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Applied

Ceramic
Technology

Volume II
Copyright 2005 SACMI IMOLA s.c. a r.l.
Via Selice Provinciale 17/A - 40026 Imola (BO) Italy
Tel. 0542/607111 - Fax 0542/642354
www.sacmi.com
e-mail: sacmi@sacmi.it

Not for sale

All rights reserved. Translation, electronic storage, reproduction or adaptation by any means
(microfilm and photocopy included), whole or partial, is prohibited.

ISBN 88-88108-55-6
Editrice La Mandragora s.r.l.
Via Selice 92 - Cas. Post. 117 - 40026 Imola (Bo) Italy
Tel. 0542/642747 - Fax 0542/647314
e-mail: info@editricelamandragora.it
INDICE

Introduction ................................................................................................................................ 13
Evolution of ceramic tile production technology ............................................................. 13
Evolution of ceramic tile plant engineering ....................................................................... 16
Grinding ....................................................................................................................................... 17
Pressing ........................................................................................................................................ 19
Porcelain tiles and production line innovations ................................................................. 22
Firing ............................................................................................................................................ 25

Chapter I - Grinding .............................................................................................................. 29


Definition and purpose of solid material grinding ........................................................... 29
Properties of solids ................................................................................................................... 29
What happens during grinding; choosing the right machine ........................................ 30
Dry grinding and wet grinding ............................................................................................. 32
Machines commonly used in the grinding department ................................................... 33
Wet grinding theory ................................................................................................................. 36
Discontinuous wet grinding theory with Alsing or ball mills ....................................... 38
Note n. 1 ....................................................................................................................................... 45
Note n. 2 ....................................................................................................................................... 45
Practical load calculation for discontinuous wet grinding mills .................................... 51
Calculating the load for a discontinuous mill (example) .................................................. 52
Continuous wet grinding ......................................................................................................... 53
The continuous wet grinding plant ...................................................................................... 53
Continuous grinding technology ........................................................................................... 55
Description of continuous mills; how to choose the right size ...................................... 56
Description of the mill ............................................................................................................. 56
Mill sizing .................................................................................................................................... 60
Mill productivity ........................................................................................................................ 60
Control and production parameters in the continuous and discontinuous
grinding department ................................................................................................................. 62
Definitions and units of measure .......................................................................................... 64
Appendices ................................................................................................................................... 66
The continuous wet grinding mill and the porcelain tile industry ............................... 66
Technological and managerial parameters .......................................................................... 67

Chapter II - Spray drying of ceramic slips .................................................................... 71


Classification of spray driers .................................................................................................. 72
General description of nozzle-type spray drier ................................................................. 74
How it works ............................................................................................................................... 74
The spray drying cycle ............................................................................................................. 75
Description of main spray drier devices .............................................................................. 77
Dust separator device ............................................................................................................... 86
The dynamics of “dried granulate” formulation ................................................................ 87
Characteristics of spray dried powders ............................................................................... 92
Morphology of the grain and particle size distribution of the powders .................... 92
Grain size ..................................................................................................................................... 92
Powder flowability ..................................................................................................................... 93
Variations in physical characteristics of spray dried powders ....................................... 96
Relationships regulating working conditions of spray driers ....................................... 96
Energy consumption ................................................................................................................. 98
The heat transfer diagram ....................................................................................................... 98
Essential parameters and examples for the evaluation of energy
consumption and spray drier output capacity ................................................................. 100
Calculating heat energy consumption ............................................................................... 100
Practical method for calculating evaporating power of a spray drier ....................... 101
Calculating the size and output of the spray drier ........................................................ 101
Energy savings ........................................................................................................................ 103
Energy recovery ..................................................................................................................... 105

Chapter III - Pressing ......................................................................................................... 107


Introduction ............................................................................................................................. 107
Pressing systems ..................................................................................................................... 107
Pressing semi-dry powders .................................................................................................. 108
Different press types .............................................................................................................. 108
Toggle press ............................................................................................................................. 108
Friction press ........................................................................................................................... 108
Hydraulic presses .................................................................................................................... 110
Requirements for a modern press ....................................................................................... 110
Different types of press for different tiles ........................................................................ 111
Machine devices ...................................................................................................................... 114
Machine structure ................................................................................................................... 115
Different types of die used to form the tiles .................................................................... 116
The pressing sequence ........................................................................................................... 119
Main parts of the die ............................................................................................................. 120
Different punch types ............................................................................................................ 121
Characteristics of the ceramic powders used in pressing ............................................ 121
Variables in the pressing cycle ............................................................................................. 122
Definition of terms ................................................................................................................ 122
Physical characteristics of the particles ........................................................................... 123
Powder fluidity ........................................................................................................................ 126
Powder particle size distribution ........................................................................................ 126
Bulk density, tapped density and Hausner index as a function of variations
in powder parameters ............................................................................................................ 129
Ceramic powder pressing: technological aspects ............................................................ 129
Relationship between bulk density of the pressed material and green bending
strength (practical aspects) .................................................................................................. 135
Effect of forming pressure on firing performance of ceramic powders
(practical aspects) .................................................................................................................... 138
Future developments in pressing........................................................................................ 142
Appendices ................................................................................................................................ 145
Green physical-mechanical characteristics of tiles obtained from different
powders (spray dried/granulated/dry ground) .............................................................. 145
Particle size distribution of powders produced using different systems .................. 145
Compaction and uniformity of pressing ........................................................................... 147
Green and dry bending strength ........................................................................................ 149
Porosity and fired tile bending strength ........................................................................... 149

Chapter IV - Drying ............................................................................................................ 153


Conventional hot air driers for ceramics........................................................................... 154
Technological considerations............................................................................................... 155
Glossary .................................................................................................................................... 159
Machines ................................................................................................................................... 161
Rapid vertical driers ............................................................................................................... 162
Horizontal driers .................................................................................................................... 166
Evaporating conditions ......................................................................................................... 169
Infrared rays............................................................................................................................. 170
Microwaves .............................................................................................................................. 171
Technological aspects ............................................................................................................ 171
Relationship between drying cycle and tile thickness/size .......................................... 171
General observations ............................................................................................................. 172

Chapter V - Glaze and decoration application techniques................................... 175


Glaze preparation ................................................................................................................... 175
Preparing screen printing pastes ........................................................................................ 182
The glazing department ....................................................................................................... 182
Glaze application and glazing lines .................................................................................... 184
Key units on the glazing line ............................................................................................... 188
Other units ............................................................................................................................... 190
The glazing line ...................................................................................................................... 190
Printing machines ................................................................................................................... 191
The scraper blade (squeegee) ............................................................................................... 191
Flat screen printing ................................................................................................................ 192
Rotary printing machines ..................................................................................................... 192
Roller decoration ..................................................................................................................... 195
Screen mesh types................................................................................................................... 196
The frame .................................................................................................................................. 198
Emulsion ................................................................................................................................... 199
Photoengraving ....................................................................................................................... 200
Silk screen printing inks ....................................................................................................... 200
Mixing the paste ..................................................................................................................... 201
Refinement ................................................................................................................................ 201
Screen printing vehicles (medias) ....................................................................................... 202
Screen printing decoration techniques .............................................................................. 203
On-glaze decoration ............................................................................................................... 203
Under-glaze decoration ......................................................................................................... 203
Colour gradation ..................................................................................................................... 204
Plain tiles .................................................................................................................................. 204
Colour overlap ......................................................................................................................... 205

Chapter VI - Firing ............................................................................................................. 207


General ...................................................................................................................................... 207
The transformations that take place during firing ......................................................... 207
The firing cycle ....................................................................................................................... 213
Different types of firing ........................................................................................................ 215
Fuels ........................................................................................................................................... 216
Ceramic firing kilns ................................................................................................................ 220
Heat exchange ......................................................................................................................... 220
Heat transmission by convection ........................................................................................ 220
Kiln construction .................................................................................................................... 221
Combustion system ................................................................................................................ 223
Controls ..................................................................................................................................... 232
Rollers ........................................................................................................................................ 234
Metal rollers ............................................................................................................................ 234
Ceramic rollers ........................................................................................................................ 236
Raw materials and formulations .......................................................................................... 236
The most common causes of roller breakage .................................................................. 237

Chapter VII - Sorting, packaging and palletizing lines ......................................... 243


Introduction ............................................................................................................................. 243
Analysis and classification of tiles ...................................................................................... 243
Automatic tile inspection ...................................................................................................... 252
Introduction ............................................................................................................................. 252
Tile vision systems: characteristics .................................................................................... 253
Installing an automatic sorting system ............................................................................. 258
Defects detected by an automatic sorting system .......................................................... 259
Automatic sorting systems: performance and advantages ........................................... 260
Automatic sorting systems: other uses ............................................................................. 261
Classification and stacking ................................................................................................... 262
Packaging .................................................................................................................................. 264
Printing and labelling zone .................................................................................................. 267
Palletizing zone ....................................................................................................................... 267
Sizing a sorting and palletizing line .................................................................................. 271
Production control software ................................................................................................ 272
Sorting line configurations for porcelain tiles ................................................................. 273

Chapter VIII - Polishing .................................................................................................... 275


Introduction ............................................................................................................................. 275
Past developments and current trends .............................................................................. 275
Lines and machines for the rough flattening - polishing - squaring of
porcelain tiles ........................................................................................................................... 276
The work cycle ........................................................................................................................ 276
Glazed wall tile squaring lines ............................................................................................ 282
Polishing - satin finish - semipolishing lines for glazed, unglazed and third
firing ceramic ........................................................................................................................... 282
Appendices ................................................................................................................................ 283
Water treatment and recycling ............................................................................................ 283
Recovery/re-utilisation of porcelain tile polishing sludge .......................................... 283
Polishing sludge ...................................................................................................................... 284
Difficulties in using the sludge ............................................................................................ 286

Appendix 1 - The environmental impact of the ceramic industry..................... 289


Pollutants in raw materials for bodies ............................................................................... 291
Pollutants in glazes ................................................................................................................ 292
Pollutants in gaseous emissions .......................................................................................... 292
Atmospheric pollution ........................................................................................................... 294
Prevention and separation .................................................................................................... 295
Bag filters .................................................................................................................................. 296
Fume filtration......................................................................................................................... 297
Abatement of organic substances....................................................................................... 297
Water pollution ....................................................................................................................... 298
Water treatment (separation) ............................................................................................... 303
Porcelain tiles ........................................................................................................................... 305
Solid waste and residues ....................................................................................................... 305

Appendix 2 - Production controls .................................................................................. 309


Controls on raw materials or bodies .................................................................................. 309
Body preparation department controls ............................................................................. 321
Spray dried powder controls ................................................................................................ 322
Press department controls ................................................................................................... 323
Controls on dried tiles ........................................................................................................... 326
Controls on the biscuit (double fire only) ......................................................................... 327
Controls in the glazing department ................................................................................... 328
Controls on the finished product ........................................................................................ 329
Laboratory controls on raw materials for frits and colours ......................................... 330
General criteria for quality control tests on raw materials for glazes ...................... 332

Appendix 3 - Defects ........................................................................................................... 333


Defects associated with raw materials ............................................................................... 335
Problems attributable to the technological characteristics of the body ................... 347
Problems associated with the nature of the raw materials that appear
after firing ................................................................................................................................. 349
Other defects associated with raw materials .................................................................... 349
Body preparation defects ....................................................................................................... 350
Pressing defects ....................................................................................................................... 352
Glaze and glazing defects ..................................................................................................... 354
Defects caused by the glaze .................................................................................................. 354
Application defects .................................................................................................................. 356
Poor glaze-body match .......................................................................................................... 357
Glazed surface defects ............................................................................................................ 357
Nature and formation of gaseous emissions .................................................................... 358
The influence of stains .......................................................................................................... 361
Glaze application defects ....................................................................................................... 363
Decoration defects .................................................................................................................. 367
Firing defects with effects on the glaze ............................................................................. 368
Firing defects ........................................................................................................................... 370
Tile bursts in the pre-kiln (explosions) ............................................................................. 370
Breakage during preheating ................................................................................................. 370
Cooling breakage (or “cooling cracks”) ............................................................................. 375
Identifying the point of tile failure .................................................................................... 375
Crazing ...................................................................................................................................... 376
Uniformity of shrinkage over the kiln cross-section .................................................... 377
Glaze brilliance and shade .................................................................................................... 380
Pin holes - holes - bubbles in the glaze ............................................................................. 381
Degassing ................................................................................................................................. 383
Degassing in double fire processes ..................................................................................... 384
Black core .................................................................................................................................. 384
Planarity defects ...................................................................................................................... 386
Downturned corners .............................................................................................................. 387
Upturned corners ................................................................................................................... 388
Convexity .................................................................................................................................. 389
Concavity .................................................................................................................................. 392
Roller effect .............................................................................................................................. 395
Priest hat ................................................................................................................................... 397
Asymmetric deformation or warping ................................................................................ 399
Monoporosa ............................................................................................................................. 401
Convex planarity (Monoporosa) ......................................................................................... 401
Non-uniform planarity across the kiln load in monoporosa ........................................ 405
Non-uniform planarity over time (Monoporosa) ............................................................ 406
Non-uniformity of size across the load cross-section in monoporosa ...................... 407
Production contamination .................................................................................................... 408
Introduction

INTRODUCTION

Evolution of ceramic tile production technology

The developments seen in the ceramic industry since the end of the Second World
War, have, quite simply, been extraordinary. The way in which building bricks, sani-
taryware, tableware and ceramic tiles are produced has changed radically. This is
especially true of tiles, where production plants and markets have been revolution-
ised; on the one hand, this has come about as a result of the enormous demand for
industrial and residential building materials and, on the other, continuous efforts to
increase productivity and improve health and safety standards for workers in the ce-
ramic industry itself.
Not so long ago the ceramic industry was an almost craft-like affair (fig. 1) that
depended on an abundant supply of manual labour. Progressively, yet rapidly, it
soon became a mechanised industry, thus eliminating much of the pure physical toil.
From here rationalisation of the work process led to gradual replacement of com-
plex control and organisational activities via the application of electronic automation.
Generally speaking, such changes have resulted in uniformity of output and the
transformation of the human role, the latter now largely being limited to supervision
and control of highly automated – even robot-controlled – processes.
Fortunately, more uniform production results have been counterbalanced by
extremely keen interest in the development of new tile shapes, new decorations and
new products, thus avoiding the blandness of standardisation altogether.

ORGANIZZAZIONE ARTIGIANALE
CRAFT-LIKE ORGANISATION

MECHANISATION
MECCANIZZAZIONE

RATIONALISATION
RAZIONALIZZAZIONE AUTOMATION
AUTOMAZIONE

UNIFORMITÀ DIOF
UNIFORMITY PRODUZIONE
OUTPUT

MANUAL
LAVORO WORK
MANUALE SUPERVISION
ATTIVITÀ DI SUPERVISIONE

Fig. 1.

13
Applied Ceramic Technology

In fact, this demand for ever-better aesthetics has driven technological deve-
lopment onwards and upwards. Plant engineers and machine designers have been
forced to elaborate more and more complex manufacturing solutions to meet the
fast-rising demand for a creative finish.
The three most important factors that have led to attainment of high-perfor-
mance, attractive tiles and consequently high product sales are (fig. 2):
• the machines, that have succeeded in meeting ever-more demanding tolerance,
automation and performance requisites.
• extremely attentive selection of raw materials as a function of the increasing
sophistication of production machinery and rising demand for high performan-
ce tiles.
• the role of human resources, which, because of reductions in the number of workers
per unit of output caused by increased automation, has been modified significan-
tly: today’s workers, for example, need specialist training, especially in the electro-
nic control field. Forward planning has become vital: continuous efforts need to
be made to identify new technological solutions and, today more than ever, to
give one’s products a qualitative edge through constant refinement of product
aesthetics and functionality.

The result of this revolutionary expansion of the ceramic tile industry is well
known and has allowed some nations, particularly Italy, to become undisputed lea-
ders in terms of overall output, quality and worldwide exportation.

GROWTH FACTORS

MACHINES

RAW MATERIALS

HUMAN RESOURCES

Fig. 2.

14
Introduction

Furthermore, in the field of ceramic tile production Italy is advantaged by the


world’s highest concentration of ceramic plant and machinery manufacturers. In
Italy alone (fig. 3) 190 such companies employ 7,200 workers and generate total
sales of around A 1.6 billion/year (2000).
For some years now this huge production effort has hinged on an equally huge
technological effort, itself largely dependent on mutually rewarding interdepen-
dence with the Research and Development activities carried forward in a state of
delicate equilibrium by tile producers and suppliers of production plants, machine-
ry and raw materials.
The most successful companies have always been those ready to react quickly to
technological and aesthetic trends by keeping one step ahead of them and even
controlling them. Even better, some companies have managed to impose the results
of their constant application of new ideas on the market; these companies are gene-
rally aided by a highly evolved, concentrated manufacturing scenario (e.g. Italy, Spain)
and a backdrop of flexible, medium size engineering companies ever ready to follow
the developments required of them. Simultaneously, such companies have proved
adept at responding quickly to the requisites of new technical or standardisation
legislation on mechanical and physical tile characteristics (MOR, frost resistance,
water absorption etc.).
To illustrate just how the tile manufacturing industry has developed, a brief
historical aside on recent technological developments is needed.
At the start of the 1970’s certain negative aspects vis-à-vis the production process
and the final product were successfully eliminated, giving a new process and a product
that was more remunerative and suited to a much vaster market; this proved to be
good news for tiles manufacturers and suppliers of technology (i.e. presses and kilns)
alike.

PRODUCTION
PRODUZIONEPLANT / MACHINERY
DI IMPIANTI OUTPUT
E MACCHINE

ITALY
ITALIA AZIENDE
COMPANIES
ADDETTI
EMPLOYEES
190190
7,2007.200
SALES
FATTURATO 1.6 billion
3.100 miliardi
EXPORT
EXPORT 65%65%

Tableware
Stoviglieria
Sanitari
Brick Sanitaryware 0,8
Laterizi
10,3 2,5 Refrattari
Refractories
0,3 Piastrelle
Tiles
85,5

Fig. 3.

15
Applied Ceramic Technology

The way in which the industry evolved towards such innovation was typical of
the Italian economy; the industry was able to rely upon a high number of suitably
sized companies that were willing and able to experiment the new technology inter-
nally. Those companies also had the knowledge, skill and drive needed to interpret
and guide the experimentation.
As already mentioned, there were also a great many mechanical engineering
companies with autonomous research capacity and, finally, an intense exchange of
ideas and experiences within the industry.
The outcome was that Italian tile manufacturers were the first in the world to
gain possession of a new product – single-firing ceramic – that would prove to be
extremely competitive in terms of both quality and price with respect to other floor
tile types.
Compression of energy and labour costs not only made this new innovation
profitable, it also made traditional systems, market niches aside, rapidly obsolete.
In this scenario, then, the characterising aspect of output was the ceramic body
while aesthetics, conditioned by poor familiarity with the new techniques, was cha-
racterised by matt or rustic glazes designed to give an impression of strength.
Consequently there was soon a levelling out of both the domestic and export markets
for these products.
Once again, the quest for qualitative advantage gave new impetus to research
into aesthetics, giving rise to the use of new decorations, grains and granulates and
the creation of products with a glossier, more intricately decorated finish that re-
quired more and more applications and silk screen printings.
Technology suppliers reacted accordingly, providing ever-more sophisticated tile
pressing and automatic handling machines and giving manufacturers the bonus of
reduced waste, improved quality and greater production plant flexibility.

Evolution of ceramic tile plant engineering

Ceramic tiles, then, began to gain ever-larger world markets not only because
their raw materials are found all over the globe and the production process is consi-
dered to be a relatively easy one but, above all, because new technologies based on
reliable machines were able to provide finished products of excellent quality.
The dynamism of the industry also played a key role, acting as a catalyst for
continuous evolution of both process and product. Beginning in the 70’s and 80’s
(depending on the country and the degree of industrial development, see fig. 4) a
general switch-over from traditional double firing to rapid double and single firing
was witnessed.
That changeover was accompanied by the increasingly widespread use of wet
grinding, larger and larger tile sizes and fast-improving aesthetic/decorative resul-
ts; such changes clearly involved important technological changes in mills, presses
and glazing lines.

16
Introduction

TILE OUTPUT IN EUROPE (year 2000)


(Millions of m2/year)

ITALY 632
SPAIN 620
TURKEY 150
GERMANY 65
PORTUGAL 60
FRANCE 50
CZECH REPUBLIC 31
POLAND 30
RUSSIA 20

Fig. 4.

Grinding

Just twenty years ago the majority of ceramic manufacturers still used pen-
dulum mills or pin crushers. Nowadays, as a result of increased output require-
ments and demand for particle size distributions that pivot around the 10 micron
mark, with 63 µm screen residues equal to zero (and 45 µm residues of just a few
percentage points), there has been a widespread conversion to large, continuous wet
grinding mills. For at least ten years now this tried and tested solution has had all
the characteristics of a mature technology.
While, in the production of low-performance red body tiles, it might still be
possible to consider using dry grinding technology, the increasing demand for light
coloured bodies of complex formulas, together with the improved technological
characteristics of the finished tile, has oriented the market towards more and more
extensive use of wet grinding where the excess water is evaporated in spray driers.
These changes, of course, are driven by the improved quality of the semi-finished
tiles and the improved production flexibility such technology offers.
Continuous wet grinding mills (fig. 5) are also used extensively, and have been
for many years, in the world’s mining industries.
In addition to technical advantages continuous grinding has also yielded techno-
logical, energy and management advantages with respect to discontinuous grinding
because:
• it is possible to weigh and formulate the bodies continuously and automatically,
thus providing more consistent physical-chemical slip characteristics and easier
repeatability as and when necessary.
• it is possible to reduce the quantity of water in the mill because continuous emp-
tying and the higher temperature (higher by as much as 60 °C) of the usually
thixotropic slip make it possible to use suspensions that are denser but just as easy

17
Applied Ceramic Technology

Fig. 5.

CONTINUOUS
GRINDING PLANT

VANTAGGI DELLA
ADVANTAGES OF MACINAZIONE CONTINUA
CONTINUOUS GRINDING
+17,4%
+17.4% -14,8%
–14.8% -14,8%
–14.8% -80%
–80% -50%
–50%

INCREASED
AUMENTO ENERGY
CONSUMO SPECIFIC
CONSUMO LABOUR
PERSONALE REQUIRED
AREA
PRODUCTIVITY
PRODUTTIVITÀ CONSUMPTION
ENERGETICO ELECTRICITY
ELETTRICO REQUIREMENTS
RICHIESTO SPACE
RICHIESTA
CONSUMPTION
SPECIFICO
DISCONTINUOUS CONTINUOUS
MACINAZIONE
GRINDING MACINAZIONE
GRINDING
DISCONTINUA CONTINUA

Fig. 6.

18
Introduction

to unload: this results in evident energy savings at the subsequent spray drying
stage (consumption about 15% lower).
• while system output capacity has been increased, the grinding department is
now more compact than in the past and the low number of employees makes for
easier management.

Furthermore, as only turbo-dissolved clayey raw materials can be used, conti-


nuous grinding can be organised to feed pre-formed slips continuously; in this case
the productivity of the system, which then focuses its potential on the harder mate-
rials, may increase by as much as 40%.
Continuous, wet grinding mills are, of course, more suitable for production plants
of considerable size as it is here that the described advantages are greatest. They
may also be used in medium size plants as base body preparation units, with subse-
quent batch corrections; the effective load capacity of the machines currently avai-
lable on the market ranges from 40,000 litres (24 tons of silica grinding media) to
150,000 litres (100 tons of grinding media).

Pressing

Recent product innovations have seen so-called porcelain tiles gain ever-greater
market shares. Such innovations have also yielded technological improvements at
other stages of the production process. For example, enormous progress has been
made in pressing, where machines and accessory systems have been completely re-
designed to meet demand for larger tiles without reducing specific pressure (which,
has, in truth, increased).
The 30 × 30 cm and 40 × 40 cm tiles now account for more than half of total
output and sizes of 90 × 180 cm and beyond, mere oddities up until just a short time
ago, now form part of the standard product range (fig. 7).
This trend towards large tiles means that for the same surface area a smaller
number of pieces are handled; also, silk-screen printing and dry grain application
techniques make decoration much more effective and, thanks to the extensive sur-
face area of the tile, easier. Such decoration techniques now allow manufacturers to
imitate a whole range of natural stones almost perfectly. Moreover, the initial in-
vestment is amortised quickly on account of the considerable added value of these
products.
Such production plants are more “exploitable” in that there has been no slowing
down of production cycles, only increased productivity in terms of square metres
produced. The market has accepted these larger tiles willingly, not only because of
their superb aesthetics, but also because they are more economic to lay – even where
used in raised flooring or outdoor building facades (fig. 8) – and involve fewer inter-
tile joints.
Yet none of this would have been possible without the press and die develop-
ments that followed in the wake of fast-changing manufacturer needs.

19
Applied Ceramic Technology

Fig. 7.

Fig. 8.

At present, presses used to make large tiles have very high pressing forces (up to
7,000 tons - fig. 9), with die cavities now rapidly nearing 1000 × 2000 mm. The
construction parameters for such machinery must thus take into account the need
for rigidity, precision of alignment and absence of torsion etc.: those needs have
been met through the application of a various construction solutions capable of
producing non-welded, suitably pre-loaded structures.

20
Introduction

Fig. 9.

Filling systems have also changed much in recent years: they now involve a
large number of multiple operations and provide excellent filling homogeneity, even
with specially shaped die cavities.
With regard to the actual pressing phase itself, no summary of recent develop-
ments would be complete without mentioning the introduction of pressure-com-
pensating or isostatic dies (fig. 10) in which an incompressible fluid occupies a space
separating a rigid part of the punch from a flexible part that comes into contact
with the powders to be pressed: during pressing, then, this compensates for the
density differences caused by the non-uniformity of the powder filling.

ISOSTATIC PUNCH

Fig. 10.

21
Applied Ceramic Technology

The advantages offered by this simple solution (derived from the production of
technical ceramics), especially in the case of large tiles, include, among other things, a
drastic reduction in sizing variations, the disappearance of a host of other dimensio-
nal defects (often evident only after firing) and increased press efficiency.

Porcelain tiles and production line innovations

Our analysis of recent production technology innovations would not be comple-


te without mentioning the enormous success of porcelain tiles. This argument does
not concern an innovation in the production process per se but, rather, a product
innovation that has strongly influenced (and is likely to continue doing so) the wall
and floor tile market and the configuration of production plants.
This type of ceramic material is defined by its superior technological characteri-
stics and generally falls within ISO 13006 class BIa (fig. 11). In Italy it has conque-
red a significant slice of the market: in 1985 porcelain tiles accounted for just 8
million square metres while forecasts for 2001 anticipated sales in excess of 300
million square metres. In Italy, porcelain tiles now make up over 30% of total floor
tile sales. Since some 62% of such Italian-made products are exported (mainly within
Europe), it is fairly safe to assume that European and world demand will continue to
grow.
The irresistible commercial success of these tiles has had knock-on effects in the
production process. A different chemical and mineralogical composition (fig. 12)

PRESSED CERAMIC TILE CLASSIFICATION

CATEGORY WATER PRODUCT


ABSORPTION (%) TYPE

B III > 10 MONOPOROSA OR RAPID


DOUBLE FIRING TILE

B II b 6 – 10 SINGLE FIRED TILE


(SEMI-POROUS)

B II a 3–6 VITRIFIED SINGLE


FIRED TILE

BIb 0.5 – 3 FROST-RESISTANT


SINGLE FIRED TILE

BIa < 0.5 PORCELAIN TILE

Fig. 11.

22
Introduction

PORCELAIN TILE COMPOSITION


Feldspar

Plastic Clay

Kaolin
Quartz
Talc

KAOLIN
PLAS. CLAY
FELDSPAR
QUARTZ
TALC

Fig. 12.

has, as seen, necessitated better grinding machinery performance; this is because


the high degree of compactness and vitrification that characterises these tiles is
dependent not only on accurate raw material selection but also optimum particle
size distribution: the latter provides the extensive inter-particle surface area needed
for proper sintering at the firing stage.
Pressing parameters (and machines), via which compaction – and thus reactivity
at high temperatures – is optimised, have also been influenced. Standard porcelain
tile pressures now stand at around 350-450 kg/cm2.
Hence the growth in demand for the larger tiles has increased the requirement
for larger, more powerful presses.
Another key development in the production process associated with the success
of porcelain tiles concerns decoration.
Given its characteristics of surface hardness and abrasion resistance porcelain
tiles were, up until about 3 or 4 years ago, produced without any glaze-like vitreous
covering as the latter would have been detrimental to performance. This posed the
question of how to obtain an aesthetic result that would free the manufacturer from
the relative banality of plain colours and so-called “granito” ceramics, obtained
simply by colouring bodies with appropriate oxides and mixing different combina-
tions of coloured powders together (fig. 13).
New decoration techniques have thus been perfected which, without compro-
mising the cited technical performance, have allowed the creation of entirely new
product types and led to marked differentiation of products available to the consu-
mer. Such techniques have also allowed porcelain tiles to make inroads in areas
traditionally reserved for products of very high aesthetic quality.

23
Applied Ceramic Technology

VARIABLY SHADED VARIABLY VEINED


PORCELAIN TILE PORCELAIN TILE

Fig. 13.

Such innovations have also permitted the re-introduction of glazing lines spe-
cially designed for porcelain tiles.
Given the possibility and need, as is often the case in full-body products like
porcelain tiles, of effecting post-firing polishing to increase the tile’s aesthetic
qualities, there has been intense development of both application-type decoration
and decoration with pigmented substances dispersed in appropriate vehicles (wa-
ter, glycols, PEG, polycarboxylic acids etc.). The latter are absorbed in a control-
led manner into the semi-finished product (tiles that have been pressed and dried
or pre-fired at 900-1000 °C), and colour it from within the body. This has resulted
in a far-reaching reassessment of aesthetic aspects, allowing, for example, the re-
introduction of silk-screen printing decoration (fig. 14), without in any way alte-
ring the body and, above all, surface features of the material.
Furthermore, final polishing can now be performed as a function of just how far
the pigments are absorbed into the ceramic body and as a function of the need to
obtain the shading effects that give the finished tile a natural look.
These new needs, all aimed at enhancing the aesthetic quality of the product,
have stimulated enormous innovation within the accessory machines field; these
carry out tasks such as granulation, re-granulation, micronization, multiple die ca-
vity filling on the press, application, decoration. Such needs have also driven intense
research into precursors, raw materials, pigment and soluble pigmenting salts etc.
(fig. 15).
Fast-growing demand for a wider range of products and better aesthetics has, in
very recent years, resulted in the widespread reappearance of surface glazing tech-
niques for porcelain tiles; this is largely performed with special glazes or glass-
ceramics that are extremely resistant to chemical aggression, staining and exhibit
very good bending strength. This form of decoration, together with a seemingly
endless flood of imaginative solutions put forward by designers and applicators, has
gone hand in hand with the increasingly diffused utilisation of porcelain tiles on

24
Introduction

PORCELAIN TILE
DECORATED WITH SALTS

Fig. 14.

TYPES OF POWDER THAT CAN BE PRESSED

SPRAY-DRIED
DRY GROUND
MICRONIZED
PIGMENTS
RE-GRANULATES
FLAKES
GRAINS
PELLETS

Fig. 15.

walls as well as floors. Porcelain tiles now provide a high quality touch in many
public buildings (outdoors and indoors) and are sometime used on external facades
where their technical and geometric qualities (porcelain tiles can be ground to size
and chamfered) are ideal.

Firing

The popularity of large tiles and high-density, almost fully sintered materials
has inevitably produced changes in that most critical stage of the production pro-
cess, firing.
Firing has undoubtedly been affected by more technical innovations and plant
engineering developments than most other stages of the production process, espe-

25
Applied Ceramic Technology

cially over the last few decades. As mentioned in the introduction, this has also
involved the development of specially formulated bodies suitable for the new firing
cycles.
The advent of single-layer roller kilns, which began to appear in the mid-70’s,
shortened firing cycles to 25-65 minutes for a whole range of items, from the sim-
plest double fired product to the densest, thickest porcelain tile body. Moreover,
flexibility in terms of load and regulation allowed manufacturers to adjust firing
curves to suit tile size and thickness and the glaze type.
While the reader will certainly be aware of much more recent developments
concerning flexibility, electronic control, energy consumption, productivity and
adaptability to certain products, it is nevertheless worth taking a brief look at the
latest innovations which have provided manufacturers with even better performance.
In particular, there has been much progress in the optimisation of temperature
distribution across the cross-section and length of the kiln via the use of tubed or
boxed burners (fig. 16).
In addition to supplying a mix of convective and radiated heat, these also allow
the heat to be directed to more sensitive sections of the kiln, such as side walls or at
the centre of the chamber as required.
Moreover, these devices make it possible to programme temperature regulation
during initial preheating of the tiles by using low temperature air. Fine regulation
of cooling zones – clearly advantageous where large or high mass tiles are pro-
duced – is also being developed.
The ability to adjust temperatures and times allows for the creation of special
cycles that yield certain colouring effects (where iron, manganese and other colouring
elements are present) in glaze applications or special body compositions.
The innovative technological aspects illustrated here represent just a few exam-
ples of a continuous upgrading process that involves everything and everyone in

INNOVATIVE BURNERS

Fig. 16.

26
Introduction

the ceramic industry – from raw materials to rheological and silk screen printing
additives, from glaze manufacturers to tile producers. Suppliers of complete plants
and machinery are especially committed in this regard as they play an ever-greater
role as “vehicles of know-how” and are a driving force in the industry’s R&D sector.
Recent efforts aimed at optimising sorting, packaging and storage lines (fig. 17)
illustrate this point perfectly: sophisticated electronic control systems using intelli-
gent vision systems that effect on-line product classification are increasingly com-
mon as are automatic laser or wire-guided tile transfer systems etc. (fig. 18).
So far nothing has been said about key innovations in glazing and screen printing,
now available as continuous systems or about the huge efforts that have been made to
bring the industry into compliance with environmental standards; this last aspect is

Fig. 17.

Fig. 18.

27
Applied Ceramic Technology

particularly important in highly industrialised areas and is a key factor when it comes
to designing a new product or production line.
This second volume examines each stage of the ceramic tile production process,
from grinding all the way to sorting and packaging. Its aim is to provide clear,
concise, comprehensive and updated explanation of production technology and com-
plete the preliminary information on materials, products and reactions provided in
the first volume.

28
Grinding

Chapter 1

GRINDING

Definition and purpose of solid material grinding

Grinding involves a whole series of tasks intended to reduce the dimensions of


solid raw materials.
It begins by crushing the raw materials to produce smaller lumps and ends with
the creation of a fine powder.
Hence grinding is not just a simple, preliminary affair. It is a complex process
that aims to produce a material of a desired average particle diameter and particle
size distribution appropriate for a specific final product.
Broadly speaking, while there are a variety of reasons for reducing the dimen-
sions of a solid, the most important aspect is that the increase in specific surface
area gives the mass a high degree of homogeneity and results in more complete,
faster chemical reactions during firing (see relevant chapter in Vol. 1).

Properties of solids

Solid materials have certain properties that significantly influence the efficiency
of the grinding process. The most important of these are:

a) Linear dimensions of the particles of the materials to be ground. These concern:


– the diameter, where particles are spherical
– the side length, where particles are cube-shaped etc.
Clays are usually supplied to ceramic manufacturers as lumps no larger than 10-20
cm.

b) Dimensions of the external surface of the particles to be ground


Surface area can be calculated easily for spherical or cubic shapes, even those of
irregular form. Quarried clay lumps are frequently rounded or laminated; the lamina-
ted ones can sometimes be very hard (“shale-clays”). Other materials are spherical,
rectangular or cubic such as the harder materials: calcite, dolomite, feldspar and silica.

c) Hardness
This is one of the most important parameters in grinding.
It is essential to have an understanding of:
– compression resistance: especially important in the dry grinding of hard mate-
rials.

29
Applied Ceramic Technology

– impact resistance: comes into play in the dry grinding of clays and wet grind-
ing of hard materials.
– abrasion resistance: important in the wet grinding of hard materials.

d) Material structure
May be compact or heterogeneous, with casual fracture planes or well determi-
ned cleavage fractures.
Clays generally have a compact structure but some often have fracture planes.
The ceramic industry also uses schistose clays with evident, well defined cleavage
fractures.
Hard materials are generally compact; these include materials such as quartzites,
feldspars, chemical sedimentary limestones and highly fissured metamorphic rocks
such as homogeneous-sedimentation calcites and dolomites that have not been exces-
sively modified by diagenesis.

e) Specific weight
Not a particularly important factor in the grinding of compact solid materials.
However, in the case of natural mixes or blends with particles of different miner-
alogical composition, specific weight takes on more significance regarding the possi-
bility of segregation during transportation within the plant.
There follow some specific weights for several ceramic materials:

Clays from 2.5 to 2.8 g/cm3


Quartz 2.65 g/cm3
Feldspars from 2.53 to 2.67 g/cm3
Calcite 2.75 g/cm3
Dolomite 2.95 g/cm3

f) Moisture content and hygroscopic characteristics


Both exert considerable influence on grinding in that they reduce the efficiency
of the grinding machinery.
As moisture content rises grinding output capacity falls (for the same fineness).

g) Tendency to agglomerate or flocculate


Reduces grinding efficiency.
Other factors which influence grinding considerably, especially where ceramic
materials are in their natural state, are shown in fig. 1.

What happens during grinding; choosing the right machine

The grinding process involves the following:


a) simple compression (crushing)
b) percussion
c) impact

30
Grinding

MORPHOLOGICAL AND PHYSICAL CHARACTERISTICS OF CERAMIC


RAW MATERIALS INFLUENCING THE GRINDING PROCESS

CLAYS
• MINERALOGICAL NATURE
• PLASTICITY
• ELECTROSTATIC INTERACTION WITH WATER

THESE CHARACTERISTICS ARE IDENTIFIED VIA ANALYSIS OF:


• PERCENTAGE AND NATURE OF RESIDUAL MATERIALS
• CLAYEY PARTICLE DIMENSIONS
• SPECIFIC SURFACE AREA
• IONIC EXCHANGE CAPACITY
• PRESENCE OF SOLUBLE SALTS

NON-CLAYEY MATERIALS
• SIZE AND PARTICLE SIZE DISTRIBUTION
• BASE STRUCTURE

Fig. 1. Morphological and rheological factors influencing grinding.

d) abrasion
e) cutting.

All the machines used in the grinding process involve the above-listed principles.
Comminution can be sub-divided into two main phases:
– crushing, the range of which extends from the rough blocks extracted in the
quarry to pieces just a few millimetres in size. Crushing itself may be divided
into primary crushing (or pre-crushing), effected on materials that range from
the tout-venant quarry blocks to pieces about 100 mm in size, and secondary
crushing that produces “grains” with a size of about 10 mm.
– grinding, instead, has a field of application that extends down into the microns.

This stage of comminution is divided into primary grinding, which involves


pieces as small as 0.5 mm, secondary (or fine) grinding, which yields particles with
a size of some tens of micrometers, and final micronization, which reduces the
particles to a size of just a few microns (fig. 2).

31
Applied Ceramic Technology

BASIC GRINDING OPERATIONS


SIZE
PEZZATURA
• CRUSHING
FRANTUMAZIONE: IN OUT
30-20 mm 5-10 mm
- FRANTUMAZIONE
– PRIMARY CRUSHINGPRIMARIA 100 mm

– SECONDARY CRUSHING
- FRANTUMAZIONE SECONDARIA 5-10 mm

• GRINDING
MACINAZIONE: IN OUT
5-10 mm < 50 µmm
MAYPUÒ
BE SUB-DIVIDED INTO:IN:
ESSERE SUDDIVISA
– PRIMARY GRINDING
- MACINAZIONE PRIMARIA ~ 0.5 mm
– SECONDARY GRINDING
- MACINAZIONE (FINE)(FINE)
SECONDARIA 20-100 µm

– MICRONIZATION
- MICRONIZZAZIONE < 50 µm

Fig. 2. Grinding: different stages and relative piece/particle sizes.

In the case which is of most interest to us (i.e. grinding of raw materials for
ceramic tile bodies), it should be born in mind that highly heterogeneous materials
are often used; these may be heterogeneous from both a mineralogical and a physi-
cal standpoint. Certain necessities thus need to be taken into account:
– dispersion of the various components in the clay or mix must be all but perfect.
– some mineralogical components need to be ground to different degrees.
– certain impurities contained in the raw materials need to be removed from the
mix before grinding it.

Dry grinding and wet grinding

The raw materials used in ceramic bodies can be ground using either dry or wet
grinding technology.
As a rule it can be said that wet grinding is preferred as it reduces in-mix particle
size greatly and provides better homogenisation. Dry grinding technology may be
used where raw materials are homogeneous from both a morphological and hard-
ness standpoint, when the final product is of modest quality or with double-firing
products in general.
With wet grinding the raw materials are initially ground together as a suspen-
sion of solids to reduce the size of the natural particles even further. The substance
obtained at the end of this grinding process is called slip. Chemical deflocculants
(which can also reduce the quantity of water in the slip, thus providing economic
gains) allow manufacturers to produce particles with a diameter of even less than
one micron (almost zero residue on a 63 µm screen).

32
Grinding

The choice of grinding technology, however, depends only in part on the degree
of particle fineness needed to obtain a certain final product; other factors need to be
taken into account. Dry grinding, in fact, is used for mixes made up of a maximum
of two or three clays that are similar to each other in terms of both mineralogical
constitution and physical characteristics.
Any silt, sand or coarse residue must only be present in very limited quantities.
Dry grinding can thus be used to produce double fire biscuit (i.e. to be fired a
second time) and in the production of wall tiles (majolica). Its application in the
production of floor tiles (e.g. porcelain tiles) or monoporosa is somewhat limited as
wet grinding is generally preferred.
Wet grinding is used with natural mixes of clays and hard materials, that is, with
heterogeneous blends sized in such a way as to make their refinement with even the
most efficient dry grinding systems impractical; bodies are, above all, prepared using
wet grinding technology where ceramic compositions consist of various compo-
nents, specific weights and particle sizes.
Wet grinding is also preferable where clays contain impurities that need to be
eliminated from the bodies: the preferred procedure is to disperse them and then
sieve the slip through a suitable mesh.
Finally, wet grinding is preferred for the manufacture of vitrified products or
those utilising very fast firing cycles, in that the wet process makes composition
corrections easier and provides powders that, once spray dried, have good fluidity.
Fluidity is important as it ensures good die cavity filling performance at the pres-
sing stage (fig. 3).
From the above, then, it is evident, from a purely technological viewpoint, that
there can be no real competition or dualism between dry and wet grinding: they
exist only as separate alternatives. Once the raw materials have been analysed and
the technical characteristics of the tile to be produced have been taken into account,
only one technology will prove feasible.

Machines commonly used in the grinding department

Dry grinding plants


a) Clay grinding
Ceramic tile manufacturers generally use clays with a maximum moisture con-
tent of 4-5%; in mills heated with hot air (which performs a drying function), this
figure can be as high as 10%.

Primary crushing reduces the size of the incoming materials from about 20 cm
to about 6 cm max. This is normally done in pin-type or toothed-wheel crushers.
Subsequent crumbling (secondary crushing) is performed in impact crushers; here,
the material is reduced to a maximum particle size of 5 mm.
Grinding itself is carried out in centrifugal pin mills, fixed or mobile hammer
mills and, above all, in pendulum mills, depending on the required degree of parti-
cle fineness.

33
Applied Ceramic Technology

FACTORS INFLUENCING THE CHOICE OF PROCESS


(DRY OR WET GRINDING)

- TECHNICAL CHARACTERISTICS OF THE FINISHED PRODUCT


- TYPE OF RAW MATERIAL
- QUANTITY OF COMPLEMENTARY COMPONENTS
- MORPHOLOGICAL CHARACTERISTICS OF AVAILABLE RAW MATE-
RIALS
- COST OF FINISHED PRODUCT
- OVERALL INVESTMENT
Fig. 3. Factors determining the grinding method.

b) Grinding chamotte or other hard materials


Materials with a maximum moisture content of 1.0-1.5% are used.
Primary crushing is done in jaw crushers; starting with a piece size of about 15-
20 cm, the material is reduced to a tout-venant with a maximum particle size of 4-6
cm.
Subsequent granulation is effected in impact mills where maximum particle size
drops to 0.5-1.0 cm.
Final grinding is generally effected in annular gap mills where medium particle
size distribution is required or in pendulum mills should greater refinement be re-
quired.

Body preparation (dry grinding): machines


In defining the machines needed for the grinding process and, more generally,
those needed to prepare powders for the pressing of ceramic tiles, three essential
aspects need to be taken into consideration:
1) the nature of the material to be ground, that is, the type of component (e.g. clays
and, chamotte, etc.) and its relative physical characteristics (size, moisture con-
tent, hardness and impact strength).
2) the final particle size distribution to be attained.
3) the technology adopted for the transformation of the ground material into a powder
suitable for pressing: wetting and any re-granulation (or, better, agglomeration).

From the above it follows that no one machine is able to perform all the required
functions: production plants therefore use a range of machines to deal with specific
situations as and when they occur.

34
Grinding

The key machines in dry grinding are:

Pre-crushers
PIN-TYPE LUMP CRUSHERS

Crushers
JAW CRUSHERS
IMPACT CRUSHERS
HAMMER MILL

Refiner mills
PIN CRUSHERS
ANNULAR GAP MILL
PENDULUM MILL
VERTICAL ROLLER PULVERIZER

As stated previously, grinding involves the following:


a) simple compression
b) percussion
c) impact
d) abrasion
e) cutting.

All the machines used in the grinding process perform one or more of the above-
listed actions. Fig. 4 shows particle size distribution ranges for the dry ground
powder and compares it to the granulate obtained from spray drying.

In dry technology, regulation of the degree of grinding depends on the classifi-


cation system (dynamic air flow sizing for pendulum mills and vertical roller pulve-
rizers, mesh for pin mills).
Note that the machine efficiency decreases over time because the grinding media
is subject to wear. Such wear progresses at a rate proportional to machine producti-
vity, which is, in turn, dependent (except for vertical roller pulverizers) on mill
RPM.

Wet grinding plants


Raw materials generally have a maximum moisture content of 14% for clays and
6% for the harder materials and are reduced in size as follows:
– for clays: maximum piece size 6-10 cm
– for hard materials: maximum piece size 0.3 cm.

The clays can be dissolved with the aid of high speed or turbo dispersers and con-
tinuous or discontinuous drum mills.
Hard raw materials, instead, are normally ground in continuous or discontin-
uous drum mills.

35
Applied Ceramic Technology

Fig. 4. Particle size range of semi-finished products with dry and wet grinding.

The extent of grinding varies enormously depending on the type of product


being manufactured.

Wet grinding theory

There are various grinding theories, all of which tend to explain machine opera-
tion in terms of laws expressed as mathematical formulas; the most important of
these are Kick’s law and Rittinger’s law:
a) Kick’s law: states that the energy needed to crush a solid material to a specified
fraction of its original size is the same, regardless of the original size of the feed
material.
This energy is also proportional to the logarithm of the ratio between the initial
and final diameters of the material. The law can be expressed mathematically as
follows:

W = κk lg (D/d)

where
W = required energy
Kk = constant dependent on type of material
D = average size of particles before grinding
d = average size of particles after grinding.

For example, the quantity of energy needed to reduce a given weight of mate-
rial from 1 cm3 to 0.5 cm3 is equal to the energy needed to reduce the same weight
of material from 0.5 cm3 to 0.25 cm3 and so on.

36
Grinding

b) Rittinger’s law: states that the energy needed to reduce the size of a solid particle
is directly proportional to the resultant increase in surface area. The law can be
expressed mathematically as follows:

W = κr (1/d - 1/D)

where
W = required energy
Kr = a constant dependent on particle shape and energy per unit of surface
d = average side length of particles after grinding
D = average side length of particles before grinding.

In other words, the quantity of energy needed to reduce the size of a given
weight of material still depends on the initial and final size of the ground product.
For example, it can be estimated that, if it takes 2.5 hours to grind the material from
1 mm to 100 µm (reduction ratio 10:1), in another 2.5 hours the material will pass
from 100 µm to just 53 µm (reduction ratio 2:1) because the change in surface area
remains the same.
It should, however, be observed that, in practice, the amount of energy absorbed
by the machines is always greater than the amount of energy calculated via the
above formulas because the work also involves:
1) Energy needed to overcome the cohesion linking the particles in the pieces being
ground.
2) Deformation energy (plastic and elastic deformation).
3) Energy absorbed in attrition between grinding media.
4) Energy absorbed by vibration.
5) Energy lost as heat.

More recently a further theory has been developed by Bond. He observed that
the energy required to reduce a material from an initial size of d0 to a final size of d1
is defined by the difference between the total quantities of energy needed to pass
from a theoretically infinite size to sizes d0 and d1 respectively. This evaluation has
given rise to the identification of a “Work Index”: an example of values obtained
semi-experimentally is given below:

Calcined clay 1.43 Quartzite 12.67


Glass 3.08 Spodumene 13.70
Raw clay 8.16 Nepheline syenite 14.90
Pyrite 8.90 Silica sand 16.46
Dolomite 11.31 Magnesite 16.50
Limestone 11.61 Basalt 20.41
Feldspar 11.67 Mica 134.50

37
Applied Ceramic Technology

These figures give a good idea of how the “grindability” of a material depends
not only on its hardness or abrasion resistance.

Discontinuous wet grinding theory with Alsing or ball mills

The purpose of wet grinding is, as mentioned earlier, not only to reduce the
particle size of the raw materials in the bodies to a few microns but also to achieve
perfect homogenisation and dispersion of the various components throughout the
mix.
Wet grinding is almost exclusively performed in Alsing or ball mills (fig. 5).
This type of mill has a discontinuous work cycle. The entire work cycle is divi-
ded into three phases:
1) Loading of raw materials, water and rheological additives (usually defloccu-
lants).
2) Grinding.
3) Unloading of the obtained slip.

Proper grinding and good mill performance depend on the observance of basic
rules and the understanding of some basic concepts. The most important of
these are:
a) Mill speed
A mill of diameter D metres, rotating at “n” revolutions per minute has a peri-
pheral speed of:

v = (π/60) D n = metres/sec.

Fig. 5. Discontinuous Alsing or ball mills.

38
Grinding

The speed of the mill exerts a centrifugal force on the pebbles (i.e. the grinding
media) lying against the drum wall; this force raises the pebble of mass “m” by an
angle α with respect to the horizontal: this is the point at which the force of gravity
is equal to the opposing centrifugal force.

cf = m v2 (D/2) = mgsen α

This equality indicates that the angle to which the pebble is raised is indepen-
dent of the mass “m” of the pebble and depends only on the rotation speed of the
mill.
Once the lift angle α is exceeded the pebbles up against the drum wall fall away
from it because, at this point, gravity overcomes the centrifugal force. They thus fall
back into the mill, tracing a parabola as they do so. The angle β that the pebbles
achieve beyond the lift angle α is known as the “cascade angle”.
The pebbles that are not against the drum wall but located closer to the axis of
rotation have a lower peripheral speed than the outermost ones, are not lifted as
high and are enveloped by more external layers as illustrated in fig. 6.
The overall motion of the grinding media in a mill thus consists of a “cascade”
drop plus a rolling action: these two movements cause grinding.
The angle of lift a can also be expressed as a function of mill RPM:

v = (π/60) D n metres/sec

and centripetal acceleration expressed by the formula:

ca = 0.0055 D n2 m/sec2 therefore sen α = (ca/9) = 0.000561 D n2

Where acceleration ca is considerably lower than g the load is raised only a little
above the horizontal and the pebbles tend to slide backwards on the mill lining;
grinding action is low and the pebble wear rate high (fig. 7).
Tests have shown that grinding is optimised at an angle of 45° - 60° because the
pebbles then fall back into the drum in “cascade” mode, roll against each other and
thus maximise grinding; moreover, wear on the pebbles and the mill lining is mini-
mised.
Where acceleration ca is approximately equal to g, the pebbles closest to the mill
lining “stick” to it (partial centrifugation) while the inner layers of grinding media
trace a parabola and fall back against it.
The produced grinding action is still high but wear on both grinding media and
mill lining is intense.
The pebbles closest to the lining will, of course, continue to “orbit” the mill
without ever falling as they are subject to a centrifugal force equal and opposite to
the force of gravity.
The peripheral speed at which partial centrifugation begins and pebbles start
“sticking” to the lining is called critical speed (cs).

39
Applied Ceramic Technology

Fig. 6.

Fig. 7.

40
Grinding

When ca is sufficiently stronger than g even the innermost layers of grinding


media will adhere to the mill lining as centrifugal force overcomes gravity (total
centrifugation).
Under these circumstances grinding does not take place at all.
The above leads us to conclude that a progressive increase in mill speed (i.e.
RPM) initially results in increased grinding efficiency; then, as centrifugation co-
mes into play, further increases in mill speed diminish grinding efficiency.
There is thus an optimum mill speed at which grinding time is minimised (fig. 8).
Nevertheless, optimum mill performance does not correspond to minimum grin-
ding time but is, rather, achieved at that speed at which the energy lost in friction
and impact is minimised and the energy spent on actually grinding the product is
maximised. This occurs when the grinding media fall into the mill in “cascade”
mode at an angle of 45° - 60°.
As experienced production personnel will be well aware, the noise made by the
grinding media can provide important clues as to whether the mill is running at the
right speed.

Tempo di time
Grinding
macinazione

VelocitàMill
del speed
Mulino

Fig. 8.

Fig. 9 shows critical and correct speeds as a function of the internal diameter of
the mill.
All the mills that run according to the graph in fig. 9 have a constant centripetal
acceleration = 50-75% of gravitational acceleration (g).
However, to apply the same acceleration values to mills of different diameters is
wrong; large-diameter mills are more efficient and acceleration can, and should, be
slightly reduced to make the lining and grinding media (subject to more stress than
in smaller mills) last longer. Mills are thus run not at constant centripetal accelera-
tion but at constant peripheral speed; at most, such speed will vary within a very
tight range. For example:

41
Applied Ceramic Technology

Giri
RPM metri
metres
min’ min’
130 180

120 170
110 160 _
1 Vc = 133 √D m/min
100 150
90 140 2 Vk = 75% Vc

80 130 3 Vk = 50% Vc
70 120 _
4 nc = 42.3/√D
60 110
5 nk = 75% nc
50 100
40 90 6 nk = 50% nc

30 80
20 70
10 60

0.5 1.0 1.5 2.0 2.5 metres


metri
Diametro utile
Effective deldiameter
mill Mulino (m)
in metri

Fig. 9.

a) for low and medium density grinding media


(2.4 - 2.7 g/cm3)
Vk = 95 - 125 m/min, that is:
nk = Vk/πD = (30 - 40)/D RPM

b) for high density grinding media


(3.4 - 3.5 g/cm3)
Vk = 85 - 95 m/min, that is:
nk = Vk/πD = (27 - 30)/D RPM.

Fig. 10 shows these values.


Of coarse, the above should be taken only as a rough guide; in the final analysis,
it is the cascade angle (which should always be around 45°) rather than the mill
speed which counts.
The cascade angle now depends not only on the peripheral speed but also the
type of product (solid or liquid) and, where liquid suspensions are being ground,
the density and viscosity of such suspension.
b) Grinding media
Mill rotation generates not just the overall “cascade” motion of the pebbles but
also reciprocal rotation between them.

42
Grinding

RPM
Giri metres
metri
min’ min’
130 130
Vk = 125 m/min
120 120

110 110

100 100
Vk = 96 m/min
90 90
Vk = 85 m/min
80 80 _
1 nk = 42,3/√D RPM
70 70
_
60 60 2 nk = 40/√D RPM
_
50 50 3 nk = 30/√D RPM
_
40 40
4 nk = 27/√D RPM
30 30
A Porcellana-steatite
Porcelain-steatite
20 20 (densità
(density 2.4
2,4+2,75 gr/cm33))
- 2.75gr/cm

10 10 B Sintered
Allumina alumina
sinterizzata
(density 3,4+ gr/cm3)
(densità 3.4+
0.5 1.0 1.5 2.0 2.5
Effective mill diameter (m)

Fig. 10.

Such rotation is particularly grinding-effective where grinding media consists


of spherical or cylinder-shaped balls.
Much less efficient are silica pebbles on account of their irregular shape, which
makes rolling discontinuous and heterogeneous (fig. 11).

Rolling and attrition between pebbles of different morphologies


The most important aspect of grinding media is its specific weight (normally
referred to as density). Classification is as follows:
a) low density media (specific weight = 2.4 - 2.7 g/cm3), such as standard porcelain
or silica.
b) medium density media (specific weight = 2.7 - 3.0 g/cm3): such as steatite, porce-
lain with a high alumina content etc.
c) high density media (specific weight = 3.4 - 3.6 g/cm3), such as sintered alumina,
alubit©.

The higher the specific weight, the greater the kinetic energy freed during rol-
ling and falling (grinding media volume being equal) and the more effective the
grinding action.
Moreover, in wet grinding, because of hydrostatics, the force of gravity is pro-
portional to the difference pc-ps (between the specific weight of the media and the

43
Applied Ceramic Technology

Fig. 11.

specific weight of the product). The greater this difference, the greater the grin-
ding action. Fig. 12 shows how the specific weight of the grinding media influences
grinding times.

c) Grinding media load (pebbles)


The amount of grinding media loaded into the mill has a strong influence on
grinding times; if the quantity of pebbles in the mill is increased progressively,
grinding time initially falls and reaches a minimum when the pebbles fill about half
the mill. Beyond this point grinding times start to increase again.
Reciprocally, absorbed power initially increases and reaches its peak where the
grinding media occupy about half the mill and then starts to drop (fig. 13).
According to P.E.I. minimum grinding time corresponds to a pebble load of
about 60% of mill volume. In practice, though, the recommended pebble load is 50-
55% (i.e. apparent volume of pebbles equal to 50-55% of mill volume).

% di
of Residuo 10.000 mesh/cm 2
a 10,000
residue at
Maglie/cm3
100

90
1 Porcellana normale (densità = 2,4)
80 1 Residuo porcelain
Standard = 0 dopo (density
24 ore = 2.4)
2 Steatite=(densità
Residue = 2,6-2,7)
0 after 24 hours
70
2 Residuo
Steatite = 0 dopo
(density 20 ore
= 2.6-2.7)
60 3 Porcellana
Residue = 0 ad alto
after 20contenuto
hours
3 di Allumina
Porcelain with(densità
high = 2,7-2,76)
50 Residuocontent
alumina = 0 dopo 16 ore= 2.7-2.76)
(density
Residue = 0 after 16 hours
40

30

20

10

2 4 6 8 10 12 14 16
Tempo di macinazione
Grinding in Ore
time (hours)

Fig. 12. Influence of specific weight of grinding media on grinding time.

44
Grinding

Grinding
time

Absorbed
power

Empty Full

Level of pebbles as % of mill diameter

Fig. 13. Grinding times and absorbed power as a function of grinding media load.

The corresponding level of pebbles is 50-54% of mill diameter as illustrated in


table n. 1 and fig. 14.

Note n. 1

The angle between the two tangents at the pebble-particle contact points is cal-
led the grip angle; it depends on the diameters S and p (of pebbles and particles
respectively, see fig. 15).
Calculations show the optimum grip angle to be about 17°: this means that the
diameter of the pebbles should be 90 times the average diameter of the particles.
For example, where particles have an average initial diameter of 0.7 mm, the peb-
bles should be approximately about 60 mm in diameter.
After a certain time, though, these pebbles will no longer provide efficient grin-
ding.
An assortment of pebbles is thus needed: the large pebbles grind the larger
particles into smaller ones and the small pebbles refine those smaller particles even
further. Pebble diameter should not, in any case, exceed 60-70 mm.
The real volume accounted for by the pebbles in a completely full mill is only
about 60% as the remaining 40% consists of the gaps between them.

Note n. 2

This data (tab. 1) refers to a stack of pebbles of a differing diameter that is


intermediate between real volume cubic stacking = (π/6) 100 = 52.4% (stacking by
minimum density) and real volume tetrahedral stacking = √(2π /6) 100 = 74%
(stacking by maximum density) (for pebbles all having the same diameter).

45
Applied Ceramic Technology

Percentage del
Percentuale of mill volume
volume del Percentage
Percentuale delofdiametro
diameterdel
occupied
mulino occupato dalla carica di of mill taken
mulino raggiunto dalla carica
by pebble load up by pebble load
biglie delle biglie
5 10
15 21
25 30
35 38
45 46
55 54
65 62
75 70
85 79
95 90
100 100

Tab. 1.

55% of volume
50% of volume

50-54% of mill diameter

a) Apparent volume of pebbles = 55%


b) Free volume of mill = 44%

b)
a)

54% D

c) Real volume of pebbles = 33%


d) Volume of gaps between pebbles = 22%

Fig. 14. Mill filling diagram.

46
Grinding

Fig. 15.

It thus follows that for a pebble load occupying 50% of mill volume, the real
volume of the pebbles is approximately 50 × 0.6 = 30% and the volume of the gaps
between the pebbles approximately 50 × 0.4 = 20% of mill volume.
Summing up:
Apparent volume Real volume Volume of gaps Free volume
50% 30% 20% 50%
55% 33% 22% 45%

Apparent pebble volume, real pebble volume and the level of the spheres in the
mill are interconnected as illustrated in fig. 16.
e
volume

vo n t
m
Free

le re
lu
bb pa
pe Ap
pebbles
of product
above
Volume

le
bb
l pe e
a m
Re volu
Volume

gaps
of
% of mill volume

volume
pebble
Real

% of mill diameter reached by level of the pebbles

Fig. 16.

47
Applied Ceramic Technology

Once the load volume occupied by the pebbles is known it is easy to calculate the
weight per unit of volume, i.e. the so-called load ratio.

Load ratio = Real vol. % × specific weight (g/cm3)

A load occupying from 50 to 55% of mill volume gives, depending on specific


weight, the following load ratios:

Pebbles Specific weight Real volume Load


in g/cm3 % ratio kg/m3

Low density ð 2.4 ð 30-33 ð 720-800


porcelain

High density ð 2.7 ð 30-33 ð 810-900


porcelain

High density ð 3.4 ð 30-33 ð 1080-1120


alumina

Fig. 17.

These load ratios are not always observed. It is common for mills to be loaded at
much lower ratios, such as 500 kg/m3, according to the well known formula: pebble
load in kg/m3 = mill volume in litres/2. This ratio is much too low because even
with high density porcelain the real pebble load is just:

500/2.4 = 208 litres/m3 = 21%

This means an apparent volume of approximately 35% (as opposed to 50%) and
a level of about 37% of mill diameter (13% below the half-full line).
This ratio (even less favourable where medium and high density grinding media
are used), involves longer grinding times and wears both pebbles and lining faster.
Pebble size/assortment must be chosen on the basis of the following factors:
a) Mill size: mills of small volume must be loaded with a smaller-sized assortment
of pebbles than larger mills. An assortment of three different pebble sizes is
generally used, as follows:
45-50% smaller diameter pebbles
25-30% intermediate diameter pebbles
25-30% larger diameter pebbles.
b) Particle size distribution of the substance to be ground and the ground substance: where
the substance to be ground is made up of coarse particles large-diameter pebbles
will be needed. If that substance is to be fine-ground smaller-diameter pebbles
will be needed to increase the number of contact points and the total surface
area of the pebbles themselves.

48
Grinding

Table 2 gives contact/surface area data for pebbles of different diameters.


c) Specific weight of the substance to be ground (wet grinding): in wet grinding, where
the specific weight of the product is high (e.g. greater than 2.5 g/cm3), high
density pebbles must be used; thus the difference 3.4 - 2.5 = 0.9 is in the same
order as that between a pebble of specific weight 2.4 and a product of specific
weight 1.5.
d) Product load. As with pebble load, there are no hard and fast rules, only general
guidelines. The product (wet or dry) must at least cover the pebbles completely.
Quantities any lower than this would be ground too quickly and could overheat.
Moreover, wear on both pebbles and lining would be intense.
The lower product load volume limit is thus given by the volume of the gaps
between the pebbles. For example, where pebble load = 50% of mill volume the
product must account for at least 20% of mill volume, that is (20/100) 1000 =
200 litres per m3.

However, there should really be more product than this so as to cushion the
pebbles cascading back into the mill.
Bear in mind that the more “excess” product is added, the longer the grinding
time.
Fig. 18 shows how grinding time is influenced by product load P, expressed as a
percentage of mill volume.
The upper product load limit is given by the minimum free space that must be
left in the mill; this space represents approximately 25% of drum volume and the
upper product load limit is thus about 20 + 25 = 45% of mill volume.
Of course, if the mill is this full grinding times will be lengthy and grinding
output (kg of product ground per hour) low.
In some cases, though, manufacturers are not so much concerned with maxi-
mum grinding output as they are with the fact that the mill has to be run for a
certain time, perhaps because the product so requires or simply because the factory
does not always have personnel at hand to empty and reload the mill; hence it often
makes more sense to use the available mill volume completely.

Diameter of pebbles in mm 20 30 40 50 60
2
Surface area of pebbles in cm 12.56 28.27 50.26 78.54 113.10
Volume of pebbles in cm3 4.19 14.10 33.50 65.25 113.00
3
Number of pebbles per dm (1) 143.10 42.57 19.91 9.19 5.31
Number of contacts per dm3 (2) 858.70 255.42 107.46 55.15 31.85
Surface area of pebbles
in m2 per m3 179.73 120.34 90.01 72.20 60.05
(1) Calculated according to real volume = 60% of apparent volume, which represents a practical load factor,
owing to the average between best and worst possible pebble settling.
(2) Calculated according to tetrahedral stacking (with 6 contacts per pebble).

Tab. 2.

49
Applied Ceramic Technology

Grinding time

Product load (% of mill volume)

Fig. 18.

e) Lining and grinding media


Both lining and the grinding media can be made of several different materials.
The table below shows the most commonly used lining/media combinations for
ceramic body and glaze mills.

MILLS FOR BODIES


Lining Grinding media
– Silica – Silica
– Alumina – Alumina
– Rubber – Silica
– Rubber – Alumina

MILLS FOR GLAZES


Lining Grinding media
– Porcelain – Porcelain
– Alumina – Alumina

Such materials generally have the following specific weights


SILICA: 2.65 kg/l
PORCELAIN: 2.75 kg/l
ALUMINA: 3.57 kg/l

f) Conclusions
The concepts described so far may be summed up as follows.
The main factors influencing grinding are:
– mill speed.

50
Grinding

– pebble load (load ratio, assortment, type).


– product load (load ratio, type, initial and final particle size distribution). Rational
use of a mill involves regulation of the above factors so as to minimise the ener-
gy absorbed in the wear of the lining and the grinding media and the energy
dissipated as heat generated by friction and attrition.

These optimal conditions are achieved when:


– mill speed produces falling-rolling of the pebbles; peripheral speed should ap-
proximately be:
95-125 m/min for low density pebbles
75-85 m/min for high density pebbles.

The pebble load level should be half the diameter of the mill or a little more (50-
55% by volume, that is 50-54% by diameter).
This involves the following load ratios:
700-800 kg/m3 of low density pebbles (2.4)
800-900 kg/m3 of medium density pebbles (2.7)
1000-1100 kg/m3 of high density pebbles (3.4).

– The assortment of pebbles must be selected as a function of the initial and final
particle size distribution of the product; mill size also needs to be taken into
account.
As a rough guide, the assortment for silica pebbles should be as follows:
45-50% of smaller diameter pebbles (20-30 mm)
25-30% of intermediate diameter pebbles (40-50 mm)
20-25% of larger diameter pebbles (50-60 mm).

– There should be at least enough product to fill all the empty gaps between the
pebbles (20-22% of mill volume): it is highly advisable to add some excess pro-
duct (up to a maximum of 25% with respect to mill volume).

Practical load calculation for discontinuous wet grinding mills

An exact calculation of the quantity of raw material to be loaded in the mill


requires certain information; this is usually found in the mill instruction manual or
the raw material test lab reports.
The required data is:
1. Effective mill capacity This is the space available to the raw materials, water and
grinding media. Expressed in litres.
2. Slip density to be prepared in the mill. Expressed in kg/l.
3. Content of solid material in the slip. Expressed as a percentage.

51
Applied Ceramic Technology

The load for body grinding can be calculated with the following formula:

Kg of dry material = 0.55 (0.67) × Vu × d × y/100

where
Vu = effective mill volume
d = slip density kg/l
y = dry material percentage in slip
0.55 = filling coefficient of mills with silica grinding media
0.67 = filling coefficient of mills with alumina grinding media.

Calculating the load for a discontinuous mill (example)

The mill to be loaded and the slip to be prepared have the following characteri-
stics:
– mill capacity = 30,000 l
– silica lining
– silica grinding media
– effective volume 24,000 l
– slip density 1.6 kg/l
– dry material in the slip 64% (water = 36%)

Kg of dry material = 0.55 × 24,000 × 1.6 × 64 / 100 = 13,500

If the body composition is:


Clay A 10%
Clay B 23%
China Clay 12%
Feldspar C 17%
Feldspar D 18%
Feld. sand 20%
the quantity of each dry raw material can be obtained from the proportion

Weight of dry material X = (% of dry material X in the body) x (Mill dry load)
i.e. where X is china Clay its weight is 12% of 13,500 = 1,620 kg

Since raw materials stored in the factory are seldom dry, it will be necessary to
determine moisture content and bear this in mind during batching via the propor-
tion

Wet batch weight = Dry weight × 100 / (% of dry content in raw material)

This calculation provides the sum of the weights of the individual raw materials
which, depending on their moisture content, will exceed the theoretical weight cal-

52
Grinding

culated as mill capacity: loading moist raw materials means loading water. The pre-
sence of such water will have to be taken into account when calculating the quanti-
ty of grinding water. This is calculated as follows:

36 (% H2O) : 64 (% raw materials) = Z (theoretical litres or kg of water to be loaded)

therefore:

Z - [(Ytot Total weight moist materials) – (Xtot Total weight dry materials)] =
kg or litres of H2O to be added

Rheological additives (deflocculants) are normally added together with the wa-
ter in appropriate quantities, calculated in the laboratory as described in Volume 1;
in any case such quantities represent only a small percentage (0.2-0.4%) of the total
weight of the dry raw materials.

Continuous wet grinding

Recent years have seen a steady increase in the number of continuous wet grin-
ding plants being installed.
These plants use tubular mills. Raw materials (body components and water) are
fed continuously from one end of the mill while the slip exits from the opposite end.

The continuous wet grinding plant

The first section of the plant consists of a continuous computer-controlled weigh-


ing and batching system. Each of the different raw materials making up the body
composition is stored in a silo.
Each of these silos features an extractor which regulates, on the basis of a si-
gnal, the quantity of material released onto the weighing conveyor belt. The weighing
belt measures the difference between the actual outflow and the set-point and tran-
smits it to the computer. In the event of an anomaly the computer modifies the
release rates to ensure that the ratio of components – and thus the body formula –
remains constant.
The thus-batched raw materials merge together on a conveyor belt which carries
them to the mill pre-loading silo; the latter has a filling cycle regulated by a level
control sensor.
A mechanical extractor unloads the material from the silo constantly and places
it on a weighing conveyor which compares silo outflow rate with the mill infeed set-
point and corrects any fluctuations by adjusting conveyor speed (fig. 19).
Just before the mill feed screw there is a device that pre-mixes the raw-material
and the deflocculant with the aqueous suspension containing re-circulated screen-
ing residue.

53
Applied Ceramic Technology

GRINDING DEPARTMENT: FLOW DIAGRAM

Fig. 19.

At the mill outlet the slip is first passed through a sieve with a mesh size of a few
mm to trap any large, solid lumps (including small pebbles); a smaller-mesh sieve
set follows.
The sieving residue is carried away by the pre-batched water to be recycled into
the mill while the slip is sent to a constantly stirred holding tank.
From here it is pumped directly into the spray drier or put through a colouring
process.
Generally, all the raw materials (clay and non clay) making up the body are fed at
the pre-mixer stage and subsequently to the mill.
However, in some cases a part of the clay (generally the wettest most plastic
part) and any colourless unfired scrap is dispersed in a turbo mixer.
Possible system configurations associated with this technology (fig. 19) are,
essentially:
– configuration in which a part of the clayey components by-pass the mill; the mill
is fed with a mix rich in components that are hard with respect to the formula-
tion of the body, but containing a certain percentage of plastic raw material for
suspension purposes.
– configuration with pre-dispersed clayey materials (and any unfired scrap), fed
into the mill after mixing with the other slip components.

These solutions are particularly appropriate in cases where the body has a sub-
stantial proportion of very plastic, very moist clays (moisture greater than 15-20%),

54
Grinding

as they are difficult to mix with other body components and can lead to aggregation
phenomena which reduce grinding efficiency.

Continuous grinding technology

Constant research into innovative control equipment has resulted in the deve-
lopment of precise, highly reliable weighing and batching systems (raw materials,
deflocculants, water).
Such microprocessor-controlled systems have led to the introduction of conti-
nuous mills in the body preparation plant.
Consequently, manufacturers are now able to provide excellent consistency of
slip characteristics such as composition, water content, density, viscosity and, last
but by no means least, grinding residue.
The reasons behind the ceramic tile industry’s adoption of the continuous pro-
cess – already used in the mining industry extensively – are twofold: technological
and technical-managerial.

From a technological standpoint the most immediate advantages vis-à-vis pro-


duct quality are:
– greater consistency of slip characteristics thanks to automated in-mill batching
of the various materials (body components, water and deflocculants) that are
much more reliable than manual procedures.
– greater grinding media efficiency thanks to optimisation of pebble assortment
in the different chambers and a grinding media/loaded material weight ratio of
at least 2.5:1 (for a 3-chamber mill in silica - silica - alumina) compared to a
maximum of 1:1 for discontinuous mills with high density alumina media.
– as a result of the above, grinding times have been reduced drastically: for por-
celain tile bodies, which contain a significant amount of hard, comminution-
resistant materials, grinding times vary from 2 to 3-4 hours (depending on
whether the pebbles are made of alumina or silica).
This is a huge gain on the 10 hours or more (up to 30 hours with silica media)
associated with discontinuous mills - improved rheological characteristics of the
slip, thus making sieving easier even when density is increased and slip water
content drops by 2-3%; the latter can be sieved directly at the mill outlet without
having to interrupt agitation, thus preventing the thixotropic phenomena which
can disturb sieving; furthermore, slip outlet temperature, on average 20-30 °C
higher than in discontinuous mills, keeps viscosity within the required range
(about 3 °E) and ensures good fluidity.

From a technical-managerial viewpoint the main advantages are:


– approximately 15% less heat energy is required in the spray-drying process be-
cause water content is reduced by about 2% and the slip is warmer (20 °C ap-
prox.): the former translates into latent heat savings and the latter in sensible
heat savings.

55
Applied Ceramic Technology

– thanks to reduced grinding times, machine-specific productivity increases by up


to 70% per unit of volume.
– less personnel are needed to run an automated process.
– up to a 50% less grinding department space is required per unit of output, favoured
by the economies of scale that allow containment of the number of auxiliary
machines.

Description of continuous mills; how to choose the right size

The machine (fig. 20) is essentially made up of:


– A cylindrical structure with a rigidly bolted base. This has hubs for the support
of the entire mill and concentric ports arranged inside the hubs for loading/
emptying. The cylinder is made of thick, special stainless steel that has been
precision welded and quality-checked using X-rays and ultrasound.

The bases are made of high-strength, precision-made cast iron on the cylinder
connection flanges and the bearing drive fits.
– A series of supports, made of steel profiles and thick sheet metal, are anchored
rigidly and partially sunk into the cement foundations.

Mill supports are equipped with bearings of the double roller type to sustain rol-
ling load adequately.
– A drive unit made up of one or two DC (or AC) motors, which, via a series of
reducers, moves the mill cylinder: the reduction system may be of the gear or
belt type.

The drive unit thus provides:


a) soft and gradual mill start up with low current absorption.
b) a wide range of rotation speeds, thus making it possible to set the most suitable
grinding speed for the specific body type (for DC motors).
c) gradual mill deceleration with final halt in correct position.

– An internal cylinder lining made of wear-resistant rubber specially shaped to


maximise grinding efficiency.
– A series of forced oil or grease lubrication systems to lubricate all drive parts.

Description of the mill

The continuous mill is, then, made up of a cylindrical sheet steel structure with
ports for inspection, maintenance and introduction of grinding media; bases featur-
ing ports for continuous infeed of raw materials and unloading of slip, a drive unit,
a series of oil/grease lubrication systems and a PLC control panel.
The anti-wear rubber lining on the interior of the cylinder usually incorporates

56
Grinding

Fig. 20. Continuous mill.

protuberances known as lifters: these are specially designed to optimise grinding


and increase the dynamic effect of the pebbles on the material. The mill is sub-
divided into two or three chambers by bulkheads featuring adjustable-aperture throu-
ghways to control the axial flow of the slip and regulate how long the slip stays in
the different zones.
Sub-division of the cylinder means that grinding media materials and pebble
assortments can be optimised for each different stage of grinding:
– heavy grinding media of varying size for mixing of the heterogeneous material
near the mill infeed point.
– heavy grinding media of varying size, for the crushing or primary comminu-
tion of the harder coarse material: this stage does not necessarily necessitate
high-density grinding balls (although they would undoubtedly improve per-
formance).
– spherical or rounded media (to provide the rolling that optimises refinement of
the material through abrasion and cutting): during the body refinement stage
these pebbles should be small (to ensure a high number of media-media contact
points) and high density (to keep dynamic input high and so maintain a vigorous
impact action).

In practice, in-mill grinding media separation is not so clear: primary crushing


and mixing, already partially begun in the pre-mill feed devices, occur simultaneously
in the first chamber and continue, to a lesser extent, in downstream ones.

57
Applied Ceramic Technology

Production of single-firing, porous or vitrified tile bodies generally involves mills


with just two chambers, while porcelain tile manufacturers almost always use 3-
chamber models.
The third chamber is generally used for extreme refinement of the body and is
loaded with small grinding media.
The first two chambers will usually contain medium density media (d≅2.6 g/
cm³) made up of rounded silica pebbles of varying size (from 30 to 100 mm); the
third chamber generally contains high density sintered alumina balls (d≅3.5 g/cm³),
quite small in size (1-1½”), that refine the materials efficiently and ensure high pro-
ductivity.
Costs associated with grinding media wear in a continuous 3-chamber silica-
silica-alumina mill are generally less than those incurred with discontinuous mills
having alumina grinding (i.e. pebbles+lining).
Optimising the grinding process via appropriate distribution of in-mill silica
pebble assortment allows the desired particle size distribution to be achieved fast
enough to meet output requirements without having to use costly sintered alumina
media.
Porcelain tile manufacturers generally use one of two different types of conti-
nuous mill that meet very different managerial and production needs. These are:
– very high capacity mills of enormous output potential which generate enor-
mous economies of scale vis-à-vis auxiliary equipment and running costs. Mills
of this type may, for example, have an effective internal capacity of 150,000
litres and yield an average output of 14-16 tons/hour of dry porcelain tile body.
– low capacity mills that are more flexible and easily adaptable to already-opera-
tive grinding departments. For example, these include mills with an effective
internal capacity of 35-40,000 litres that provide average hourly outputs of 3.8
tons/h of dry body for porcelain tiles.

Assuming average unfired scrap to be 5%, overall L.O.I. (loss of ignition) to be


5% and fired tile weight to be 20 kg/m², output for the above mill types may, in
practice, be calculated as approximately 15,700 m²/day and 4,100 m²/day respecti-
vely.
Self-classification of grinding media and grinding type is also possible: this is
seen on cylindrical-type continuous mills featuring a helical classifying lining or
those that have a range of diameters (i.e. the cylinders are conical).
The operating principle of the cylindrical drum with helical classifying lining is
based on the fact that large grinding media tend to remain at the periphery of the
mass rolling inside the mill owing to the combined effect of gravity, rolling and
centrifugal force.
However, the lining lifters push the bigger pebbles backward towards the load-
ing material inlet where larger pebbles are needed.
Such mills do not have any partitions or separated chambers and the pebbles can
be introduced during feeding together with the raw materials and water etc (in
other words, “on the run”) instead of having to stop the mill to re-charge media into
the separate chambers.

58
Grinding

Fig. 21. Continuous mill with cylindrical drum and helical classifying lining.

Fig. 22. Continuous conical section mill.

The operating principle of the conical mill is based on the fact that large grin-
ding media, thanks to gravity, rolling and centrifugal force, tend to move towards
the large mill diameter zone (feeding side). The main problem with this type is
lower efficiency of final refining near the outlet due to decreased diameter (and
volume) in this part of the mill.

59
Applied Ceramic Technology

MILL SIZING

Mill productivity

a) Sizing
Continuous mill size and productivity are functions of a coefficient Ks that de-
pends on the type of body to be ground and is defined on a case-by-case basis.
This coefficient is assumed to be inversely proportional to the grinding time of
the body in question in a standard-compliant discontinuous mill.
It follows that the formulas for hourly output (H.O.) and mill size (effective vo-
lume) are:

H.O. = Vu × d × s × Ks/GT

where
Vu = effective mill volume in litres
H.O. = hourly output in kg/h
d = slip density in kg/l
s = % of dry material in the slip
Ks = coefficient
GT = grinding time in standard-compliant discontinuous mill where it mathe-
matically follows that:

H.O. × GT
Vu = 
d × s × Ks

b) Grinding time GT
The time the body takes to reach the desired residue logically coincides with the
time it is left in the mill.
This time is defined as:

Vu × d × s × Kr
GT = 
H.O.

where
GT = time in mill expressed in hours
Vu = effective mill volume in litres
d = slip density in kg/l
Kr = filling coefficient (ratio)
H.O. = hourly output in kg/h.

As already observed for discontinuous mills, there are also certain principles and
regulations for the efficient running of continuous mills:

60
Grinding

a) Rotation speed
To determine the correct speed at which a continuous mill should be run the
already-explained rules and formulas for discontinuous mills can be applied.

b) Lining shape
Previous descriptions of the grinding process refer to mills with an essentially
smooth lining in which there is no added lifting force between the lining and the
grinding media.
The point at which the grinding media “detaches” from the lining – a key de-
terminant of grinding efficiency – can be changed by modifying the profile of the
lining.
Continuous mills are normally fitted with rubber protrusions that aid lifting of
the grinding media.
The distance between the lifters is constant on all types of lining.

c) Different lining types


A description of linings should take into account three factors: lining material,
lining profile and lining attachment systems. The most commonly used lining ma-
terials are:
– high quality cast steel and rolled steel
– rubber
– stone (e.g. microcrystalline quartz)
– a combination of wood and steel
– porcelain.

Generally speaking, the most widespread materials are rubber and steel, which
complement each other.

Fig. 23. Left: illustration of mill interior (note the diaphragm between the two chambers). Right: two
different lifter profiles.

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None of the above materials is ideal for all applications.


When coarse material is ground with large pebbles, a steel lining is generally
preferred (not for ceramic bodies).
Properly designed rubber linings have a particularly wide field of application
and are, today, the most common.
Rubber is, as a rule, the best material for working temperatures of 80-90 °C.
Another important factor in the choice of lining material is the potential for
contamination.
Rubber is preferred in the grinding of ceramic materials to avoid even very small
quantities of iron grains, which can lead to post-firing colour alterations.
Rubber coated stone linings and the first rubber-lined mills featured completely
smooth profiles.
Yet to give the grinding load sufficient kinetic energy, smooth-surfaced mills
have to rotate at a higher RPM than those with shaped linings. Moreover, high
wear rates are caused by the material rubbing against a smooth lining as its slides
backwards. A gradual increase in grinding media lift can, by choosing an appro-
priate lining profile, be obtained at even medium RPM.

d) Grinding media
Bear in mind that ceramic bodies can be divided into two main categories: white
(or clear) firing and coloured firing.
White bodies must not in any way be contaminated by colouring substances
while, of course, there is less of a problem with coloured bodies. This distinction
influences the choice of grinding media, the specific weight and abrasion resistance
of which must be as high as possible.
There are two possible solutions:
1) White bodies: grinding media in alumina or silica.
2) Coloured bodies: grinding media in silica (or steel).

With coloured bodies, then, it is also possible to use steel grinding media, which
provides high grinding efficiency. However, trials have shown that only iron parti-
cles smaller than 100 microns do not cause contamination problems; hence use of
steel is only possible where the manufacturer has the equipment needed to eliminate
the coarser iron grains.
As far as linings are concerned a heterogeneous-profile rubber lining is prefer-
red for abrasion resistance and noise dampening purposes.

Control and production parameters in the continuous and


discontinuous grinding department

a) Particle size distribution (residue)


This parameter – the benchmark indicator of grinding process efficiency – is of
fundamental importance.

62
Grinding

The particle size distribution of a ceramic body drastically influences its beha-
viour during firing as it affects:
– specific surface area and reactivity
– shrinkage-vitrification curve
– deformation
– water absorption
– black core
– defects caused by contamination.

Particle size distribution is generally determined by sieving a slip sample (on a


sieve set of known mesh) corresponding to a known dry quantity and then measu-
ring the cumulative dry residue on the sieves.
A single sieve will not on its own be sufficient to determine the particle size
distribution of a body.
It is often preferable to use the residue percentages from two meshes having
apertures of 63 µm (230 mesh, 10000 maglie/cm²) and 45 µm (320 mesh, 16000
maglie/cm²) respectively. However, as long as raw material characteristics or grinding
conditions do not change, residue % at 63 µm constitutes a valid process control
parameter.

Product type Residue % at 63 µm Residue % at 45 µm


Red monoporosa 5–8 15 – 25
White monoporosa 5–8 15 – 25
Red monovitrified 5 – 10 15 – 25
White monovitrified 5 – 10 15 – 25
Fast double firing 5 – 10 15 – 25
Porcelain tile 0.6 – 0.8 1.8 – 3.0

Checking frequency: every shift/every mill.

b) Density and water content (%)


Variations in density and water content affect:
– mill productivity
– viscosity
– particle size distribution
– settling
– spray drier energy consumption.
Slip water content can be periodically checked by measuring the density of the
slip with a container of known volume (e.g. a pycnometer). Water content depends
on:
– the nature of the body
– the quantity of deflocculant added
– characteristics of the water.

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Product type Discontinuous mills Continuous mills


Red monoporosa 35 – 37 33 – 35
White monoporosa 34 – 36 32 – 34
Red monovitrified 38 – 40 36 – 38
White monovitrified 33 – 35 31 – 33
Fast double firing 35 – 38 33 – 36
Porcelain tile 33 – 35 31 – 32

Water content (%)


Checking frequency: every shift/every mill.

c) Viscosity (and thixotropy)


If viscosity is too low it can lead to:
– sedimentation of the slip
– excessive quantities of water
– excessively fine spray-dried powders.
Excessive viscosity, instead, can cause:
– longer grinding times
– mill unloading difficulties
– sieving difficulties
– excessively coarse spray-dried powder.

The nature of the body, particle size distribution (especially as regards the clayey
particles), density, temperature and pH all have significant effects on viscosity.
Optimal viscosity is: 2.5-3 °E (250 - 400 cP).
Checking frequency: once/twice per shift, every mill.

d) Temperature
Influences viscosity of the slip and often improves its rheological characteristics.
Excessively high temperatures can:
– cause intense thixotropic phenomena
– damage the rubber lining.

Optimum temperatures are 50-60 °C for discontinuous mills, 70-80 °C for conti-
nuous ones.
Checking frequency: once/twice, every mill load.

Definitions and units of measure

While the rheological behaviour of suspensions of solids in liquids has already


been described in detail in Volume I, it is worth mentioning some parameters com-
monly used in grinding departments.

64
Grinding

– VISCOSITY = the resistance a fluid opposes to movement


F/S = η (Vmax - Vmin /x)
where
F = force applied to the liquid (N)
S = surface area of application (m2)
vmax-vmin = change in speed (m/s)
x = thickness of liquid (m)
η = absolute viscosity (N s/m2 = Pa s)
N.B.: viscosity diminishes as temperature increases.

– SPECIFIC WEIGHT (DENSITY) = Weight (mass) per unit of volume


(grams/litre)
Examples:
water olive oil slip
viscosity mPa s 1 20 °C 100 300
density g/l 10004 °C 918 1700

Practical units of measure of viscosity


°Engler
Corresponds to the ratio between outflow time for 100 cc of slip and outflow time
for 100 cc of water from a standardised funnel.
This is the standard check for body slips.
Example: outflow time for 100 cc of slip = 12 sec.
water outflow time = 5 sec.
slip viscosity: 12/5 = 2.4 °E.

Ford Cup
Measurement corresponds to time taken for 100 cc to flow out of a Ford cup with a
∅ 4 mm nozzle
Mainly used with glazes and engobes.
Example: slip viscosity = 25 sec Ford cup.

°Gallenkamp
Measurement corresponds to “return rotation degrees” (generated by of a twisted
metal support wire) travelled by a cylinder that has been immersed in the slip and
rotated 360°.
Mainly used for casting slips (sanitaryware).
Example: slip viscosity = 320 °G.

cPoise (Brookfield)
A measure of viscosity effected with a fixed-speed rotating viscosimeter.
Example: slip viscosity = 300 cP
1 centiPoise (cP) = 1 milliPascal second (mPa s)

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APPENDICES

The continuous wet grinding mill and the porcelain tile industry

In the context of porcelain tile manufacturing the continuous grinding system


initially appeared to be marred by a certain rigidity as there were difficulties in
making the slip colouring process flexible.
Today, most companies equipped with a continuous drum mill use it to produ-
ce a colourless base slip, which, after sieving, is sent to a holding tank with an
agitator.
Concentrated colouring syrups are then added to the tank; alternatively, the syrups
are batched into the slip by devices installed on the tank feed line or, more rarely, in
the pressurised piping that leads to the spray drier.
Thanks to the advent of reliable automatic batching systems continuous grin-
ding has now become extremely versatile and has rapidly gained ground in the
porcelain tile sector too.
The base slip is coloured by using devices (e.g. adding batchers that operate by
weight or volume) that add colouring slips to the base body. These are installed on
the spray drier service tank feed line and thus allow a microprocessor to generate a
signal proportional to density: this signal can be displayed automatically, both local-
ly on the instrument and on the batching control system.
The measuring system thus operates independently of temperature, pressure,
viscosity, conductivity and fluid rheology.
Note: concentrated colorants are, by definition, slips characterised by a very high
concentration of colouring pigment. Use of such “concentrated” products means
that the coloured slip preparation department takes up very little space yet provides
maximum productivity, optimises the degree of grinding of the pigment and gives
optimum slip storage capacity.
As there is high pigment concentration in the slip, it will, of course, be very
dense and therefore the rheological properties of colouring suspensions must be
monitored carefully to prevent sedimentation.
Nevertheless, some companies do produce, for some periods, white or super-
white bodies directly in the continuous mill.
The rheological characteristics of these bodies differ from those of standard
base bodies in that they feature a higher non-clayey complementary content, which
is, as a rule, counterbalanced by the use of especially plastic clayey raw materials
(e.g. clays with a montmorillonite content); the latter influence the viscosity of the
slips and their tendency towards thixotropy.
Furthermore, the abundance of grinding-resistant hard components may incre-
ase process times, lowering the output potential of the body preparation depart-
ment considerably.
So, while the continuous machine is, of course, ideal for defined, constant opera-
ting conditions, it is also capable of providing a certain versatility.

66
Grinding

Technological and managerial parameters

The slip can be fluidised with the aid of solid additives such as sodium poly-
phosphate, introduced in quantities amounting to 0.3-0.4% of the dry body. Alter-
natively, where body type allows, liquid mixtures based on organic substances and
sodium silicates can be used; these are introduced in slightly higher percentages
(approximately 0.4-0.5%).
Liquid mixtures are advantageous in that they can be adapted to suit a certain
body and act faster thanks to the ease with which they are dispersed throughout the
aqueous vehicle; batching systems are also more reliable.
The water content of the slip generally falls within the 31-34% range. Bear in
mind that:
– as a rule, the amount of deflocculant being equal, a higher in-body clay content
increases the amount of water needed to disperse the material.
– high plasticity of clayey body components (e.g. montmorillonite clays) raises
viscosity, which must then be controlled by increasing water or fluidizer content
(white bodies, generally featuring a higher percentage of hard complementary
components and a clayey fraction of higher plasticity, are subject to the contra-
sting effects of the plasticity of the clays and their percentage in the body).
– recycled water that has undergone chemical-physical clarification-flocculation
treatment and has consequently been enriched with flocculating ionic substances
may work against the effect of the fluidizer and increase the required quantity
of water.
– using greater quantities of deflocculant allows the quantity of water to be re-
duced; consequently there are heat energy savings at the spray drying stage.
– attaining a high degree of body refinement means dissipation of large amounts
of mechanical energy in the form of heat; the slip thus exits the mill at high
temperature (often higher than 70 °C), keeping viscosity low.

At room temperature, slip density varies between 1690 and 1740 g/l (at mill
outlet temperatures much lower densities are observed): the lowest densities are
generally observed in colourless bodies, the highest in white ones.
Viscosity generally falls between 2.5 and 3 °E, although slips outside this range
that can still be sieved easily are certainly not uncommon. The fluidity of a suspen-
sion, in fact, should also be viewed in light of its yield point and thixotropy.
In any case, good fluidity means good sieving on small-mesh screens (net aper-
tures of 130-160 µm), indispensable in ensuring body quality and preventing im-
perfections such as dimples and dots which only show up after firing.
Production line checks should, of course, be completed by particle size distribu-
tion data from laboratory tests, which, for the most part, consist of sieve residue
analyses. The reference figures usually adopted for porcelain tiles are:
– 0.7-1% of sieve residue with net mesh opening 63 µm
– 2.5-4% of sieve residue with net mesh opening 45 µm.

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More accurate, reliable analysis – obtained with the aid of a laser diffraction gra-
nulometer – allows the user to evaluate cumulative curves and the average numerical
diameter of samples. Results are generally as follows:
– average numerical diameter of particles: 17-20 μm.
– percentage of particles passing through at 20 μm: 70-75%.

Specific electricity consumption on mills in porcelain tile plants usually stands at


50-70 kWh per ton per of dry ground body.

The table below compares porcelain tile body production in continuous and di-
scontinuous mills (grinding media quality being equal):
Continuous mill Discontinuous mill
Gross capacity (l) 40,000 38,000
Volumetric ratio 1.053 1
Grinding media Silica/Silica/Silica Silica
Lining Rubber Silica
Dry output (kg/h) 3,500 -
N° of cycles (cycles/day) - 1
Slip load (l) - 17,000
Slip density (g/l) - 1,690
Water content (%) - 34
Dry load (kg) - 18,900
Daily dry output (kg) 3,500x24=84,000 18,900/1=18,900
Output/day per unit volume (kg) 84,000/1.053=79,800 18,900/1=18,900
Total consumption/ton 63.7 kW/h 103 kW/h (*)
(*) This considerable difference is caused by the silica/silica combination (which
is quite common). Where alumina is used, grinding times are halved and electricity
consumption remains similar.
Productivity ratio, gross volume and grinding media quality remaining equal:
79,800/18,900 ≅ 4.2 (in any case this figure will always be greater than 3).

Therefore, gross mill volume and grinding media being equal, at least 4.2. discon-
tinuous mills are needed to do the work of a single continuous one. Similarly, overall
gross mill volume and grinding media being equal, continuous mill productivity is
approximately 4.2 times higher than discontinuous mill productivity.
The nature of the grinding media influences efficiency considerably: sintered
aluminium media raises machine productivity but also raises costs. However, bea-

68
Grinding

ring in mind that the benefits of sintered alumina are largely perceived at the re-
finement stage, such additional costs can be mitigated by using such media in the
refinement zone only.
Significant economies can thus be obtained simply by changing the grinding
media, without excessively penalising productivity.

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70
Drying

Chapter II

SPRAY DRYING OF CERAMIC SLIPS

Spray drying has been used in the foodstuff and pharmaceutical industries for
over a century; its introduction into the ceramic industry is a somewhat more re-
cent affair. In ceramics, spray-drying has simplified the overall production process
by replacing filter-pressing, drying, grinding, re-moisturising and classification (fig.
1) and has also reduced labour and maintenance requirements.
The slip obtained from grinding raw materials in an aqueous suspension is
dried by way of a continuous, automatic process that provides a product of con-
trolled moisture content, shape and particle size distribution that is ideal for pres-
sing.
Thanks to spray drying, these advantages have been available to the ceramic

RAW MATERIALS

PRE-TREATMENT

WET GRINDING

SIEVING

FILTER PRESSING

DRYING

SPRAY DRYING CRUSHING

RE-MOISTURISING

CLASSIFICATION

SILOS

PRESSES

Fig. 1. Comparison of the spray drying and filter-pressing processes.

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industry for some years now. Spray drying is carried out in machines called spray
drier atomisers, or, more simply, spray driers (see fig. 2).

Fig. 2.

Classification of spray driers

As a rule, there are two categories of spray drier:


a) Direct heat spray driers
In these spray driers the heat needed to bring the water in the slip to evaporation
point is introduced in the form of combustion gasses or heated air, which comes
into contact with the droplets and causes evaporation by convection. This is the
type generally used by the ceramic industry.

b) Indirect heat spray driers


In these machines the heat is transferred to the material to be treated by conduc-
tion.
The greater the surface area via which evaporation can take place, the faster the
evaporation process.
The heart of the system consists of a sprayer device that is generally of the
rotary (turbine) or fixed (nozzle) type. Atomisation of the suspension is achieved
through the use of kinetic energy (in the former) or the pressure exerted on the
fluid (in the latter).
There are, then, several different types of spray driers, each defined by the sus-
pension atomisation system and the heat flow route (upward or downward).

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Spray drying of ceramic slips

Fig. 3. Different spray drier configurations.

Fig. 3 illustrates four different types of spray drier configuration:


– Downward uniflow type, atomisation with nozzles.
– Downward uniflow type, atomisation with turbine.
– Counterflow type: atomisation with downflow nozzles, air upflow.
– Counterflow-uniflow type, upward nozzle atomisation, air downflow.

Ceramic production plants generally utilise the so-called pressure centrifuge


“nozzle” system to atomise the suspension; here, the pressurised flow also imparts,
by way of volute-shaped inserts, rotary movement of the particles as they exit the
nozzle.
Other devices known as lances can also be used to atomise the slip.
Within these different nozzle and turbine systems, then, the quality of atomisa-
tion depends on the degree of concentration of the solid, viscosity, surface tension
of the slip and the equilibrium between several other factors such as pressure, tower
volume, nozzle size (in the first case) and the characteristics and speed of the tur-
bine (in the second).
A nozzle-type atomisation system has the advantage of providing good particle
size distribution control and repeatability.
Once the flow rate and the characteristics of the incoming suspension have been
determined it is easy to exercise control over all the variables: powder particle size
distribution is changed simply by changing the nozzles.

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A nozzle-type spray drier with compressed air atomiser is rarely used to dry
ceramic slips.
For products with a very high specific weight, or where very fine particle size
distribution is required, the centrifugal disc system is the most suitable.
Fig. 4 summarises the complete spray-drying process, from slip infeed to purifi-
cation of the exhaust gases.

Fig. 4. Illustration of spray drying plant.

General description of nozzle-type spray drier

How it works

In spray drying, continuous and automatic atomisation and hot air drying of the
slip produces powders of controlled particle size distribution and moisture content
that can then be pressed in a semi-dry state to make tiles.
The spray drier essentially consists of a chamber of shape and volume designed
to promote heat exchange between the finely sprayed slip and the hot air/com-
bustion fumes.
There are, as illustrated on the previous page, several different types of spray
drier: the one most commonly used in the ceramic industry is the mixed-flow type
where the air is directed downwards from the top of the chamber and the slip is
projected upwards from the base.
This solution maximises the time spent by the particles inside the drying cham-
ber: because they first encounter the hot air in counterflow and then in uniflow, heat
exchange efficiency is high (fig. 5).

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Spray drying of ceramic slips

Fig. 5. Illustration of the spray drying process. General view of plant.

The finest powders in the spray drier chamber are first separated by cyclones,
then a dust collector. Finally, the fumes exit the stack.

The spray drying cycle

The diagram in Fig. 6 illustrates a spray drier with nozzle-type atomisation and
shows the position of all the main devices.

1. Slip feed pumps 8. Burner


2. Filters 9. Hot air duct
3. Nozzle holder ring 10. Annular hot air distributor
4. Drying tower 11. Centrifugal ventilator
5. Powder outlet valve 12. Wet dust separator
6. Separator cyclones 13. Stack
7. Pressurisation

The main body of the drier is cylindrical. Hot air is introduced into the chamber
from above and distributed tangentially; the initial counterflow stage of heat ex-
change takes place as this hot air meets the atomised slip being projected upwards
from the bottom of the cylinder via nozzles mounted on a ring which is concentric
to the chamber perimeter.
As the powders lose their momentum and fall back towards the lower, conical
section of the chamber the final uniflow stage of drying begins. Kinetic energy is
provided by a pair of piston pumps (which operate at 20-30 atm) that impart a
nozzle exit speed of about 30 m/sec, sufficient to overcome the low viscosity (about
3° Engler) of the slip, “shear” it into minute droplets and direct it upwards.

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The cone-shaped upward spray does not travel in a straight line but, rather,
spirals upwards on account of the movement imparted by internal devices, nozzles
and spirals of varying shape and size.
A simplified description of the overall drying process can be provided with the
aid of fig. 6: the slip is fed at constant pressure by the pump (1), passes through
the filters (2), and reaches the distributor ring (3) inside the tower (4).
The finely atomised slip jet is hit by a vortex of hot air produced by a natural
gas or LPG air-flow burner (8) and an intake fan (7) (or by a direct combustion
burner using liquid fuel).
The air is conveyed to the upper part of the tower via a heat-insulated steel duct
(9) and is set in rotation by the annular distributor (10). Dried powders are unloaded
via the outlet valve (5) onto a conveyor belt.

13

9
10

8
12

11 4

3
7

1 5
2

Fig. 6. Illustration of main parts and devices of a spray drying system.

76
Spray drying of ceramic slips

The fine powder residue that remains suspended in the air exhausted by the
main fan (11) is, in part, separated out by the cyclones (6) and, in part, by the wet
dust separator (12).
The exhausted air is then expelled via the stack (13).

Description of main spray drier devices

Slip feed pump (1)


The purpose of the pump is to transfer the slip – at a set pressure – towards
the atomisation devices. It is of the hydraulic piston type, powered by a hydraulic
unit.
The pistons are made of alumina, a material highly resistant to abrasive fluids.
Working pressure (regulated simply by adjusting the valves) is generally in the
order of 22-28 bar, depending on the characteristics of the slip and the type of
atomisation nozzles.

Slip filters (2)


Two filters are generally installed on the slip feed line: these trap any impurities
or foreign bodies.
It is important that these filters operate efficiently because if such impurities/
objects reach the atomisation devices they can clog the nozzles. The filters consist
of a cylindrical container containing a perforated cylinder which acts as a support
for the filtration mesh.
Filters are washed automatically and alternately (where of the automatic type).

Distributor ring (3)


Made of a stainless steel ring with spray nozzles attached, connected to the slip
feed piping via a reinforced rubber flex hose.
A simplified illustration of a stainless steel nozzle holder ring, relative feed pi-
ping and the ring extraction device is given in fig. 7. A more detailed view of the
nozzle ring is shown in fig. 8.
As an alternative to the ring system the slip can also be atomised by lances
(fig. 9).
These are arranged around the tower perimeter and protrude towards its centre.
One or more atomising nozzles can be fitted on each lance. Fig. 10 illustrates two
different spray driers equipped with ring-mounted and lance-mounted nozzles re-
spectively.
a) with ring-mounted nozzles
b) with lances.

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Fig. 7. Diagram of nozzle ring and extraction device.

Fig. 8. View of nozzle ring.

Atomisation nozzles
The nozzles are generally of the so-called “coil” type in which a spiral-shaped
insert causes the fluid, driven by the pressure behind it, to rotate in a way that
facilitates dispersion of the jet as it impacts with the air.
An exploded drawing of a nozzle is given in fig. 11.
The spiral is not the only important nozzle part: equally important are the disk
inserts with central holes.
The (upper) table in fig. 11 shows disc hole diameters and the lower table the
spiral heights.

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Spray drying of ceramic slips

Fig. 9. Lance atomiser.

Fig. 10. Cross section and plan of two different spray drier types: a) ring atomising nozzles b) with
lances.

In addition to the spirals and discs the other main nozzle parts are:
1. Head
13. Discs without hole
14. Distributor
15. Container with coupling

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Fig. 11. Nozzle parts.

The perforated discs, made of tungsten or diamond-coated, have calibrated clear-


ance. Most perforated discs have an orifice diameter of 2.5 mm.
The “coils” are located in the interior of the nozzle. These impart a rotary mo-
tion and are thus used to narrow or widen the atomised slip cone. The most com-
monly used types are between 8 and 15 mm high. The number and type of nozzles
depend on the type and quantity of spray-dried powder to be produced.

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Spray drying of ceramic slips

Drying tower (4)


This constitutes the actual evaporation chamber (fig. 12).
Made up of a conical collector, a cylindrical evaporating area and an upper sec-
tion containing the annular hot air distributor.
The internal walls of the tower are made of stainless steel and the outer walls
of polished aluminium. A heat insulation layer is sandwiched between the inner and
outer walls.
A stainless steel duct connects the tower to the separator cyclones. A thermo-
couple installed on this duct allows the exhaust air temperature to be monitored as
it relates to the moisture content of the dust produced.

Powder outlet valve (5)


This cooler-equipped valve is of the counterweight type; it cools and discharges
the spray-dried (or atomised) powder.
Ambient temperature air flows through a series of adjustable-aperture slits and
comes into contact with the outflowing spray dried material, thus lowering its tem-
perature.
There is also another type of cooler known as the enhanced performance type
(fig. 13).
This allows the external air, drawn in by low pressure, to contact the hot granu-
late downflow several times and uses special surface geometry to improve cooling
performance.
Lowering the temperature of the spray dried granulate even further reduces the
condensation problems generally encountered later in conveying systems, sieves
and silos.

Fig. 12. Cut-away diagram illustrating the tower interior.

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Fig. 13. Enhanced-performance spray dried powder cooler.

Separator cyclones (6)


These are made of stainless steel and equipped with a counterweight powder
discharge valve and inspection hatches. These perform initial powder separation
from the exhaust air exiting the tower (fig. 14).
They work constantly and are always switched on before the main fan so as to
prevent the latter being damaged by powder. Before entering the cyclones the exhaust
air powder content is in the order of 2-4000 mg/Nm3. When the air leaves the
cyclones content is just 400 mg/Nm3.

Fuel feed system


The type of fuel feed system essentially depends on the type of fuel (gaseous or
liquid, light or dense, high or low viscosity). Systems using light liquid fuel (e.g.
light oil) do not require heating devices for correct atomisation at the burner nozzle
in that their low viscosity allows them to be atomised by way of pressure alone.
Systems using, instead, heavy liquid fuels require nozzle pre-heat and special in-
burner apparatus.
Where the fuel is a very thick liquid the pumping duct and the holding tank will
also need to be heated.

Burner types (7)


The different combustion systems adopted in spray driers are as follows:
– Flu-fire burner (gaseous fuel) with cogeneration system.
– Air-flow (or in-vein) burner (gaseous fuel).
– Direct combustion Weishaupt burner (liquid fuel).

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Spray drying of ceramic slips

Fig. 14. Diagram illustrating flow routes within the fine powder separationcyclones.

Air-flow burners are suitable for gaseous fuels and forced-draught burners are
suitable for liquid fuels. In both cases the flame is adjusted via a system that modu-
lates the quantity of fuel as a function of required in-tower temperature.
Fig. 15 shows an air-flow burner. They provide excess combustion air (about
150% of stoichiometric air).
FLU-FIRE burners, instead, do not have their own combustion air fan.
Gas combustion thus occurs with process air, which must have a minimum oxy-
gen content.
Fig. 16 illustrates the structure of the FLU-FIRE burner.
These burners are also suitable in cogeneration plants and, depending on their
specific characteristics, may act as after-burners where standard generators are in-
stalled (fig. 17).

Hot air distributor (8)


The hot air distributor, installed in the upper part of the evaporation tower,
consists of a peripheral, tangential inlet and a system of spiral ducts that force
the air to move towards a corresponding series of inward-facing apertures (fig. 18).

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Fig. 15. Air-flow burner structure.

Fig. 16. FLU-FIRE burner structure.

The resulting air flow generates a vortex which facilitates heat exchange with
the slip (fig. 19).

Main fan (9)


The main fan, of the centrifugal type, draws in the air needed for the drying
process. A partial vacuum is thus present in the section of duct preceding it.

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Spray drying of ceramic slips

Fig. 17. FLU-FIRE burner coupled to cogeneration plant.

Fig. 18. Cut-away diagram showing the hot air distributor.

Fig. 19. The hot air vortexes formed in the distributor (computer generated image).

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The stack (10)


The stack constitutes the final section of the air circulation system and connects
the spray drying plant to the exterior.

Dust separator device

The wet abatement device is located downstream from the main fan. It constitu-
tes the second stage of dust separation and is where the finest dust particles are
removed.

Spray drier operation (temperature and pressure)


Working temperatures and pressures are illustrated in fig. 20.

– The slip, which exits the mill at 20-70 °C, is pumped at a pressure of 20-30 bar
towards the spray drying system.
– Pressure P1 in the drying tower is approximately -0.5/-1.5 mbar.
– The hot air intake temperature is in the 550-650 °C range.
– The temperature of the spray-dried powder is generally in the 40-70 °C range.

fume temp.
with abatement unit 60-80 °C
without abatement unit 80-120 °C

fume outlet
gate

gate

fume outlet temp.

spray dried powder temp.

slip

Fig. 20. Temperatures and pressures in the spray drying system.

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Spray drying of ceramic slips

– The air directed towards the cyclones (T1) falls within the 80-120 °C tempera-
ture range.
– The partial vacuum inside the cyclone is in the order of –10/–20 mbar.
– The temperature of the fumes exiting the stack may be 60-80 °C where a dust
separator device is installed or 80-120 °C where it is absent.
– Stack smoke pressure is in the order of +10/+15 mbar.

Since the situation varies on a case by case basis all the above figures should be
viewed as approximate.

The dynamics of “dried granulate” formulation

At the precise instant in which the slip is atomised into droplets, the latter are
split, projected upwards, captured in the turbulence generated by the downflow of
hot air and forced to follow trajectories that involve collisions, aggregations, new
splits and impacts against the tower walls.
Computer-generated flow models have allowed researchers to study just how a
spray drier works by examining the trajectory of the particles and how long they
remain in the chamber; researchers have also been able to investigate temperature
and humidity ranges both in the process area and the slip droplets themselves (see
fig. 21).
Like all “interfacial” phenomena, the relationship between mass (volume) and
surface area is crucial. Here, the phenomenon of evaporation is directly propor-
tional to the droplet surface area available for exchange and the temperature, sur-
face tension and other parameters.

Fig. 21. Computer generated image of particle trajectories inside a spray drier.

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At the same time, the size of the droplets and the direction and speed of
the atomised flow dictate the suitability of the type and size of the drying
chamber.
In the ceramics industry droplets generally range in size from just a few microns
to 900-1000 microns with a classic statistical distribution centred around 300-400
microns.
During the average life of a droplet (5-6 seconds, the contact time between the
two phases) high-energy heat exchange at the liquid interface, with air that has
been heated to over 500 °C (maximum air temperatures may be as high as 650 °C),
causes evaporation of the water in the droplet and thickening of the particles sus-
pended in it.
The size and shape of the dried product obviously depend on the nature of the
solid phase (note that the case in hand refers to a ceramic body where the percenta-
ge of inert material is very high with respect to the clayey parts).
Depending, then, on the size of the droplets, the generated granule types may be
classified as follows (see fig. 22):
a) For droplet diameters up to 70 microns drying is absolute and the finest parti-
cles, in the form of powder, are captured by the outgoing air flow and then re-
covered by the powder collection device. The smallest particles consist of indivi-
dual grinding residue particles.
b) For measurements in the 70-400 micron range drying conforms to average over-
all moisture content values and generates a granule, already spherical in shape
with a cavity of varying size, that drops into the conical cooling/collection zone
of the spray drier.
c) Over 400 microns, drying produces a granule with a moisture content higher
than the overall average; this is because, on account of its volume, it spends

Fig. 22. Possible particle size distribution of a spray dried body and morphological aspect of grains of
different sizes.

88
Spray drying of ceramic slips

less time in the drying chamber. This large granule nearly always has the clas-
sic shape described above yet also has a net tendency towards agglomeration
and inclusion of particles as a result of its high residual moisture content (fig.
23).

Fig. 23. An individual particle (left) and an example of agglomerated particles.

Granule formation mechanism


The typical hollow sphere shape generally derives from complex phenomena;
these are examined in detail below.
Tests have shown that once the drying process has begun the particle maintains
it trajectory without rotating: thus one side of the particle always faces forwards as
it travels through the air. It is on this side that initial heat exchange takes place.
This involves the first, violent superficial evaporation and consequent hardening of
the external film of the grain being formed: simultaneously the droplet contracts
as the solid particles suspended within it draw closer together (fig. 24).
Fig. 25 illustrates, stage-by-stage, the grain formation sequence starting from
the moment in which the droplet is expelled from the nozzle.

At this point the parameter which determines the final form is the duration of
heat exchange between the two phases. If this time is too short the water vapour
formed inside the droplet, unable to exit the already hardening film, shatters the
grain which, on microscopic examination, takes on the appearance of a split-apart,
layered, thickly walled egg shell.
If the heat exchange lasts longer, the water vapour forming in the interior can
leave the droplet through its rear, which is cooler and has a film still at the forma-
tion stage (thinner and less compact). This is why the rear wall collapses inwards
and the grain takes on the characteristic hollow sphere appearance, maintaining a
residual moisture content.
Of course, not all the grains take on the classic spherical shape as there may be
small percentages of agglomerates and other, finer particles.

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Fig. 24. The dynamics of particle-hollow formation.

It is the spherical fraction that provides the best results in terms of uniformity,
average composition and good flow performance.
It is interesting to note that the particle size distribution of the spray dried
grains compared to that of the wet sprayed droplets is smaller by about one third.
Starting with a slip having a litre weight of 1.6-1.7 Kg, total evaporation of the
water yields a solid with an apparent weight of about 1 Kg/l on account of the
empty gaps within the granules and between them (corresponding to the contrac-
tion undergone by the droplets as they dry).
While the solid parts contained in the initial droplet end their passage through
the spray drying system here, the liquid fraction, which has been transformed into
water vapour, is exhausted together with the air in the chamber (now cooler after
yielding the heat necessary for evaporation). After passing through the cyclones
and the wet separators, the so-called fumes exit via the stack at controlled tempera-
ture and humidity, taking with them any residual solid particles compatible with
environmental protection laws. Transformation of the relevant phases is illustrated
in fig. 26.
The final powder added to the fine powder recovered by the cyclones is sieved: it
is then stored in silos.
After an “ageing” period, which homogenises moisture content and temperature
throughout the silo, the powder can then be drawn off and sent to the pressing
department.

90
Spray drying of ceramic slips

Fig. 25.

SLIP HOT FUMES


liquid phase gaseous phase
T 35/60 °C - P 20 - 30 bar T 500/600 °C
solid 65% dry air
liquid 35% CO, CO2

POWDER COLD FUMES


solid phase water vapour phase
T 40/65 °C T 90/115 °C
solid 95% air, water vapour,
liquid 5% fumes, suspended dust

Fig. 26. Characteristics of materials and fumes (phases) entering and exiting the spray drier.

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Characteristics of spray dried powders

Morphology of the grain and particle size distribution of the powders

The spray dried grain is, then, more or less spherical in shape with a hollow
“dimple” of varying size; it contains the residual moisture necessary for pressing
and this is generally found inside the hollow. Fig. 27 compares the grain morpholo-
gy of a spray dried powder with that of a dry-ground powder. The spray dried
powder (left) appears as a set of spherical grains of varying size while the dry
ground powder (right) is an agglomerate of needle-like, acicular particles.
This difference clearly implies different mould filling characteristics at the pres-
sing stage: the best results are generally obtained with spray dried powders.

Grain size

Spray dried powder grains are generally of a diameter in the 100-600 micron
range, with much of the statistical distribution falling inside the 180-300 micron
band. Maximum particle concentration, though, is generally found in the 250-300
micron range (fig. 22).
The three factors
– grain morphology
– residual moisture content
– particle size distribution
are extremely important in defining the “flow characteristics” of the powder, which
play a key role in mould filling.

Spray dried powders derived from different bodies, such as vitrified single-firing
(white and red), porous single-firing, and porcelain tile bodies have, on the whole,

Fig. 27. Grain morphologies of spray-dried (left) and dry-ground powders.

92
Spray drying of ceramic slips

similar particle size distribution since it depends more, in fact, on the physical cha-
racteristics of the slip (viscosity and density) than it does on the composition of the
body.
Tab. 1 shows spray dried particle size distribution ranges for different bodies
commonly used in the ceramic industry.

1 2 3 4

GRANULOMETRIA:
PARTICLE SIZE DISTRIBUTION:
mgl/cm22
mesh/cm µum
m
sopra
above 100 600 2 6 2 1
“ 196 425 10 20 13 9
“ 400 300 11 13 13 10
“ 576 250 43 41 44 42
“ 1050 180 15 12 14 17
“ 2500 125 12 7 9 14
below
sotto 2500 125 7 2 6 7
Disperso
Lost 0 0 0 0
Total
Totale 100 100 100 100
Approx. average
Diam. medio diam.(µm)
approx. (µm) 283 344 295 272

Particle size distribution of different spray dried powders (different bodies).


Note: the differently numbered spray dried powders correspond to the following commonly used
industrial products: 1 white vitrified single-firing body, 2 red vitrified single-firing body, 3 red porous
single-firing body, 4 porcelain tile body.

Tab. 1. Spray dried powder particle size distribution of different bodies.

Powder flowability

The flow properties of spray dried powder are of fundamental importance to


the efficient filling of the press moulds and the subsequent tile quality.
Conceptually, measurement of powder flowability involves various factors such
as particle size distribution, specific weight, shape, mutual adhesions and degree of
packing.
In practice, however, flowability is measured by quantifying the time taken for a
given amount of powder to flow out of a funnel-shaped container.
With ceramic powders the tool proposed by AICE consists of a funnel of known
volume (fig. 28).
This measurement allows the user to obtain and evaluate the following informa-
tion:
– fluidity relative to volume (expressed in cm3/s), obtained by dividing volume by
emptying time.
– apparent density (expressed in g/cm3), obtained from the ratio between powder
weight and volume occupied (i.e. funnel volume).

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Fig. 28. Instrument for measuring powder flowability.

– angle of fall (expressed in degrees), obtained by measuring the angle of the


cone formed by the powder falling from the funnel.

Tests carried out on spray dried powders obtained from different bodies made by
different producers show very similar fluidity/volume and fluidity/mass values.
It has also been observed that the most important factor influencing powder
flowability is the residual moisture content of the spray dried powder; note that
flowability decreases as residual moisture increases (see tab. 2).
Slightly different flowability values are seen in laboratory-prepared mixtures,
obtained by mixing together very different granulometric fractions (tab. 3).
Observation of the table shows that a mix consisting of a preponderance of
“medium” particles flows better than other mixes classified as “coarse” or “fine”.

Umiditàmoisture
Powder delle polveri % %
content 3.2 5.1 5.9
Fluidità rel.
Fluidity rel. to
al VOLUME
VOLUME
3
16.1 16.1 14.8
cm3/s
cm /s
Fluidità rel.
Fluidity rel. to
alla MASSA g/s
MASS g/s 17 16.9 15.3
3
Densità apparente
Apparent density g/cm
g/ cm3 1.06 1.05 1.03
Angolo
Angle ofdi caduta °
fall (°) 30 29 31

Tab. 2. Flowability values for spray dried powders of different residual moisture content.

94
CAMPIONE SAMPLE T.Q. COARSE
GROSSO MEDIUM
MEDIO FINE
FINE C+M
G +M M+F
M +F C+F
G +F
PARTICLE
GRANULOMETRIA:SIZE DISTRIBUTION:
mgl/cm2 um

ferent particle size distributions).


above
sopra 100 600 1 6 0 0 3 0 3
“ 196 425 8 44 0 0 22 0 22
“ 400 300 9 50 0 0 25 0 25
“ 576 250 45 0 100 0 50 50 0
“ 1050 180 16 0 0 45 0 23 23
“ 2500 125 12 0 0 34 0 17 17

95
below
sotto 2500 125 7 0 0 21 0 10 10
disperso
lost 1 0 0 0 0 0 0
Total
Totale 100 100 100 100 100 100 100
Approx. average
Diam. medio approx.diam. (mm)
(µm) 267 456 275 162 365 218 308
Spray drying of ceramic slips

POWDER
UMIDITÀ POLVERI
MOISTURE CONTENT % % 4.2
FLUIDITY
FLUIDITÀ rel. VOLUME
rel.altoVOLUME cm3cm
/s 3/s 17.0 15.3 17.7 16.5 16.2 17.4 16.4
FLUIDITY
FLUIDITÀ rel. to MASS
rel.alla MASSA g/s g/s 18.4 15.8 18.8 18.0 17.2 19.1 18.8
APPARENT DENSITY
DENSITÀ APPARENTE g/ 3cm3
g/cm 1.08 1.03 1.06 1.09 1.06 1.10 1.15
ANGLE
ANGOLO OFDIFALL
CADUTA (°) (°) 27 30 27 28 29 27 28

Tab. 3. Flowability measurements of a spray dried powder and artificially produced grain blends (dif-
Applied Ceramic Technology

Variations in physical characteristics of spray dried powders

To obtain satisfactory results in downstream production processes the spray dried


powders must, then, have certain residual moisture characteristics.
As mentioned above, particle size distributions for spray dried powders produced
with different bodies (e.g. vitrified single fired, porous single fired, porcelain tile)
are, to a large extent, similar.
Residual moisture content may vary from 4 to 7 % depending on the plasticity of
the body. It is, to an extent, possible to act on certain variables concerning both the
working conditions in the spray drier and some of the slip parameters so as to vary
and optimise aspects such as particle size distribution, residual moisture content,
spray drier output, quantity of powder reaching the stack, temperature of spray
dried product.
Fig. 29 shows how these variables (causes) act on the characteristic parameters
of the spray drying process (effects).
The information in the table is, of course, indicative rather than absolute in that
the cause-effect variables are presented individually while, in practice, they interact
with each other.
In an actual factory several variables are usually altered simultaneously to pro-
duce a final result that benefits from such interaction.

Relationships regulating working conditions of spray driers

There follows a description of the most important theoretical relationships re-


gulating the spray drying process.
Although the diagrams in figures 30 and 31 were obtained by atomising water,
the results are similar to those that would be obtained by spraying a slip.
In spraying water similar spray angles and lower volumetric flow rates are ob-
served.

Relations regulating flow rate


The volumetric flow rate of the slip is proportional to its density.
1
Volumetric flow ratecaá
Portata volumetri
density
densità

Flow rate, by volume or weight, is proportional to pump pressure.

Volumetric flow
flowrate
Portata volumetri
Volumetric ca 
rate á pressione pompa
pump pressure

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Spray drying of ceramic slips

Fig. 29. Variables which control and condition the spray drying process.

Output comparison
Confronto between
tra produzione slip andewater
tra barbottina acqua
- spacers15-7
-Torrette 15-7spirale
coil 13-6
13-6Pp=
= 20
20 bar

25
x 10

20
ratex 10

15 Slip
Barbottina
Portata

10 Water
Acqua
Flow

0
1 2 3 4
Nozzle
Diametro diam.
ugelli

Fig. 30. Variation in flow rates as a function of nozzle diameter.

Outputproduzione
Confronto comparison with
con slip
barbottina
-- spacer
Torretta15-7
15 - 7Pp=
= 20 bar
bar

70
60
Angoloangle
cono

50
40 coil 10-4
spirale 10 -4
Cone

30 coil 13-6
spirale 13-6
20
10
0
1 2 3 4
Nozzle diam.
Diametro ugello

Fig. 31. Variation in cone angles as a function of nozzle diameter.

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Flow rates increase as coil clearance increases. Fig. 30 shows flow rates (y co-
ordinate) with coils of different heights in relation to the adoption of nozzles of
different diameters (x coordinate).

Relationships regulating particle size distribution


Using higher pressures results in a smaller particle size distribution.
Greater slip pressure => smaller particle size distribution

With higher viscosities larger particle size distributions can be obtained.


Higher viscosity => larger particle size distribution

Energy consumption

The optimisation of energy costs during the spray drying process depends on a
number of plant engineering and technological factors.
The most important of these are:
– size and type of spray drier
– continuity of operation
– conditions on the machine and essential devices such as burners, fans, insulation
systems
– optimisation of overall working conditions
– technological characteristics of slip (density, viscosity, droplet drying rate).

The minimum relative specific consumption (Kcal/kg) and its output capacity
expressed in Kg/h - essentially depends on two factors:
– percentage of solid contained in the slip hence the proportion of water to be
evaporated
– hot air inlet temperature.

The heat transfer diagram

Fig. 32 illustrates the heat (energy and material) balance in the spray drier. Note
that the heat effectively used for evaporation of the water accounts for little more
than half of the total heat introduced into the chamber; the rest is, instead, heat
loss, mainly through the walls and with the exhaust air and, to a far lesser extent,
with the dried product.

As tab. 4 illustrates, optimum specific fuel consumption is, on average, about 370
Kcal/kg.

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Spray drying of ceramic slips

Fig. 32. Heat (energy and material) balance in the spray drier.

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Essential parameters and examples for the evaluation of energy


consumption and spray drier output capacity

Calculating heat energy consumption

The parameters and data which need to be taken into account in evaluating ener-
gy consumption are given below (tab. 4).

Average specific heat energy consumption is thus as follows:

G e, A .Q
qA = = 372.7
438.5 kcal/kg
Gp

ATM

Gp Kg/h Hourly pressing


Produzione orariapowder output
di polveri per pressatura 10000

Ub l/kg Umidità
Slip della barbottina
moisture content 0.35

Up l/kg Pressing powder


Umidità della moisture
polvere content
per pressatura ---

Consumospecific
Average specificoheat
medio di energia
energy consumption
Q Kcal/l 850
1000
per litreper
termica of water evaporated
litro d’acqua evaporata

Ge l/h Hourly flow rate


Portata oraria of water
di acqua to be evaporated
da evaporare Ge,A

Consumospecific
Average specificoheat
medio di energia
energy consumption
Q Kcal/kg qA
per Kg of
termica perpressing powder
kg di polvere per pressatura

Tab. 4.

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Spray drying of ceramic slips

Practical method for calculating evaporating power of a spray drier

Of all the spray drier parameters, evaporation rate is the one that provides the
most immediate information as regards its efficiency and the one that will lead to
full exploitation of its potential.
Table 5 shows a series of formulas with which it is possible to calculate the
amount of water evaporated by the spray drier.
H 2O ev. = Pf × Y

Ui% − Uf%
Y =
100 − Ui%
Key to symbols:
Ui% Water contained in the slip (%)
Uf% Water contained in the spray dried product (%)
Pf Final spray dried product, including residual moisture (kg/h)
H2O ev. Water evaporated (litres/h)
Y Coefficient for calculation of evaporated water (see also table 5)

Thus a very simple formula to calculate the maximum output is:


H 2O ev.
Pf =
Y

Calculating the size and output of the spray drier

There is often a need to know data as regards the output the spray drier will
effectively be expected to provide; such data is used to size the machine in line with
effective production plant needs and to run checks on production during routine
operation.
The following two examples show how some of the sizing questions can be
resolved.

1 - If hourly wet powder output is known the quantity of water to be evaporated by the
spray drier can be determined.

a) Known data
Qp – quantity of spray dried powder = 6800 kg/h
Up – powder moisture content = 6%
H2O – slip water content = 38%

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Tab. 5. Table for calculation of evaporative capacity of a spray drier and the quantity of spray dried
product.

b) Calculation
– Determining the quantity of dry powder produced (Qs)

Qs = 6800 × 94/100 = 6392 kg/h

Where 94 is given by 100–% of water in the spray dried powder (i.e. the 94 is the
% of solids of the powder derived from the 6% water needed to press it).
It is also known that the quantity of water in the powder and thus not evapor-
ated by the spray drier is:

6800 - 6392 = 408 l H2O/h

– Determining the quantity of water contained in a slip with a 38% water con-
tent and 6392 Kg of dry material

38 : 62 = × : 6392
× = 3917 l H2O/h

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Spray drying of ceramic slips

where
38 = % of water in the slip
62 = % dry material in the slip.

– Determining the quantity of water effectively evaporated by the spray drier

3917 - 408 = 3509 l H2O/h

N.B. This calculation is also used to establish the required drying capacity of a
spray drier to be installed in a plant of specific capacity.

2 - If the evaporative capacity of the spray drier is known the quantity of moist spray
dried powder produced can be determined.

a) Known data
– spray drier evaporative capacity = 3500 l/h
– spray dried powder moisture content = 6%
– slip water content = 38%

b) Calculation
– Determination of the apparent dry percentage and the water in the slip

62 × 100 / 94 = 65.95% (dry)

Where 94 is given by 100–% of water in the spray dried powder (94% dry mate-
rial in the powder and 6% water).

– Determining hourly spray died powder output at moisture content of 6%

34.043 : 65.95 = 3500 : ×


× = 6798 kg/h
where
34.043 = % of water to be evaporated (from 100 - % apparent dry material in the slip)
65.95 = % apparent dry material in the slip
3500 = evaporative capacity of spray drier in l/h of water.

Energy savings

Energy savings at the spray drying stage can be obtained by varying the working
conditions of the machine and the technological parameters of the slip.
The main variables which have a significant effect on energy savings are:
a) incoming hot air temperature
b) difference in temperature between incoming air and outgoing air
c) air recycling
d) increase in the slip solids content.

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a) Effect of temperature of incoming hot air


Increasing the temperature of the incoming air reduces the amount of heat energy
needed to dry the slip, for the same air flow rate. Alternatively, where the tempera-
ture of the air exiting the spray drier remains constant, the lower the hot air flow
rate the lower the energy loss at the stack and the better the thermal efficiency.
Fig. 33 illustrates how specific consumption varies as incoming hot air tempera-
ture increases.

b) Effect of the difference in temperature between inlet air and outlet air
The greater the difference between the inlet and outlet air temperatures, the
lower the energy consumption per unit of product output.
This difference can be widened either by increasing the temperature of the inlet
air or decreasing that of the outlet air.

c) Effect of recycling air


In most cases the air exiting the spray drier is released into the atmosphere.
This is undoubtedly a waste of energy, especially where its temperature exceeds
120 °C.

Fig. 33. Specific consumption of a spray drier as a function of hot air inlet temperature.

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Spray drying of ceramic slips

Recycling a part of the outlet air (from 10 to 50%) could provide considerable
energy savings.
However, recycling more than 50% of outlet air could, instead alter in-chamber
hygrometric parameters to the extent that the drying speed of the atomised drop-
lets is reduced.
Trials have shown that energy savings of up to 20% can be obtained by re-
cycling outlet air with a temperature of 120 °C.

d) Effect of increasing the percentage of solid material


A higher proportion of solid material in a slip can yield considerable energy
savings; however, this option is not always open to the manufacturer in that an
excessive percentage of solid can thicken the slip and cause mill unloading difficul-
ties.
However, recovery of waste spray dried material along the production line (e.g.
in sieving, pressing etc.) or the fine material separated out by the cyclones is always
possible. In a normal production plant this recovered material accounts for some 3-
5% of the total and can be added into the agitated tank, thus preventing mill un-
loading problems.
Nevertheless, it is important that the addition of this extra solid material does
not cause excessive variations in slip viscosity and thixotropy and consequent pro-
blems at the spray drying stage.
Recycling this recovered “waste” powder and collected dust back into the spray
drier slip tank provides energy savings in the order of 3 and 7% respectively.

Energy recovery

Where the size and power of the spray drying system allow, the plant can be
integrated with a cogeneration system. This uses the excess heat produced by an
electricity generator (smoke from turbine or combustion engine) as hot air for the
spray drier. The electricity can thus be used internally or, if there is a surplus,
reintroduced into the mains grid. Recent legislation has provided incentives in this
regard.
Moreover, it is evident that where a cogeneration system provides a flow of hot
air, a recovery system will be able to provide (necessary air temperature and flow
rate remaining equal), a considerable reduction in fuel consumption per unit of heat
generated.

105
Chapter III

PRESSING

Introduction

Pressing is that stage of the production cycle in which ceramic products are
formed by compacting semi-dry granular powders.

Pressing essentially involves:


– forming of the tile: to give it the required geometry.
– powder compaction: to confer certain mechanical characteristics.
– densification of the powders: to limit the empty spaces within the pressed item.

Compared to other forming systems (extrusion, casting, etc.) pressing has consi-
derable advantages:
– high productivity
– excellent repeatability of size parameters
– pressed pieces are easy to dry
– limited drying and firing shrinkage.

Pressing systems

Pressing powders generally have an evenly distributed moisture content which


is important as it confers plasticity on the system and thus aids inter-particle cohe-
sion.
Depending on the remaining percentage of water, then, materials may be for-
med:
in a plastic state: the mix has a residual water content of some 20-25%.
Pieces are formed, for instance, by extruding the plastic mass through highly
polished metal moulds having orifices corresponding to the finished tile dimen-
sions:
– in a “semi-dry” state: these powders have a residual moisture content of around
10-15%.
– in a dry and/or semi-dry state: in this case powder moisture content ranges from 3
to 7%.
Loose powders of varying grain size and morphology are normally used, but
they must have good flow properties.

Flowability largely depends on the shape of the grain and thus on how the powder
was prepared, that is:
Applied Ceramic Technology

– by dry grinding followed by granulation


– by spray drying of a ceramic suspension (slip).

Compaction and densification of the powders is influenced not only by maxi-


mum press power but also by the intrinsic plasticity of the body, moisture content
and particle size distribution.
There are essentially three different kinds of press, each of which features a
different energy application system:
– mechanical press
– hydraulic press
– isostatic press.

Pressing semi-dry powders

Different press types

In industrial tile manufacturing processes that involve the pressing of semi-dry


powders, only fully automated presses are used.
Historically, it should be noted that, before the advent of hydraulic presses, toggle
(or knuckle-joint) and friction presses were used.

Toggle press

This is a mechanical press featuring a system of two interconnected rods that


reproduce a knee-like joint. During pressing the speed of fall of the punch decrea-
ses steadily as pressure increases (fig. 1).

Friction press

Friction-type mechanical presses are characterised by a fast, violent pressing


action with a highly dynamic instantaneous impact. The fall and rise of the shaft
that transfers motion to the mobile cross-beam is controlled by two rotating verti-
cal discs located to the side of the screw-coupled flywheel (fig. 2).
Contact with the flywheel takes place first with one disc then the other, one disc
driving the punch down, the other raising it. The friction press is a high-output
machine (up to 30 cycles/min) and, given the installed electrical power, features an
excellent energy-productivity ratio.

Of simple design, it is also easy to maintain. Its limitations lie in the difficulties
of maintaining constant, uniform pressing.
Hence it has now largely been abandoned in favour of more reliable hydraulic
pressing systems.

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Pressing

Fig. 1. Toggle press.

Fig. 2. Friction press.

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Hydraulic presses

The hydraulic press functions by way of a fluid that exerts a pressure inside a
cylinder. The operating principle is based on the pressure increase obtained when
the pressure exerted by a narrow column of fluid is connected to a cylinder with a
piston of much larger cross sectional area. The greater the differential between the
area of the two cylinders the greater the total force on the larger one compared to
the narrow one.
Modern presses, which use oils with special viscosity characteristics, have a
hydraulic control unit that supplies the oil under pressure: once the oil is introduced
into the circuit it exerts the compression force of the accumulator and multiplier
through the cylinder on the material. This unit consists of two independent cir-
cuits, a high pressure one which feeds the actual pressing mechanism and a low
pressure one which serves auxiliary units. A single or double-action cylinder unit
is installed on the upper structure of the press; this shifts the cross-beam vertically
as required and exerts high pressure on the punches at just the right moment.
Summing up, the pressing action is effected by transforming hydraulic pressure
into a deformation force as per the following formula:

F=S×P
where
F = Deforming force (in Kg)
S = Surface area (in cm2)
P = Oil pressure (in Kg/cm2).

It is thus possible to calculate:


Po (oil pressure kg/cm2) = St (punch surface cm2) × Ps (specific pressure kg/cm2) /
Sp (piston surface cm2)
Ps (specific pressure kg/cm2) = Po (oil pressure kg/cm2) × Sp (piston surface cm2) /
St (punch surface cm2)

The main characteristics of the hydraulic press are:


– evenly distributed pressing force
– absolute repeatability of pressing cycles over time.

The above characteristics make hydraulic presses especially suitable for use in
highly automated production plants and – as regards final product technical re-
quirements – in the pressing of products with high levels of firing shrinkage.

Requirements for a modern press

A modern ceramic press must:


– be reliable
– provide high output

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Pressing

– be automated
– be flexible
– be extremely precise at every stage of the cycle
– maximise energy savings
– be versatile.

“Versatility” refers to the possibility of choosing between a work cycle with max-
imum energy savings and a cycle with maximum speed.
For a detailed description of the main parts of a “press system” it is best to refer
to the specific technical manuals which accompany every machine. Nevertheless,
note that a dry-pressing machine essentially consists of the press itself and equally
important complementary devices such as:
– filler box feed devices
– die cavity loading devices
– dies
– powder removal devices.

Fig. 3. First-generation hydraulic press.

Different types of press for different tiles

Generally speaking, ceramic tile manufacturers use three different machine ran-
ges for the following purposes:
1. Presses for small tiles and trims. Low tonnage machines (< 500 tons) with sophisti-
cated control devices and precision cross-beam movement, filler box movement
etc. Moulds are complex and ejection of the formed piece may involve move-
ment of the die box. Powder filling and pressing force can also be applied hori-
zontally, with the mould closed. Installed power is generally low (20 or 30 kW).

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Fig. 4. A modern hydraulic press (series 2000).

2. Presses for modern standard size pieces, i.e. single fire floor or wall tiles of up to
40×40 cm.
These presses account for the bulk of the market and have maximum pressure in
the 600-4000 ton range; characterised by very high productivity (up to 18-20
complete cycles per minute) and flexibility to meet the ever-increasing variabili-
ty of production lots, often involving several size changeovers per week. For this
reason die changeover, filler box or feed unit adaptation and machine adjustment
tasks need to be as fast and simple as possible. A powder loading system that
uses a filler box with a traditional grating (grid) is already seen as obsolete and
can now be replaced by floating gratings supported directly by the die box anti-
friction inserts. Thus the filler box and load hopper effectively form a single unit
and all that needs to be changed during a tile size changeover is the grating (figs.
5 and 6).
3. Presses for medium-large sizes. This range covers larger tiles (e.g. 30×60, 60×60
cm or larger) or tiles decorated on the press itself and not glazed downstream;
these items require slower cycles and it is important that energy efficiency is not
sacrificed.
This is why more suitable, lower productivity presses have been developed, es-

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Pressing

Fig. 5. Traditional filling system.

Fig. 6. Filling system with floating grating.

pecially now that medium-large tiles of this type are steadily becoming more
popular.
As a rule, hydraulic systems use proportional valves, or servovalves, and not the
on-off circuiting seen on earlier models. This means that electronic setting sys-
tems can be used, thus guaranteeing precision and quality. The load-bearing
structure is normally of the column and/or welded type. Presses in the 600-
1500 ton range have column structures, either of the pre-stressed type (to counter-
act lengthening of the structure at the moment of maximum load) or arch-like
ring frames (made with rings either welded together or linked with threaded
bars).

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4. Presses for large tiles (fig 7). Pressing forces range from 4000 to 7000 tons and
beyond [specific loads are generally in the order of 400-650 Kg/cm2 depending
on the overall surface area being pressed. Higher pressures are only used on very
lean (non-plastic) bodies or very dense granules]. Such presses are characterised
by very wide clearance and, of course, sophisticated accessory systems (filler
boxes, dies etc.).
They are not used to make tiles as such but, rather, very large ceramic slabs (e.g.
120×180 cm); hence reliability takes precedence over speed. Feed systems are
specially designed to ensure even distribution of the powder. The dies are made
of several parts so that they can be moved around the plant with standard fork-
lift trucks (they would otherwise be too bulky). Production cycles may be lower
than 10 cycles per minute.

Machine devices

Ejector
Newly designed piston ejectors have played a key role in making presses more
flexible: recent years have, in fact, seen a switch from traditional ejectors, installed
underneath the press, to ejectors fitted on the press bed directly beneath the die
itself. Because this new design has shorter pistons movement is more precise. More-
over, proportional hydraulics and a greater number of lift points (where there used
to be one there are now at least two) give more accurate ejection. To ensure maxi-
mum production flexibility, ejectors have even been integrated into the individual
dies. This means that the latter can be adjusted outside the press, thus reducing
plant downtime.

Fig. 7. A PH 7200 press for large slabs.

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Pressing

Machine structure

1 Load bearing
structure
2 Mobile cross-beam
3 Fixed cylinder
support beam
4 Hydraulic piston
5 Mould air filter
6 Traditional ejector
(SMU ejector on
more modern
machines)
7 Multiplier
8 Hydraulic SMU
ejector (traditional
ejector on older
machines)
9 Filler box support
10 Filler box
11 Hopper
14 Filler box drive
15 Mechanical buffer,
guards
16 Aspiration hood
17 Spring dampener
18 Hydraulic hoses
19 Hydraulic leak fluid
container
20 Logic elements plate
21.1 Valve bank
21.2 Braking unit
22 Ejector and filler box
control
27 Hydraulic control
unit
28 Cooling pump
29 Guards
30 Electrical wiring
31 Electronic control
unit
32 Electrical cabinet
33 Cross-beam position
controller
34 Mould/die
35 PLC keyboard

Fig. 8. Main parts of a hydraulic press.

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Different types of die used to form the tiles

There are several traditional types of tile forming die, each of which have well-
defined operating principles. Two such types are the entering punch die and the
mirror die.

Entering punch die


The most widespread technological solution: during pressing the upper punches,
fixed to the mobile cross-beam, penetrate the corresponding cavities of the die, which
is fixed to the lower part of the press. The pressed tile is then removed from the cavity
by raising the lower punches.
Fig. 9 shows the various parts of an entering punch die (liners, punches etc.).

Fig. 9. Cut-away diagram of an entering punch die: 1) upper punch, 2) lower punch, 3) die box.

Mirror dies
In this case, instead, the upper punch contacts the top of the die box, which is, in
turn, mobile with respect to the die as it is connected to the lower part by elastic
systems (fig. 10).
The key characteristic of a mirror die, then, is that the die box is shifted by the
force exerted by the upper punches on the die box itself.
The resulting advantage is that as the tile is made the right way up the top (or
face) side of the tile no longer scrapes along the die box. However, it is no longer
possible to produce tiles with edge spacers either. Upper punches and box liners last
much longer than they do on entering punch dies.
Undoubtedly more complex from an engineering viewpoint, the mirror die is
also more costly and relatively more difficult to assemble than an entering punch
die.

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Pressing

Fig. 10. Cut-away diagram of a mirror die: 1) upper punch, 2) lower punch, 3) die box, 4) base plate,
5) pusher.

Upper forming die (SFS)


In the wake of increased demand for solutions that allow the tile to exit the
press face-up (e.g. because decoration at the press is becoming increasingly popu-
lar), other types of die with special mechanical control systems for punches and
die walls are becoming more common: such highly technological systems allow
the tile to be produced face-up with a spacer, thus avoiding contact of face and die
box (fig. 10a).
This type of die solves a great many technological and aesthetic problems,
allowing the manufacturer to produce high quality products such as coarse grain
porcelain stoneware in which the larger particles remain in the upper layers.

Fig. 10a. Cut-away diagram of an upper forming press: 1) upper punch, 2) lower punch, 3) upper die
box, 4) lower die box, 5) pusher.

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Mirror die with pushers


Very large tiles cause more marked expansion problems during pressing.
Hence solutions have been developed that allow pressing at the same level as the
die; this involves the interposition of spacers between the die box and the punch to
aid degassing during the compaction phase.
The mechanical set-up is optimised so that no alignment work is required
(fig. 11).
Ever-more sophisticated decoration at the press (especially in the porcelain tile
field) has led to the development of ejectors that can be adjusted to different, electro-
nically controlled positions.

clearance mobile cross-beam


adjuster spacers

pusher

mirror top die


clearance

lower
die box punch

box liners

hydraulic
support piston

press bed

Fig. 11. Cross-section illustrating a mirror die with pusher.

Isostatic dies
For some time now special isostatic (or, more properly, isostatic-effect) die sets
have been used to optimise filling homogeneity right across the surface of the die
cavity; isostatic dies have reduced finished tile defects considerably.
Compression is achieved by way of a punch with a rigid back and a hard, yet
deformable polymer front that comes into contact with the powders to be pressed; a
chamber between the punch and the polymer membrane contains an incompressible
fluid. Fig. 12 illustrates the operating principle behind these punches.

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Pressing

Oil

Powder

Fig. 12. Isostatic punch operating principle.

Isostatic punch

Fig. 13. Cross-section of an isostatic punch designed for industrial use.

The pressing sequence

A general description of the filling, pressing and ejection sequence for the va-
rious kinds of die follows.
The pressing cycle begins with ejection of the tile formed during the previous
pressing; this ejection consists of the tile being raised by the lower punches from
the bottom of the cavity until it is above and level with the surface of the die box.
Figures 14, 15 and 16 illustrate the different stages of the pressing cycle (filling-
pressing-ejection) for entering punch, mirror and upper forming dies respectively.
The cycle is as follows: the grating-equipped filler box moves forwards and shunts
the just-formed tiles away from the die box. Then the lower punches drop (first fall)
and the cavities are filled with powder; the filler box returns to its “home” position.
The lower punch then drops further (second fall) and the mobile cross-beam begins
its descent. Initial first compression of the material then takes place: this is not
violent, as its main function is to expel the air from the powder particles (de-airing)
The second compression gives the tile its definitive shape and brings the material to
the required degree of compaction. The cycle then recommences, with ejection of
the pressed tile and a new filling of the die cavities.
Electrical impulses emitted by proximity sensors installed at certain points on
the press allow precision control and thus automation of all press movements by

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Traditional mirror die


Filling Pressing Ejection

Fig. 14. Tile forming sequence: mirror die.

Entering punch die


Filling Pressing Ejection

Fig. 15. Tile forming sequence: entering punch die.

S.F.S. upper forming die


Filling Pressing Ejection

Fig. 16. Tile forming sequence: upper forming die.

way of a feedback system. The impulses are sent to an electronic controller which
recognises the process being carried out at that moment, calculates the next move-
ment and relevant execution times and, in turn, transmits the necessary impulses to
the hydraulic control unit which governs the pressing sequence.

Main parts of the die

The main die parts are:


– upper punch
– lower punch
– die box.

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Pressing

For a more detailed explanation of parts the reader should consult the specific
machine handbooks.
There follows an overview of the main characteristics that distinguish the various
types of pressing punch.

Different punch types

Hardened, polished steel


Generally used where a high quality tile finish and very high resistance to wear
are required.
The polished surface of the punch gives an excellent tile finish and is therefore
particularly suitable for porcelain tiles.

Punches with moulded rubber surface


The rubber surface (available in varying degrees of hardness) eliminates the
need for systematic cleaning of the punches and thus the need for the brushing
systems that perform this task.
A rubber face is also an effective means of creating surface effects (indentations,
rustic effects etc.).
Even quite complex surface patterns or embossments (structures) can be achieved
economically in this way.

Punches with cast resin lining


As above, cleaning times are reduced significantly. Unlike rubber surfaces, those
in cast resin can be smoothed to give perfectly flat surfaces.

Isostatic punch
A tile back punch with a membrane on its face which uses the incompressible
nature of the oil in its internal channels to compensate for uneven cavity filling.

Characteristics of the ceramic powders used in pressing

Pressing is intended to:


a) provide tiles of a set size without generating defects on either fired or unfired tiles that
are the result of pressing itself.
One such defect is lamination (the formation of air pockets in the body); this
shows up as fissures and surface damage that may appear at any stage of the pro-
duction process. Also to be avoided are size, geometric and flatness (planarity) de-
fects on the fired tile.
All these problems can be traced, together with other causes, to density varia-
tions at different points on the same tile or from one tile to another.

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The main causes of such variations are uneven die cavity filling and changes in
press performance.

b) contribute to the formation of a microstructure in the unfired tile that gives:


– the bending strength needed at subsequent stages of tile production: that
strength must be available immediately after pressing and after drying.
– an unfired tile with a mass that is permeable and allows the gases formed
during pre-firing and/or firing (combustion of organic substances, dissocia-
tion of carbonates etc.) to escape.
– gives a fired product of standard-compliant technological characteristics (firing
shrinkage, porosity, bending strength) with normal firing cycles.

Variables in the pressing cycle

To meet the requisites in points a) and b) the characteristics of the spray dried
powder and the working conditions of the press must be correct and comply with
accepted standards.
The main factors influencing pressing are thus:
a) Characteristics of the powder being pressed.
b) Characteristics of the pressing cycle.

a) Characteristics of the powder being pressed.


Before analysing the powders that are suitable for pressing and the relationship
between their characteristics and those of the pressed tile, some clarification is re-
quired as regards:
• definition of terms
• physical characteristics of the particles
• technological characteristics of the powders.

Definition of terms

Particle: may be a primary particle or a cluster of primary particles; the latter is


referred to as an agglomerate.
Agglomerate: term associated with a small mass of primary particles kept com-
pact by surface forces and/or inter-particle bonds.
Grain/Granule: terms used frequently in ceramics where agglomerates are pro-
duced deliberately by adding an agent that aids re-granulation (in most cases the
agent is water).

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Pressing

Physical characteristics of the particles

Powder characteristics
BULK DENSITY
Weight per unit of volume of powder; includes solid phase, porosity (internal
air gaps) of individual grains and air between individual particles.

SINGLE GRAIN BULK DENSITY


Parameter that defines the weight per unit of volume: includes solid phase and
internal voids in the individual grain.

TAPPED DENSITY
The bulk density of a known volume of powder after controlled vibration.

Characteristics of powders – definitions and measurements


HAUSNER INDEX
This is the ratio between tapped density and bulk density of the powder in que-
stion.

Dv
I.H.
H.I. =
Da

where
Dv = tapped density (g/cm3)
Da = bulk density of powder (g/cm3).

BULK DENSITY
Ratio between mass and apparent volume (M and V).

M M
Bulk dens. = –––––– = ––––––––––––––
V tot Vpores + Vsolid

REAL DENSITY
Ratio between mass (i.e. quantity of material) and actual occupied volume.

M
Real dens. = –––––––
V solid

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TOTAL POROSITY
Ratio between pore volume and total volume.

Vpor Vtot –Vsol 1 – Vsol 1 – Dbulk


Porosity = –––––– = ––––––––––– = –––––––– = –––––––––
V total Vtot Vtot Dreal

OPEN POROSITY
Ratio between the volume occupied by the open pores (i.e. those connecting with
the outside) and total volume.

CLOSED POROSITY
Ratio between the volume occupied by the closed pores (i.e. those not connecting
with the outside) and total volume. This value is negligible.

COMPRESSION RATIO
Ratio between apparent and compacted volume.
Mass
V app. Dapp. D compacted
Compressio n ratio = = =
V compacted Mass D apparent
D compacted

Characteristics and microstructure of pressed tiles depend on:


• nature of the particles (shape)
• particle size
• characteristics of the agglomerates
• pressing additives (percentage of water, binders, plasticizers).

In turn, the above factors determine and condition the properties and technolo-
gical characteristics of the powders, namely:
• bulk density
• fluidity
• compression ratio
• friction angle of the powders.

As mentioned, consistent distribution of the powder in the die cavity is a must


for good pressing results.
To attain this goal the powder must have good fluidity; this also allows manu-
facturers to use faster press cycles without compromising pressed tile homoge-
neity.
Yet good fluidity is not, in itself, sufficient: the powder must also be of suitable
bulk density.
Excessively low bulk density generally means that large volumes of air have to

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Pressing

be expelled during pressing or a thicker powder filling layer has to be used. Both
cause difficulties in the pressing cycle.
– The bulk density of a powder depends on the volume of the intergranular spa-
ces and the density of the granule or agglomerate. This value is determined by
weighing a known volume of powder.
– Agglomerate density depends on how the powder was prepared (dry grinding,
re-granulation, spray-drying) and on the shape and size distribution of the par-
ticles in the agglomerate.

Bulk density values for different powders (granulates or spray dried powders) of
specific grain size are given in fig. 17 and table 1.
They illustrate that spray-dried grains have lower densities than agglomerates.
Note also that re-granulate density increases slightly as grain size increases while
for spray-dried powders the opposite is true because of the existence of the hollows
inside the particles, which increase as particle size increases. Such cavities depend
on particle shape and size distribution.
The “agglomerates” obtained from dry grinding do not have any such cavities.
Table 1 shows bulk density values for:
– spray dried powder
– dry ground powder (traditional)
– re-granulated powder.

Fig. 17. Bulk densities for different (granulates and spray-dried) semi-finished products.

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APPARENT
DENSITÀ TAPPED
DENSITÀ PER
MOISTURE
UMIDITÀ APPARENTE VIBRAZIONE
DENSITY DENSITY
(%)
(g/cm 3) (g/cm3)
Regranulated
Granulato body 5.90-6.0 1.1-1.15 1.470-1.480
Spray dried body
Atomizzato 5-7 0.33-1.00 1.240-1.260
Dry ground
Macinato bodytradizionale
a secco 6-10 0.75-0.8 1.320-1.350

Tab. 1. Bulk densities for different types of powder (spray dried, dry ground and re-granulated for a
given composition).

Powder fluidity

Powder fluidity is one of the most important pressing parameters.


It is generally expressed as:
– flow speed
– a Hausner index value.

Flow speed is defined as the time taken for a certain volume of powder to flow out
of a funnel-shaped container via a calibrated orifice and is expressed in cm3/sec.

The Hausner index is based on the increased density of powder on vibration. The
higher the inter-particle fluidity the higher the tapped density and the Hausner
index.
Although this is the most suitable scale for characterisation of powder fluidity, it
is not generally used in routine powder characteristic checks.
The effect of residual moisture content and grain size on powder fluidity is illu-
strated in figs. 18 and 19.
In Figure 18 note that fluidity falls as moisture content rises, especially in the 5-
8% range. A similar graph is obtained with agglomerates prepared using dry grin-
ding methods.
Fig.19 shows the effect of specific diameter for powders prepared by spray drying
and granulation. In both cases smaller grain sizes give lower fluidity. With dry
ground granulates particles that are less than 200 microns in diameter reduce flow
speed to nearly zero. Those between 200 and 500 microns produce the optimum
flow speeds.
With spray dried powders higher fluidity levels are seen where particles are in
the 125-400 micron range. Both spray dried powders and granulates are affected by
the presence of low percentages of small grains.

Powder particle size distribution

Fig. 20 shows the particle size distribution of a dry ground powder after granu-
lation while fig. 21 gives that of a spray dried powder.

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Pressing

Fig. 18. Variations in powder flow speed against changes in the moisture content of a spray dried
powder.
FLOW SPEED (cm3/s)

GRAIN SIZE (µm)

Fig. 19. Changes in fluidity for spray dried and granulated powders of specific diameter.

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GRAIN SIZE (µm)


Fig. 20. Particle size distribution of a dry ground, re-granulated powder.

GRAIN SIZE (µm)


Fig. 21. Particle size distribution of a spray dried powder.

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Pressing

Note that the granulate (dry ground and re-granulated) has a relatively high
content of particles in the low-fluidity band (i.e. less than 200 microns). Compared
to the spray dried powder (usually around 5% below 125 microns) the differences
produced by the two powder production processes are very significant.

Bulk density, tapped density and Hausner index as a function of


variations in powder parameters

Fig 22 shows, for a spray dried powder, variations in:


– bulk density
– tapped density
– Hausner index.
as moisture content changes. Note that an increase in moisture content reduces
both the bulk and tapped density: the former is most affected.
Hausner index values increase.
Fig. 23 shows how spray dried powder grain size influences the Hausner index.
Note that the Hausner density curve is similar to the flow speed curve, having
similar values in the 200-500 micron particle size band (corresponding to the maxi-
mum).
Grains outside the 125-400 micron range give the lowest bulk density values.
Those inside have the higher density and best packing characteristics.
Fig. 24 shows how particle size influences the above-mentioned parameters, this
time for a granulate.
Again, the Hausner density curve is very similar to that for flow speeds (i.e. for
particles larger than 300 microns the Hausner index remains fairly constant).
Fig. 25 shows the linear correlation between the Hausner index and flow speed.
For powders that do not flow easily and for which flow speeds cannot, therefore, be
accurately measured, the best indicator of fluidity is undoubtedly the Hausner index.
To see how moisture content influences the fluidity of traditionally prepared
powders (wetted dry ground powders), Hausner density values were calculated for
industrial powders of different residual moisture content. The results are shown in
fig. 26 (with figures for spray dried powders for comparison).
Note that moisture content has much more effect on the fluidity of traditionally
prepared powders than on spray dried powders. This “low grain flowability” effect
seen with dry ground/re-granulated products is due to the irregular shape of the
particles and the high percentage of fine material.

Ceramic powder pressing: technological aspects

Evaluating how pressing pressure and powder moisture content interact in the
compaction of spray dried powders is of great interest to ceramic manufacturers. It
is, however, complex and difficult to interpret.

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Fig. 22. Variations in bulk density, tapped density and Hausner index as a function of residual moistu-
re content (spray dried powder).

Fig. 23. How variations in particle size influence bulk density, tapped density, and fluidity in a spray-
dried powder.

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Pressing

Fig. 24. Influence of particle size distribution on bulk density, tapped density and powder fluidity (dry
ground re-granulated powder).

Fig. 25. Relationship between Hausner index and flow speed.

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Fig. 26. How changes in moisture content affect fluidity (Hausner scale) in spray dried, dry ground
powders.

During pressing, powders, whether spray dried or dry ground, tend to resist
external forces as illustrated in fig. 27 which shows how bulk density changes as
forming pressure increases (pressure is expressed on a logarithmic scale).
Here, medium-low pressures result in almost uniform densities while higher
pressures result in steadily increasing bulk densities.
With simple ceramic powders the above relationship is generally a linear one.
Whether the product is dry or includes lubricants or binders, during the press-
ing cycle, at lower pressures, the particles or grains are rearranged, while at higher
pressures there may be elastic and plastic deformation, sliding and abrasion or even
actual fracturing and grinding of the particles or grains.
This evidently involves the actual simple strength of the material itself hence
the cited density-strength relationship.
Powder compaction curves (e.g. fig. 28) may therefore show changes in gradient
against pressure for different products, namely:
– dry ground powder (V)
– re-granulated powder (G)
– spray dried powder (A).

Here, the first change in gradient (near-linear tract) for powders G and A occurs

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Pressing

Fig. 27. Relationship between forming pressure and unfired density (logarithmic scale).

Fig. 28. Compaction diagram for different semi-finished products - (A) spray dried powder, (G) re-
granulated powder, (V) dry ground powder.

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where bulk density of the compacted powder Pt, corresponds to a forming pressure
of Pf.
At this point re-arrangement of the grains is nearly complete (end of phase I)
and fracturing and/or deformation of the grains begins (phase II). The flow pres-
sure is considered to be a measure of the simple strength of the agglomerate. The
second evident change (where the gradient drops towards the end of the graphs)
takes place when the pressed spray dried granules, as a whole, reach densities close
to those of the individual granule (Pg, see fig. 28).
In this state the pores on the outside of the granule have been all but eliminated
(end of phase II) and reduction of intergranular porosity begins (phase III – new
flattening out of the curves).
The compaction diagram is one of the most appropriate tools for checking the
behaviour of a granulate material during the compaction phase.
Normally, though, to see how the characteristics of the spray dried powder (par-
ticle size distribution and moisture content) influence powder behaviour during com-
paction, simpler checks are run.
Results from tests with a spray dried powder for the production of low porosity
floor tiles are shown below.
Tab. 2 shows its particle size distribution.

The spray dried powder was separated into several particle size bands to evalua-
te the impact of a specific size band on the degree of compaction at the pressing
stage.
Tab. 3 shows these bands together with the average granule density (Pg) and
bulk density compacted by vibration (Pv).
The increase in bulk density was determined by plotting the compaction curve
using the following variables:
– forming pressure of up to 600 Kg/cm2
– changes in residual moisture content from 3 to 10%
– semi-finished powders of different particle size distribution.

These tests demonstrated that the behaviour of an agglomerate during compac-


tion and its resulting bulk density essentially depend on its moisture content, for-
ming pressure (figs. 29 and 30) and, to a much lesser extent, on particle size distri-
bution (fig. 31 - average grain size).

As far as the mechanics of powder compaction are concerned, observe the fol-
lowing:
1. Increased bulk density of spray dried powders during compaction is in line with
the models that have been put forward, studied and perfected in the case of non-
plastic agglomerates.
2. Flow resistance (or flow pressure) Pf falls linearly as average particle size de-
creases and moisture content increases (fig. 31).
3. The compaction pressure (Pj) of the agglomerate decreases as moisture content

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Pressing

Dimensione grano
Grain size (%)
(µm)
>750 0.5
750-500 2.5
500-400 11
400-300 23
300-200 31
200-125 25
<125 7

Tab. 2. Particle size distribution of the spray dried powder on which tests were carried out.

Grain density
Densità (Pg) and
del granulo (Ρg)bulk density
e densità of spray
apparente dried powdersemicompattato
dell’atomizzato semi-compactedper
byvibrazione
vibration (Ρv)
(Pv)
Fraction
Frazione Ρg (g/cm3) Ρv (g/cm3)
Mix (I)(I)
Miscela - 1.110
125 - 200 µm (F) 2.047 1.130

300 - 400 µm (M) 1.990 1.090

500 - 750 µm (G) - 1.035

Tab. 3. Grain density (Pg) and bulk density of spray dried products, semi-compacted by vibration, of
uniform particle size.

increases (exponentially). The size of the particles is less significant for a given
standard moisture content (fig. 32).
4. The behaviour of the spray dried agglomerate at the compaction stage and the
bulk density of the pressed tile essentially depend on the residual moisture con-
tent of the powders (figs. 29 and 33); grain size is less significant (where medium-
low forming pressures are applied)(fig. 30).

Relationship between bulk density of the pressed material and green


bending strength (practical aspects)

Fig. 27 illustrated how the bulk density of the pressed material is generally
linked linearly to the logarithm of forming pressure.
These theoretical considerations aside, it is, at this point, important to quote
some data obtained from experience at a semi-industrial level; such data concerns
the pressing of spray dried powders for vitrified single fire tiles. The graphs in
fig. 33 show the pressed tile modulus of rupture at different forming pressures
and moisture contents. They illustrate how pressing force and moisture content
act synergistically on the bulk density values of the pressed materials, thus al-

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Fig. 29. Changes in bulk density (d) as a function of pressing force and powder moisture content.

Fig. 30. Bulk density as a function of pressing force and particle size distribution.

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Pressing

2 4 6 8

Fig. 31. Changes in flow pressure (Pf) of a powder as a function of its particle size distribution and
moisture content.

2 4 6 8 10

Fig. 32. Changes in compaction pressure (Pj) as a function of particle size distribution and moisture
content.

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GREEN BENDING STRENGTH (Kg/cm2)

PRESSURE

PRESSURE

PRESSURE

PRESSURE

MOISTURE (%)

Fig. 33. Relationship between moisture content and green breaking load.

lowing attainment of uniform (bulk) density values by modifying one variable or


the other.
The graphs in figs. 34 and 35, instead, show green and post-drying bending
strengths for spray dried powders of different moisture contents pressed at differ-
ent pressures. In this case note how an increase in forming pressure and moisture
content (improving powder plasticity and flow) give rise to increased green and dry
bending strengths.
This behaviour can be explained by the fact that the particles are brought closer
together, thus reducing the volume of voids between particles. There is also increased
inter-particle contact, forming “bridges” and “links” between them.

Effect of forming pressure on firing performance of ceramic powders


(practical aspects)

The graphs on the preceding pages show the relationship between forming pres-
sure and bulk density.
However, in order to illustrate the full complexity of the problem, it is, at this
stage, important to introduce data on the relationship between semi-finished pro-
duct characteristics, conditions at the press and the final product that has been ob-
tained in laboratories and test plants.

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Pressing

Residue 3.7% Residue 3.7%


Density (g/cm 3)
Pressure (g/cm2)

Density
Moisture
content

Pressure (Kg/cm2) Moisture content (%)

Fig. 34.

Residue 3.7% Residue 3.7%


Bending strength (N/mm2) Bending strength (N/mm2)

Moisture
Moisture
content
content

350
Pressure (Kg/cm2) Pressure (Kg/cm2)

Fig. 35.

The relevant variables are:


– pressing force
– green pressed tile bulk density
– powder moisture content
– working conditions at the press
– characteristics of the product after firing (shrinkage and porosity).

Observations and data refer to vitreous bodies, where the relationship between
the above parameters is more evident.
Fig. 36 shows vitrification curves for materials of different bulk density at diffe-
rent firing temperatures.
Note that for any given firing temperature higher bulk densities correspond to
lower shrinkage and water absorption values.
Other observations:

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Dbulk
Dbulk
Dbulk
Dbulk

SHRINKAGE %

WA %
TEMPERATURE °C

Fig. 36. Vitrification curves for vitrifiable bodies of different bulk density.

a) The lower shrinkage seen on samples of higher bulk density is attributable to a


lower percentage of pores in the unfired material.
b) Close to vitrification temperatures, lower shrinkage and lower porosity give
greater product stability.

Fig. 37 highlights the relationship between unfired tile density and linear shrinka-
ge even more clearly.
Yet variations in density are not dependent on pressing force alone. A change in
moisture content in the order of 1.5% is equivalent to a change in dry bulk density
of 0.03 g/cm3.
Another factor that causes variations in pressed tile bulk density is pressing speed
(see fig. 38).
Different bulk densities in different zones on the same tile – a variation attributa-
ble to non-uniform filling or other factors discussed previously – may cause uneven
shrinkage within the same tile and thus dimensional defects.
Fig. 39 gives a quantitative example of shrinkage variation where samples of
different bulk densities are fired at the same temperature. Note that differences in
bulk density of 0.06 gr/cm3 correspond to shrinkage differences in the order of
about 0.3%; on a 330×330 mm tile this means up to 1 mm variation on the length of
a side.
Fig. 40 illustrates the problems that arise where a press cavity is incorrectly
filled, resulting in different bulk densities over the tile.

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Pressing

SHRINKAGE %

TEMPERATURE °C

Fig. 37. Relationship between unfired bulk density and linear shrinkage.

Pressure (Kg/cm2)
Fig. 38. Variations in bulk density as a function of pressing speed.

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Fig. 39. Shrinkage as a function of bulk density.

Future developments in pressing

Current trends (2001) indicate that demand for very large, rectangular tiles –
with aesthetic characteristics ever-more similar to those of natural stone – is set to
increase further.
On the manufacturing side this is sure to mean increased demand for larger
pressing areas and higher tonnages so that even larger slabs can be produced: ever-
more sophisticated on-press decoration is likely to involve widespread use of body/
coloured granule mixes, glaze grains and other dry decoration techniques. In this
regard there already exists a new technology that uses a double pressing process.
This consists of a relatively simple first press, which forms and, where required,
decorates the slab at a preliminary level of compaction; the slab is then conveyed to
a small-scale dry decoration line before being compacted in a second press to give a
green tile of the required definitive compaction.
The advent of larger slabs, which realistically resemble natural stone, has also
led to the appearance of new production technologies, which, in a certain sense,
have much in common with the technology used in the cutting and preparation of
natural materials. For example, there is no longer any need for a spacer gap or

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Pressing

Fig. 40. Size defects caused by heterogeneous die filling.

chamfered edge as the slabs are laid without an inter-tile gap. In fact, the idea of
producing mainly large slabs is beginning to gain consensus: this is because diffe-
rent tile sizes can be produced by cutting the green slab with specially designed
conveying and cutting systems, thus allowing the manufacturer to by-pass compli-
cated – and costly – die changeovers. This technology is also likely to have a signi-
ficant impact on die manufacturing technology as slab-size dies need to be extremely
long lasting.

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Further improvements are also expected on the units that feed the powder into the
die, while hydraulic circuits have already been optimised to confine high pressure to
the main circuit only and thus prevent overloading of more delicate components: this
reduces unscheduled maintenance, a factor that can seriously undermine production
line efficiency.

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APPENDICES

Green physical-mechanical characteristics of tiles obtained from


different powders (spray dried/granulated/dry ground)

Preparation of raw materials


Body preparation involves a series of tasks that aim to provide a homogeneous
material with an appropriate, relatively fine particle size distribution and a moi-
sture content suitable for the employed pressing system (in the case in question
powders with a moisture content of 4-7 % were pressed). The following processes
were used:
– dry grinding process, consists of dry grinding the raw materials and then wetting
them with suitable machines.
– wet grinding process, consists of in-water grinding of the raw materials and sub-
sequent spray drying of the obtained slip.

In dry grinding the (very finely) ground powders are treated to aid agglomera-
tion of the particles.
This is done with the aid of:
• standard wetting machines
• re-granulators.

The observations and data below refer to tests that aim to compare the post-pres-
sing characteristics of differently prepared materials (all intended for the manufactu-
re of the same product). The following preparation methods were used:
– cycle with traditional dry grinding, wetting and re-granulation
– cycle with dry grinding and grain selection
– cycle with wet grinding and spray drying.

Particle size distribution of powders produced using different systems

Figures 41 and 42 compare the particle size distributions of dry ground powders
to be wetted and granulated respectively.
As mentioned, the fine particle size of dry ground powders has a considerable
(and sometimes negative) influence on downstream production processes. While, in
fact, fineness generally improves firing conditions because of the increased specific
surface area, pressing conditions are generally worsened on account of the excess-
ive quantity of very fine talc-like powders; this can lead to considerable de-airing
problems (lamination).
These difficulties disappear with granulation as the fine particles are agglomer-
ated.
Both granulation and spray drying agglomerate the particles obtained from grind-
ing. The particle size distributions of the respective agglomerates are, nevertheless

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Fig. 41. Particle size distribution of dry ground powders destined for wetting and granulation.

Fig. 42. Particle size distribution of spray dried powder and grains.

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Pressing

(with the machinery and under the conditions in question) quite different: fig. 42
clearly shows that the particle size distribution of the spray dried material is largely
concentrated around the middle of the spectrum (0.125-0.5 mm) while that of the
granulate is, instead, spread more widely across it.

Compaction and uniformity of pressing

In order to evaluate pressing compaction and the uniformity of such compaction,


penetrometer readings were taken on the pressed tiles and permeability measure-
ments were made on the dried tiles.
Fig. 43 illustrates typical penetrometer data distributions for the various raw
material preparation technologies; pressing pressure is nearly identical, as is the
position of the punch in the respective press.

Observe that:
– tiles made from spray dried powders have the lowest penetrometer imprint depths
(generally around 0.8 mm, against an overall average of 1.2 mm for the other
types of pressed tile). The former are thus more compact.
– tiles made from spray dried powders are not only more compact, they also featu-
re a compaction that is more uniform; the source of this greater uniformity is
not attributable to different press management or control methods but, rather,
the morphological and structural characteristics of the spray dried powder its-
elf (more homogeneous cavity filling).

This data confirms the superior quality of spray dried powders and their posi-
tive influence on compaction performance: that superiority stems from the optimal

Penetration (mm)

Dry ground Granulate Spray dried

Fig. 43. Distribution of penetrometer readings for different body preparation technologies.

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die cavity filling offered by the spherical shape and physical characteristics of the
granules.
The entity and distribution of penetrometer readings on tiles made from dry
ground and granulated powders differ only marginally.
On the other hand, permeability measurements on dried tile samples give a some-
what different picture (see fig. 44).
Forming pressure remaining equal, the permeability readings for dried tiles made
from granulated powder are higher (i.e. outflow times are shorter) than those ob-
tained on tiles made with dry ground and spray dried products (N.B. flow time
refers to the time taken for air compressed at 6 Atm to flow through the entire
thickness of the tile: outflow time is inversely proportional to permeability). Once
again, then, granulated powder is shown to produce tiles that are relatively less
compact than their spray dried counterparts.
Yet another important aspect regards the uniformity of permeability distribution
and, therefore, compaction. Readings for granulates are, in this regard, very similar
to those for the spray dried product, yet the dry ground tile is characterised by
much greater discrepancies between the readings taken on different parts of the
same tile; the tile is, in fact, generally more compact at the centre than at the sides.
The fact that the granulate tends to be similar to the spray dried product in this
regard can be attributed to the shape, particle size distribution and consistency of
the granules, which provide good die filling performance. While this does not deci-
sively and definitively show the granulate to be of high quality, it is, nevertheless,
an aspect of some importance.

Outflow time (s)

Dry ground Granulate Spray dried

Fig. 44. Distribution of permeability readings for different raw material preparation technologies.

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Pressing

Green and dry bending strength

Green bending load is important not only as an indicator of the achieved degree
of compaction but also as a performance parameter: it is an important qualitative
requisite for tiles that will be moved and handled in their unfired state (as in single
firing processes).
Fig. 45 shows, for the three materials in question, green and dry bending strengths
as a function of forming pressure; the diagram clearly illustrates the superior perfor-
mance of the spray dried product, especially for dried tiles. At pressures of 230-240
Kg/cm2, the dried tile made with spray dried powder has a breaking load of 4 N/mm2,
against approximately 3 N/mm2 for tiles made from granulate and 2 N/mm2 for tiles
made from dry ground material.
Once again the data seems to indicate that spray dried powders are of higher
quality than granulates and that granulates are of much higher quality than dry
ground materials.
(N/mm2 2)
VALUE(n/mm
LOADVALUE
BREAKINGLOAD
BENDING )

Fig. 45. Green and dry bending strengths as a function of forming pressure for the three material
types.

Porosity and fired tile bending strength

The graphs in figs. 46 and 47 give, respectively, the porosity (expressed as WA


%) and bending strengths of the analysed materials.

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Fig. 46. Water absorption (WA%)values for pressed tiles made with spray dried powder, powder granu-
lates and dry ground material.
BREAKING LOAD VALUE (N/mm2)

Fig. 47. Bending loads of fired tiles as a function of forming pressure for the three material types.

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Pressing

The best porosity values are obtained with spray dried powder, then powder
granulates and, finally, dry ground powder.
Only at very high forming pressures (over 250 Kg/cm2) do the tiles made with
dry ground powder feature a porosity similar to that attainable with granulates.
Bending strength tells a similar story: the best results are obtained with spray
dried powders, then powder granulates and, finally, dry ground powder.
As with porosity, the bending strength of tiles made from dry ground materials
only begins to near the performance obtained with granulates where forming pres-
sures are higher than 250 Kg/cm2.

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Spray drying of ceramic slips

Chapter IV

DRYING

As explained in Volume 1, the term “drying” refers to removal of the water


contained in a solid by way of evaporation (i.e. its conversion from a liquid to a
gaseous state).
The tendency of a liquid to become gaseous largely depends on its chemical-
physical properties. Kinetic energy causes molecules to leave a liquid as vapour
while, simultaneously, vapour molecules condense.
The number of molecules abandoning the liquid depends on temperature; the
number condensing depends on the number of molecules in a gaseous state that
come into contact with the surface of the liquid in a given time and thus the number
of molecules in a determined space and their speed (i.e. vapour pressure).
To a lesser extent, dying also involves the so-called crystallisation, zeolite or struc-
tural water contained in certain minerals (such as montmorillonite, etc.).
As it absorbs energy, water, like all liquids, has a tendency to become gaseous.
This transformation does not continue indefinitely; it will cease when the vapour
reaches saturation point (i.e. when an equilibrium between the number of water
molecules evaporating into vapour and the number of vapour molecules conden-
sing into liquid is reached). This equilibrium corresponds to a certain pressure,
known as saturation vapour pressure, which increases with temperature.
When, by increasing temperature, vapour pressure is raised to a point where it
equals atmospheric pressure, boiling occurs (i.e. the vapour escapes not only from
the surface of the liquid but also from its interior as bubbles).
For all substances, lower ambient air pressures correspond to lower boiling points
and every substance has, at a given temperature, its vapour pressure. The saturation
vapour pressure of water at 100 °C is 1 Atm (fig. 1).
Taking into account the amount of energy absorbed during liquid-vapour tran-
sformation, it can be seen that the amount of energy involved during drying is
often underestimated.
Drying is a process conditioned by three main factors:
– “drying power” of the environment: relative humidity, air flow speed etc.
– forces acting at capillary level.
– dimensional changes caused by release of moisture.

The drying process, then, involves transfer of heat energy from the surrounding
environment to the ceramic piece and simultaneous transfer of water in the opposite
direction.
The heat (energy) needed for the former may be received by the piece by way of
convection, radiation or conduction: normally all three are involved. The most com-
mon of the above three – hot air convection – can, as a rough guide, be broken down

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Vapour tension mm Hg

Temperature °C

Fig. 1. Saturated vapour pressure of water at different temperatures.

into the following stages:


• transfer of heat contained in air to piece
• transformation of water from liquid to vapour
• removal of vapour from surface of piece
• water transported in liquid state from piece interior to surface.

When the evaporation rate at the surface exceeds interior-to-surface capillary


transfer capacity, a further drying stage, during which the evaporation front shifts
towards the interior of the piece itself, begins.
This is generally represented by the classic convection drying curve for porous
hygroscopic materials, which features three stages, each corresponding to different
drying speed gradients and different depth levels.

Conventional hot air driers for ceramics

Drying speed is largely determined, then, by the capillary diffusion of water


inside the tile.
When drying starts (i.e. at the drier inlet) the temperature of the pressed tile is
low and diffusion is very slow; evaporation speeds thus need to be contained so as to
prevent compaction of the surface layer.
This is why, in conventional driers, the incoming material is placed in contact
with hot air that is relatively humid. Up to the surface of the pressed tile (i.e. the
drying interface), heating occurs by convection; inside the pressed tile heating

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Drying

occurs by conduction (note that a pressed tile generally has very low thermal
conductivity). Heating speed is generally adjusted by modifying air temperature
and flow rate.
For a given material of defined porosity, the time needed for attainment of uni-
form heating temperatures that result in proper diffusion kinetics essentially depends
on tile thickness.
The drying cycle, of course, is influenced not only by thickness but by moisture
content. Extruded or cast products, on account of their high moisture content, go
through the phases of shrinkage drying, diminishing-shrinkage drying and zero-
shrinkage drying; drying of pressed tiles only involves a fraction of the second
phase and the entire third phase.
Overall shrinkage is therefore much lower and the risk of tension caused by
heterogeneous shrinkage thus relatively low.
Such low moisture contents and the correlating “shrinkage insensitivity”, have,
in recent years, resulted in the development of machines that employ extremely
high heating rates.
The purpose of this approach is to counteract natural shrinkage (which can cau-
se fractures) with the opposite tendency of the material to expand when heated
intensely: the tile is thus kept in a sort of dynamic equilibrium that allows use of
extremely fast drying cycles (lasting just a few minutes).

Technological considerations

In any case, bear in mind that:


– diffusion towards the interface requires a moisture gradient.
– the speed of diffusion increases with the gradient; the pressed tile has an
initially homogeneous moisture content which is subsequently reduced at the
surface, thus aiding transport kinetics: there exists an upper technological
limit to this phenomenon on account of the fissuring that occurs where drying
is violent, although this can be avoided by taking the precautions mentioned
above.
– diffusion speed is proportional to green permeability, itself dependent on the
chemical-physical properties of the body (composition, particle size distribu-
tion, quantity and size distribution of non-plastic hard materials) and on the
forming process and work parameters.
– water flow rates decrease as the migration route lengthens: thus very thick tiles
have slower drying speeds.
– water viscosity inhibits transport kinetics by increasing resistance to flow. To
reduce viscosity and aid diffusion the water is heated (heating involves the whole
tile).

Surface evaporation. This is the kinetics of the process and actually involves two
elementary processes:

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1. Interface evaporation (liquid-vapour equilibrium phenomenon).


2. Removal of the vapour (diffusive transport by way of concentration gradient),
which is a function of temperature (or, rather, the vapour pressure of the water)
and ambient thermo-hygrometric conditions (at the interface and in the gaseous
phase).

In conventional drying processes the hot air:


– carries the heat to the tile body and causes evaporation
– takes the vapour away.

Thus water evaporation and vapour removal rates increase as air temperature
and flow speed increase and are aided by low air humidity.
Good quality drying is achieved when the two processes (diffusion and evapora-
tion) have kinetics that allow the quantity of water evaporated per unit of time to
be replaced by an equal quantity of water from the interior of the pressed tile
(evaporation rate = diffusion rate); under standard process conditions the slower of
the two is internal diffusion.
For any given material (of established geometry, permeability, moisture) the only
diffusion parameter that can be adjusted (via heating) is water viscosity.

Drying speed = flow of water per unit of pressed tile surface area [Kg/(m2h)].

This last observation illustrates the direct relationship between temperature and
pressure (or vapour pressure). At the above equilibrium the vapour is referred to as
“saturated vapour”; if the pressure is below the equilibrium point the vapour is said
to be “unsaturated”.
In the case of saturated vapours pressure is merely a function of temperature.
To shift the equilibrium a certain quantity of heat energy equal to the latent heat of
the substance being evaporated needs to be applied to the system. This heat is pecu-
liar to every substance and is defined as “the heat needed to transform a standard
unit of weight”.
Vapour condensation causes the latent heat to show up as calorific energy. The
heat of vaporisation is very high if one considers that, theoretically, 605 Kcal are
needed to evaporate 1 Kg of water once the water temperature has been raised to
100 °C.
Water evaporation obviously diminishes as the degree of saturation of the space
overlying the water increases.
In ceramics evaporation problems are related to the fact that the water to be
evaporated is combined with solids, thus restricting evaporation. The water forms a
sort of reticule made up of numerous capillaries that wind their way in between the
solid particles.
The problem is how to transport this water from the interior of the piece, through
the capillaries, to the surface where it can evaporate freely.
To resolve this problem two factors – and their respective speeds – need to be
taken into account: diffusion and evaporation. The problem of drying can said to

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Drying

have been largely resolved when the evaporation speed does not exceed the speed
with which the water is diffused from the interior of the piece to the surface and
thus the water can evaporate at a speed that is high enough to be economically
viable yet not so fast as to cause product damage.
Drying is thus piloted by the DIFFUSION SPEED of the water in the interior
of the pressed tile and the subsequent EVAPORATION SPEED.

The major evaporation conditions are therefore:


• SURFACE EVAPORATION: occurs under conditions of thermodynamic equi-
librium with the surrounding environment, with liquid water being drawn from
the interior of the pressed tile in quantities equal to those being evaporated.
• EVAPORATION UNDER PLASTIC CONDITIONS: occurs in capillaries and
interstices at the liquid-vapour interface under equilibrium conditions, with va-
pour being simultaneously transferred to the surface via the capillaries themsel-
ves. The process occurs under dynamic conditions, with transfer of the interface
zone deeper and deeper into the piece.
• INTERNAL EVAPORATION WITHOUT FLOW: similar to the above but there
is not enough moisture to generate flow or settling of the clayey particles and
thus removal of the water generates interstitial porosity.

A study of the graphs found in specialist literature shows that:


– the volumetric stability that follows drying-induced shrinkage corresponds to a
full/empty volume ratio of approximately 75/25.
– the interstitial water which has reached post-drying stability varies from 10% to
12% by weight of the solid.
– dimensional variations corresponding to moisture contents below 10-12% are
virtually negligible.
– pressed tile dynamic equilibrium is achieved when the degree of water evapora-
tion corresponds to the degree of interstitial water diffusion in the tile interior;
thus in each situation there is a certain evaporation speed, said to be “critical” in
that beyond this speed dimensional variations can create tensions which can, in
turn, cause damage.
– evaporation speeds above the 1st critical Bigot point essentially depend, tempera-
ture remaining equal, on ambient conditions; below the 2nd point they depend
only on the chemical-physical characteristics of the ceramic material.

DIFFUSION SPEED depends on:


– mineralogical characteristics of the material, which directly influence the orienta-
tion of the water molecule and thus its ability to migrate.
– particle size and shape, which influence width and shape of the capillaries via whi-
ch the water is diffused.
– percentage of water content in the piece: as water content drops the solid particles
converge (shrinkage only stops when the particles touch each other). This con-
vergence narrows the empty capillaries and seals some of them off, resulting in
increased obstruction.

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– pressed tile temperature


– speed and extent of shrinkage, itself a function of evaporation

surface tension of the liquid to be evaporated


– relationship between ––––––––––––––––––––––––––––––––––––––––––––
vapour pressure of atmosphere, hygrometric state,
relative humidity

During shrinkage the capillaries narrow and some of them are sealed off, thus
increasing resistance to diffusion of the water through the mass of the tile. Accord-
ing to some researchers this resistance is inversely proportional to the fourth power
of the diameter of the capillaries.
However, it has been found that the shape of a capillary affects diffusion more
than its size and that this shape depends on the size and structure of the surround-
ing particles.
Finally, diffusion can only occur if there is evaporation on the surface of the
piece.
Since evaporation depends on the ratio between the surface tension of the liquid
and the atmospheric vapour pressure overlying the system, it is obvious that diffu-
sion speed also depends on this ratio.

EVAPORATION SPEED depends on:


– air temperature: the higher the air temperature the greater the quantity of water
it can hold in suspension
– air speed
– hygrometric state of air: determines, at a given temperature, the quantity of water
that can be removed from the material
– surface area exposed to air and angle at which piece is tilted with respect to direction of
air flow
– diffusion speed of the liquid in the material

surface tension of liquid to be evaporated


– relationship between ––––––––––––––––––––––––––––––––––
vapour pressure of atmosphere

Control of air volume, temperature and speed is made easier if its hygrometric
state is known.

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Drying

Glossary

• ABSOLUTE HUMIDITY
the quantity of water per Kg of dry air.

vapour pressure of air


• RELATIVE HUMIDITY –––––––––––––––––––––––––
saturated vapour pressure

quantity of water vapour per Kg of dry air


• PERCENTAGE HUMIDITY ––––––––––––––––––––––––––––––––––––––
quantity of water vapour that would contain
a Kg of dry air if it were completely saturated

• VAPOUR PRESSURE
The vapour pressure in equilibrium with liquid pressure.

• SURFACE TENSION
The force that acts on the surface of a liquid, tending to minimise its area.

• WET BULB TEMPERATURE


Temperature obtained by immerging the bulb in water, the surface of which is
exposed to the air. The sensible heat transferred from the air to the water is
equal to the latent heat of evaporation of the water.

• HEAT OF VAPORISATION
The quantity of heat energy needed to evaporate a unit of liquid, at constant
pressure and temperature. Also known as enthalpy of vaporization, heat of eva-
poration and latent heat of vaporization.

• SPECIFIC HEAT
The quantity of heat needed to increase the temperature of a material by 1 °C,
without any chemical or phase changes.

• PSYCHROMETRIC (OR HYGROMETRIC) CHART


A graph, each point of which represents a specific condition of a gas-vapour
system (such as air and water vapour) with regard to temperature (horizontal
scale) and absolute humidity (vertical scale); other characteristics of the system,
such as relative humidity, wet-bulb temperature, and latent heat of vaporization,
are indicated by lines on the chart (fig. 2).

From the above it is evident that the drying process is conditioned by the hygro-
metric state of the air at different temperatures. Rational use of a drier thus re-
quires that air humidity, especially in critical zones, be monitored carefully. Since

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Fig. 2. Psychrometric chart.

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Drying

evaporation results in cooling, the temperature of the solid is lowered to an extent


that depends on the dryness of the air.
The device used features two thermometers: one has a naked bulb and measures
ambient air temperature directly and the other has a bulb sheathed in a cotton cover
that keeps it constantly wet.
The two bulbs give the same temperature reading only when ambient air is satur-
ated (100% relative humidity) because in this situation water evaporation ceases
altogether. Vice versa, the difference between the two temperatures is at its greatest
when ambient air is completely dry.
Wet bulb and dry bulb thermometric measurements allow researchers to trace
charts that show the humidity of air-vapour mixes at a constant total pressure of 1
atm (fig. 2).

Proper drying requires:


– careful evaluation of thermo-hygrometric process parameters
– proper body formulation

which translates into


• reduced shrinkage and limited deformation.
• the bending strength needed to oppose the stress of drying and allow handling during
subsequent stages of production.

Thus the main parameters that need to be taken into consideration in body for-
mulation are:
• percentage of plastic raw materials: these increase the cohesive strength of dried
objects, but also increase shrinkage.
• mineralogical nature of the clays: deflocculated clays in their natural state form
a compact, impermeable tissue during drying. They adsorb cations with some
difficulty, thus forming more open, permeable structures that allow faster
drying.
• percentage of non-plastic raw materials: these worsen unfired bending strength but
help contain shrinkage (especially where particle size distribution is fine).
• water content: increases shrinkage and plasticity. Particle fineness is, in fact, pro-
portional to the hygroscopic value of the body.
• forming pressure: influences drying behaviour in that higher pressures reduce per-
meability and water diffusion.
• piece geometry: this is very important. Drying is faster for high surface area/volume
ratios (thinner tiles dry faster).

Machines

The driers used in the ceramic tile industry are of both the horizontal and verti-
cal type. Although the technological principles behind them are essentially the same,
the dynamics are somewhat different in that variations in the cycles significantly

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alter the times over which shrinkage, increased bending strength etc. exert their
effect.
Working conditions on the machine and air parameters (maximum temperature,
speed, volume and hygrometric values) are, therefore, necessarily different on the
two drier types.

Rapid vertical driers

High performance rapid vertical driers are ideal for automatic tile production
lines. They are designed to provide optimum technological results: low residual
moisture content, uniform tile temperatures, good product bending strength and
low energy consumption (fig. 3).
An automatic vertical drier is essentially made up of a vertical framework in
which a chain drive system moves a series of racks (or baskets), which consist of a
set of rollers to carry the tiles.
Tiles are loaded automatically – without touching each other – onto the racks by
the rollers as they rotate.
An air flow generated by burners and fans dries the tiles by convection; this
process yields a product that is suitable for the subsequent stages of the production
process (glazing, firing etc.), that is, one which has:

Fig. 3. Rapid vertical drier.

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Drying

– low moisture content


– good bending strength
– a set temperature.

The diagram below (fig. 4) illustrates the main parts of a vertical drier.
Fig. 5, instead, shows a plan for a vertical drier with a pre-ventilation unit and a
cooling unit at the outlet.
Operative conditions in the drier (air temperature, humidity and flow rate)
are controlled by three independent units that form three differentiated drier
zones.
In the first zone (where the material enters the drier and is lifted) the tiles are
exposed to an air flow, produced by a fan and burner, which runs parallel to the
tile surface. Intake and outlet gratings are used to distribute the air and direct it

1 Load-bearing structure 10 Internal ducting


2 Insulating panels 11 Burner fan
3 Rack (basket) chain 12 Burner
4 Drive unit 13 Stabilisation unit
5 Racks (baskets) 14 Stack
6 Rollers 15 Pneumatic system
7 Lubrication unit 16 Electrical system
8 Service platform 17 Electrical cabinet
9 Upper service platform 18 Control panel

Fig. 4. Cut-away diagram showing main parts of a vertical drier.

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SECOND
ZONE FIRST
ZONE

COOLING
ZONE

STABILISATION
ZONE

Fig. 5. Air circulation with cooling unit.

to the various rack levels throughout the drier. Once the air has traversed the
racks, it is re-aspirated into the internal ducting where most of it is re-circulated
by the fan and a small (adjustable) portion is expelled by the exhaust fan into the
atmosphere.
The circuit in the second zone (where the tiles are lowered) is similar to that in
the first zone yet independent from it, in that it has its own fan, burner and external
air intake damper.
A further fan controls the stabilisation zone, the last area dedicated to the actual
drying cycle. Significant resources have been channelled into the development and
perfection of this section and so meet the need for uniform tile temperatures.
To achieve stabilisation the tiles need to be exposed to a correctly directed flow
of constant-temperature air, obtained by mixing cold external air – in quantities
batched by a modulating valve – with the hot air exiting the second zone.

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Drying

This “stabilisation” process controls the tile properties required at subsequent


stages of the production process (glazing, application of soluble salts, dry polishing
etc.).
The drying cycle normally exposes tiles to high temperatures immediately
(assuming they can withstand initially fast water removal) so that a lower tempe-
rature (closer to the final one) can be set in the second zone. This maximises
stabilisation efficiency and produces high bending strengths.

Where tiles are somewhat fragile the cycle can be modified accordingly: this is
achieved by creating (via dampers) an initial tile heating zone with reduced air flow
that allows temperature to rise gradually.
To obtain very low outgoing tile temperatures (below 65 ºC), the drier can also be
equipped with two axial fans that introduce ambient temperature air into the lower
drier zone. It is also possible to reach an outgoing tile temperature of 40-50 °C.
Smooth tile loading and unloading and versatile tile size accommodation are
provided by infeed and outfeed rollers, precise on-rack tile arrangement, a twin
roller drive system which prevents slippage and the encoder which controls rota-
tion.

Rack movement is controlled by an inverter on the chain drive motor; this system
provides maximum precision and also protects against overloads. Furthermore, guides
placed along the entire rack route ensure proper positioning at all times.
The racks are supported by special arms fixed to the chain: these make move-
ment friction-free and thus reduce energy absorption.
Thick insulation reduces heat loss to a minimum. The potential of these driers is
illustrated in the following graphs and tables (fig. 6 and tab. 1).
Drying time (minutes)

6 rows
5 rows
4 rows
3 rows
2 rows
1row

Press speed (cycles/min)

Fig. 6. Relationship between press output capacity and drying time.

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UNFIREDCRUDO
FORMATO SIZE (mm.)
(mm) TEMPO DI ESSICCAMENTO
INDICATIVO
APPROX.DI RIFERIMENTO
DRYING TIME (min.)(min.)
larghezza
width lunghezza
length Spessore
thickness
161 161 6 30
161 215 7 35
215 215 7 35
269 269 8 41
215 323 8 44
323 323 8 44
355 355 9 49
323 430 9 50
430 430 10 53
538 538 11 58
645 645 12 64

Tab. 1. Drying times for tiles of different size and thickness.

Horizontal driers

Experience acquired with the first fast driers has led to a greater understanding
of some fundamental concepts vis-à-vis drying of pressed tiles with very low re-
sidual moisture content (4-7%).

1. Ventilation: air flow must be as parallel to the tile faces as possible to ensure that
heating is homogeneous and vapour is efficiently removed from the tiles.
2. Drying air temperature: plays a key role in evaporation speed.
3. Water evaporation speed: less influenced by speed and relative humidity of air than
on vertical driers.

Horizontal driers can have from just one to as many as five layers of rollers
(channels).
They are enclosed in an insulated chamber fed with hot air generated by dedi-
cated burners and/or exhaust air recovered from the kiln (see figs 7 and 8).
Figures 9, 10 and 11 chart the influence of the main tile drying variables. These
are:
W = Tile moisture percentage by weight
V = Speed of air over the flat tile surface
Wr = Relative humidity of the drying air
T = Temperature of the drying air.

Note: the term drying speed refers to the weight (Kg) of water freed from the
surface of one square metre of tile surface in one hour.
The graphs show that drying speeds are much higher where samples have a very
high water content (e.g. 12%).

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Drying

Fig. 7. Multi-level horizontal drier.

Fig. 8. Horizontal drier.

Note also that where pressed tile water content is quite low (5-7% or lower) the
relative humidity of the drying air is no longer significant.
This is an advantage since fast driers sometimes operate discontinuously and
relative air humidity can vary considerably, especially during drier start up and
stoppages.
In (fast cycle) horizontal drying the tile behaves, from a technological viewpoint,
more or less as described in the theoretical explanation of drying given in Volume
1.

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Drying speed (Kg/m2h)

Air speed (m/s)

Fig. 9. Relationship between air speed and drying speed expressed in Kg/m2h (W = tile moisture %).

Drying speed (Kg/m2h)

Air humidity (%)


Fig. 10. Relationship between air humidity (%) and drying speed expressed in Kg/m2 h (W = tile
moisture %).

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Drying

Drying speed (Kg/m2h)

Air temperature (°C)


Fig. 11. Relationship between air temperature (°C) and drying speed expressed in Kg/m2 h (W = tile
moisture %).

It may be the case, however, if pressed tile moisture content is very low, that
evaporation can be accelerated using a non-standard drying cycle that raises tile
temperature to over 100 °C, changing the water into steam while it is still in the
capillaries.

Evaporating conditions

Table 2 shows maximum water evaporation speeds for certain materials as a


function of treatment temperature.

MAXIMUM DRYING SPEEDS (Ve MAX)


(Kg/m2h) as a function of treatment temperature

Body type (spray dried products) Treatment temperature


180° 220° 260°
Red monoporosa. 5.3 mm thick, moist. cont. 4% 1.2 1.5 2
White single fire 8.8 mm thick, moist. cont. 4.7% 1.6 2.2 2.9
Red single fire 8.8 mm thick, moist. cont. 5.8% 1.7 2.4 3.1
Tab. 2. Maximum evaporation speeds as a function of treatment temperature (Ve max Kg/m2 h).

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Fig. 12, instead, indicates – in graph form – how maximum evaporation speed
(Ve max, Kg/m2h) changes as a function of treatment temperature.
By taking into account drying speeds attainable for tiles of different size and
thickness, it may be affirmed that high evaporation speeds can be obtained without
any damage to the tile using hot air alone, without having to use other drying
systems (described below).

Fig. 12. Evaporation speed (Kg/m2h) as a function of treatment temperature.

Infrared rays

Rather than drying, this is simply heating, because when electromagnetic ra-
diation with a wavelength of 0.8-3 microns encounters a ceramic body it only
penetrates a few tenths of a millimetre as even water blocks rays of this wave-
length.
The surface of the tile thus heats up more quickly than the interior as heat is
diffused inside by conduction.
While actual drying always requires an air flow to remove the water vapour, it
can only take place quickly where the temperature of the tile is high enough to
reduce the water viscosity in the capillaries significantly.
However, this method has two major drawbacks: firstly, it uses high temperature
radiation sources that can cause the material to overheat should the tile stop under
the source and, secondly, electricity costs are prohibitive.

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Drying

Microwaves

Ceramic bodies could be heated with microwaves in the 2.5 GHz range. These
are directed at the material via specially designed wave deflectors.
Water molecules, which behave as resonating dipoles, dissipate energy and it is
thus possible to heat the whole of the piece at once (albeit heterogeneously as there
is the side effect to take into consideration).
The thus-generated vapour is carried away by a hot airflow.
Drawbacks:
a) Very high plant investment costs.
b) Very high drying costs in that the energy, although used efficiently, necessarily
requires an electrical source.
c) Possible safety and environmental hygiene problems in that radiation leaks can, at
such wavelengths, be harmful in many ways and damage the human central ner-
vous system.

Technological aspects

The technological aspects of fast horizontal driers are, on the whole, similar to
those of vertical driers.
As before, body formulation needs to take into account the aspects described
previously and the main drying parameters (drying cycle times, speed, humidity
and temperature of drying air).
As with vertical machines, drying requires:
– attentive evaluation of thermo-hygrometric process parameters
– proper body formulation

which translates into


• reduced shrinkage and limited deformation.
• a bending strength that will withstand drying stress and allow handling during subse-
quent stages of production.

The parameters to be taken into account for correct body formulation are the
same as those listed for vertical drying.

Relationship between drying cycle and tile thickness/size

Drier size and drying cycle duration depend, to a large extent, on the dimen-
sions of the tiles. Pilot plant tests and comparisons with results obtained on an
industrial scale have led to the establishment of a simple formula which gives
appropriate drying cycle times as a function of tile thickness and longest side
length.

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These formulas are given below and refer to two different lay-outs:

PRESS ➪ DRIER ➪ GLAZING

Teo = [(S)3/2 + (0.02 × Lm)1.3] × Ko

where
Teo : drying time in minutes
Ko : coefficient of material: 0.40 white and red single fire
0.45 white and red monoporosa
0.55 porcelain tile (soluble salts)
S : total thickness mm
Lm : longest side in mm

PRESS ➪ DRIER ➪ STORAGE

Teo = [(S)3/2 + (0.02 × Lm)1.3] × Ko

where
Teo : drying time in minutes
Ko : coefficient of material: 0.50 porcelain tile (plain, salt and pepper)
0.55 porcelain tile (large grains)
S : total thickness mm
Lm : longest side in mm.

General observations

It is possible, then, to use very high evaporation speeds without damaging the
product.
Hence there is a clear temptation to build driers with very fast cycles. Yet, on
modern driers, the most desirable technological parameter is not so much short
cycle duration as constant temperature of the outgoing pieces.
This is because any variations in this parameter can seriously compromise glaz-
ing results.
Utilisation of air at temperatures that provide control – via special thermoregu-
lation devices – over outgoing piece temperature, even where the process has been
complicated by lengthy stoppages, is only possible where the drying cycle is of a
certain duration.
From a thermodynamic viewpoint, the use of very high temperature air would
force manufacturers to operate with very high vapour contents so as to prevent
excessive loss at the stack but this could result in undesirable condensation on the
pieces themselves.
The key requirements with this type of drying are, then:

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Drying

1) Drying cycles must be suitable for tile thickness and temperatures must not be excessively
high.
2) Outgoing piece temperature needs to be controlled.
3) Specific energy consumption must be contained.
4) Mechanics must be simple and the machine compact.

Generally speaking, all types of press have their own matching drier with an
inlet frequently designed to accept twice the number of tiles produced at each
pressing cycle; this results in less costly, simpler feed units. Moreover, less space
is needed.
Installation of machines with wider cross-sections has been made possible
thanks to a device that allows roller removal even where very little side space is
available.
The multi-layer horizontal drier system is hardly an original one as it has been
used by the heat treatment industry for decades and, moreover, had already been
adopted (in part) on vertical tile driers in split ventilation models (i.e. the drier is
designed as a series of ventilations cells as illustrated in fig. 13).

Fig. 13. Multi-layer horizontal drier (the diagram illustrates air flow routes).

Here, each cell is, from a thermo-hygrometric point of view, fully independent as
it is equipped with its own circulation fan, hot air generator, air intake and extrac-
tion port (which carries exhaust air to the stack).
Re-circulation air enters and exits the cell via hopper-like ducts through the side
walls opposite the drive units, thus providing more space and a well balanced air
feed on the different levels.
The system also employs an “upside down” emission/intake system over the full
length of the drying cell.
Air flows through openings of variable aperture while specially positioned ducts
and deflectors ensure uniform cross-flow.
During drying the tiles are exposed to an air flow parallel to their faces; each

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drier level is bordered by a series of removable metal sheets that define the treat-
ment cell.
The exhaust air is extracted at a point designed to yield maximum thermodyna-
mic efficiency (i.e. where the enthalpy – or total heat – of the re-circulation air is at
its minimum).
Machines of this kind thus make it possible to construct proper drying curves
that include a final stabilisation zone, extremely useful for the control of outgoing
piece temperature.
In the event of a glazing line stoppage the material may halt inside the drier.
This could cause temperature fluctuations on outgoing tiles so regulation logic
sets a “holding temperature”, attained via settable gradients; moreover, internal
temperatures can be lowered quickly by servomotor-operated ambient air intake
valves.
Roller drive units, of the traditional type used on kilns, feature helical gears in
closed oil-bath casings. This system is very reliable and is virtually maintenance-
free.

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Drying

Chapter V

GLAZE AND DECORATION APPLICATION TECHNIQUES

Glazes can be used in several physical states: as aqueous and non-aqueous


suspensions, granulates (sintered or pelletized grains) or powders.
Solid, granulate and powdered glaze preparation techniques are generally the
domain of glaze manufacturers. Ceramic plants themselves mostly handle the
grinding of composite glazes to make them suitable for the delicate application
stage.

Glaze preparation

1) The glaze preparation department


This department should suit the specific plant and logically be sited, where pos-
sible, between the storage areas and the glazing lines to minimise transport.
In the past glaze preparation departments were often situated in underground
areas below the glazing department so that the latter could be supplied directly.
Today a system with all the tanks and machines above ground level is preferred:
other solutions, generally more expensive and less ergonomic, are used only where
space is restricted or there are insurmountable logistic problems.
A modern preparation department should be a well organised operation, working
to precise specifications so as to supply the application station with a reliable, consi-
stent product.
To be economically viable it will necessitate a variety of different sized ma-
chines.
Taking an average size factory as an example (2 million m2 of single fire tiles per
year), the required machine pool must include at least:
– 2 mills of 5000 l capacity
– 2 mills of 2000 l capacity
– 2 mills of 1000 l capacity
– 1 mill of 500 l capacity
– 1 mill of 200 l capacity.

The department may be producing many different glazes at any one time, re-
quiring at least 2 agitator-equipped tanks (each capable of holding two mill loads)
for every ball mill.
This allows grinding to be carried out mainly at night, thus reducing energy
costs and noise-related problems.

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Fig. 1. Alsing mill: cross-section, internal view and close-up showing grinding media and lining.

2) The machines
Preparation departments usually have the following:
– Alsing mills, of various capacities. While the 5,000 litre models are the most
common, mills can range from the small 300 litre units used for experimental or
control tests to the 12,000 litre units for large-scale production runs. Generally
equipped with sintered alumina grinding media (which wears at a rate of 500-
2000 g/ton of ground glaze) and a sintered alumina lining that lasts about 20,000
hours.
Rubber and silica are no longer employed in this field. The discharge plug must
be made of stainless steel.
Energy consumption is in the order of 10 kW/ton of ground glaze per grind-
ing hour at 17 RPM.
– Agitator tanks. Available in a range of types: octagonal, plastic or tile-lined ce-
ment, stainless steel cylinder. Average holding capacity is 5 m3 (approximately
equivalent to the contents of two 5,000 litre mills). Tanks must be covered and
are equipped with agitators to prevent settling: these consist of a gearmotor
mounted directly on the shaft that supports the glaze stirring device.

The agitators rotate slowly (about 20 RPM) and sometimes discontinuously (from
10' to 20'/h).
Hence the gearmotor system must be designed to withstand the stress caused by
repeated restarts.
Modern agitators feature inverters that allow RPM to be adjusted as and when
desired.
A splash pan should be installed between the gearmotor and the shaft to catch
any leaking oil and thus prevent contamination of the glaze.
The agitator blades should be shaped and sized so that they pass as close to the
sides and, most importantly, the bottom of the tank as possible: this prevents sedi-
mentation or, even worse, solidification.
Helix and turbine agitators also exist, but these are generally employed as mo-
bile units.

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Glaze and decoration application techniques

As these run at high RPM they must be used cautiously because the glaze could
overheat or air bubbles could get into it, with serious consequences vis-à-vis rheolo-
gical behaviour.
There must be enough tanks to allow proper storage of the glaze. Generally
speaking, there should be one tank for current use (from which the glaze is withdrawn
and sent to the application stations) and a holding tank, where checking and correc-
ting are done.
Emptying operations are best performed with the aid of flex hoses and rapid ball
couplings with butterfly valves as these are less likely to jam. Couplings and valves
should be made of stainless steel: anything containing copper, bronze or brass must
be avoided.
– Pumps. Several types are used. The most common are:
• Diaphragm pumps for low pressure glaze emptying and transfer operations.
These have the advantage of being very safe, having no electrical system and
a wide range of flow rates.
• Peristaltic pump. Squeezes the slip through a wear-resistant rubber flex hose
by way of a rotor with three or more “spokes”, each tipped with a roller. Has
a less marked “pulse” than the diaphragm pump and is self-priming. Has be-
come very popular over the last decade thanks to good performance even
under difficult conditions and low maintenance costs.
• Centrifugal pump. The most economic type. Rubber lined and stainless steel
versions are available to prevent contamination. Not self-priming. High pres-
sure unattainable. Frequent, yet inexpensive maintenance required.
• Mono pumps of the displacement type. Pressure is provided by a spiral steel
screw rotating inside a rubber seat.
They must never be run empty and require rather a lot of maintenance.
Now used sparingly for both glaze and slip transfer because of high costs.
Suitable for long distance transfers on account of high pressures (from 5 to
7 Atm).
– Vibrosieve. High efficiency circular vibrosieves are now the norm. Efficiency de-
pends on sieve diameter and vibration frequency, which can be optimised throu-
gh use of an inverter.
However, as yet, there are no machines capable of sieving efficiently between 80
and 90 microns at high flow rates and densities. By using the largest diameters
available (about 120 cm) it is just possible to reach 110 microns, and even then
not for every kind of glaze.
– Magnetic separators. Removal of magnetic impurities from the glaze is essen-
tial. While progress has been made on the technological side, much still de-
pends on the attentiveness and skill of the worker. If, in fact, static magnetic
separators are not washed at the right moment they can actually cause the
every damage they are intended to prevent: this is because tiny particles,
harmless on their own, can agglomerate to form needles, which, once they
reach a certain size, could detach and be carried away by the glaze flow, thus
damaging output.

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There are several types of iron remover. The most common are:
– Bars. Generally consist of cartridges, with three cylindrical, magnetic bars welded
to its cover. Limited contact area, but can be installed in groups or series. Easy to
clean and inspect.
– Honeycomb. These provide more surface area. Made up of permanent magnets in
the form of overlaid perforated discs. More difficult to clean.
– Roller. The most recently developed – and most costly – solution. Consists of a
roller (diameter 250 mm, length 800 mm) partially immersed in the glaze. The
electromagnetic roller rotates on its own axis and extracts magnetic impurities
from the glaze; these are then removed by a scraper. Operation is continuous.

On more recent models the 3000 gauss electromagnetic roller, which heats up
and loses efficiency to the point where it supplies just 1500 gauss, has been replaced
by a 5000 gauss permanent magnet. Magnetic separator efficiency is, of course,
inversely proportional to glaze flow rate and viscosity.

3) Scales and weighing systems


On the whole ceramic companies would be well advised to have a clear under-
standing of how their glazes are composed. This would allow them to optimise use
of frits and other components, thus avoiding excessive stocks and the correspond-
ing control and management problems. However, this involves more work on the
weighing side and the possibility of error. Moreover, a system that allows accurate
monitoring of materials purchased becomes indispensable.
Intermediate solutions exist: for example glaze manufacturers can supply alrea-
dy made-up sacks or bags that can be modified by adding other components in the
ceramic factory. This makes weighing tasks easier yet control of incoming compo-
nents more difficult. Finally, it is even possible to purchase fully pre-packaged com-
pounds.
In many cases these three systems co-exist, with the best “mix” being chosen on
a case-by-case basis. Note that the glaze preparation department is generally equip-
ped with a series of electronic, digital display weighing units with the following
weight ranges:
– 2000 or 3000 Kg floor platform unit
– 300 Kg floor platform unit.

The weighing units can be connected to a printer.


PC-connected weighing units that optimise formula weight control and automat-
ically provide information for stock control are increasingly used. These systems
can also supply important information and make the switch to new formulas (and
their cost calculation) smoother.
While weighing systems, then, have evidently evolved, the same cannot be said
of mill loading systems. Apart from the cited ready-mixed sacks, all other composi-
tions require several stages of manual handling involving the transfer and lifting
of bags and containers. In any case, the extreme variety of the compositions rules
out automatic loading.

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Glaze and decoration application techniques

A possible solution is the rationalisation of the glazes used in production, conse-


quently lowering the number of components in their formulation, which could lead
to semi-automatic silo storage and weighing systems.
Today, in virtually all glaze preparation departments, packs are weighed or even
counted on the assumption that they are of constant weight. The mill load is pre-
pared and then placed on pallets which are raised to the mill infeed level with eleva-
tors or fork-lift trucks.
Alternatively, the contents of the various packs are poured into a ground level
container (with a discharge valve) which is then raised to the level of the mill infeed
port and emptied into it. Weighing operations must, of course, take into account
both moisture content and the weight of packaging.

4) Observations on glaze grinding


From an energy viewpoint, grinding is the most costly task in the whole depart-
ment, with mills accounting for some 10% of plant electricity consumption. This
explains why grinding is generally carried out at night using cheaper rates.
With glazes, optimisation of grinding is near impossible because compositions
vary so much.
Nevertheless, much attention can and should be paid to the means that are at the
manufacturer’s disposal: water and additives. These are usually already included in
the formulation of the glaze and include CMC-based glues, various sorts of fluidi-
ser (STPP, hexametaphosphate, polyacrylates, etc.) and suspension agents (general-
ly NaCl).
Water also plays a key role: if it is drawn from the mains ionic exchange can,
where necessary, be performed; if, instead, it is drawn from a well it must be treated
according to its inherent impurities: sand or active carbon filtration, hydrocyclones
and/or ionic exchange may be required. In any case it is good practice to pass all
glaze water through a 63 micron sieve.
Using recycled water for glaze preparation or dilution is highly inadvisable: even
where this water appears innocuous it will still be characterised by very high con-
ductivity and a high content of rheologically active soluble salts with surface-
active agent characteristics.
Use of additives must be limited to the indispensable, because anything extrane-
ous to the formula itself generally creates problems during downstream stages of
the production process.
The grinding media load must be kept constant through the regular (weekly or
every charge) introduction of balls equal to the medium-to-large sizes of the origi-
nal charge.
Checks are carried out at least once a month by measuring the distance between
the surface of the load and the mill hatch.
Should the presence of contaminants be suspected (these usually show up on the
tiles as coloured specks), the mill must be emptied and the grinding media checked.
The latter can conceal a whole range of foreign bodies: coarse frit residue, alu-
minium (skeets or scoops), electrical wiring, various types of iron, plastic, wood,
etc. Checking the grinding media load, by emptying the mill, should be carried out

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methodically at least once every six-months. It is best not to remove the smaller
grinding elements via sieving at this time as this would disturb equilibrium, alter
grinding times and modify particle size distribution. Broadly speaking, grinding
times are regulated by setting mill running time or revolutions and depend on the
type of glaze being ground.
One of the most delicate stages of grinding is mill start-up, when the transmis-
sion belts are subject to maximum stress. Over the first 30 minutes this stress may
actually increase and if the belts are not properly tensioned, they can slip and wear
very fast. They can even overheat and catch fire, a scenario to be avoided at all costs
as the consequences are extremely costly. Hence mills must be started under the
control of qualified personnel. Anti-slip products to be sprayed on the belts at the
time of mill start are best avoided as they actually damage the belts.
Above all, when grinding coloured glazes, it is good practice to stop the mill and
clean any coarse residue from the fissure between hatch and lining as this traps
unground particles that can act as a contaminant.

5) Unloading the mill


Once grinding is over the mill is unloaded. Because this task is potentially danger-
ous certain precautions need to be taken: friction between the grinding media and
the glaze generates heat and temperatures as high as 35-50 °C may be reached, thus
raising in-mill pressure considerably. If the lid is removed without due caution the
pressure could eject it with considerable force. The mill operator must, therefore,
first vent the pressure via the bleed valve or vent the lid a little at a time by holding
it in place with the clamps.
The hatch is then replaced with a discharge port having a stainless steel outlet
valve and a coarse mesh to stop the grinding media being carried away by the out-
flow.
Once the mill has been rotated so that the discharge port is at the lowermost
point and the venting valve on the opposite side has been opened, the mill can be
emptied.
Following a quick residue check, the glaze is unloaded while still hot (i.e. under
optimum sieving and iron removal conditions). It can be passed through the finest
sieve possible (only if sieving time does not occupy the mill for too long) and then
pumped into holding tanks where it is checked again. These tasks can made easier
by using a mobile sieve and pump unit.
No attempt should be made to accelerate gravity-assisted drainage of the glaze
by pumping air into the mill: use of compressed air is strictly forbidden as mills are
not pressure-tested vessels. Once all the glaze has drained the mill is washed.
This delicate task has two important purposes: recovery of the glaze captured
by the grinding media and preparation of the mill for the next load without any
risk of contamination.
Achieving the former requires one or two washings with just limited quantities
of water. The first washing (about 100 litres of wash water) still contains a high
percentage of solids and can usually be added to the emptied glaze directly. The
second washing (700-800 litres of wash water), has a solids content of just 1-1.5%

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Glaze and decoration application techniques

(the first washing will already have recovered some 99% of the trapped glaze).
More thorough washing is only necessary following the grinding of very strong
colours.
With monoporosa and double fire glazes the use of only moderate quantities of
wash water is essential as these glazes must be applied at high density.
The glaze is then pumped into a holding tank and checked.

6) Feeding the glaze to the glazing line


The method will depend on the size of the glaze application department and its
location with respect to the glaze production unit.
Quite often the glaze is transferred from the main tank into smaller ones that are
then transported to the glazing department by fork-lift truck and positioned at the
point of use.
This practice is always used for flashing applications and intensely coloured
glazes or where the glaze preparation department is large enough to allow storage
of a suitable number of containers.
However, it is an inconvenient system in that there is a continual and dangerous
movement of trucks through often narrow passageways; bear in mind that the con-
tainers are bulky and require manpower. Moreover, it involves the laborious, time-
consuming task of container washing.
As an alternative glazes can be pumped from the preparation department into
intermediate storage tanks in the application area. When, for logistical reasons,
pumping is utilised, the system must be set up with care to prevent leakage, an all
too common problem.
Pipes should have a diameter of at least 2 or 3 inches (depending on length) and
should, at least along their initial tract, be made of stainless steel.
Each pipe can feed a number of tanks (usually 3): it should not have any ball or
throttle valves, but simply an initial gate valve and a pneumatic-type external valve,
fitted on the flex hose section at the end.
Piping may cover considerable distances, (100 metres or more), with each 100 m
tract containing some 250-280 Kg of dry glaze. Following an initial, vertical tract,
pipes must follow as steep a gradient as possible down to the discharge point within
the limitations of building height.
Washing the pipes is not easy: pumping controlled quantities of water behind
the glaze is inadvisable because, given the considerable distances, the water tends to
mix and layer with the glaze, thus making it difficult to decide when the flow needs
to be diverted into the drains or sedimentation tanks.

7) Glaze storage
All glazes – especially alkaline glazes – are subject to hydrolysis. The migration
of soluble salts from the frits may cause serious defects on the finished tile. This
sometimes occurs on monoporosa and fast double firing products, yet can also gener-
ate various degrees of pin-holing on other glazes.
Glues also deteriorate rapidly, losing their characteristics and thus causing ser-
ious application difficulties.

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For many glazes, then, high temperatures (during summer) and lengthy storage
times are the ceramists feared enemies.
Hence it is best not to rely too much on leftover glazes that have been in stock for
a long time just because “they were all right before”. Overstocking certain glazes is
therefore inadvisable and manufacturers must always make sure that glazes are used
in the order they were produced.
Recovery of altered glazes is, in monoporosa and fast double firing plants, ex-
tremely difficult.
The altered glaze can usually be mixed with fresh-prepared glaze to reduce solu-
ble salts.

Preparing screen printing pastes

Recent years have seen the widespread adoption of screen printing techniques.
First used with glossy single fire glazes, screen printing soon spread to rustic pro-
ducts, its popularity being aided by the rapid evolution of graphics.
Screen printing and, for some years now, flexography, provide excellent repeata-
bility and let manufactures renew their product ranges with relative ease.
Over time screen printing has come to be characterised by a constant reduction
in applied weights: before such improvements the most commonly used floor tile
screens fell in the 30-50 wires/cm range and wall tile screens were generally 50
wires/cm. This meant high glaze consumption and the appearance of black core
problems on single fire products caused by the presence of organic vehicles.
This in turn, meant slower firing cycles and poor decoration definition (especial-
ly with graduated shades).
Serigraphic paste preparation techniques were very approximate. The ground
base was generally purchased from colour suppliers and then, once mixed in with
the vehicle and the necessary additives, passed through a grinder. From here it was,
at best, screened in a rotating scraper sieve at 5-6,000 mesh/cm2 (75-80 microns)
before being deemed ready for use.
More sophisticated serigraphic techniques and materials will be discussed in
greater depth further on.

The glazing department

The glazing department is usually situated between the pressed tile drier outlet
and the kiln feeders (or, in double firing, between the two fires, possibly being pre-
ceded after the first fire and followed before the second fire by storage systems).
Proper spacing apart of the various application stations along the glazing line is
essential.
The floor, which must have a non-slip surface, must slope towards drainage chan-
nels so that glaze spills are collected. Lighting must be adequate.
The department must also be equipped with shelving for storage of the seri-

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Glaze and decoration application techniques

graphic screens, the visual check panels (one per line) on which production samples
and standard tiles are displayed, and an area for small spare parts storage and minor
maintenance work.
In a properly managed glazing department, the fast flow of defect information is
essential. Defects do not necessarily show up on selected test samples, hence moni-
toring at the kiln outlet is also required as is continuous statistical tracking of such
defects.
Other important elements in a glazing department include:

Electrical system
The power supply on the glazing line itself should not exceed 50 V (if no diffe-
rential safety device is used).
The lines are supplied from overhead 380 or 60 V cables.

Compressed air system


Compressed air requirements vary enormously from one glazing line to another,
generally ranging from 100 to 300 m3/h per line.
This air is used to power spray guns, pneumatic controls (on screen printing
systems), fixative application systems (though these can use high pressure airless
pumps) and tile surface blowers.
The compressed air feed line generally consists of a 1” pipe supplying air at 6-8
Atm.

Water supply system


There are normally two water circuits in the glazing department, sometimes
three.
One circuit is generally fed with water from a well or mains pipe and is usually
used to dilute the glazes; the second is recycled water for washing purposes.

Fume aspiration system


Extraction of the fumes that form inside the application units is essential as they
contain glaze particles.
Proper modulation of shutters and, therefore, extraction performance inside the
glazing units (especially disc and spray gun units) not only safeguards worker health,
it also shields the tiles themselves from certain application defects: lumps, glaze drop-
lets, condensate.
An individual glazing line generally requires a fume aspiration capacity of some
8,000-10,000 m3/h.

Data gathering system


The glazing line must be equipped with sensors that allow manufacturers to
monitor efficiency and other important production control parameters.

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Speed
Conveying speeds are in the order of 20-25 m/min, but may reach 60 m/min
along certain tracts (e.g. the gap preceding the box storage system).

Glaze application and glazing lines

Once prepared, glazes can be applied to dried, single fire tiles (now almost
universal) or biscuit (double fire) tiles in a variety of ways. The successful out-
come of unfired tile glazing largely depends on dried tile bending strength, as the
tile must be strong enough to withstand multiple applications/decorations without
breaking.
Applying an engobe (a semi-glaze composition) under the glaze is useful in that
it limits degassing phenomena and also prevents the glaze coming into contact with
contaminants in the body.
A uniform film of suitable engobe is sometimes applied to the back of the
tiles to stop direct contact with rollers and so reduce the rate at which dirt
builds up on them.
Generally speaking, a glazing line consists of a belt conveyor: a feeder is instal-
led at one end of the conveyor and a collection unit at the other, with the application
stations in between.
Tiles are conveyed on trapezoidal cross-section belts, preferred because they are
easy to clean, have a limited tile-belt contact area and are versatile.
The belts are supported by pulleys mounted on a metal support frame. This
conveying system works as a series of interconnected sections each independent
from the other in terms of speed (e.g. different speeds may be required during tile
preparation, glaze application, decoration operations etc.).
In addition to actual application units, conveyor lines may also include auxiliary
equipment items such as compenser units (which automatically allow tile collection
and release), turntables to rotate the tiles 90°, spacers, side guides, tile cleaning
devices (fans, brushes, suction units), scrapers, etc.
The main glaze application devices are:
a) bell unit
b) waterfall unit
c) rotating discs
d) spray guns
e) drop feeders
f) dry application units.

Bell unit
Essentially a convex metal dome. As the glaze runs off its surface it forms a
constant, uniform waterfall-like curtain. Glaze is applied to the tiles by passing
them through the curtain
The glaze, which can be relatively dense and viscous (1950-2000 g/l) tends to
deposit in slightly greater quantities on the sides of the tile.

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Glaze and decoration application techniques

The size of the bell on an individual glazing station depends, of course, on the
size of the tile being produced (fig. 2).
Bell units are the most widely adopted continuous application solution, allowing
manufacturers to obtain very smooth surfaces, a prime requisite for certain tile types.
The glaze flows out of the apex of the bell, with feed parameters being adjusted
to suit the characteristics of the glaze being applied.
A circular ring bordering the top of the bell allows the user to apply one or two
coats simultaneously.
Once set up, the unit generally requires little monitoring but it does involve
numerous parameters.
One of the most common defects is the formation of bubbles or depressions
on the glaze surface. This defect has a number of possible causes: bubbling in
glaze transfer and agitation, erroneous fluidification, unsuitable viscosity and
density.
As the variables in play are so many, there is no easy solution to bell application
problems.
For example, high glaze density makes sieving difficult. It is now possible to
sieve as the glaze returns to its container using large-diameter 4000 mesh vibro-
sieves. The latter remove the lumps that sometimes detach from the figure-of-eight
container or from recycled glaze. Another problem is that bell units are adversely
affected even by slight vibration, so the bell support pole must be isolated from the
rest of the line.

Waterfall unit
Consists of a triangular hopper: the glaze flows out through a slot of adjustable
aperture, thus creating a “waterfall”.
Tiles are glazed by passing them underneath the waterfall. These units come in
different lengths to cover the full range of tile sizes.

Fig. 2. Bell unit (note – at right – the erroneous flow of glaze highlighted by the hole in the veil).

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The glaze feed unit is similar to the one used on bell systems: vibrosieve, hopper,
feed tube with flow adjuster.
Performance is sometimes undermined by waterfall obstruction problems, espe-
cially lumps in the glaze and air bubbles.
An excessively liquid glaze can also cause problems (irregular stripes): this de-
fect can be corrected by reducing the in-hopper load and narrowing the waterfall
slot.

Pressurised injection system


Glazes, or other slips (even where quite dense), can also be applied by way of a
recently developed technique that involves pressurised injection through newly de-
signed waterfall units.
This system, called Vela®, makes it possible to apply glaze more homogeneously
across the width, yet waterfall-type defects often remain.
A special feed system allows several coloured products to be introduced together
with the base glaze, thus providing a variety of decorative elements, the shape,
position and overlap of which can all be adjusted.
Where required, injection can be electronically controlled to ensure good repeat-
ability.
Blending the base glaze with the coloured injection products confers considera-
ble creative flexibility.
Manufacturers can also apply large quantities of material per unit of surface
area per unit of time, allowing them to build up layers of considerable thickness on
the tile.

Rotating disc system (single or double disc)


Applies the glaze by centrifugal force through packs of disks of varying diame-
ter (120-180 mm); they rotate at high speed, about 40-50 cm from the surface of the
tile.
Characterised by excellent flexibility, this system can apply glazes of greatly
differing densities and viscosities as well as those with coarser particles and also
provides very good flexibility in terms of applied quantity.
The discs are generally arranged as circular “packs”, fed axially via a holed
tube.
Drive transmission is provided by belts and pulleys of different diameters that
allow adjustment of disc RPM.
The latest versions feature inverter control, thus allowing more precise speed
and atomisation control.
Most packs have a rotation speed of 3000-4000 RPM; while higher speeds are
possible, wear rates increase accordingly.
Discs, while versatile, are not able to produce a perfectly smooth surface. More-
over, disc application is sometimes marred by defects such as:
– drops: these form as a result of incorrect glaze rheology, condensation, unsuit-
able booth configuration, clogged holes etc.
– lumps: caused by excessively fast drying of the glaze or excessively violent glaze

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Glaze and decoration application techniques

intake; may also derive from a low feed rate, inadequate for the size of the pack,
thus allowing the glaze to dry on the discs.
– stripes: weight too low, irregular disc rotation, erratic feed.

Attempts to prevent the formation of drops and lumps have, over the years, led
to the construction of booths of every possible shape and size (fig. 3).
The discs are fed at a constant flow rate by way of an aperture that is regulated
by an overflow control system and an adjuster valve.
The glaze is passed through mesh filters on the feed line and through vibro-
sieves on the return circuit.

Drop device
Applies rather large drops (approximately 1 cm in diameter) to obtain certain
(e.g. rustic) aesthetic effects. Drop applicators may be of the tube or cup type.
Tube feeders resemble disc units, but instead of a disc pack there is a 3-4 cm
cylindrical holed tube.
Cup feeders, instead, feature small, continuously fed crenelated cups, which
rotate around a vertical axis, throwing the glaze against the tiles in a way that
depends on the characteristics (density and viscosity) of the glaze itself, the shape
of the cups, their height, rotation speed and drive speed.

Spray gun
Allows the application of small quantities of glaze via an atomiser. Flashing
effects can be obtained by oscillating the guns (sometimes two differently oriented
guns are used in the same booth). Intensity could be varied by way of an inverter on
the feed pump.

Fig. 3. Disc application booth and close-up of lamellar disc pack.

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Where uniform flashing effects are required, constant glaze feed rates are essen-
tial.
Spray gun glazes, generally used at low densities, require certain rheological
properties to prevent the formation of lumps and drops.
With spray guns the main inconveniences are deformation of the jet (nozzle
dirty or damaged) and droplets which either run off the booth walls onto the tiles
or are carried away by the turbulence generated by the injected air.
To combat these defects a variety of differently shaped booths have been desi-
gned in line with a host of volumetric theories, thus leading to changes in wall
angles, positioning of intake ducts etc.
Air pressure, which needs to be kept constant, is generally kept in the 2-6 Atm
range.
High atomisation pressures provide finer droplets but also tend to pressurise
the booth, thus creating considerable extraction problems, with the aerosol (har-
mful to both workers’ health and the environment in general) exiting the apertu-
res.

Dry applicators
These are used to apply granular glazes (grains) with a vast range of particle
size distributions or various kinds of sands. The grains are re-circulated by way of
a pneumatic loop or a sealed-in cup elevator (the latter creates less dust).
The grains are loaded into a hopper; this is fitted with an extractor which causes
the glaze to fall as a uniform veil onto a roller, belt or distributor sieve (fig. 4). If
stripes or steaks – defects often stemming from errors at the hopper loading stage –
are to be avoided, the grain distribution system must work perfectly.
Before reaching the grain applicator, specific areas of the tile surface are coated
with a glue or wet glaze.
As the grains fall onto the tiles they adhere to the glue-coated areas only; excess
grains are then blown off the tile surface and returned to the feed circuit.
Because they mimic granite almost perfectly and most manufacturers feel that a
thick layer of glaze generally provides the product with a certain “added value”,
grain applicators are very popular (1985-2000).
Universal grain/powder applicators which provide streaked effects by using rol-
lers or embossed belts are also available.

Key units on the glazing line

Conceptually, the glazing line consists of a series of individual machines assem-


bled together to form modules which, in turn, make up the line. A description of the
main modules follows.

Wetting unit: in the traditional version, connected directly to the water mains, or
pneumatic version (minimum constant water pressure at least 1 bar). Mainly used on
double firing or airless-type single firing lines. A pump feeds up to 3 different appli-

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Glaze and decoration application techniques

Fig. 4. Dry grain/powder applicator.

cation points. Used on monoporosa and single fire lines where the engobe or glaze
is applied with a bell.

Glaze scraper module: this module is inserted some 12-15 metres after the last bell
application, thus allowing the glaze to dry.
The module consists of 2 glaze scraper stations (which scrape parallel sides of
the tile), 2 turntables and 1 fan.
Manufacturers use different glaze scraper types for single and double firing
operations. With the former, any flashing is cleaned off the sides with felt discs so
as not to wet the edges, while the latter employs water-bath rubber discs.

Screen printing modules: standard screen printing modules are 6-9 metres long
and consist of a fixative spray gun (traditional or airless), a compenser and the
screen printing unit.
The module may incorporate several drive units and usually has two air feed
points, one water feed point and a suction intake.

Tile back engobe applicator: applies engobe to the back of the tile; fitted on a mo-
dule about 3 m long. Recommended for use with all production technologies as it is
an effective way of protecting the kiln rollers.

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Other units

Rustic effect brushing unit: mostly used on lines producing single fire and porcelain
tiles with structured or relief surfaces.
The device consists of several abrasive discs or brushes generally positioned at
least 6 m downstream from a spray gun unit.

Bark effect discs: these may be modified traditional discs (the disc pack is replaced
with a holed tube) or special booths designed to confer a granito look.

Grain or powder applicators: generally positioned at the end of a line, 3 m after a


single or double disc unit. In this case the disc applies the glue that attaches the
grains to the surface of the tile.

The glazing line

Line composition varies as a function of production technology. The tables be-


low give a general idea as to how module compositions change accordingly.

SINGLE FIRE LINES

approx. length glaze applicators optional decoration optional


applicators
80 – 100 m 1 water spray 1 bell 2 serigraphic units 1 roller unit
3 double discs 1 single disc 1 serigraphic unit
1 spray gun 1 grain applicator

MONOPOROSA LINES

approx. length glaze applicators optional decoration optional


applicators
80 – 100 m 1 water spray 1 single disc 2 serigraphic units 1 roller unit
1 double disc 1 dry applicator 1 serigraphic unit
2 bells
1 spray gun

DOUBLE FIRE LINES

approx. length glaze applicators optional decoration optional


applicators
70 – 90 m 1 airless water spray 1 single disc 2 serigraphic units 1 roller unit
1 double disc 1 dry applicator 1 serigraphic unit
2 bells
1 spray gun

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Glaze and decoration application techniques

PORCELAIN FIRE LINES

approx. length glaze applicators optional decoration optional


applicators
60 – 80 m 2 double discs 2 flat serigraphic 1 drier*
units
1 application

* where soluble salts are produced.

Printing machines

Screen printing is the most common tile decoration system used by the ceramic
industry.
Its popularity stems from the fact that it allows manufacturers to obtain a large
number of identical pieces at high output rates.
Generally involving the use of a fabric screen, the system works by squeez-
ing the ink through the mesh of the open part of the fabric (which forms the
pattern) by means of a scraper blade, thus reproducing the same pattern on the
tile surface.
It is a technique that can be used both on fired tiles and dried pressed tiles (where
they have sufficient bending strength), above or below the glaze.
A silk screen printing station must have the following characteristics:
• high piece/minute output to match the output capacity of the latest generation
of presses
• versatility with regards to pattern/decoration types
• low running costs
• limited manpower requirements
• faithful image reproduction.

The most common printer types are:


• Flat (figs. 5, 5a)
• Rotary (fig. 6)
• Roller (fig. 6a)

The scraper blade (squeegee)

This is the blade that pushes the ink through the mesh of the fabric and brings
the latter into direct contact with the tile surface (except where the “contact” tech-
nique is used).
The scraper blade (or squeegee) is a flexible resin strip attached to a rigid support;
the profile of its edge (i.e. the part that touches the fabric) depends on the printing
technique.

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As it is subject to wear, which might ultimately lead to faults in the pattern


(stripes, colour changes), the blade edge must be kept sharp at all times.
The main printing parameters are:
• imprinting speed
• scraper pressure
• angle of imprint a (angle between scraper and screen).

Imprint angles, which depend on scraper flexibility, the pressure exerted and the
profile of the scraper edge, have an important influence on the quantity of applied
ink.
In particular, the lower the angle of imprint (soft, round-edged squeegees) the
more ink is deposited.

Flat screen printing

On flat screen machines the scraper can move both parallel and at right angles to
the glazing line during printing and pushes down hard on the screen as it not only
has to squeeze the colour through the fabric but also bring the latter into contact
with the tile surface (no-contact screen printing, see fig. 5).

Rotary printing machines

Rotary printing has provided an effective response to the limitations posed by


flat screen printing.
The principle uses patterns on a screen wrapped around to form a cylinder which
rotates over the tile passing beneath (fig. 6).
This system provides constant print speeds; thanks to an electronic sensor,
which signals the arrival of the tile and its position, screen speeds are varied to
make sure the start of the pattern coincides precisely with the leading edge of the
tile.
Compared to flat screen printing, the main advantage of the rotary method is
increased output capacity, mainly because the tiles do not stop but move through
continuously.
Another key feature of this machine is that the decorative pattern is spread over
the entire circumference of the cylinder/has more extensive distribution along the
cylinder circumference.
Increasing the number of designs on the same cylinder increases the possibili-
ties for product diversification.

That’s why, in so-called “random” printing, rotary printers provide a greater


number of graphic combinations compared to flat screen machines. Working condi-
tions being equal, rotary screens also last longer.

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Glaze and decoration application techniques

Fig. 5. Flat screen printing technique: 1) scraper blade, 2) ink, 3) screen, 4) frame, 5) tile.

Fig. 5a. Flat screen printer.

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T) conveyor belts
L) line belts
FT) photocell.

Fig. 6. Rotary screen printing: A) feeder, D) imprint roller, P) tile.

Fig. 6a. Roller printing machine.

Rotary screen manufacture can be carried out in two different ways:


1) The traditional way is to stick the film and impress it on the cylinder using
lasers, which align and sub-divide the pattern and define the exposure times; this
allows the screens to be impressed as they rotate, allowing for greater precision.
2) A more innovative solution impresses the fabric as it lays flat; the fabric is then

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Glaze and decoration application techniques

attached to the cylinder. This technique can be used with all rotary printers and
combines the excellent print definition typical of flat screens with the versatility
and durability of rotary systems.

A specially designed wrap-around unit allows screens to be fitted in the ceramic


production plant, thus saving on storage space, transport and disposal costs.

Since its introduction, rotary screen printing has evolved steadily and now al-
lows manufacturers to make prints that are as true as possible to the originals.

Roller decoration

Here, the images to be reproduced are engraved into a polymer or silicon cylin-
der with a laser; faithful reproduction of the original image is provided by digital
processing of the laser-engraved image, giving fine resolution, excellent uniformity
of colour shade, high quality definition and constant repeatability over time. Re-
petitive patterns, shaded effects and infinite reproduction of the original design
can all be obtained.
Development of standard laser engraving processes has led to the creation of
the High Definition (HD) system, a new technique that allows an image to be repro-
duced on a tile without a base screen or tilts as it is reconstructed point by point.
The absence of a screen eliminates all colour overlap problems and allows the origi-
nal image to be reproduced in the finest detail.
In fact, the main advantage of the HD system is that detail, instead of being lost,
is enhanced; moreover, softness of colour gradation makes this type of incision
especially suitable for marble-like effects, the detailed nuances of natural stone and
geometric patterns.
With rotary roller systems, the tile is decorated as it comes into direct contact
with the surface of the roller; they both move at exactly the same speed so there is
no need to stop the tile, thus speeding up the decoration process and reducing the
corner damage, cracking and other defects often associated with start-stop systems.
It is, then, a decoration system in which movement of all components – cylinder,
colour, pressed tile – is synchronised.
Silicon roller engraving creates cavities that contain the colour to be applied to
the tile; at every turn of the roller, even before it touches the tile, a scraper removes
any excess printing paste.
Two mechanisms release the colour from the cavity: the first is “assisted gravity”
whereby the low viscosity colour is transferred to the surface of the tile quickly by a
combination of gravity and the centrifugal action of the rotating roller; the second,
much more important, mechanism depends on the fact that the colour, when it comes
into contact with the tile, is absorbed by it and thus “sticks”.
Another key advantage of this system is roller durability, itself influenced by a
number of factors such as scraper pressure (silicon abrasion) and the nature of the
glaze (e.g. coarse glazes increase friction between cylinder and tile), especially its

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moisture content. A still-moist glaze can provide efficient lubrication for the silicon,
thus extending the working life of the cylinder.

Screen mesh types

Whether flat screen or rotary systems are used, it is the mesh that provides the
support for the image to be printed and the mesh which ultimately determines the
level of definition.
To be suitable for high quality printing, a mesh must have the following cha-
racteristics:
a) uniform weave.
b) high abrasion/wear resistance to withstand the mechanical stresses of the print-
ing process.
c) high tensile strength to withstand the stresses of print frame construction.
d) a fabric appropriate to the type of pattern/decoration and the quality of the tile
being produced (this involves such factors as mesh density, mesh aperture and
mesh thickness).
e) resistance to the chemical products used in printing (e.g. screen printing pastes,
water, degreasing agents).
f) elasticity so that the screen reverts to its original position after being stretched
by the scraper blade.
g) resistance to pressure and impact.
h) the mesh threads must swell as little as possible in order to prevent changes in
aperture and thus paste flow-through parameters.
i) it should adhere well to all photosensitive emulsions.

The range of meshes – the “instruments” by which passage and deposition quan-
tity of colour are controlled – is extensive, giving the user a vast choice in terms of
fabric, fibre and mesh density.
The most important factor characterising fabric type is mesh density (the number
of threads per unit of linear measure, usually per centimetre). It should always be
born in mind that “colour” deposit and consumption are influenced by mesh density
directly as the colour has to pass through the mesh.
As the mesh is the only support for the image, it must be of a density able to repro-
duce even the finest details. Thread diameter is also an important factor in this regard.
Another factor to be taken into consideration when choosing the fabric is mesh
aperture: this becomes crucial when using pastes with very coarse particles.
Fabric type is determined by thickness, a value that is a combination of mesh
density, thread diameter and on-frame fabric assembly.
Theoretical parameters regarding the maximum amount of colour (expressed
in cubic centimetres per square metre) left on the tile after the passage of the scra-
per blade, are referred to as theoretical volume of colour.
This varies from fabric to fabric and depends on mesh aperture and fabric thick-
ness.

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Glaze and decoration application techniques

Colour consumption/deposit is also influenced by other factors:


– on-frame fabric assembly
– screen manufacture and design technology
– hardness, profile, pressure and angle of scraper blade
– imprint speed
– fabric tension
– printing pressure in relation to machine type (flat or rotary)
– number of emulsion applications.

Fabric types
The following section takes a look at the fabrics most commonly used by screen
manufacturers, products with synthetic fibres capable of withstanding the mecha-
nical, physical and chemical strains of printing (fig. 7).

a) Polyester fabric
This fibre has good tensile strength and, consequently, has limited thread stretch,
thus making it ideal for high definition printing, where alignment accuracy is crucial.
It has excellent heat resistance and limited sensitivity to sharp changes in tempera-
ture and humidity. Polyester also has very good resistance to abrasion, solvents, min-
eral/organic acids and is insensitive to light. Monofilament (single wire) polyesters
provide excellent colour passage performance thanks to the smoothness of the threads,
hence screens last a long time.
It should also be pointed out that specially developed technical polyesters also
exist; these innovative products offer:
– homogeneous results that remain constant over time
– a longer screen life thanks to improved emulsion adhesion
– excellent uniformity and smoothness of the applied emulsion
– optimum image resolution and definition
– reduced work times as the fabric is self-lubricating, reducing screen cleaning
requirements considerably.

b) Nylon fabric (polyamide)


This highly elastic fibre provides excellent mechanical resistance, although this
does depend on the degree of extension and polymerisation. Another feature of

Fig. 7. Various fabric types (polyester, nylon and metallic wire).

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nylon is the fact that its tensile strength and stretch diminish as temperature in-
creases.
Highly resistant to abrasion, it is nevertheless, a material that absorbs moisture
easily, causing it to swell.
On account of their excellent elasticity, monofilament nylon meshes are espe-
cially suitable for printing on irregular surfaces.

c) Metallic or metallized fabric


Metallized high precision fibre is made by coating monofilament polyester with
metal (usually nickel). Dimensional stability makes it especially useful where high
registration accuracy is required; it differs from stainless steel meshes on account
of its elasticity. Surface conductivity prevents any electrostatic build-ups and the
metallized surface is also highly resistant to abrasion.
Consequently, it is ideal for use with the abrasive colours used in ceramics.
Since the colour passes through the mesh smoothly, it is possible to obtain prints
with extremely well defined edges.
The steel fabric is now used rarely because it has been replaced by new nylon
types.

The frame

The frame provides the necessary support for both flat and rotary printing scre-
ens and has a direct influence on screen quality (i.e. uniformity and constancy of
tension).
As it is subject to continuously changing chemical and mechanical forces, it is
best made of stainless alloy so rust does not cause catalytic damage to the mesh.
Two types are available:
a) steel, which offers the advantages of high specific weight, durability (where pro-
perly protected), relatively low costs and good mechanical strength; on the down-
side steel frames are difficult to handle where large and, unless coated with paint
or varnish, may rust.
b) aluminium, which has the advantage of being light, easy to handle, rust-resistant
and highly suitable for small and medium size frames; however, aluminium offers
only limited resistance to acids and alkalis, and is somewhat less appropriate for
large sizes in that it is not always rigid enough to withstand the tension of the
mesh itself. Aluminium frames are also relatively expensive.

Tensioning
This is one of the most important tasks in the preparation of a printing screen
frame, as it has a direct influence on final results. Only a correctly tensioned screen
will provide the desired outcome, namely:
– good mechanical strength
– optimum adhesion of the emulsion
– good image colour.

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Glaze and decoration application techniques

Tensioning may involve one of the following systems:


– pneumatic: clamps stretch the mesh to the required tension, control being effected
with an instrument that measures pressure (in Atm).
– mechanical: simple and manual, or more sophisticated, with an electric motor
coupled to an automatic programming system. Uses different lock systems such
as pins, bars and pincers, which hold the screen in place and cover its perime-
ter.

Good printing results depend on uniform tensioning of the screen right across
the entire area enclosed by the frame.
Workers can measure screen tension during frame preparation via the pressure
gauge on the pneumatic pincer tensioner: the pincers are worked by a pressure re-
gulator and the gauge itself.
Note that mesh producers supply fabrics complete with tensioning data tables:
this information is used to calibrate the tensioning machines accordingly. Tension-
ing measurements are expressed in atmospheres (bar).
More commonly, a tensometer is used. This is a small electronic or mechanical
instrument equipped with a blade that comes into contact with the mesh and measu-
res its tension (in Newton/cm).
Improper tensioning can lead to defects such as lack of multi-colour printing
alignment precision, shifting about of the screen, a “stretched out” image, premature
mesh wear and heterogeneous colours etc.

Emulsion

The emulsion (or gelatine) is a key component in the screen printing process. It
is spread over the tensioned screen with the aid of a scraper blade and the design is
impressed on it using a photoengraving procedure.
Note that until the mid-80’s meshes for the ceramic industry were made with a
chrome emulsion; this cost less but offered little resistance to the strains of the
printing process and was a source of serious water pollution. Since then, as part
of an effort to reduce environmental impact and meet the growing demand for
innovation, a diazo gelatine (a photosensitising agent) has been introduced into
the production cycle and adapted to the special printing needs of the ceramic
industry.
Still used for the production of printing screens, this article offers good photo-
sensitised product duration, high definition and is much more environmentally
friendly.
Technological and graphic developments in the ceramic sector, greater openness
to new applications and the need to respond to ever-greater demand for high quali-
ty have all led to the development of new emulsions with good printing resistance
and high definition.
These highly light-sensitive photopolymers provide fast incision, excellent defini-
tion and good resistance to the glazes.

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Photoengraving

Once the emulsion has been applied the frame-mesh assembly is left to dry be-
fore being photoengraved.
Exposure has a direct influence on definition, resolution of the finest details,
thickness and the chemical/mechanical resistance of the pattern produced in the
emulsion.
Correct exposure depends on two important factors:
– exposure time, essential in conferring quality and resistance
– intensity and quality of the light.

Keeping the light at the right distance during the photoengraving process re-
sults in homogeneous distribution over the entire surface area. However, if the light
source is too close the light tends to be concentrated in the middle, with diminished
intensity at the sides. Likewise, a light source that is too far away causes underexpo-
sure and areas with poor mechanical/solvent resistance.
Results also depend on photograph image density (which must maintain the fin-
est details), the thread density of the screen fabric and the characteristics of the
photosensitive emulsion (on the basis of which the exact UV exposure time needed
for complete emulsion penetration is calculated).
The most appropriate exposure time can, however, be found by effecting a series
of positive test exposures, increasing or decreasing exposure times until results are
optimum.
Another factor influencing exact reproduction of the design on the screen print-
ing frame is the subsequent development, which influences mesh aperture and thus
the passage of colour onto the tile.
A catalysing stage follows to reinforce the fabric.

Silk screen printing inks

These are pastes or liquids of varying viscosity, made up of solid particles dis-
persed in a fluid “vehicle” and any complementary substances that may be required.
Easily transferred onto the tile, they are deposited in layers about one tenth of a
millimetre thick.
The solid part consists of colorants that change into glass during firing.
Essentially crystalline or fluxing blends with oxidants and pigments, they are
prepared via a wet grinding/drying process.
The liquid part, which acts as a vehicle for the colorants, generally consists of
products such as glycol and polyethylene glycol, characterised by extensive tile co-
vering capacity.
Vehicles must have good binding, plastifying and stabilisation qualities; those
vehicles with better adhesive performance, especially suitable for use with single
fire products, can be prepared with carboxymethyl cellulose in solution, to which
polyvinyl alcohol, glycols or polyglycols are added.

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Glaze and decoration application techniques

The solid base is generally prepared by way of a wet grinding method similar to
that used with glazes; it is then dried gradually (using an optimised thermal cycle),
powdered and stored.
Thus obtained, the powder is then mixed and homogenised with the liquid vehi-
cle.
Mixing usually takes place in an agitator, with a certain powder weight being
added to a pre-determined quantity of vehicle.
The paste is then put through final refinement, a procedure that may involve a
series of machines (sieving units, cylindrical refiners or roll mills, grinding refiners
or micro-ball mills).

Mixing the paste

Once each of its components has been accurately weighed, the paste must be
homogenised before it can be put through the refinement procedure.
Mixing takes place in simple cylindrical containers equipped with slow-stir pad-
dles and outflow valves on the bottom.
Examples of various screen printing paste compositions used with different pro-
duction technologies are given in the table below.

Double fire Monoporosa Single fire Porcelain tile


paste paste paste paste
Base frit Transparent Transparent Transparent Transparent
~ 1030 °C ~ 1120 °C ~ 1180 °C ~ 1200 °C
Frit % 95 95 95 95
% Kaolin 5 5 5 5
Colouring pigments 0–50 out of 0–50 out of 0–50 out of 0–50 out of
100 100 100 100
Vehicle: base 20-100 out of 20-100 out of 20-100 out of 20-100 out of
(media) 100 100 100 100

Refinement

Performed with the aid of several different machines. Refined pastes must have
the following characteristics:

Flat Rotary Roller


Residue % at 45 mm 0 - 0.2 0 - 0.2 0 - 0.2
Density g/l 1500 - 1700 1500 - 1700 1500 - 1600
Ford Viscosity at Ø 4 > 150” > 150” 25 - 30”
mm Ford

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Refinement of the screen printing paste (or ink), once carried out in simple grind-
ing units which did not always provide efficient dispersion, is now carried out in
more sophisticated machines such as micro-ball mills. The latter are made up of:
– a cylindrical tank with a sealed lid.
– a grinding chamber lined with hard alumina containing 5 mm grinding balls.
– a sealed motor, the shaft of which has two rotors positioned at different heights
in the tank; the bottom of the grinding chamber acts as a centrifuge.

The roughly mixed screen paste is introduced into the tank and from here is
aspirated into the grinding chamber via a circular aperture.
Most grinding takes place in the peripheral zone, where grinding energy is max-
imised by the centrifugal forces acting on the balls and the paste. Driven by the
centrifugal force, the paste is circulated through helical fissures on the bottom of
the tank.
The ceramic quality of the ink is checked by way of sampling procedures which
involve both individual raw materials (frits, colorants) and the paste: the latter gen-
erally requires adjustment to maintain desired chromatic effects.

Screen printing vehicles (medias)

The vehicle acts as an ink solvent, transforming the powdered colours into a
fluid suspension.
From a ceramic viewpoint, such substances are of extremely limited importance
in that they do not actually influence the final product. Yet from a printing stand-
point they play a key role in establishing the characteristics of the ink and ensuring
good image reproduction.
The most commonly used vehicles are glycols and polyglycols with an ethylene
oxide, propylene and polymer base.
These commercially available chemical composites have high powder wetting
capacity, are optimum binders and disperse the colour perfectly, creating a mass of
good flowability that sticks to tile surfaces well. Vehicles are mixed with dry powders
in ratios that depend on the specific application technology.
Optimum print conditions must be tested in a production context.
The dry base/vehicle ratio can be varied within the following intervals:
– flat or rotary screen printing: base 20-100, vehicle 100.
– roller screen printing: base 80-120, vehicle 100.

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Glaze and decoration application techniques

SCREEN PRINTING DECORATION TECHNIQUES

On-glaze decoration

The most important factor influencing this type of decoration is the moisture
content of the glazed surface on which the image is to be printed; if it is excessive
it may cause “stickiness” between glaze and screen, resulting in clogging of the
mesh.
If, instead, the glaze is too dry, it diminishes cohesion between the glaze and the
underlying layers, causing the former to “dust” the screen (i.e. stick to it); fixatives
normally provide an easy solution to this problem.
Glazed surface moisture content largely depends on the time that elapses be-
tween glaze application and printing (line length and conveying speed), the nature
of the glaze (composition and particle size distribution), the porosity of the tile and
the presence of under-glaze decorations.
Drying times are best modified by adjusting line speed (maximum speed is defined
as the speed at which tile breakages begin to occur) and glaze composition: to adjust
the latter the percentage of plastic substances (kaolin, clay) is usually altered, or addi-
tives are used.
Drying times can also be adjusted by making slight changes to glaze grinding
parameters, taking care not to alter post-firing properties. In any case, this approach
is much less effective than the first two.
In addition to the moisture content of the glazed surface, another factor which
influences on-glaze decoration is scraper blade pressure; if it is too low decoration
may be imprecise or incomplete; if excessive the first colour may stick to the screen
of the second application; if inconsistent it may lead to deposits of varying thick-
ness that result in non-uniform colour shades.
Identical defects may have a number of different causes; for example, a colour
may stick to the underside of the next screen if application stations are too close
together or if the first ink has an excessively long drying time. Imprecise/incom-
plete decoration may be caused by faulty screens, an excessively wide screen-tile
gap or improperly levelled tile guides.
Variations in decoration thickness are caused by differences in squeegee speed,
tiles of non-uniform thickness, worn screens and variations in the composition and/
or viscosity of the ink.
Other possible defects include the differences associated with use of colour re-
agents (caused by absence of parallelism between the screen planes and the scraper
blade) and streaks or stripes (blunt scraper blade or worn screen).

Under-glaze decoration

This type of decoration is applied directly to the tile, which must be cleaned and
sprayed with a thin film of water beforehand so as to even up wettability and water
absorption.

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It is also good practice to apply a preparative undercoat to provide a base for the
screen printing ink.
In addition to the above-described defects (encountered with on-glaze decoration)
small dimples, holes or cracks may appear at decoration points, especially where deco-
ration layers are very thin.
These problems may be caused by excessively large grains (inefficient powder
grinding) or very slow drying which causes the ink to be repelled.

Colour gradation

Graduated colouring is reproduced on the screen by creating a set of points of


various shape, size and arrangement.
Graduated decorations, whether printed on top of the glaze or directly on the
tile, require particular attentiveness in the choice and preparation of materials (es-
pecially the screen printing glaze), the type of scraper blade and above all, the type
of mesh.
The glaze should be fine-ground to residues of about 0% at 16,000 mesh/cm2,
while the scraper blade should be sharp edged so as to obtain maximum image
resolution with minimum wear: the blade should also be fairly hard.
The mesh – which must have a highly regular weave – should be selected on the
basis of tests aimed at optimising the results required in final production.
Generally speaking, the best fabric for this sort of application is polyester with a
density of 100-120 threads/cm.
Note that this type of decoration, when printed directly on the unglazed tile
surface, highlights defects such as a scratched surface; hence it is good practice to
equip the press with mirror dies.

Plain tiles

When a large number of tiles are to be printed all the same colour, the surface
on which the colour is to be applied must be perfectly uniform, clean and free from
even the slightest defects.
If printing on top of the glaze it is essential that the latter does not transfer dust
onto the screen.
A dust-contaminated tile surface can cause colour variations, “shadows” and/or
pin-holing.
Once again, polyester screens are to be preferred on account of their dimensio-
nal stability over time (density should not exceed 77 threads/cm).
Silk screen printing pastes should have good flow properties so that the spaces
corresponding to thread cross-overs are filled in.

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Glaze and decoration application techniques

Colour overlap

Overlapping two colours will evidently produce a third one. Screen printing al-
lows manufacturers to take advantage of this simple concept and thus generate a
number of colours far greater than the number of actual application stations.
In general, decorations of diminishing thickness – in any case very thin (60-70
threads/cm) – are applied so as to aid drying and allow the use of soft scraper
blades; fluxing colours are sometimes used on top of refractory colours.
When printing directly on the surface of the tile it is possible to overlap two
colours and insert a layer of transparent glaze (crystalline) between them.

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Glaze and decoration application techniques

Chapter VI

FIRING

General

Firing is, perhaps, the most important stage of the whole production process as
it actually creates the ceramic material by transforming the raw materials in the
body into new crystalline and vitreous compositions that confer key properties: in-
solubility and solidity to maintain shape, bending strength, porosity or impermea-
bility, resistance to chemicals etc.
Firing also causes the vitreous coating to melt and form a continuous layer that
is solidly anchored to and interlocked with the tile body, thus providing the required
chemical, physical and aesthetic characteristics.
Firing consists of heating, and thus transferring energy, to the pressed, dried tile,
up to a fixed temperature for a set time, so that chemical and physical transformations
cause the body and glaze to acquire the properties required of the final product. In
the past the target temperature, the firing time and the firing methods were decided
on the basis of experience; nowadays the same parameters are established on the
basis of chemical knowledge, an understanding of the technical behaviour of the
relevant raw materials and preliminary analyses of the latter, especially thermal
analyses (see Volume 1).
The equipment available to the modern producer allows him to control manu-
facturing conditions ever-more precisely and effect the finely-tuned firing cycles
that are indispensable for standardised mass production.

The transformations that take place during firing

Firing takes place by introducing heat into the kiln interior and thus into the
ceramic products themselves.
Heating increases the vibration amplitude of the atoms in the material, thus
causing it to expand.
The extent of this expansion depends on the chemical nature of the material, its
crystalline or vitreous structure, their relative quantities and the transformations
that take place during heating; it has been demonstrated that crystalline composi-
tions expand more than vitreous ones, just as compact structures expand more than
porous ones.
As firing progresses, certain compounds in the materials disappear and new ones
are created; these changes show up as expansion or shrinkage.
The exact nature of such phenomena depends on the initial composition of the
body, the transformations that occur, and in-kiln temperature; this explains why

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bodies can behave so differently during the first and second firings even where the
achieved final temperature is the same: the thermal expansion generated during a
first firing is irreversible while that of a body which has already been fired and
heated is reversible (fig. 1).
Another physical transformation that takes place during firing is the melting of
the fluxes in the body and glaze compositions. In the ceramic industry eutectic mixes
are melted to allow the creation of a liquid phase at temperatures lower than those
actually needed to melt the individual materials; it has been shown that the more
numerous and complex the eutectics among the oxides supplied by the raw mate-
rials, the more easily the composition melts.
When melting takes place, it counteracts the previously described expansion,
and causes a series of closely correlated transformations: reduced porosity à in-
creased density à solid-solid and solid-liquid reactions à improved technological
properties.
As temperature rises so the quantity of molten material increases steadily, si-
multaneously resulting in a reduction of system viscosity. Gradual softening of the
tiles and a series of events associated with the formation of the liquid phase follow:
infiltration of the liquid into the cavities of the mass, solution of the granules,
diffusion of dissolved material throughout the rest of the liquid phase, crystalliza-
tion of the solute in equilibrium with the solvent once saturation point has been
reached.
Simultaneously, there is an increase in reactions caused by the reduced viscosity
of the piece, making control of the material vitrification curve (shrinkage and ab-
sorption of water as a function of temperature) more difficult and possibly leading
Expansion (‰)
Expansion (‰)

Fig. 1. Unfired and fired tile expansion curves.

208
Firing

to curvature defects (e.g. pyroplastic deformations) caused by the imperfectly leve-


led support surface of the tile as it advances on the moving rollers.
With glazes the composition is richer in fluxing agents and nearly all the mate-
rial is transformed into a liquid of a certain viscosity: some substances, added for
the purpose of creating certain effects such as glaze opacity, or pigments intended
to give colour, may remain undissolved.
Infiltration, dissolution, diffusion and crystallization also occur in the glaze-body
contact zone and are responsible for the creation of an intermediate layer which
anchors the glaze to the body.
The depth of this layer depends on the refractoriness of the body and its perme-
ability (fig. 2).
As firing progresses and kiln temperatures increase, the material passes through
a number of critical thermal zones, generally defined by the chemical reactions that
take place within them:
– up to just over 100 °C: hygroscopic water is eliminated (this is the moisture
content left behind after imperfect drying or water reabsorbed during glazing or
from the environment).
– up to 200 °C: the zeolite or crystallization water, the molecules of which are
bound by absorption into the crystalline structures, are eliminated.
– between 350 °C and 850 °C: combustion of organic substances in the clays and
oxidative dissociation of the mineral sulphides (e.g. Pyrite FeS2) with freeing of
sulphur dioxide.
– between 450 °C and 650 °C: elimination of structural water and consequent
destruction of the clayey crystalline lattice.
– at 573 °C: allotrope transformation of quartz α to quartz β, causing a sharp
increase in volume.
– between 800 °C and 950 °C: decarbonation of limestone and dolomite with free-
ing of CO2.
– above 900 °C: formation of new crystalline phases made up of SiO2, silicates and
silica-aluminate complexes.

Fig. 2. Intermediate layer anchoring the glaze to the tile body.

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– above approximately 900 °C: thermal dissociation of other salts such as sulpha-
tes and fluorides.
– if temperatures exceed 1000 °C some body and glaze components such as alka-
line oxides, lead oxide, zinc oxide and boric oxide may evaporate.

During cooling the molten materials provide both body and glaze with cohesion
and solidity.
This consolidation may – depending on the components in the molten material
and the cooling parameters – lead to the formation of vitreous and/or crystalline
structures. In ceramics, the two circumstances usually co-exist in that the molten
material is made up of several components. The ions of certain molten materials,
owing to the loss of solubility caused by the drop in temperature, settle according
to the geometry of their crystalline structure, while the rest of the liquid solidifies
to form a vitreous phase in that cooling times, while lengthy, are not long enough to
allow its complete crystallisation.
With glazes the molten glass becomes progressively more viscous and takes on a
paste-like aspect; simultaneously, it contracts.
Yet because it has attacked and penetrated the surface porosities of the tile it
remains securely anchored to it. Initially the glaze shrinks but, as it is highly vis-
cous it adapts to the tensions that arise between it and the tile; once the vitreous
transition point has been passed, the glass “locks” and if its shrinkage subsequently
fails to match that of the tile, tensions may arise and generate defects such as cra-
zing or flaking. Such tensions sometimes remain hidden and only show up later
(latent crazing).
Another physical phenomenon caused by increased temperature is the reversible
polymorphous transformation that changes quartz α into quartz β (at 575 °C) and
then, at even higher temperatures, into tridymite and cristobalite. These trans-
formations entail structural rearrangements, expansive during heating, contractive
during cooling.
While the overall structure of the tile is, during heating, still elastic and loose
enough to absorb expansion without too much difficulty, the contraction associated
with the quartz β à quartz α transformation during cooling takes place in a tile
that is already rigid and rich in new fragile phases: cooling cycles therefore need to
be planned carefully, especially around these temperatures.
The same argument applies to materials that have already been fired to a high
degree of vitrification and are then fired a second time: in this case similar pre-
cautions need to be taken during pre-heating.
Applying heat energy to the raw materials causes them to decompose; the
compounds that arise from these reactions then become the reagents responsible
for the formation of the minerals that constitute the final ceramic article: these
changes occur at different temperatures as a function of the energy needed to
trigger them.
Such reactions can lead to the formation of compounds in a gaseous state, which
have a tendency to escape via intergranular interstices: a suitable degree of tile
compaction is, then, essential, as it not only optimises sintering but also provides

210
Firing

the permeability needed for expulsion of these pyrolysis and oxidation gases while
allowing gaseous exchange with the in-kiln atmosphere (especially the air and the
oxygen it contains).
In fact, the gases cointained in the in-kiln atmosphere can react with materials
in the body, the glaze and even the products of those same reactions.
The air is usually directed so as to steer reactions in the desired direction; for
those transformations that generate gas or require oxygen air flows are designed to
aid gaseous turnover and create an oxidising atmosphere.
Vice versa, when an oxygen-poor atmosphere is required, or when the level of
oxides needs to be reduced, air circulation can be decreased and/or substances that
produce reducing gases such as CO and H2O are introduced into the firing atmo-
sphere.
This can be done by varying air inflow via regulation of the burner’s secondary
air ducts or by modifying the relative gas pressure settings in the various kiln sec-
tions (keeping settings stable by increasing or decreasing pressure in different parts
of the kiln).
For example, as seen, organic substances burn between approximately 300 and
850 °C, producing carbon dioxide and water vapour; if heating is gradual, air circu-
lation is good, surface vitrification does not take place and combustion is completed
at around 800 °C, resulting in minimum residues and fine porosity.
Vice versa, if heating is too fast the organic substances could undergo distilla-
tion accompanied by the production of carbon and other reduction products, which
blacken the tile (black core defect).
Only at higher temperatures does the carbon react with the surrounding oxides
which reduce as follows (Me = generic metal):

Me2O3 + C à 2MeO + COá or MeO + C à Me + COá

These reactions involve gaseous formation of carbon monoxide and cause a colour
change towards grey-black, local increase of volume in the mass and local over-firing.
Within the same temperature interval (350-500 °C) oxidation of the pyrite (possibly
present as an impurity) begins, being completed at higher temperatures:

FeS2 + O2 à FeS + SO2 á


4FeS + 7 O2 à 2Fe2O3+ 4 SO2 á

If the atmosphere is oxidising the sulphur dioxide changes into SO3 and, in re-
acting with the basic oxides (CaO) of the body and the glaze, sulphates may be
formed:

CaO + SO3 à CaSO4

The presence of calcium sulphate in the fired tile is damaging as it could dis-
solve in the water contained inside the body and appear as saline efflorescence: this
emerges on the surface of the pre-fired biscuit and can also cause glaze detachment.

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Decomposition of alkaline earth carbonates involving the release of carbon di-


oxide and the formation of the metal oxide takes place between 650-950 °C: the first
to decompose are the magnesium carbonates, followed by calcium ones (for a same
type, the imperfect or non-crystallised structures decompose first and then the well
crystallized ones):

CaCO3 Æ CaO + CO2Ç

As this is a reversible reaction, decomposition is aided by elimination of the


products from the kiln atmosphere: good air circulation and the presence of clayey
minerals that react with the calcium oxide by forming silicates and calcium silica-
aluminates aid gradual, total dissociation of the carbonate with completion of its
fluxing action.
Fine particle size distribution also aids decomposition: coarse limestone particles,
in fact, decompose only superficially or, in any case do not allow the calcium oxide
to fully react with the other oxides.
The constitution, at high temperature, of neo-formed crystalline composites such
as silicates and calcium silica-aluminates can cause the body to expand, thus counter-
acting the shrinkage that occurred previously during the destruction of the crystal
lattice of the clayey minerals.
This increase in volume remains after cooling and explains why products with
these body compositions, when fired at the above temperatures, do not shrink in size
but, rather, expand.
Thanks to the presence of feldspars rich in alkaline elements, the liquid phase
formed at high temperatures is initially very viscous and this allows the products to
maintain their shape well.
Viscosity then decreases as temperatures rise further (this change in viscosity
occurs faster in sodium bodies than potassium bodies).
Feldspars are thus the vehicle of that vitrification which characterises products
with low porosity: the liquid phase, in fact, fills the pores and, as temperature increases,
absorbs the clayey mineral oxides more and more, causing considerable shrinkage
and increase of density within the mass.
Once the liquid saturation point has been reached, the needle-like mullite crystals
and aluminum silicate separate, intertwining with each other in the vitreous body to
form a structure of high bending strength.
This type of mullite (known as secondary mullite) is typical of bodies with a
high alumina content, such as porcelain (50% kaolin, 25% quartz, 25% feldspar),
fired at very high temperatures (1350 °C) with the formation of an abundant liquid
phase.
Crystallisation persists as long as the liquid has sufficient fluidity.
As regards glazes, compositions consisting mostly of frits do not involve any
particular chemical reactions in that these occur during fritting (melting tempe-
rature in frit kiln higher of 250-400 °C). Glaze compositions with a higher raw
material content have a reactivity that depends on the chemical nature of the mate-
rials themselves: sometimes the formation of eutectic mixes causes fusion, while in

212
Firing

The mullite formed in a porcelain body - S primary mullite, A secon- Viscosity of feldspars as a function
dary mullite formed from the feldspathic vitreous phase, V vitreous of T.
phase, Q dissolving quartz granule.

Fig. 3.

other cases dissolution of the materials takes place without them undergoing chem-
ical transformations (e.g. frit to which compounds such as zirconium silicate and
quartz have been added). The most significant chemical reactions concern the form-
ation of new compounds which crystallise in the vitreous mass (making the glass
opaque or the surface matt) or those that give rise to formation of colorants or
certain decorative effects.

The firing cycle

As firing progresses the product is exposed to different temperatures of varying


duration: this temperature-time sequence constitutes the firing cycle.
In ceramics a firing cycle is divided into at least three stages:
a) heating, up to a maximum temperature that optimises the required ceramic pro-
perties (determined via trials): the rate of temperature increase is adjusted ac-
cording to parameters intrinsic to the material and kiln performance.
b) holding (or “soaking”), at maximum temperature: duration depends on the size of
both product and kiln; the larger the tile, the greater the need to homogenise the
temperature in order to ensure that the required physical and chemical trans-
formations take place.
c) cooling to ambient temperature: occurs at a rate that takes into account the sensi-
tivity of the tile to thermal gradients; other needs must also be considered (e.g.

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at this stage it may be necessary to aid crystallization phenomena by slowing


down the cooling rate within certain temperature intervals).

Depending on whether they are endothermic or exothermic, the chemical and


physical reactions triggered by firing cause further temperature changes within the
body, changes that must be allowed for by firing cycle planners.
Generally speaking, decomposition and dehydration reactions and phenomena
leading to a more or less condensed state (e.g. fusion or evaporation) are endother-
mic; oxidations, combustions and the switch from a disordered to a more ordered
state (as in crystallization) are exothermic transformations.
Within certain temperature intervals tensions can arise within the piece and it is
here that the temperature increase/decrease rate (∆T/time = thermal gradient)
should be slowed down accordingly, while other intervals may permit much faster
temperature change rates.
Attainment of appropriate firing cycles (i.e. temperature-time curves) is depen-
dent on a thorough understanding of firing phenomena and the temperatures at
which they are triggered.
Yet heating gradients and soaking times depend not only on factors concerning
the material; of equal importance are the size of the tile (i.e. different cycles for
differently sized tiles), load parameters (the heat spreads more efficiently if load
density is lower) and the heat diffusion rate of the material given its surface area,
thermal conductivity/specific heat and density.
Planning a firing curve is thus the difficult art of reconciling kiln productivity
with product quality.
For centuries kilns with huge chambers – and lengthy firing times – were used
to homogenise heat penetration into the product and so eliminate any internal ther-
mal gradients.
Towards the mid-70s, with the advent of single-layer roller kilns, industrial firing
times were drastically shortened (to just a few tens of minutes).
Nevertheless, studies on rapid firing have shown that even where heating rates
are accelerated the chemical-physical transformations are “delayed” because of
the gradient that forms between the temperature of the kiln and that of the pro-
ducts.
This phenomena is explained by the fact that it takes time for the kiln heat to
spread uniformly through the product mass. It has also been demonstrated that
such temperature differences can be diminished by increasing heat transmission
coefficients in the material.
Thus the practice of holding maximum firing temperatures once they have been
achieved is as valid in fast firing as it is in slow firing because it homogenises tempe-
ratures and allows reactions to progress and complete.
Rapid firing has led to radical changes in kiln loading, kiln structure and the
formulation of both bodies and glazes.
Tiles subject to rapid firing are introduced into the kiln in a way that maximises
the surface area exposed to the heat; tiles are arranged in a single layer so that they
can receive heat from every direction as uniformly as possible.

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Firing

Heating/cooling rates are slowed down only within critical temperature in-
tervals (as explained above) while for other intervals steep gradients can be
used.
Kilns are now made of refractory materials of low thermal inertia which accu-
mulate little heat, the latter being well distributed throughout the kiln by a series of
burners.
Thanks to these modifications manufacturers are able to keep output levels high.

Different types of firing

Firing can be performed in a variety of ways that depend on the sort of product
being manufactured.
Firing may involve the tile body, the glaze and decorations or glaze and body
together.
The first involves firing of the dried tile, the second the firing of the glaze – as
part of a double firing process – and the third the single fire process (fig. 4).
Body firing involves attainment of temperatures that determine the final quali-
ties of the product (i.e. bending strength, porosity or impermeability, colour). For
certain items such as terracotta, refractory, red gres, unglazed klinker and unglazed
porcelain tile this fire is the first and final one.
In the double firing process the first fire represents only the initial stage of heat
treatment, conferring the solidity, bending strength and chemical-thermal inertia
needed at the glaze application stage.
Once the glaze has been applied the tile can be re-fired at even lower temperatu-
res (usually 30-40 °C less, to prevent the vitreous glaze being affected by any reac-
tions originating from the body).
This process concerns faience, earthenware and soft porcelains (i.e. wall tiles and
low compaction/cohesion tableware).
Single firing allows manufacturers to obtain the desired body and glaze proper-
ties simultaneously.
This technique offers significant advantages, both economic (faster production
process, lower capital investment, energy and labour requirements) and technical
(during firing an intermediate layer forms between glaze and body, thus improving
body-glaze adhesion).
However, the advent of this new firing technique, back in the 70s, necessitated
changes to both plant hardware and body/glaze formulation.
The body necessitates a composition that is, already in its unfired dried state,
solid and strong enough to withstand the stresses of moulding/pressing, glazing
and decorating; during firing it must release a minimum quantity of gas before the
glaze becomes completely molten so as to prevent the formation of bubbles and
pin-hole defects.
The body must also maintain open porosity up to about 800-850 °C to allow
gaseous exchange with the in-kiln atmosphere and thus prevent black core pro-
blems.

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Curve in presence of black core


Temperature (°C)

Lower zone

Upper zone

Firing time (min.)

Fig. 4. Vitrified material firing curve (single firing).

Finally, the body must be formulated so as to minimise the shrinkage that can
cause distortion of decorations.
The glaze, which also includes decoration, must be of a composition that “ma-
tures” at the same temperature at which the body attains its final characteristics,
must melt when the body has already ceased to generate gases and must spread and
level quickly so as to coat the tile evenly; moreover, it should not be affected by the
gases/steam in the kiln and must be aggressive enough to react with the body and
form the intermediate layer.
The “hardware” changes brought about by single firing largely involve the kiln
and automation both upstream and downstream from it.
For instance, storage and handling systems for glazed-decorated materials
(waiting to be fired) and kiln feeding/unloading units have been extensively auto-
mated.

Fuels

The heat needed to fire the tiles is normally produced by burning solid, liquid or
gaseous fuels or even by using electricity.
Combustion is a fast oxidation reaction and thus exothermic enough to be used
for the production of heat. Because of this reaction the fuel, made up of compounds
such as carbon, hydrogen, sulphur, carbon monoxide, hydrocarbons, combines (follow-
ing ignition) with oxygen in the air to produce reaction products and heat.

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Firing

C + O2 → CO2↑ + 94.2
94,2 kcal/mole
CH4 + 2O2 → CO2↑+ 2H2O↑ + 192 kcal/mole
H2 + ½O2 → H2O↑ 58.6 kcal/mole
+ 58,6

The heat triggers and continues the combustion. In terms of commercial worth,
the main thing that differentiates fuels is their calorific value; this depends on the
composition of the fuel and is defined as the quantity of heat (kcal) liberated on
complete combustion of 1 Kg of solid or liquid fuel or 1 m3 of gaseous fuel (see tab.
1).
During combustion some substances may subtract heat by activating endother-
mal processes such as changes of state (e.g. liquid-gas) or simply by heating up (e.g.
the nitrogen in the combustion air).
For the fuel to express its full calorific value it needs to be mixed as well as
possible with the combustion air; the latter must also be present in quantities at
least equal to the theoretical values indicated by the combustion reaction.
In practice, apart from situations that require a reducing atmosphere, imperfect
mixing with combustion air can be compensated for by adding excess air: this sur-

Density High-Cal. Low-Cal. Oxygen Combustion


Molec.
Gas Symb.
W. Kg/Nm3 value value requirement products
Kcal/Nm3 Kcal/Nm 3 CO2 H 2O N2
Hydrogen H2 2 0.090 3050 2570 0.5 2.38 - 1 1.88
12.770 10.760
Methane CH4 16 0.717 9520 8550 2 9.52 1 2 7.52
39.858 35.797
Ethane C2H6 30 1.356 16820 15370 3.5 16.66 2 3 13.16
70.422 64.351
Propane C3H8 44 2.019 24320 22350 5 23.80 3 4 18.80
101.823 93.575
Butane C4H10 58 2.703 32010 29510 6.5 30.94 4 5 24.44
134.019 123.552
Ethylene C2H4 28 1.261 15290 14320 3 14.28 2 2 11.28
64.016 59.955
Propylene C3H6 42 1.915 22540 21070 4.5 21.42 3 3 16.92
94.370 88.216
Butylene C4H8 56 2.501 29819 27840 6 28.56 4 4 22.56
124.808 116.560
C. Oxide CO 28 1.250 3020 3020 0.5 2.38 1 -- 1.88
12.644 12.644
Oxygen O2 32 1.428
Nitrogen N2 28 1.250
Carb. Dioxide CO2 44 1.997
Sulph. Dioxide SO2 64 2.926
Water H2O 18 0.804
Dry air -- 29 1.293

Tab. 1. Properties of gases involved in combustion under normal conditions (0 °C, 760 mm Hg, dry).

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plus is in the order of 40-150%, 25-60% and 10-50% for solid, liquid and gaseous
fuels respectively.

Gaseous fuels are particularly advantageous in that they blend completely with
the air, hence combustion can occur with air quantities only slightly above theoreti-
cal levels. Moreover, they can be burnt close to the products without causing any
damage, do not produce ash, do not need preheating and thus burners of relatively
simple design can be used.
Gaseous fuels provide very high temperatures because of their high calorific
value and because pre-heated air can be used; they also make control of heating and
the in-kiln atmosphere more efficient.
Natural gas is a mix of methane, ethane and limited quantities of other light
hydrocarbons: it is found both in gas-only deposits and in oil deposits as a gaseous
phase.
Having a calorific value of around 8500 kcal/m3, it burns with a very pure flame
and contains negligible quantities of sulphur. It is thus the most commonly used
fuel in open flame kilns (where combustion gases come into direct contact with the
product).
Generally supplied to factories via pressurised piping, it goes through an inter-
mediate decompression stage before reaching the burners.

Liquid fuels also have certain advantages: easier batching and distribution through-
out the various kiln sections, good mixing with the combustion air by way of atomisa-
tion, limited ash production, small efficient burners.
To ensure efficient combustion two fuel-air mixing methods may be used:
– atomisation of the liquid in a fan-blown air stream (the most widespread sys-
tem)
– the liquid is vaporised by using a part of its own combustion heat.

The liquid is atomised by pumping it into a duct which ends in a nozzle. Burners
may be fitted on the walls or the roof of the firing chamber; in the latter case
burners that inject a given quantity of fuel at set time intervals are used.
Ceramic kilns can also use liquid fuels such as the so-called “light oils” and oil
distillates, generally available as either kerosene or naphtha: the latter is usually
preferred on account of its price. Combustion is generally good, yet the combustion
system as whole is an expensive one and maintenance is more frequent than with
natural gas systems.
At ambient temperature “heavy oils” generally have the consistency of tar and
must therefore be preheated to at least 60 °C to make them fluid enough to circulate
through the ducts and then heated to at least 110 °C to ensure good atomisation.
Combustion is poorer and produces a considerable quantity of carbon residues, sul-
phur dioxides and other pollutants.
Because of these problems heavy oils are only used where better fuels are either
unavailable or unaffordable.
Where fuels of better quality are unavailable, it may also be possible to use “poor”

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Firing

gases of low calorific value, such as gases derived from the treatment of coke, or
mixtures of hydrogen, methane and CO etc.
The most suitable liquid fuel for modern burners is undoubtedly liquid petro-
leum gas (LPG). It is clean, of high calorific value and, in most cases, requires
burners similar to those used with natural gas; however, storage and distribution
systems are required, and a good understanding of its technological behaviour is
necessary as it is commercialised in liquid form but used as a gas. This necessitates
the installation of special vaporising units (electrical or with burner). Feeding the
fuel that spontaneously evaporates inside the tank directly to the kiln is not feasible
as it is impossible to keep the composition of the gas consistent (the more volatile
elements evaporate first).
To stop the fuel entering the distribution network while still in its liquid state
and prevent any ice forming when the fuel is decompressed to the standard 500-600
mm H2O, it is good practice to follow the values given in the following tables (tables
2 and 3).

Mains By-weight percentage composition of LPG (propane/n-Butane)


pressure Propane n Butane
BAR 100/0 0/100
90/10 80/20 70/30 60/40 50/50 40/60 30/70 20/80 10/90
0.5 6 6 6 6 6 6 9 12 15 18 21
0.75 7 7 7 7 7 9 12 16 19 22 25
1 8 8 8 8 9 13 16 20 23 26 29
1.5 9 9 9 10 14 19 22 26 29 32 35
2 10 10 10 15 20 24 27 31 34 38 41

Tab. 2. Minimum LPG temperatures and pressures in burner feed lines.

3 3
Gas (m ) produced by the stoichiometric combustion of 1 m
Gas of gas with (dry/humid) air.
CO 2 N2 H 2O Totale
Methane 0.998 / 0.998 7.470 / 7.470 1.934 / 2.046 10.491 / 10.603
Ethane 2.011 / 2.011 13.174 / 13.174 2.924 / 3.121 18.266 / 18.463
Propane 3.052 / 3.052 19.041 / 19.041 3.945 / 4.229 26.265 / 26.549
Butane 4.147 / 4.147 25.226 / 25.226 5.025 / 5.401 34.698 / 35.074

Tab. 3. Combustion products.

The temperature of the gas depends on by-weight percentage composition of the


LPG, expressed as a mixture of propane and n-Butane and the effective pressure
upstream from the kiln control unit (expressed in bars).

Example: if the LPG is made up of 30% Propane and 70% n-Butane, and the pressure
in the feed line is 1 bar, the temperature of the incoming gas must not be less than 20 °C for
the safety margin to be acceptable. With the same composition at a pressure of just 0.5 bar, a
temperature of 12 °C would be sufficient.

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Where LPG is used its by-weight composition is not always known and varies
over time: hence it is always advisable to use pressures of around 0.5 bar to prevent
the formation of liquid phases or ice in the equipment or system.

CERAMIC FIRING KILNS

Heat exchange

The kiln is the machine in which the tiles are fired to obtain the desired product
characteristics. During the various stages of firing heat exchange takes place between
the heat sources, the fluids, the kiln structure, the products being fired and the at-
mosphere surrounding them: this involves conduction (of limited importance), con-
vection (the main form of heat transmission) and radiation (relevant only in the
high temperature zones).

Heat transmission by convection

Convection transports the heat via air circulation (hot air rises, cool air descen-
ds), transmitting a quantity of heat which, other conditions remaining equal, is:

Q = ρ . S . ∆T

where S is the surface area in contact with the heat, ∆T is the temperature diffe-
rence between ceramic body and gas and P represents a convection coefficient whi-
ch varies widely depending on circumstances: this coefficient also indicates how
heat exchange depends, to a limited extent, on the temperature difference between
the air and the heated solids, while controlling the movement of that air is, instead,
very important for heat exchange. Air circulation depends on the position of the
heat source with respect to the fume intake duct, high speed burners and forced-
draught circulation fans.
Convection is also aided by loading the tiles so that the air can circulate freely
between them; also, mounting high-speed burners on opposing kiln walls in a stag-
gered pattern aids convection by producing turbulence and gas circulation at right
angles to the direction of product feed.
Heat is also propagated by way of radiation, transmitted via the infra red rays
emitted by all hot bodies. The quantity of heat emitted depends on temperature as
per the following equation:

Q = σ (T24 – T14)

where T2 and T1 are the temperature of the emitting (usually flame or in-kiln
walls) and the receiving material (usually tiles or cooling air) respectively.

220
Firing

Logically, the higher the kiln temperature the more important this phenomenon,
to the extent that in some cases, especially where flames are in the immediate vicini-
ty of the tiles, their surfaces are protected with refractory material. Heat transmis-
sion by radiation is typical of muffle kilns and where products are contained in
saggars. It is, in fact, the refractory material that radiates its accumulated heat to the
tiles.
Radiation can also be used to accelerate cooling of items that have been fired at
high temperature. In this case the radiation given off by the bodies is captured by
silicon carbide tubes (with a high infrared absorption capacity) through which am-
bient air is circulated.

Kiln construction

Today, the most common type of tile firing kiln is the single layer type, where just
one layer of material is passed through the kiln on a set of rollers. Its length corre-
sponds to the required firing time. Double layer roller kilns are still used as they
require less space (fig. 5).
On entering the kiln the tiles are fed through zones of steadily increasing temp-
erature (preheating) until they reach the maximum temperature zone. Subsequently
the tiles enter a fast cooling zone where the gradient flattens out a little to prevent
problems associated with the presence of quartz and steepens again until the kiln
outlet, where temperatures vary between 40 and 60 °C. The firing cycle is defined
as the time taken by the tiles to travel from one end of the kiln to the other and,
together with cross sectional load capacity and number of channels, is a key deter-
minant of output capacity.
The tiles usually pass through the kiln at constant speed.

Fig. 5. Double layer roller kiln.

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Generally, tiles are transported through the kiln on rollers. The kiln is divided
into modules, each about 2 metres long, assembled end to end; they are made of
tubular frames and sheet metal panels which support the insulating layer, made of
refractory brick and insulating mortar on the floor and refractory slabs and Z-blocks
on the walls and roof. Fig. 6 shows how kiln insulation consists of layers of diffe-
rent materials and illustrates the resulting insulation performance.
Module composition varies enormously depending on production requirements:
in general, single fire tile production involves kilns 60-120 m long, with effective
cross sections of 1.3-3 m (usable area of 80-360 m2), sub-divided, approximately, as
follows:
Pre-kiln (10% of total kiln length)
Preheating (31%)
Firing (19%)
Fast cooling (6%)
Slow cooling (20%)
Final cooling (14%)

Fig. 6. Illustration of kiln wall showing thermal insulation.

222
Firing

The vertical cross section of the chamber is kept to an absolute minimum so as


to accelerate fume speed and thus increase fume-tile heat exchange. Air flow is pro-
vided by fans (there are usually six) which have, starting from the kiln infeed, the
following functions:
– fume exhaust
– combustion air input
– rapid cooling air input
– slow cooling heat exchanger exhaust
– final cooling hot air exhaust
– final cooling cold air input.

Fig. 7 shows side view, plan and cross-sections for a typical single layer kiln of
the latest generation.
This diagram also illustrates the efficient use of combustion gas; in most kilns
the firing zone is characterised by a flow of fumes that runs against the direction
of tile feed, the fumes being exhausted through the main stack located in the kiln
entrance zone.
This set-up is of prime energy management importance because it allows the
heat generated in the firing zone to be used for preheating purposes; where toxic or
undesired emissions are present in the preheating zone, they are sent to the stack
directly for depuration treatment.

Combustion system

Gaseous or gassified fuels such as methane and LPG are burnt directly in the
combustion chamber and then expelled as fumes into the kiln interior. The burners
mix the fuel with air drawn in through ducts by fans. Such air may be defined as
either primary (the burner comburent air) or secondary (used to fine-tune the firing
atmosphere).
In most cases, however, fuel-air mixing takes place directly at the nozzles: by
varying the diameter of the primary combustion chamber outlet different cross-
sectional heat distribution patterns can be obtained.
The extreme temperatures in the combustion chamber necessitate utilisation of
specially designed materials, such as silicon carbide (SiC) or sometimes SiSiC. Adju-
sting the air flow makes it possible to obtain hot gases that exit the burner at
speeds of 100 m/s and more, producing directional jets than maintain uniform
temperature along almost their entire length, which usually corresponds to kiln
width. As the burners are arranged in an alternating, staggered pattern above and
below the rollers, fume turbulence is maximised, thus ensuring maximum heating
uniformity.
The traditional burner modulation systems are:
– fixed air / modulated gas
– modulated air / modulated gas.

223
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Kiln stack Firing Fast Slow Final


pre-heating section cooling cooling cooling
section

Fig. 7. Side view and plan of single layer kiln showing how cross section changes from zone to zone.
Firing

In the former the quantity of air arriving at the burner, once adjusted, remains
constant independently of changes in load or anything else which might alter the
temperature in the firing zone: temperature settings are maintained via gas modula-
tion only. With this system, it is obvious that the burner will operate at a correct
gas/air stoichiometric ratio only within a narrow operating range, as the most com-
mon situation is one of excess air. This system is of simple design, gives good
pressure stability in the kiln where there are gaps in the load, yet is costly in terms
of fuel consumption.
In the latter both gas and air can be modulated (at a constant ratio) to compensa-
te for gaps in the in-kiln tile load or other factors that might alter temperatures in
the zone.
Temperature is maintained by varying air and gas flows simultaneously and con-
sequently acting on the volumes inside the kiln. Note also that with this system the
burners generally operate at a stoichiometric ratio which optimises fuel consump-
tion.
However, negative aspects such as pressure instability caused by gaps in the load,
greater constructive complexity and difficulties in avoiding temperature peaks can
cause serious problems, especially where kilns are particularly wide and long.
High output (wide infeed) kilns and very fast firing cycles demand narrow tile
size tolerances. Consequently the use of pulse-type systems with burners stagge-
red on opposing kiln walls and adjustable flame distribution systems, which use
refractory ducts or deflectors, are becoming increasingly common. Both these solu-
tions optimise heat control, which, thanks to the development of ever-more reliable
control electronics and measuring systems, limit temperature fluctuation to just a
few degrees Celsius, thus providing excellent results in terms of wall to wall hea-
ting homogeneity.
To sum up our description of the combustion system it should be pointed out
that enormous efforts have been made to reduce energy consumption. This is high-
lighted by the simple fact that in 1980 it took 967 Kcal to produce 1 Kg of 300 ×
300 mm glazed tiles with a water absorption of 5-6%, while today just 450-500 Kcal
are needed.
One simple, highly effective solution in this regard is use of pre-heated combu-
stion air. Even where air is heated to just 100 °C fuel savings are in the order of 5-
6%. More radical heat recovery (from the cooling zone) allows combustion air to be
used at temperatures as high as 230-250 °C, resulting in savings of some 12-14%
(see tab. 4). Without entering into the merits of different plant layouts, the fol-
lowing table shows specific consumption for a kiln with a 2.5 m wide infeed and a
total length of 110 m, a 47 minute firing cycle, Tmax 1220 °C for the firing of porce-
lain tiles, shrinkage 8%, weight 20 Kg/m2, output 6400 m2/day (5350 Kg/h fired
product):
The heating sequence and the corresponding kiln structure can be described in
terms of the reactions that occur at certain temperatures. The following paragraphs
chart the progress of the tile through the various kiln zones.

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COMBUSTION
TEMPERATURA
AIR
ARIA 30 °C 100 °C 160 °C 220 °C
TEMPERATURE
COMBURENTE
SPECIFIC
CONSUMO
CONSUMPTION
SPECIFICO 485 456 440 420(-(–13.4%)
420 13,4 %)
Kcal/Kg unfired)
(Kcal/Kgcrudo)

Tab. 4. Specific consumption in a single layer kiln as a function of combustion air temperature.

1 - Pre-kiln
This is the kiln inlet, designed to eliminate any residual hygroscopic water left
behind by the drying process, picked up during glazing or absorbed following unsu-
itable storage: maximum permitted water content is 2% by weight. Here, elimina-
tion of the zeolite water in the clay also begins.
This part of the kiln does not usually have its own heating apparatus, but relies,
instead, on transfer of fumes from the downstream firing zones via stack ducts
located above and below the pre-kiln rollers. Temperature is monitored by a ther-
mocouple in the roof.
Pre-kiln temperatures range from 200 to 500 °C, but considering the speed of
the cycle and the endothermal nature of evaporation the material itself reaches
temperatures of just 50-200 °C.
The only temperature regulation device is an air intake located in the roof and
floor of the pre-kiln, adjustable by way of a gate valve. The vertical height of the
kiln interior at the early end is minimised so as to accelerate fume speed and conse-
quently increase fume-tile heat exchange.
Both walls and roof are insulated with rigid slabs made of special fibres, ancho-
red to the metal frame of the module. The floor, instead, is shielded with harder
insulating bricks capable of withstanding the wear generated by the periodic re-
moval of tile debris.

2 - Pre-heating
Here, the key event is the degassing of the ceramic body, indispensable for the
prevention of swelling, bubbling and cratering of the glaze/body and colour alte-
rations.
The relevant temperature range depends on the type of product being fired and,
even more importantly, the type of glaze. Conceptually, preheating ends where glaze
melting begins and the surface porosity of the tile begins to drop, causing a sudden
fall in gas permeability.
Pre-heating temperature ranges may be in the order of 500-700 °C or, if the
glaze is of good quality, 500-1000 °C. For exceptionally high-fluxing bodies and
glazes it may extend as far as 1100 °C.
Pre-heating also involves the delicate allotrope transformation of quartz α in
quartz β. This must be completed without the tension generated by the sudden
increase in the volume of the ceramic body causing any breakages: in short, prehe-
ating must be efficient and suited to the characteristics of the tile.
The pre-heating zone has a series of burners, mounted on the walls above and

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Firing

below the rollers. Kilns for the second glaze fire do not have burners below the
rollers, except in the firing zone. The burners are sub-divided into several multi-
burner sets on two kiln modules, staggered symmetrically along the right and left-
hand sides of the kiln.
Burner sets above and below the rollers are always adjusted separately.
Compared to the pre-kiln, the pre-heating section is higher and modules are
larger as they require thicker insulation. The innermost layer of the walls is made
of insulating brick and a secondary layer of fibre. The roof is lined with lightwei-
ght refractory blocks, anchored by metal couplings to the tubular structure on the
module frame. In addition to the blocks there is also a second layer of refractory
fibres and a third layer of insulating cement.
The floor consists entirely of various types of insulating brick or compressed
refractory. To shield it from any mechanical impact, the floor is lined with thin, dry-
mounted tiles made of dense refractory materials. Wall insulation is completed by
plugging the roller seats with insulating fibre.

3 - Firing
This is where temperatures breach the 1000 °C barrier and are at their maxi-
mum.
Insulation: the innermost layers of the wall are made of refractory-insulating
bricks of maximum refractory performance; insulating fibres complete the shiel-
ding. Note that insulation thickness varies as a function of the temperatures re-
quired for specific product characteristics. To insulate properly at temperatures of
1100-1250 °C three different layers of insulation are used, thus providing good kiln
performance at optimised running costs.
The entire firing zone is equipped with wall-mounted burners both above and
below the rollers.
It is in the firing zone that virtually all the final size, flatness, vitrification and
glaze characteristics of the tile are established. Hence fine temperature control and
a perfectly flat roller plane are essential, as tiles can soften considerably.
The influence of the adjoining cooling zone also needs to be attenuated: this is
achieved by inserting two barriers at the end of the firing zone, each consisting of
a wall that cuts off the lower part of the firing channel between floor and rollers
and rigid insulating fibre slabs (chicanes) inserted through an aperture in the kiln
roof to divide the channel above the rollers.
Inserting similar barriers in the firing or pre-heating zones, while often a source
of frequent and sometimes costly maintenance work, rarely gives appreciable re-
sults. Hence they are only installed where essential (e.g. in very short kilns or kilns
for products with special requirements).

4 - Rapid cooling
This phase covers the interval between maximum firing temperature and about
600 °C.
The process is designed to cool the tiles as fast as possible, but must not continue
to the point at which allotrope transformation of quartz takes place (573 °C).

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Because this stage involves a sharp drop in temperature and the return of both
body and glaze to a solid state, it is undoubtedly one of the most critical in the
entire firing process. Rapid cooling is achieved by way of blower pipes housed in the
walls, both above and below the rollers: the air exits the pipes and enters the kiln
chamber where required via a series of aligned holes, which ensure even air distri-
bution over the load and are generally made of austenitic steel or, where exposed to
very high temperatures, silicon carbide.
Temperature control in the fast cooling zone is provided by thermocouples in-
stalled both above and below the rollers.
Equally important is the heat exchanger, consisting of a series of steel pipes
running transverse to the kiln below the roof; the air flowing through these pipes is
actually the combustion air on its way to the burners.
Hence the exchanger has the dual function of cooling the tiles and pre-heating
the burner combustion air, normally to 100-120 °C.
At these temperatures the air is already sufficiently expanded, is moisture-free
and thus will not damage the kiln interior in the event of a burner shutdown.
Wall insulation in the rapid cooling zone consists of an initial layer of refractory-
insulating brick and then a layer of insulating fibre. Insulation is thinner here as a
result of the relatively low temperatures.

5 - Slow cooling
This is the stage at which the highly delicate allotrope transformation of quartz
takes place, an event that involves a sharp decrease in the volume of the ceramic
body.
As the above subtitle implies, cooling must proceed slowly and gradually so that
this transformation takes place simultaneously throughout the tile: otherwise the ten-
sions generated in the already-rigid ceramic tile can easily reproduce the characteri-
stic “cracking” which, in medium-high vitrification, gives the fracture a smooth, shiny,
conchoid look with sharp edges.
Temperatures in this part of the kiln are in the order of 600-450 °C, correspon-
ding to actual tile temperatures of 700-500 °C.
Heat exchange is provided by a nest of tubes running widthways beneath the
roof of the kiln; a fan draws in cold ambient air and circulates it through the tubes.
The flow is routed so that air in adjoining tubes flows in opposite directions. Some
tubes can be excluded by closing valves on the hot air ducts.
As in the pre-kiln, the roof of the kiln is lower and the modules are smaller
because lower temperatures require thinner insulation. The roof chamber is insula-
ted with rigid fibre slabs anchored to the module frame while the walls are insulated
with brick on the innermost layer and then fibre; the floor is made of insulating
brick.
In this part of the kiln the refractory plays a secondary heat insulation role, by
ensuring that temperatures remain sufficiently high when there are gaps in the tile
flow. The end of the slow cooling zone is marked by two transverse barriers, po-
sitioned closely together.
Both consist of a wall sectioning off the below-roller level and austenitic steel

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Firing

slabs slotted through apertures in the kiln roof above it; the extremities of these
chicanes are hinged so that accidentally overlapped pieces can pass through.
The purpose of these barriers is to control air counter-flow in the final cooling
section.

6 - Final cooling
At this point the tile has passed the critical quartz transformation point. Final
cooling is thus designed to lower the latent heat of the product as much as possible.
Cold air is introduced directly above and below the tiles by blower sets consi-
sting of holed triple-tubes running widthways. Flow rates on individual sets can be
adjusted by means of a gate valve on the air feed system.
A second fan withdraws the air that inevitably heats on contact with the tiles,
removing it via ducts in the kiln roof fitted with adjustable throttle valves.
These intakes extend into the slow cooling zone: one is positioned between the
two barriers separating the slow and final cooling zones and another is located
upstream from the barriers themselves: this last intake is useful when the kiln is
being heated and in establishing the necessary equilibrium regarding air volumes
flowing towards the firing zone.

Roller drive units


The rollers are generally driven by a gear transmission system, usually a worm
screw driving an angular gear.
The series of motor gears is fixed by grub screws to a steel shaft, one for each
kiln module. The drive shafts in two, three or four modules can be coupled to-
gether.
The shaft (or group of shafts) is driven by a gearmotor and chain transmission
system. Speed is adjusted automatically by software. Motor reducers piloted by fre-
quency modulators are also becoming common.
All gears are shielded by sealed casings which also act as oil bath sumps.

Circulation of air volumes and pressure in the kiln


Balancing the air volumes in the kiln is of considerable importance, as implied
by the sheer size of the fans. The combustion air fan, the fast cooling fan and the
final cooling air blower all introduce significant volumes of air into the kiln. Simi-
larly, the fume fan and hot air removal fan in the final cooling zone extract signifi-
cant volumes.
The fume intakes at the start of the pre-kiln are arranged symmetrically above
and below the rollers (see first cross section in fig. 7). They are not angled towards
the incoming fume flow: they simply generate a vacuum towards which the fumes
flow automatically.
Intake flow is adjusted – individually above the rollers and as a set below – by
throttle valves: these allow the user to balance flows and depressions above and
below the rollers.
The fume fan flow rate can be adjusted in several ways: usually, a manually con-
trolled throttle valve is installed upstream from the fan intake. Alternatively, valves

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Applied Ceramic Technology

can be adjusted by servomotors (controlled via the kiln control panel) or frequency
modulators (inverters) on the fan itself: these systems may also include an automa-
tic kiln pressure adjustment device.
An ambient air intake on the fume stack is also present: this is usually a manual
throttle valve and allows fume temperatures to be lowered when excessively high
for the fan; it also acts as a fine adjuster of exhaust fume quantities.
However, the systems which distribute fume suction between the above-roller
and under-roller sections are of limited efficiency: even when some 10-12 metres
from the intakes the fumes already tend to follow the “natural” route above the
rollers. This tendency is aided by the intercommunication afforded by the inter-
roller gaps (where uncovered by tiles).
The exact amount of combustion air supplied to the burners (quantities usually
vary between 5 and 35 m3/h) depends on requirements. Dilated by the high tempe-
ratures, this air represents a significant proportion of the volumes that need to be
evacuated.
To these volumes at least a part of the fast cooling air is added; the air blown
into the fast cooling section is partially or wholly exhausted by the fume fan or the
hot air intakes in the final cooling section.
Where removed by the fume fan this air has a positive effect on fuel consumption
because it is already heated (so less cold air is fed to the burners) and provides good
oxygenation in the kiln interior (fig. 9).
Where, instead, it flows towards the final cooling zone in the same direction as
the tiles, this air can be of considerable importance in keeping the kiln interior hot
in the event of extensive gaps in the tile load; this protects the leading row of tiles
in the kiln from the effects of the volume changes associated with the quartz tran-
sformation (fig. 8).
The quantity of air introduced is modulated automatically so as to maintain
correct temperatures in the fast cooling zone; consequently, especially where tile
feed is discontinuous and thermoregulator default parameters are not optimal, kiln
pressure may oscillate. The final cooling air is blown in through widthways blower
ducts arranged both above and below the rollers. The air exits through blowholes
positioned perpendicular to the tile load.
This final cooling arrangement optimises efficiency and enhances the opportuni-
ties for energy recovery as air volumes at 110-160 °C are easily employed elsewhere.
Pressure is important for kiln regulation purposes but does not, in itself, have
much influence on firing results (except for planarity).

Combustion air Cooling air

Pre-kiln Preheating Firing Fast Slow cooling Final cooling


cooling

Fig. 8. Air circulation with partial exhaust of cooling air.

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Firing

Combustion air Cooling air

Pre-kiln Preheating Firing Fast Slow cooling Final cooling


cooling

Fig. 9. Air circulation with conveyance towards main stack.

When a kiln pressure reading is taken it only refers to a single point in the entire
firing channel: bear in mind that pressure is at its minimum at the fume extraction
points in the pre-kiln and at maximum in the fast cooling zone on account of the
large volumes of air being introduced. Within a given zone, pressure is higher at
the roof level, minimum at floor level, the differences often being considerable. For
purposes of convenience, kiln pressure is detected at the burner level, above the
rollers just before the last firing zone module.
Another, less technical yet more practical and meaningful method consists of
localising the ± 0 pressure point between the partial vacuum of preheating and the
pressure of the firing zone.
The following diagram illustrates how pressure changes from zone to zone
(fig. 10).
In any case, kiln pressure should not exceed a limit of approximately 0.3 mm
and draught should be balanced so that fumes produced in the firing zone are not
drawn towards the kiln tile outlet: the latter can increase fuel consumption and
cause degassing problems in pre-heating.
cooling
Slow
air
Pre-heated

air
Combust.
stack
To the

cooling
Final
cooling
Fast
air output
Cooling

Preheating Firing Fast Slow Final


cooling cooling cooling

pressure

partial vacuum

Fig. 10. How pressure varies in the various kiln zones.

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Controls

Proper running of a ceramic kiln involves a whole range of controls: composi-


tion of fumes exiting the stack, composition (or at least oxygen content) of the
atmosphere in the kiln, fan speeds and flow rates etc. Yet the key parameters re-
quiring monitoring are pressure and temperature.
Pressure can be controlled with simple instruments that indicate the low levels
of pressure/vacuum in the various kiln zones. Simple glass-tube manometers, with
one end open and in communication with the ambient atmosphere and the other end
connected to the firing chamber by a special heat resistant tube, can be used. Even
water can be used as a filling medium, the difference in level with respect to equili-
brium indicating the degree of pressure or vacuum. Inclined-tube manometers, which
operate according to the same principle, are also used and give good resolution (up
to 1/20 mm).
Several temperature monitoring instruments exist, each using different princi-
ples of measurement. The main problem is getting an accurate picture of how the
heat is distributed between the tiles and the kiln structure, in that measurement
generally takes place without direct contact because the tiles are moving and the
firing chamber is large and sealed.
One of the simplest and most widespread high temperature measurement devices
is the thermoelectric pyrometer, also known as a thermocouple; this consists of two
dissimilar conductors joined together at their ends which, by way of the Seebeck
effect, generate a thermoelectric voltage between the two junctions proportional to
the temperature difference between the junctions.
Different types of metal are coupled depending on the temperature interval being
monitored. Up to 600 °C a copper and copper/nickel alloy match is usually em-
ployed; up to 1000 °C chrome/nickel alloy (cromel) and aluminium/nickel alloy
(alumel) are used, while for higher temperatures, up to about 1600 °C, various plati-
num alloys with rhodium (Pt/Pt-Rh) are preferred.
However, as mentioned, the problem lies in obtaining a “contact” measurement:
thermocouples are generally used for continuous control of the various kiln zones
and occasional material checks (e.g. by inserting them inside rollers to different in-
kiln depths).
Optical pyrometers are also an effective means of measuring temperature. These
instruments determine the temperature of a very hot surface from its incandescent
brightness; the image of the surface is focused in the plane of an electrically heated
wire, and current through the wire is adjusted until the wire blends into the image of
the surface.
Even better performance is attainable with IR ray measurement pyrometers. In
this case proper calibration of the instrument, effected via the choice of a suitable
emissivity (ε) coefficient, is extremely important.
Tile temperature can be estimated by passing certain ceramic objects of a known
temperature-shrinkage ratio through the kiln.
Manufacturers generally use Buller rings with a porcelain body, which have a
diameter of about 63.5 mm. After firing the ring is measured again and size diffe-

232
Firing

rences can be translated into temperature via a conversion table. However, such
measurements are of limited use as they depend heavily on the amount of time
taken for the rings to pass through the kiln, thus giving a relative rather than an
absolute indication of temperature.
Nevertheless, they are useful monitors of cross sectional temperature stability.
Bear in mind that the unfired ring diameter is not calibrated so the effective diffe-
rence between unfired and fired diameters must be recorded accurately, without
conclusions being drawn on the basis of fired diameters only.
Finally, specially shielded recorders can be passed through the kiln together with
the tiles. Throughout the firing cycle, these receive and record signals from various
connected thermocouples.
Correct positioning of the thermocouples thus provides valuable information on
the thermal inertia of the tiles and how temperature is distributed between their
interior and exterior.
An in-depth treatise of optimal kiln management, especially specific fuel and
electricity consumption etc., is beyond the scope of this volume.
However, the reader will undoubtedly find the heat balances in figures 11 and 12
useful as they provide a good overview of how energy is distributed and consumed.
The diagrams illustrate tile manufacturing situations with combustion air at am-
bient temperature (fig. 11) and preheated to 200 °C (fig. 12).

17.3% 14% 10% 55,7%

Hot air
Structural Endo- 12 Kg
1.62 Kg of
dispersion thermic
fumes + air
70 reactions T= 126 °C
T=250 °C
89 Kcal/kgp kcal/kgP 276
50 Kcal/kgp
Kcal/kgp

1 Kg of fired
mat. 3%
1 Kg of mat T= 90°C
Roller Kiln 15 Kcal/kgp
to be fired

Combustion Fuel
air
500 Kcal/kgp
T=30°C
e=1.10

Combustion air T = 30 °C Indicative heat balance of a roller kiln

Fig. 11. Approximate heat balance for a roller kiln with combustion air at 30 °C.

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Applied Ceramic Technology

10.8% 16.7% 12% 57%

Hot air
10.4 Kg
Structural Endother
0.82 Kg of 240
dispersion mic
fumes + air Kcal/kgp
reactions
45 Kcal/kg 70
T=250 °C T= 126 °C
Kcal/kgp 50
Kcal/kgp
Kcal/kgp

1 Kg of fired
mat. 3.5%
1 Kg of mat T= 90°C
to be fired. Roller Kiln 15
T=30 °C

Combustion Fuel
air 420 Kcal/kgp
0.74 kg
56 Kcal/kg
T=230 °C
e=1.10

Combustion air preheated


via recovery from cooling zones
T = 230 °C

Fig. 12. Approximate heat balance for a roller kiln with combustion air at 200 °C.

Rollers

The roller is one of the most important components in the kiln. Like the kiln
itself, it has changed much in recent years.
As firing temperatures have risen, kiln infeed widths have increased and firing
cycles become faster, so there has been a gradual switch from metal rollers to cera-
mic rollers.
It was the advent of firing temperatures above 1160-70 °C that led to the wide-
spread abandon of metal rollers as they deteriorate quickly at such temperatures,
even when made of expensive, quality steels such as lNCONEL 601.
Moreover a comprehensive range of rollers is now available.
Formulas, which may be both oxidic and non-oxidic, are optimised for the var-
ious kiln zones.
Ceramic rollers provide excellent quality at relatively contained cost, thus making
metal rollers virtually obsolete (they are, though, sometimes used at the kiln outlet).

Metal rollers

Initially, then, roller kilns used only metal rollers, from the simple Mannesman
roller to the stainless steel roller, with rollers of increasing quality being used towards
and in the firing zone.

234
Firing

Rollers were generally of the following quality:


– Mannesman for temperatures up to 300 °C
– Aisi 310 S for temperatures up to 900 °C
– Inconel 601 for temperatures up to 1170 °C.

Metal rollers have the following advantages:


– they are easy to clean: because they have a much higher expansion coefficient than
the ceramic materials that stick to them. Hence any ceramic dust tends to detach
from the rollers when the roller is cooled suddenly. Simply extracting a hot rol-
ler will usually be enough to clean it.
– insensitive to thermal shock: the metal roller is unaffected by emergency kiln shu-
tdowns. Heating requires fewer precautions, so kilns with metal rollers and in-
ternal fibre insulation can be switched on and off repeatedly, even weekly.
– they are long lasting: as long as there are no aggressive chemicals in the kiln atmo-
sphere.
– they stay straight: this is especially important in kiln zones with substantial diffe-
rences between above-roller and below-roller temperatures. This quality stems
from good conductivity, which prevents differentiated heating and thus deforma-
tion.

Of course, metal rollers have been abandoned because they also have several
disadvantages:
– cost: generally three/four times more expensive than ceramic rollers.
– durability: limited where kiln atmospheres are chemically aggressive; sulphur com-
pounds are particularly damaging as they react with the nickel in the steel to
form low fluxing nickel sulphide; in extreme scenarios this reaction can perfora-
te the roller in just 72 hours.
– impossibility of use at high temperatures on account of the fast deterioration and
bending that takes place above 1160 °C, thus excluding their use in the manufac-
ture of single fire wall tiles and porcelain products in general.
– impossibility of use in wide kilns as the rollers flex even under lightweight loads.

As the disadvantages clearly outweigh the advantages recent years have seen
almost total abandonment of metal rollers, except in:
– porous biscuit for double fire tile manufacture, in which the characteristics of
the body materials (without sulphurs) cause them to stick to the rollers very
quickly in the preheating zone.
– the last low-temperature part of the cooling zone, where the environment is
clean, to increase tile separation on the rollers and facilitate the work of un-
loading machines.

Since the above represent such a narrow range of the industry’s output manu-
facturers generally prefer to optimise the bodies, improve tile underside cleaning
performance and improve overall kiln control so as not to have to resort to the use
of metal rollers.

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Ceramic rollers

Developments in ceramic tile manufacturing techniques and the advent of new


tile types have driven parallel developments in the physical-chemical-ceramic com-
positions of the rollers that carry them.
Formulation of new roller compositions for use with ever-higher temperatu-
res, faster cycles and larger tiles soon became necessary to reduce tile deforma-
tion, especially flatness defects.
Producers have responded to these needs by providing specific kinds of rollers
that differ according to both temperature and the type of materials that the roller
can be expected to convey.
It should be pointed out that rollers of the same class may behave differently
where there are differences in the raw material mix of the body being fired. Analo-
gously, rollers of the same category made by different suppliers may have slightly
different formulations and thus differences in durability.
Rollers, then, are generally divided into the following classes:
– standard rollers
– semi-technical rollers
– technical rollers
– special rollers.

As expense logically varies from one category to another, it has become common
practice to use different types of roller in different kiln zones so as to contain instal-
lation costs.

Raw materials and formulations

Manufacturers use raw and semi-finished materials of high quality, which have a
considerable influence on final cost.
The following tables show standard compositions for the most commonly used
rollers:

ROLLER COMPOSITION
MATERIE
ROLLER PRIME
RAW RULLO
MATERIAL STANDARD
STANDARD STANDARD
COR- STANDARD SEMITECNICO o
MULLI- SEMI-TECHNICAL
CORDIERITICO
DIERITIC ROLLER MULLITICO
TIC ROLLER TECNICO
/TECHNICAL
ALLUMINE
ALUMINA 50 – 55 60 – 65 50 – 55
MULLITE – ZIRCONIO
ZIRCONIA-MULLITE - - 10 –- 15
CLAYS
ARGILLE 10 – 15 10 – 20 10 – 15
KAOLIN
CAOLINO 10 – 15 15 – 20 10 – 15
TALC
TALCO 5 – 10 - -

Tab. 5.

236
Firing

CRYSTALLINE PHASES IN THE ROLLERS

Tab. 6.

Firing the rollers at different cycles and temperatures causes crystalline phases
to form in different quantities and qualities, thus determining the characteristics of
the finished roller.

The most common causes of roller breakage

Rollers essentially break because of:

Mechanical problems
Being made of ceramic, rollers are rather fragile and mechanical stresses such as
knocks or excessive pressure can damage them even when new.
Hence they must be handled with care, starting with their removal from the
packaging. Another task requiring due care and attention is cleaning: this is done
using a special machine, which needs to be adjusted accurately so at not to stress the
roller. There is also a risk of breakage when the roller is inserted in the kiln: if it has
not been thoroughly dried the sudden release of water could seriously damage it.

Fatigue
As mentioned above, commercially available rollers differ in terms of mineralogical
constitution and maximum working temperature. Roller manufacturers supply tables
that illustrate these limits: yet temperature is really no more than an indicator as to
operational limits as the latter also depend on roller load, kiln characteristics and
the nature of the material being fired.
Mechanical stress on the roller can be calculated by way of the following for-
mula:
σ (N/mm2) = M/W
where
M = (P1 L/8) + [P2 (2L-I)/8]
W = 32 (
π De4-Di4
De )
M = static moment (Nmm)
W = modulus strength (mm3)
P1 = roller weight between supports (N)

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Applied Ceramic Technology

P2 = load weight (N)


L = distance between sample holders (mm)
I = load width (mm)
De = external diameter (mm)
Di = internal diameter (mm).

Chemical aggression
This is the main cause of early roller breakage and can occur inside the kiln
during routine operation, when rollers are extracted for cleaning purposes, in the
event of an emergency stop or during a scheduled maintenance stop. The damage
generally takes the form of a longitudinal crack a few tens of centimetres long or
transverse cracks which separate the roller into several cylinders, each 15-20 cm
long.
Breakage usually occurs in a kiln section some 10 m long, located between the
preheating zone and the start of the firing zone, where temperatures range from 680
°C to about 880 °C and salt deposits may be observed both on the roof and the walls.
The composition of these salts, mostly K2SO4 and K3Na(SO4)2, indicate the presence
of alkaline and sulphur vapours in the kiln atmosphere: the former originate from the
material being fired while the latter have their origin mainly in the fuel.
In-depth studies where the raw materials were clays with a high soluble salt
content, made up of sodium sulphate and lesser quantities of calcium sulphate
and complex potassium and sodium salts (SO3 = 0.8%), have been carried out. The
rollers were attacked by the alkalies, mainly potassium, resulting in the formation
of crystalline phases such as leucite, kalsilite and sanidine, totally absent in the
rollers before use. Some theories sustain that alkaline aggression occurs when the
potassium sulphate is deposited on the exposed surface and the pores of the rol-
lers where it reacts with the mullite contained therein as follows:

3Al2O3.2SiO2 + 3K2SO4 + 10 SiO2 à 6KAlSi2O6 + 3SO3


mullite leucite

Precautions
Under normal working conditions roller duration can be maximised and perfor-
mance optimised simply by observing the following.
– Always dry the rollers in as uniform a manner as possible before introducing
them into the kiln. It is advisable to dry them in the pre-kiln as placing them
above or next to the kiln is inadequate.
– To prevent moisture infiltration always store rollers in a warm, dry place, never
outdoors.
– To ensure homogeneous heating along the entire length of the roller, insert it
into the kiln module as fast as possible; insertion must only be carried out by
properly qualified personnel.
– To prevent dispersion of heat via the kiln exterior or when it is necessary to
degas the roller itself, it is good practice to plug it, at one end only (drive side),
with ceramic fibre.

238
Firing

– Hot roller rotation speed during extraction and insertion should be as close as
possible to routine running speed. After extraction the roller should be kept
turning for a few minutes.
– Extracted rollers must not come into contact with cold metal parts; they should
be handled with tools insulated with ceramic fibre. To stop rollers, especially
technical rollers, cooling too quickly, they should be blanketed with ceramic
fibre.
– In maximum temperature zones, rollers removed for cleaning purposes should
be replaced with new ones. Cleaned rollers should always be re-inserted towards
the beginning of the firing zone, taking the place of still-clean rollers that can
then be shifted to maximum temperature zones. Ideally, the temperature of the
roller should not drop below 500 °C during these tasks.

The chemical aggression caused by the “chimney effect” inside the hollow roller
interior can be attenuated by plugging it with ceramic fibre.
– To minimise roller cleaning and limit (as far as is possible) the formation of crusts,
the rollers could be engobed. The back of the tiles, instead, must be engobed. The
following types of engobe may be used.

Back engobe for carbonate base porous tiles and porcelain tiles (can also be used
for roller engobing):
ANHYDROUS ALUMINA 80.0%
KAOLIN 20.0%

Tile back engobe for vitrified tiles (only to be used for tiles, never rollers):
ANHYDROUS ALUMINA 12%
MAGNESITE (MgCO3) 88%

Universal engobe for rollers:


BROKEN ROLLERS 80%
KAOLIN 20%

N.B.: Preparation and application methods are similar for all types of engobe:
– Grinding residue: 1.0% on 45 micron mesh
– Glue: 0.3% of CMC
– Water: 70-90%
– Application density: 1100-1200 g/litre

Problems caused by rollers


The question of dirty rollers aside, it should be pointed out that even clean rollers
can cause problems regarding the feed of the material through the kiln.

Firing zone
The material moves forwards as illustrated in fig. 13.

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Applied Ceramic Technology

Cooling zone
The material is conveyed as illustrated in fig. 14, or worse still, overlapped. The
problem can be resolved by acting either on the firing zone or the cooling zone.

Firing zone
Here, two kinds phenomena can slow down the material in the middle of the kiln
with respect to the material at the sides. The first is a natural, temperature-related
effect where pyroplasticity causes the roller to sag. Even a variation of just a few
tenths of a millimetre will slow down product feed in the centre of the kiln. This
behaviour worsens at higher temperatures.
The other phenomenon stems from the way in which the rollers themselves are
manufactured; the rollers are fired in a suspended, vertical position. At high tempe-
ratures this arrangement can cause the material to flow downwards and give a rol-
ler cross section of the type illustrated in fig. 15.
The roller is then cut (as illustrated by the dotted lines) to obtain the desired
length.
The difference in central tile speeds in the firing and cooling zones can compen-
sate for each other and produce a more even line of tiles at the exit.
If the new roller arrangement still fails to produce the desired results (i.e. im-
proper tile feed), biconical rollers which maximise peripheral speed at the centre
and reduce it at the sides can be used. These rollers should be used in sets of 5-8
pieces per module towards the firing zone, for a total maximum of 30-40 rollers,
starting from the zone where central slowing is first observed.

Fig. 13. Material feed in the firing zone.

Fig. 14. Material feed in the cooling zone.

240
Firing

Fig. 15. The ceramic roller manufacturing process.

Cooling zone
With regard to direct air cooling a situation of the following type may occur (see
fig.16).
Differences in temperature above and below the rollers cause their deformation
(bending upwards), thus creating an effect opposite to that observed in the firing
zone. It follows that the tiles will then advance faster at the centre of the kiln than
at the sides.
Homogenising cooling above and below the rollers should limit the problem.

T2

Where T2 >T1

T1

Fig. 16. Roller deformation in the cooling zone.

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242
Sorting, packaging and palletizing lines

Chapter VII

SORTING, PACKAGING AND PALLETIZING LINES

Introduction

Before analysing the machines and devices used in the sorting department it is
important to point out the following: it is located at the end of the actual tile manu-
facturing process, after the tile has already acquired all its physical and aesthetic
characteristics and does not in any way influence these characteristics as it exists
only for control and classification purposes.
The sorting department allows the product to be sub-divided and packaged on
the basis of both qualitatively objective and subjectively settable parameters accor-
ding to the ceramic company’s position in the market.
In other words, the parameters which form the basis of tile classification have
much to do with commercial considerations that vary from one company to the
next, thus making them relative rather than absolute.
For a long time much of the work was manual, being entrusted to the skill of
the individual because of the difficulties of designing and building reliable, efficient
artificial vision systems; in recent years the latter have been the focus of intense
technological research, with new image acquisition systems and ever-more sophi-
sticated sensors being developed.
Hence it is extremely difficult to forecast how sorting will develop in the near
future.

Analysis and classification of tiles

Visual checks:
– to highlight tile defects
– to allow sub-division according to shade.

Dimensional and geometric controls allow:


– sub-division according to size classes
– qualitative analysis of shape defects.

It is thus necessary to distinguish between a defect (i.e. that changes the fi-
nished tile price) and dimensional or colour differences; the latter do not actually
alter the value of the tile provided sorting produces lots or packs of similar shade
and size.

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Further details can be obtained by consulting the relevant international standar-


ds (ISO 13006) and the section on finished product classification (see fig. 1).

Sorting department configuration


Far from consisting of just one machine for a certain product size, type and
output rate, the sorting department consists of a versatile series of devices. The
following paragraphs analyse the characteristics of the main machines used in sor-
ting, packaging and palletising.

Feed lines
Connection to upstream machines may consist of either a direct link to the kiln(s)
or to fired material storage systems; in both cases the product is fed by conveyors
which do not necessarily provide a consistent flow, so at the sorting infeed point,
other devices modify this into one which is smooth and uniform, eliminating dis-
continuities or non-uniformities and producing a continuous, homogeneous gap-
free tile flow.
Achieving this is essential, as any glitches in the flow will – if the sorting rate is
to be maintained – need to be compensated for by increasing the speed of the tile
conveyor, with obvious problems for the human sorter who consequently has less
time to examine the tile.
Furthermore, the feed line usually features other devices such as pressure wheels
to remove weak tiles (usually at the kiln outlet), brush and fan cleaning systems, tile
turntables (to position rectangular tiles correctly) and vertical compensators to
manage brief sorting line stoppages.

Visual inspection station


The visual inspection station (fig. 2) is the zone in which qualitative tile analysis
is carried out by one or two operators. The tiles flow through this zone as a conti-
nuous, gap-free, uniform “carpet” (see above paragraph).
Good illumination (incident and/or diffused lighting) allows the inspector to
pick out defects. At this stage the main aim is to identify those caused by production
errors (black points, glaze droplets, chipping); scanning for defects is accompanied
by analysis that aims to divide the tiles into groups of consistent shade. This allows
manufacturers to supply packs of near-identical tiles that produce the required ae-
sthetic results when laid.
After viewing the tiles the inspector marks them so that they can subsequently
be divided into uniform stacks.
They generally use fluorescent marker pens (the mark subsequently being read
by a U.V. photocell) or virtual systems which use encoder-controlled shuttles or
magnetic turntables.
With the latter system the tile is allocated a code and tracked as far as the stacking
station, where it is then placed in the code-related stack.
However, continuous observation and identification of defects or shade varia-
tions is no easy task as inspector performance inevitably varies over time and main-
taining consistency is difficult.

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Aesthetic criteria

1st QUALITY

The surface of the tile must be completely intact; aesthetic evaluation must be carried
out on a sample of at least 1 m2 or a minimum number of tiles as established by
standards.
It must involve observation of the surface of the tile at a distance of 1 m under 300 lx
lighting conditions. The result is expressed as the percentage of defective tiles.

1st Quality requisites


Percentage of tiles with defects (max 5%).

2nd QUALITY

Must involve a test sample of at least 1 m2 or 30 tiles. Evaluation must involve observa-
tion of the surface of the tile at a distance of 2 m under 300 lx lighting conditions.

2nd Quality requisites


Percentage of tiles with defects (max 5% of 3rd quality).

3rd QUALITY

Tiles of 3rd Quality are defined as those that do not meet 1st and 2nd Quality requisites.

Functional criteria

1st Quality requisites


The tiles must satisfy 1st Quality requisites as defined by relevant standards for individ-
ual product classes.

2nd Quality requisites


Dimensions
Tiles must satisfy requisites as defined by standards for individual product classes,
with a maximum permissible deviation of 25% with respect to the tolerances indicated
by the above standard.

Physical and chemical properties


The tiles must satisfy the requisites of the specific standard.

3rd Quality requisites


Tiles of 3rd Quality are defined as those that do not meet 1st and 2nd Quality requisites.

Fig. 1. Sorting criteria as defined by standards.

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Fig. 2. Manual inspection station (bench).

Given the need to employ different workers and considering the vast number of
variables, classification of output according to parameters that are not always objec-
tive – but of great commercial importance – is extremely delicate.
This “human factor” is highlighted when an increase in output makes it neces-
sary to employ two observers at a sorting station; here, the product is fed along two
lines, each assigned to a different worker; the problem here is that their separate,
subjective evaluations are blended at the packaging stage.
Manual defect and shade sorting, then, is an essential yet tricky task – yet one for
which a reliable automated alternative has yet to found. However, human error can
lead to mistakes or slow down production: the output rate of a sorting line is, in fact,
not so much dictated by automated cycle speeds but, rather, by human limitation.
It should thus come as no surprise that the ceramic industry is following the
development of automatic tile control systems with keen interest.

Dimensional control
Immediately downstream from the sorting bench comes the automatic dimen-
sional and geometric control unit, consisting of two different sections (fig. 3):
– a device for the control of size and geometric defects
– a flatness control device.

The former checks tile dimensions and classifies them within ranges set by the
machine operator: variations in tile size do not, in themselves constitute defects and
do not necessarily alter the technical specifications or commercial value of the pro-
duct.
The important thing is to sub-divide them so that tiles of significantly different
size are not laid next to each other.

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Fig. 3. Size and planarity control unit.

Optic fibres and digital linear sensors take a “snapshot” of the tile, which is then
compared to a “master” sample; precision is in the order of 0.1 mm and repeatability
is good, as is stability, despite the movement generated by the conveying system.
Other measurement solutions use photodiodes and encoders that give time/speed
readings, which are then interpolated to calculate a distance: precision is again in
the order of a tenth of a millimetre.
Measurements are carried both longitudinally and transversely (fig. 4).
Measurements X1, X2 and X3 identify the sides parallel to the direction of tile
travel, while measurements Y1, Y2 and Y3 concern sides perpendicular to it. Thus
not just one measurement but a whole series of them are made; these are processed
to attribute a single “size” value to the tile so that it can then be assigned to a group
(i.e. a calibre class) of similarly sized tiles.

The successive approximations method


This method is characterised by use of an algorithm that ensures good immuni-
ty from disturbances linked to measurement grouping (fig. 5).
It is based on the setting of central sizes that represent the “central” value of a
size class.
Calculating the difference between the central sizes and the X1-2-3/Y1-2-3 rea-
dings leads to compilation of a table, the concept of which is illustrated in tab. 1:
the top row shows the central sizes set while the first column shows the measured
axis size. The other columns show the difference between the central size and the
various X or Y measurements. Hence each field shows a deviation; the maximum
absolute value in each column (i.e. maximum deviation from the corresponding cen-
tral size measurement) is considered (bottom row) and the minimum of such maxi-
mum variation identifies the tile class.

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Fig. 4. Measurements made by the size checking unit.

Central sizes
Tile
12345678901234567890123
12345678901234567890123
12345678901234567890123
12345678901234567890123
12345678901234567890123
12345678901234567890123
12345678901234567890123
12345678901234567890123
12345678901234567890123
12345678901234567890123
12345678901234567890123
12345678901234567890123
12345678901234567890123
12345678901234567890123
Test method
12345678901234567890123
12345678901234567890123 Size class
12345678901234567890123
12345678901234567890123
12345678901234567890123
12345678901234567890123
12345678901234567890123
12345678901234567890123
12345678901234567890123

Fig. 5. The “central sizes” dimensional evaluation method.

Column maximum

Tab. 1: X1 = measured size value, C1 = central value of set size.

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Sorting, packaging and palletizing lines

An example with actual numerical data is provided in tab. 2.

Tenths of millimeter

Column maximum

Tab. 2.

Here, four different size classes have been set (top row).
The minimum out-of-size value is 12, the lower central size is chosen and the tile
is thus assigned to C2 (4493).

Average side method (as per EN 98)


The advantage of this method lies in the extreme intelligibility of assign-
ment.
As above, size classes are defined, this time as simple dimensional intervals
(fig. 6) with minimum and maximum values for each size class.
The size of the tile is the average of the tile size measurements:
= (X1+X2+X3+Y1+Y2+Y3)/6.

The class size of the tile is simply given by the interval to which the above-
calculated value belongs.

Maximum side method


Like the previous test method, this one is based on the definition of thresholds
(minimum and maximum) and assignment of detected values within certain inter-
vals: in this case that value is simply the largest of the X1-2-3/Y1-2-3 measure-
ments.

Modern control units allow the user to set any one of the above test methods as
desired.
Flatness defects are detected via telemetric sensors, calibrated with a master
plate to provide an “ideal” reference: its comparison with the actual tile surface re-
veals defects and deviations (both statistical and local) and the tile is classified
accordingly (i.e. deviation from master plate planarity constitutes a defect).
The limits of deviation for each class of tile can be set by the operator.
The figure below illustrates the most common defects detected by the above-
described unit (fig. 7).

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Tile
12345678901234567890
12345678901234567890
12345678901234567890
12345678901234567890
12345678901234567890
12345678901234567890
12345678901234567890 Test method
12345678901234567890 Size Size class
12345678901234567890
12345678901234567890
12345678901234567890
12345678901234567890
12345678901234567890
12345678901234567890
12345678901234567890
12345678901234567890
12345678901234567890
12345678901234567890
12345678901234567890
12345678901234567890

• Classification threshold

Determination of the size class requires the introduction of classification thresholds with
the following characteristics:
– thresholds must form consecutive intervals that determine the size class.
– the number of classification thresholds is equal to the number of programmed size clas-
ses minus one.

Size class Classification threshold

• Determining size:
The size of the tile is calculated as the average of the tile size measurements:
size = (X1+X2+X3+Y1+Y2+Y3)/6

All that needs to be done is to assign the calculated size to the relevant interval. As the
table shows, size classes C1 and C6 are open-ended intervals: all tiles smaller than S1 and
larger than S5 will be class C1 and class C6 respectively.

Fig. 6. Average side method.

Another recently implemented test involves measuring the squareness (ortho-


gonality) of adjoining sides. This can be measured directly as per the correspon-
ding ISO standard (i.e. by measuring the extent of deviation from the ideal position
for each side – see fig. 8).

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Sorting, packaging and palletizing lines

Different size sides Positive/negative edge Squareness Upturned or


curvature (lunette) (orthogonality) downturned corners

Diagonal and edge Diagonal and edge Warpage (global Deformation range
concavity convexity coefficient) on sides

Diagonal concavity Diagonal convexity


Fig. 7. The most common ceramic tile dimensional defects.

+/- readings

Fig. 8. Apparatus for measuring size, squareness and edge shape as per standards.

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Other devices give a squarerness evaluation by calculating the difference of the


diagonals, assuming that the edges are parallel. This last quality check is particularly
useful downstream from the edge grinding units used to rectify porcelain tile sides;
since porcelain tiles are laid without any inter-tile gap precise squareness is essential.

Automatic tile inspection

Introduction

For some years now industrial automation has been synonymous with improved
product quality and savings in terms of time and money.
The ceramic floor and wall tile industry is no exception to this rule and has
extensively automated just about every stage of the production process.
Sorting remains the only stage of that process to remain almost exclusively
manual, with inspectors classifying tiles according to shade and defects.
Workers are usually seated at an inspection station upstream from the actual
sorting line, where they can examine all the tiles moving past them.
A panel in front of the selector shows samples of the current product with diffe-
rent colour shades against which the tiles are compared and classified.
At the same time the worker also has to pick out defects which will influence the
quality category.
On the basis of his/her judgement, the worker then marks the tile with a code:
this is read by a downstream sorting machine which automatically packages the
tiles accordingly. Hence inspection and classification outcomes are entirely depen-
dent on the workers’ skill and intelligence.
To start with, it is evident that the operator’s capacity to perform this monoto-
nous task lies in his/her ability to focus on anomalies and defects while ignoring
that which is correct. The “human intelligence factor” is often a discerning one,
allowing identification of small – and sometimes new – defects, even on tiles that
have complex decorations and/or surfaces, where the distinction between what is
acceptable and what is a defect is far from obvious.
Yet human control is also inherently problematic, not so much because people
are incapable of detecting faults but, rather, because it is difficult to maintain con-
centration (i.e. objectivity and performance) over time.
The introduction of automatic shade control and defect detection systems has
the evident advantage of eliminating the above problems while raising quality and
lowering costs. This explains why, since the early 90’s, several specialist companies
and consortiums have been focussing their efforts in this direction.
The goal that these companies have set themselves is an ambitious and difficult
one, as the current trend is towards tiles that mimic the aesthetics and performance
of natural stone, or tiles of a deliberately random, heterogeneous pattern and tex-
ture that are often difficult to distinguish from actual defects.
An automatic tile sorting machine is obviously intended to mimic the tasks per-
formed by the inspectors, who, by careful observation, extract “global” information

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about the tile to identify the shade, and “local” information, used to track down
defects.
As the tiles pass by the inspector needs to maintain a certain level of concentra-
tion: if anomalies are detected concentration levels are suddenly heightened.
However, in some cases, reliance on sight alone can trick the worker and distort
his/her performance. Particles, dust, detritus or drops of liquid can sometimes fall
onto the tile along the conveyor. At first such tiles appear sub-standard, but more
accurate inspection will show that the “defect” can simply be wiped off.
In this event the inspector usually counter-checks by running his/her gloved
hand over the surface of the tile.
Nevertheless, the most important human faculty in tile inspection remains sight,
occasionally helped, in borderline cases, by touch. This visual information allows
the inspector to evaluate the tile and assign it to a certain class.
Automation of this process, then, involves imitating these human senses and
replicating certain intellectual functions: hence the employment of vision systems
that “see” the objects being examined and subsequently take the necessary sorting
decisions.
A standard vision system uses cameras, which, suitably piloted, can, in fact, ac-
quire an image of the item being inspected and then send it to a processing unit for
evaluation.
However, standard vision systems cannot emulate a sense of touch and can thus
easily be led astray by tiles that are dirty when they pass under the cameras. As this
can lead to errors and wastage, a vision system requires installation of a tile clean-
ing unit upstream from the actual point of inspection.
The complexities of designing and building an efficient, automated vision sys-
tem – the ultimate goal of which is to replace the human operator and reproduce
his/her decision-making skills – requires expertise in fields such as optics, image
processing and artificial intelligence.
Yet despite these difficulties, automatic tile sorting systems have been available
for some years now and numerous ceramic production plants have installed them to
good effect.

Tile vision systems: characteristics

The first task of any vision system designed to replace a human operator is,
then, to replicate the human faculty of sight with cameras.
High resolution video cameras are required in order to acquire the detailed ima-
ges needed for accurate detection of often small defects on sometimes very large
tiles.
The second step is the decisional one, carried out by a processor; here, through
utilisation of complex algorithms, the machine attempts to imitate the human deci-
sion-making process.
The third step is to communicate the processing outcome – for every single
image – to the automatic packing devices. To do this the inspection system marks

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the tiles with codes similar to those applied by human sorters which are easily reco-
gnisable by standard reading machines on the line.
Whatever the employed technical, optical and image processing solutions, nearly
all tile inspection systems have several aspects in common.
Since tile classification takes into account both shade differences and defects it
follows that inspection systems are generally separated into two separate modules.
This distinction stems from the fact that these different problems need to be
dealt with in different ways.
An understanding of how inspectors evaluate shade differences and defects
requires an analysis of the lighting conditions under which the tiles are obser-
ved.
Similarly, an automatic system needs to acquire, via the camera, images which
contain information useful for identification of certain characteristics and/or tile
surface defects. Hence a proper combination of lighting conditions and optics is
essential: a wrong choice can seriously compromise the efficiency of the vision sys-
tem.
During shade control, the inspector observes the tiles from above and lighting is
diffused. This overhead view allows him/her to evaluate overall shade while picking
out details that constitute decoration defects.
Automated systems generally employ the same principle.
The shade analysis module generally features diffused lighting and the camera is
mounted perpendicularly over the tile conveyor (fig. 9). This set up is largely ex-
plained by the desire to reproduce the same conditions that work so well for the
human eye.
Classification of tiles according to shade is a colorimetry problem (i.e. measure-
ment of tile colour and subsequent identification of shade as belonging to a defined
class).
In processing the camera-acquired image, a tile sorting vision system must also
be able to replicate the human faculty of colour perception.
Similarly to the human eye, automated systems perceive colour via the three
parameters of hue, saturation and intensity, which define the so-called HSI space re-
presenting colour.
In speaking of colour we are really speaking of hue. Hue allows us to distin-
guish between colours such as green and yellow. Hue is nothing more than the
perception of colour experienced by an observer when he/she is exposed to diffe-
rent wavelengths of reflected light.
Image perception begins in the eye (fig. 10). The muscles in the eyeball modify
the lens of the cornea to focus the image on the retina (i.e. the membrane lining the
interior of the eyeball).
The retina contains millions of photoreceptors, of which there are two types
with different image perception functions.
These photoreceptors convert brightness and colour information into impulses
that pass along the optic nerve to the brain where they are perceived as images.
Light-sensitive photoreceptors which allow you to see even under dim lighting
conditions are called rods. These do not contribute to colour recognition: that task,

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Fig. 9. Automatic vision system: illumination method.

Fig. 10. Human eye structure.

instead, is performed by the receptors concentrated in the fovea, the cones. There
are three types of cone (known, in simplified terms, as red, green and blue), each of
which responds to different wavelengths of light.
The intensity of cone response vis-à-vis wavelength is illustrated in fig. 11. Note
that the response peak of the cones does not always correspond to the colour with
which they are identified.
Figure 11 shows that the prevailing perception for wavelengths between 430
and 480 nanometres is blue, between 500 and 550 nanometres green and over 610
nanometres red.
The concept of saturation refers to the degree of purity of the colour (i.e. “non-
mixing” with white light). A non-saturated colour appears wan and faded while a
saturated colour is intense and vivid. For example, red is a high-saturation colour

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Wavelength (nm)

Fig. 11. Wavelengths of principle light components detected by the cones in the human eye.

and pink a very low one. For pure colours, that is, those that do not contain white
light, the degree of saturation ranges from 0 to 100%.
Intensity, instead, expresses the quantity of light reflected and perceived by the
observer.
Analysis of these parameters, then, allows recognition of shade and identifica-
tion of any shift away from a shade.
The colour video cameras used in tile inspection vision systems supply images
that are expressed as an RGB (red, green, blue) mix. These need to be converted
into HSI (hue, saturation e intensity) “format” as it is the latter which lead to accu-
rate identification of the shade.
More importantly for the tile manufacturer, analysis of local variations in hue,
saturation and intensity makes identification of colour defects such as stains, impur-
ities or glaze droplets possible.
An automatic shade sorting system has many advantages compared to manual
sorting.
For example, a worker is usually able to identify even slight differences in colour
between two tiles that appear within his field of vision simultaneously, yet not always
able to judge or remember the colour of the tile in absolute terms.
An automatic system, instead, ensures consistent shade identification judgement.
This consistency is also guaranteed by the fact that many of the available sys-
tems feature calibration mechanisms which ensure that tiles are “seen” by the came-
ras under conditions that allow constant reproduction of colour over time. This is
why automatic shade sorting is characterised by a stability and objectivity unattain-
able with manual sorting.
On the module dedicated to the detection of surface defects, instead, the best
results are obtained by viewing the tiles under direct reflection.
Fig. 12 illustrates how the light emitted by an artificial source normally (i.e.

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Sorting, packaging and palletizing lines

Fig. 12. Surface defect and the consequent light scatter effect.

where there are no defects) reflects off a tile surface and how the light is, instead,
scattered by a surface defect.
When it comes into contact with a defect the light is diverted from its normal
reflection route and only a fraction of it is reflected into the camera lens. Thus an
optical anomaly in the acquired image is used to identify a shape surface defect.
Once again, machine developers have attempted to mimic the mechanisms em-
ployed by human operators, where sorters perceive the presence of surface defects
as anomalous reflections of the light used to illuminate the tiles on the sorting
bench.
A selector will often shift his/her viewpoint of the tile so as to catch defects by
looking at the reflected light from different angles.
From the above it follows that automatic systems need to adopt two different
illumination-image acquisition modules: one for shade analysis and the other for
defect analysis.
The defects module uses simple black/white high-definition cameras so as to
identify imperfections – even small ones – such as lumps and pin-holes even on
large tiles.
Where defect classification is done manually the results depend on the opera-
tor’s skill and speed.
The ever-pressing need for higher output rates means that selectors are very
often forced to work under conditions that compromise their efficiency. For exam-
ple, the product is often conveyed across the sorting bench at a speed that gives
them very little time to analyse shade and discover defects (especially on smaller
tiles). Moreover, the tiles on the conveyor belt are often very close to each other and
the operator sees them pass by without any intervening gaps as if the control pro-
cess were a continuous one; consequently, he/she is unable to inspect the tile edges.
Even where tiles are properly separated when they reach the sorting bench it is
still impossible to inspect all the edges.
Some automatic systems get round this problem by using special optical arrange-
ments to acquire images which, through utilisation of special algorithms, allow iden-
tification of glaze shrinkage, chipping and flaking at the corners, even where such
defects are small and can escape the attention of a hard-pressed selector. These sys-
tems also help manufacturers pick out damage – invisible from above – which does not

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compromise the aesthetics of the tile but can compromise bending strength (i.e. small
cracks on edges).
Just as workers are put through a training period before they are allowed to
inspect specific products, so automatic systems have to be “taught” how to perform
certain tasks.
Machine “training” consists of acquiring a set of representative samples of a
certain shade; subsequently the machine can automatically extract those characteri-
stic parameters that identify the product in question and which will be used by the
image processing algorithms during inspection.
The automatic sorting machine supervisor has the task of setting shade and
defect tolerances (minimum size, minimum contrast, declassification thresholds etc.).
It is also possible to monitor any drifting away from the shade and set the machi-
ne so that it issues a shade warning when a certain threshold is reached, thus al-
lowing the supervisor to intervene.
The entire system can be controlled via a user-friendly graphic interface that
does not require personnel with specialised computer skills.

Installing an automatic sorting system

From the above it is clear that the best place to install an automatic tile sorting
system is on the sorting line itself in place of the traditional selection station,
upstream from the packaging machines.
If there are some products for which automatic sorting is as yet unsuitable then
both automatic and manual sorting units will be required. In this event the manual
inspection station should be installed downstream from the automatic system so
that all sorting operations can be transferred to manual (machine off) or the unit
can assist the manual workers (machine on). This arrangement allows the inspector
to see the marking deposited by the automatic system and correct, where necessary,
any evaluation errors.
Whatever the layout, insertion of an automatic system on an existing sorting
line must take into account the available space. Compatibility of system dimensions
with available space is obviously less problematic where the system is part of a new
sorting line.
Generally speaking, nearly all automatic sorting systems have their own tile feed
belts because the tiles must flow under the image acquisition units under specific
conditions (i.e. at constant speed and as undisturbed as possible by the vibration
produced by the rest of the line).
Definition of relative speeds between infeed/outfeed conveyors and the automa-
tic sorting system conveyor must ensure that the tiles are spaced apart properly so
that the cameras can acquire a separate image for each incoming tile.
Separation can be achieved mechanically by running the sorting system con-
veyor belt faster than the infeed belt so that tiles on the upstream conveyor can still
be conveyed up against each other but as soon as they reach the sorting system belt
they are accelerated to produce the necessary gap.

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Sorting system conveyor speeds may be as high as 40 metres/minute (with peak


speeds of 60 metres/min on systems with particularly fast image processing units).
Outfeed belt speed should be set so as not to “brake” the tiles exiting the sorting
system.
A mechanical alignment unit is installed at the sorting system conveyor belt
inlet: this ensures that the leading edge of the tile passes under the image acquisi-
tion unit at 90° to the direction of travel. If tiles pass under the cameras at the
wrong angle an additional image processing stage is required to “shift” the tiles
back to their orthogonal position. From a software viewpoint this is a serious com-
plication and inevitably slows down inspection rates.
The pre-sorting approach section should be equipped with guides that channel
the tiles into the actual alignment unit; the infeed conveyor should be level with the
sorting system conveyor for a distance equivalent to some 3-4 times the size of the
tile.
Evaluation of the space required for installation of a sorting system on an exi-
sting line should also take into account the space needed for the positioning of a
cleaning system with brushes and blower/suction units; this will need to be instal-
led upstream so that the tiles are already clean when they pass under the image
acquisition unit (remember that dirt and dust can modify inspection results).
Ceramic production plants are generally high temperature environments: since
electronic devices are generally destabilised by high temperatures, an air conditio-
ning system should be installed to keep temperatures in the automatic sorting area
below 40 °C.

Defects detected by an automatic sorting system

Both surface defects and shade errors are generally classified in terms of type
and severity. Within the context of a single image a defect is usually detected as an
anomalous contrast and/or alteration in the chromatic content of the image.
Yet there are limits to this defect detection capacity.
One such limit is the minimum size of the defect, dependent on the resolution
with which the image is acquired.
Each image is a matrix of pixels (or points), each of which corresponds to an
actual physical dimension on the camera’s field of vision. If, for example, the field
captured by the camera in one direction (e.g. transverse to tile motion) is 600 mm
long and the corresponding number of pixels is 2000 then the image resolution in
this plane will be 0.3 mm.
The same reasoning can be applied to the length parallel to the direction of
motion. On the basis of these two resolutions every pixel corresponds to a certain
surface area. Logically, defects any smaller than this area cannot be seen in the
image.
In general it can be said that a defect, in order to be detectable, must cover an
area of at least 0.5 mm2.
Another limit is represented by defect contrast. The higher the contrast of the

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defect the more likely it is to be detected. Reliable defect detection is therefore linked
to the contrast that such defects generate on the image under optimum lighting
conditions.
Moreover, the more complex the surface of the tile the higher the complexity of
the algorithms needed to detect defects: for example, heavily structured tiles may
have rough and/or smooth zones deliberately intermingled with matt and/or gloss
zones.
The same argument holds for the detection of colour defects where tile decora-
tion has an extensive chromatic component mixed in with random elements.
Just as size and contrast are key identification factors, so is the type of defect.
Difficulties can arise when only a part of the defect, not all of it, is detected.
This may happen when only a portion of it generates sufficient contrast. To obviate
this difficulty special algorithms which allow the defect to be reproduced in its enti-
rety are used.
Once the tile has been inspected and all the detected and identified defects have
been evaluated, the system assigns the tile to a category on the basis of the user-
applied settings.

Automatic sorting systems: performance and advantages

From a performance viewpoint (i.e. number of tiles inspected per minute) an


automatic inspection system guarantees better results than those provided by ma-
nual solutions.

Size
(side parallel to direction
of travel, in cm) 20 25 30 33 40 45 50
Vision system 125 115 100 90 80 60 50
Operator on single bench 120 96 85 75 65 52 45

The average values in the above table compare manual and automatic sorting
system performance.
Given the continuous progress in both the hardware and software fields the pro-
blem of inspection speed is negligible. Despite the complexity of image processing
operations, utilisation of more and more powerful microchips in parallel with arti-
ficial intelligence algorithms allow high-speed analysis of every single tile.
The widespread availability of such enormous computing potential means that
there are now many systems capable of examining even complex tiles. The product
types which best lend themselves to automatic inspection are:
• glazed single and double fire tiles with repetitive, random, marble-like patterns
on smooth or structured surfaces
• porcelain tiles (glossy, polished and rough)
• natural stone.

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Sorting, packaging and palletizing lines

The advantages offered by an automatic tile sorting system are:


• replacement of manual sorting
• inspection and quality control of all tiles
• a continuous kiln-to-packaging line
• reduced tile shade stock requirements
• guaranteed objectivity/repeatability over time, unattainable with manual sorting
• 24 hr/day sorting
• significant reduction in sorting staff requirements
• lower fixed production costs.

Because automated sorting can be applied to an extensive product range, with all
the consequent advantages, the ceramic industry has obviously shown great inte-
rest in such systems; their commonplace installation would inevitably revolutionise
what is still the most labour-intensive part of the production process.

Automatic sorting systems: other uses

When a ceramic plant begins a production run the ideal outcome would, of course,
be production of 1st Quality tiles only. However, the reality of manufacturing is
somewhat different. For reasons that are evident, the tiles that reach the sorting
department may well be 2nd Quality, 3rd Quality or even rejected. The higher the
percentage of low quality tiles the lower the earning capacity of the plant: lower
earnings, wasted raw materials and energy, waste disposal and stock management
problems all combine to reduce profitability. The more frequently this happens the
greater the need to identify and eliminate the causes of defects at source. Of course,
end-of-line systems do not actually solve problems of low plant efficiency: by the
time the tiles reach them the production process is already over.
However, installing automatic sorting systems downstream from specific stages
of the production process lets manufacturers identify errors before they can com-
promise the final outcome. Hence a sort of “distributed quality control system” can
be built up along the entire production line.
For example, an automatic sorting system might be positioned downstream from
the drier to check dried, unfired tiles or downstream from the first kiln in a double
fire plant. Such systems must be able to detect mechanical defects such as cracks,
corner chipping, edge imperfections and surface faults such as contamination, sunken
and raised areas, and remove such sub-standard pieces from the cycle. Consequen-
tly, the manufacturer avoids wasting any further energy/raw materials on tiles that
would certainly have been rejected at the end of the production process. Note also
that the sooner the defective pieces are identified, the greater the chance of re-
cycling them: an unfired tile is 100% recyclable, while disposing of a rejected, finished
tile is time-consuming and costly.
By analysing defects at different stages of the production process manufacturers
can track down their causes and increase production profitability by making correc-
tions and eliminating them at intermediate stages of the production cycle.

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Classification and stacking

When it exits the control area every aspect of the tile has been examined and,
whether by manual or automatic means, has been classified according to shade and
quality (the order of classification might be shade A 1st Quality, Shade B 1st Quality,
Shade A 2nd Quality, shade B 2nd Quality, 3rd Quality, Reject).
The dominant shade is not usually marked by the operator, only those shades
which deviate from it. A photocell upstream from the stacking zone, reads and de-
codes the markings.
The size measuring device assigns the tile a size and a quality class.
The planar device assigns the tile a quality class.
At this point the control and management station has all the necessary tile clas-
sification information: the final category will depend on the more negative of the
evaluations: for example, a tile deemed to be of 1st Quality shade and 1st Quality
flatness that has, however, failed to meet size criteria, will be rejected; likewise, a tile
that is perfect in terms of size and flatness will be rejected if declassed because of
surface defects.
The classified tile is conveyed to the stacking zone by two lateral feed belts (ca-
pable of carrying different sizes).
Here, the tiles are sub-divided according to the quality classes in the table above.
All tiles of the same class are directed to the same stacker, which extracts them
from the feed belts and produces a stack that can then be sent to the downstream
packaging station.
Stacking generally involves one of two different methods:
– direct stacking
– indirect stacking.

In the former the tile is usually extracted from the belts by a pair of pneumati-
cally-driven push pads that deposit it on the underlying stack being formed; the tile-
to-stack drop gap is, at this point, no further than the thickness of a single tile (see
fig. 13).
Coordinated movement of the pneumatic cylinder and the stacker plate ensures
both maximum productivity and a “soft tile landing”, in that the relative speed betwe-
en tile and underlying stack is minimized to prevent any detrimental impact or
scraping, especially for delicate materials. Precision of movement is provided by
sophisticated software which eliminates the need for any interposing buffer betwe-
en stack and tile.
The latest direct stacking machines have replaced DC motors with standard
3-phase motors controlled by an inverter; this solution maintains high perfor-
mance standards yet provides greater simplicity of operation and more readily
available spare parts.
In indirect stacking the tile is still removed from the belts by (2 or 4) pads opera-
ted by a pneumatic cylinder, but the tile is not dropped directly onto the stack from
a minimal height. It is, instead, handled by intermediate loaders which cover the gap
between extraction height and the placement height – a gap that is much wider than

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Sorting, packaging and palletizing lines

WALL FLOOR 1 FLOOR 2 FLOOR 3 FLOOR 4


Super 1st Quality – shade A – size 0
1st Quality – shade A *

1st Quality – shade B *

1st Quality – shade A – size 0 + + + +

1st Quality – shade A – size 1 + + + +

1st Quality – shade A – size 2 + +

1st Quality – shade B – size 0 + + + +

1st Quality – shade B – size 1 + + + +

1st Quality – shade B – size 2 + +

1st Quality – shade C – size 0 +

1st Quality – shade C – size 1 +

2nd Quality – shade A * +

2nd Quality – shade B * +

3rd Quality * +

2nd Quality - shade A – size 0+1 +

2nd Quality - shade B – size 0+1 +

2nd Quality - shade C – size 0+1 +

2nd Quality - shade A – size 0+1+2 + +

2nd Quality - shade B – size 0+1+2 + +

3rd Quality – shade A + B – size tol. + +

3rd Quality – shade A + B + C – size tol. +

4th Quality – shade a + B – size tol. +

Possible sub-division criteria.

Fig. 13. Stacking.

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with direct stacking. Drive units are generally of the DC step-by-step type.
Another characteristic of these devices regards the number of stacking stations.
There may be:
– lines with dynamic stackers: in this case the number of stackers is equal to the
number of quality classes + 2 reserve stackers used during unloading. A turret
arrangement ensures that all stations take the various quality classes alternately,
thus dividing the work load and spreading wear evenly among the stackers.
– lines with stacking stations which feature double autonomous movements: once
one stack is complete that same station is immediately ready to take new tiles; in
this type the number of stations is equal to the number of quality classes.

Whatever the methods of tile extraction, stack formation and on-conveyor pla-
cement the precise function of the machine is always the same: to gather classifica-
tion information and proceed with subdivision of the tiles into stacks of the same
class that can then be sent to the downstream packaging station.

Packaging

The final product can be packaged either automatically or semi-automatically;


the latter combines both machinery and labour, while the former only uses person-
nel to monitor and feed the machine with materials.
The purpose of the packaging process is to enclose stacks of the same class of
tiles in a cardboard container that will hold them together, protect them and makes
it easy to handle and transport them up until the time they are laid.
For small-medium size tiles the wrap-around system – consisting of a series of
stack pushers, carton pick-up/carry mechanisms and flap fold/seal devices – is ge-
nerally used. Note that the pack can be wrapped and sealed with the final flap (4-
point gluing) or can be closed symmetrically along the centre line of the box (5-
point gluing). Some machines allow manufacturers to adopt both solutions, thus
augmenting flexibility and versatility (fig. 14).
The wrap-around case has the advantage of producing little scrap and thus keeps
costs low, yet has its limitations in terms of tile size and is difficult to use where the
wrap-around box blank is longer than 2500 mm. Within those limits, however, it
maintains a good degree of rigidity and long-lasting handling stiffness, thus aiding
good machine reliability.
Producers of medium, large and extra-large tiles are increasingly using the co-
ver packaging method, in which the cardboard covers and wraps the stack from
above, leaving its underside exposed.
This eliminates the problems associated with case length, yet there is inevitably
a higher percentage of scrap (see fig. 15).
Wrap-around and cover packaging units may be used separately or together; in
the latter case, the manufacturer generally employs a “mix” of packaging machines
that allow him to switch from one method to another, thus making the line suitable
for a wide range of tile sizes (figs. 16-17-18).

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Sorting, packaging and palletizing lines

Fig. 14. Wrap around packaging: the 4 and 5-point gluing systems.

CARDBOARD AREA / TILE SIZE GRAPH


900000
CARDBOARD SURFACE AREA INCLUDING SCRAP

800000

700000

636804 COVER
600000

500000 512656

440896
419904
400000 404128 WRAP-
342720 AROUND
315240 302984 302984
300000 BOX
277300
BLANK
200000

100000

0
150 200 300 400 500 600

TILE SIZE
Fig. 15. Comparison of wrap-around and cover packaging performance.

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Fig. 16. Cover packaging.

Fig. 17. Wrap-around packaging.

Fig. 18. Packaging machine.

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Sorting, packaging and palletizing lines

Another important factor concerns the type of glue used to seal the cases: de-
pending on the temperature of the tiles themselves, either cold or hot-glue units
are used.
The most common of the two, hot-gluing, consists of units which melt the glue
and guns which apply it at the required points; adhesion is excellent, the system is
easy to keep clean and performance is steady and reliable.
However, it needs to be used at temperatures that bring the glue to the softening
phase, otherwise good adhesion between the materials being joined is compromised;
the limitations of this method are highlighted when packaging is carried out imme-
diately downstream from the kiln outlet and the tiles are still quite hot (maximum
60-65 °C). Under these circumstances cold vinyl glues applied with high-pressure
spray guns are used; in this case adhesion times are faster than the previous solu-
tion, yet as results are, in any case, inferior to those obtained with hot glue, cold
gluing needs to carried out in a pressing tunnel in which the flaps, once sprayed, are
squeezed by special devices to ensure good adhesion and thus prevent any subse-
quent opening of boxes and the resulting downtime.
Whatever the sealing method, the packaging machine will provide the manufac-
turer with a box of tiles that is ready to be coded and palletised.

Printing and labelling zone

On exiting the packaging machine the box is transferred to the printing zone
where it is marked with essential product data, as required by standards.
This information is generally printed on a part of the box where it can be read
after the boxes have been stacked on the pallet (usually on the side of a rectangular
or square box or on the upper side of the box).
An ink-jet printer is generally used. Black ink is preferred as it is less likely to
fade in sunlight (this is important as boxes may be left in the sun for some time).
On-box information generally includes a description of the product, its class
(size, shade, quality) and sometimes a bar code that is used either by the ceramic
company itself or later on at the distribution stage.
Bar code application requires more sophisticated devices: either the code is prin-
ted on self-adhesive labels which are then applied to the boxes or special high defi-
nition printers apply the bar code on the box directly; as application – and, more
importantly, reading – results cannot be guaranteed, a photocell is usually position-
ed immediately downstream from the bar code printer for an immediate check: a
warning is given where the code cannot be read.

Palletizing zone

After printing comes the palletizing station.


The latter generally consists of a 3-axis cartesian-coordinate robot which picks
up the packs and arranges them on pallets (fig. 19).

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Fig. 19. Palletization robot.

To complete the classification process begun during the stacking phase, all boxes
of the same code are deposited on the same pallet. Hence the number of palletizing
stations will be equal to the number of product classes, plus a reserve station which
allows the process to continue uninterrupted when a pallet is full and needs to be
removed with the aid of a manual transpallet or automatic shuttle.
Generally speaking, there are two types of palletization unit: those that run on
floor rails and those on overhead rails. The former are more widespread as they can
be adapted to the changing needs of the ceramic market more easily and at lower
cost (i.e. the length of the rails is directly proportional to the number of quality
classes on the sorting line).
The boxes are transferred to the palletizing zone by conveyors with controlled-
speed motors that allow accumulation of packs, synchronisation of different infeed
rates and consequently smooth pick-and-place operations. The box is usually tran-
sferred the same way up as it was packed (i.e. resting stably on the side of greatest
surface area): on reaching the pick-up point the boxes are rotated to the vertical
(90°), a more suitable pick-and-lift and palletization position (fig. 20).
Note that there is both a need to provide maximum box stability and, at the
same time, to deposit the tiles on their edges so that other boxes stacked on top do
not damage them: pallet loading may be seen as the art of compromise between
these two needs. Hence the two key factors are tile size and pack width. If, for
example, we take a pack containing ten 300 × 400 mm tiles, each 10 mm thick, it
will be placed on the pallet on its 400 × 100 side to give a pack height of 300. The
pack stability equation is empirically given by H (mm) × 0.2 + 40 = (mm of pack
width). Thus, in this case, we have 300 × 0.2 + 40 = 100 although other non-
geometrical factors (such as the type and quality of the pallet on which the pro-
duct is to be loaded) come into play. Packs cannot, of course, be deposited

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Sorting, packaging and palletizing lines

Fig. 20. Pack picker.

widthways individually as they could topple. In this case – and this generally
involves tiles larger than 330 × 330 mm – configuration is dictated not only by
the palletizer but also the upstream sorting line, on which a divider and stacker
unit is installed to produce a stack of tiles twice as high as normal: this is split
into two equal parts that are then packaged adjacently and given the same code.
Immediately downstream from this point another unit stacks the two boxes and
joins them together either with glue or a plastic strap (fig. 21).
Another, much less widespread alternative to turning the pack 90° at the fixed
pick-up point is to turn it to the ideal palletization position immediately at the start
of the roller conveyor on the palletizer station; the palletizer thus moves towards
the pack and lifts it only when it is as close to the destination pallet as possible;
while this method tends to speed up loading operations it requires a more extensive
base to ensure good pack stability during movement in front of the line of pallets
(sometimes tens of metres long). Moreover, this logic is unsuitable for simultane-
ous lifting of packs with different codes as they obviously need to be released in
different places.
Going back to the pick up and deposit process in a more general sense, the
pack is lifted, turned (where necessary) and then deposited on the pallet so that
the printed product information and the top of the tile face outwards and is thus
visible.
Pallet load layout varies as a function of product type, characteristics, size, tran-
sport and presentation requirements. This clearly complicated task is managed by
the sorting computer, specifically designed for simplicity, speed and user-friendli-
ness (fig. 22).

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Fig. 21. Divider-stacker unit.

Fig. 22. Visual information display facility.

The above information largely concerns standard sizes. With much larger tiles,
sometimes defined as slabs (600 × 900, 900 × 900, 600 × 1200 mm), the packaging
and palletizing processes are less standardised. When it comes to packaging, some
of these products are packed individually and manually. Subsequently the tiles are
laid directly on the pallet; overlaying them would produce stacks of considerable
weight requiring specially designed heavy duty palletizers.
Note that while palletization may, in many production plants, rely on utilisation
of semiautomatic systems, there are plenty of factories where the use of dedicated
labour makes sense, thus making all those rotation, tilting and automatic pack cou-
pling mechanisms quite unnecessary. Human intelligence is, in fact, perfectly capa-
ble of evaluating, on a case by case basis, just what needs to be done to ensure pack
or pallet load stability and should not be underestimated.
Data exchange between sorting unit and palletizer usually occurs by way of
clean contacts and the triggering of a FIFO (First In First Out) mechanism: each
pack exiting the packaging machine is entered into a memory (the FIFO memory),
while each pack picked by the palletizer exits that memory (i.e. leaves the FIFO). In

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Sorting, packaging and palletizing lines

other words the palletizer “knows”, for example, that there are 10 incoming packs,
that the first of these is code 1, that the second is also code 1, that the third is code...
and so on; every time a pack exits the packaging machine the relative class code is
sent to the robot which adds it to the chain, just as it removes it from the chain when
it picks and places it. The palletizer must be informed of every change in the memo-
rised chain otherwise loading errors will occur and packs of different characteristi-
cs will be mixed together.
The limitations of this system show up where the conveying line between sorting
and palletizing is particularly long, as this makes it easier for the above-described
errors to creep into the process.
Such problems can be prevented by controlling the type of material to be palle-
tised directly: packs exiting the packaging machine are marked with an inkjet prin-
ter (usually a high contrast spot a few millimetres in diameter) and the spot is then
scanned at the pick-up point to provide class code information.
Alternatively a bar code containing all the palletizing data can be applied and
read by a scanner at the pick-up point. If the latter system is adopted both printer
and scanner will need to be of much higher quality than those used with the “spot”
method.

Sizing a sorting and palletizing line

A sorting department is not a machine, but, rather, a set of devices some of


which are indispensable, other optional; they can be configured in innumerable ways
to produce the set up which best suits the needs of the manufacturer.
The key points to be taken into consideration are product type, output rate and
tile size range. Equally important is overall plant efficiency (i.e. full utilisation of
machine production capacity, dependent not only on the above factors but also on
line configuration and proper training of use and maintenance personnel). In other
words, while it is important to configure the devices appropriately it is also im-
portant to utilise them in a manner that ensures good overall plant efficiency, with
as little downtime (caused by maintenance problems and improper use) as possi-
ble.
Company policy also needs to be taken into consideration: is the goal one of
maximum automation or is a more labour-intensive approach more practical?
If the latter is true then we can expect to see lines characterised by semiautoma-
tic packaging and manual palletization: the high labour-intensiveness of material
transfer operations will provide good flexibility as the capacity of workers to adapt
to change is more easily managed than the corresponding software changes on a
fully automatic system. On the other hand, however, the worker’s capacity to carry
out a certain function inevitably establishes an output ceiling.
As a rough guide, then, we can calculate a tile flow rate in front of the worker of
about 20 m/min (rates for double fire and decorated products drop to as low as 15
m/min) with a corresponding packaging rate of 4/5 packs per minute: the line will
inevitably be built around these figures.

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Lines with automatic packaging and palletizing units are a more complex affair
in which the human contribution is limited to the selection station; here the opera-
tor observes the tiles passing by him/her and evaluates their shade and quality,
classifying them with an on-tile mark (for more detailed information on the impor-
tance of this process and the general lack of objectivity vis-à-vis evaluation of
shade and surface faults see the chapter on defects).
Establishing a priori how many tiles an operator can analyse per minute is no
easy task: it depends on tile size (yet is not strictly proportional to total surface
area), on the type of defects being sought out, on attentiveness in shade evalua-
tion, on the need to check any variation in shade, on product type, on the com-
pany’s strategic goals and priorities (maximum attentiveness to defects or mini-
misation of waste) plus many other variables that are too numerous to be listed
here.
Bearing this in mind a selection speed of 20 m/min should only be taken as a
rough upper limit (assuming continuous, uniform flow, with averagely skilled workers
and average sorting criteria).
Given this, manufacturers should configure sorting and palletizing lines so as to
make the most of the individual selector’s abilities (or pair of selectors where there
are dual tile feed lines or two stations). The best configuration is the one which
allows optimum employment of human skills without under-utilisation of automa-
tic units.
The manufacturer also needs to decide whether or not it is appropriate to install
devices such as stack dividers, glue/strap box joiners, turn-and-pair pick up units,
double palletizing pickers and empty pallet transfer units. The “right” combination
is the one that works best as a “team”, providing plant simplicity, maximisation of
efficiency and minimisation of both general and specific running costs.

Production control software

Production management in a ceramic company is greatly influenced by the enor-


mous number of codes needed to identify products of widely varying type, size,
colour and characteristics.
A ceramic company often distinguishes its wares according to variations that
occur within a certain product: for example, a product may be divided into 1st Qua-
lity or 2nd Quality and they, in turn, can contain different shades and sizes that give
rise to even more codes.
Following this explosion in the number of codes and the resulting complications
in stock control the industry has seen widespread application of information tech-
nology to enhance automation of production information management.
The information does not need to be created: it already exists as part of the
sorting, packaging and palletizing line logic, where qualitative and size-related sub-
division occurs and pallets containing homogeneous products are loaded. Software
enables the user to compress that information, organise it and make it readily avai-
lable (e.g. as a networked database).

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Sorting, packaging and palletizing lines

Sorting line configurations for porcelain tiles

The success of porcelain tiles has greatly influenced – and continues to do so –


sorting and palletising departments, even if indirectly: while the actual machine
functions are unaffected by the different physical characteristics of porcelain tiles,
indirect changes have been brought about because they are subject to additional
post-production processes and have generated a trend towards larger and larger
tiles (fig. 23).
With porcelain tiles, a significant amount of output is subject to polishing and
edge grinding: these are pre-sorted and stacked separately and can be diverted at
different stages along the line: the options listed below should be selected according
to the percentage of porcelain tiles the manufacturer needs to divert to these po-
lishing and/or grinding stations or the size of the production run.

2
3
4

Fig. 23. Porcelain tile sorting line layout.

Tile outlet (fig. 23 - 1)


Once identified, tiles to be polished are sent to a flat bed loader. They are then
unloaded by a transfer unit positioned at the head of the polishing line. This set up
allows the user to divert all the tiles or just some of them, the others being sent
directly to the packaging and palletizing department.

Stacker outlet (fig. 23 - 2)


Device integrated into the machine body and positioned at the sorting line stac-
ker outlet. Expels the stacks to be polished onto a holding belt before they enter the
wrap-around unit. These are then loaded onto beds or pallets and transferred ma-
nually to the lines in the polishing department. As above, the other stacks are con-
veyed to the packaging station directly.

Wrap through-passage (fig. 23 - 3)


All output is polished together: in this case the wrap-around unit can be set up so
that the stacks pass through without being packaged.

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This device avoids early wear of the wrap-around unit as the tiles transit without
rubbing against the box closure mechanisms. The stacks are then sent to the palle-
tizer which picks them (but does not, of course, rotate them) and positions them on
a pallet which is subsequently transferred to the polishing station: thus palletising
of both packaged tiles and those to be polished is performed simultaneously.

Size and squareness controller (fig. 23 - 4)


This machine classifies tiles by size and shape. Software-controlled dimensional
checks determine both the size and shape defect classes. Analysis of orthogonality
(squareness) also makes this unit ideal for checking tiles exiting an edge grinder; it
is therefore especially suitable for installation on sorting and packaging machines
downstream from squaring machines.
Another consequence of the growing demand for porcelain tiles is the progres-
sive shift towards larger and larger sizes: tiles measuring 450 × 450 or 600 × 600
mm are now commonplace, 600 × 900 or 900 × 900 mm ones are not unusual and
ultra-large slabs measuring 600 × 1200 mm are now making their appearance. Cor-
respondingly, sorting machines have been enlarged and reinforced and the extra
care required in packaging has seen manufacturers’ preferences switch towards co-
ver rather than wrap-around machines.

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Firing

Chapter VIII

POLISHING

Introduction

Ceramic tiles, whether porous or vitrified, floor or wall, are increasingly subject
to various edge grinding, flattening and polishing operations at the end of the tra-
ditional production cycle; the aim is to enhance the aesthetics of the tile and add
value.
The tiles most likely to be put through such processes are:
– PORCELAIN TILES:
• GLAZED (including single fire products)
• UNGLAZED
– POROUS WALL TILES:
• GLAZED (single and double fire).

Past developments and current trends

Polishing as an additional production process first made its appearance in the


mid-80s, being used exclusively for the surface treatment of granito porcelain (salt
and pepper) tiles.
Towards the end of the decade, as tiles steadily got larger, manufacturers began
grinding the edges in order to reduce the number of size classes and thus minimise
stocks.
At the same time manufacturers began using large grains, micronised powders,
flakes and pelletized or sintered glaze grains to produce macro granito, veined and
variable-shade effects that necessitated surface polishing and, to a greater extent,
squaring, in that such tiles were often marred by geometric variations.
Subsequently, polished and edge-ground (or rectified) wall tiles and even glazed
porcelain tiles (often confused with a well vitrified single fire product) appeared on
the market, the latter being polished with more sophisticated lapping and “ageing”
techniques designed to create specific effects.
Here the aim is to create (especially on floor tiles) products that resemble the
materials seen in old churches, castles and so on, where decades of wear and waxing
have modified the original appearance to give a “homely or rustic look” that is, para-
doxically, in huge demand in today’s high-tech society.
“Randomisation” of many production processes (body preparation, press filling,
die texturing, unfired and fired tile cutting and machining, mix-and-match packa-
ging etc.) has done much to recreate that sought-after antique look on the indivi-
dual tile but manufacturers are still a long way from giving the laid floor or wall

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that same individuality as the gaps between tiles still highlight the fact that they
have been made using modern manufacturing techniques.

Lines and machines for the rough flattening - polishing - squaring of


porcelain tiles

With machines for “traditional” tile sizes the focus is on productivity: today’s
manufacturers require lines capable of polishing 200-250 m²/h (1600-2000 m²/
shift), a figure that looks set to increase.

The work cycle

ROUGH FLATTENING (surface levelling)


Finished tiles are not always perfectly flat; rough flattening them provides the
manufacturer with products of uniform thickness. This is carried out using dia-
mond-tipped rollers, locked in chucks (mandrels) that feature vertical adjustment
(usually motor-driven and shown on the display) to facilitate positioning.
Normally, the chucks have a pneumatic system which maintains constant on-
piece pressure and also raises the roller during line stoppages and repositions it
automatically when the line restarts.
Diamond-tipped rollers need to be very sharp so as to reduce on-tile pressure to
a minimum, thus protecting the fragile ceramic from risk of breakage.
Rough flattening leaves the surface with a scoured appearance because diamond
tipped rollers are, at this stage, of the rough grain type. Combined roller + satellite
heads + roller or roller + turntable + roller systems are generally used.
On traditional tile sizes a layer of material some 0.7-0.8 mm and 0.6-0.9 mm
thick is removed for salt and pepper and penetrative soluble salt products respecti-
vely. On veined marble-like or coarse grained tiles where 1.0-1.2 mm or more may
be removed the purpose of rough flattening is not only to level the surface but
also, and most importantly, to bring out the desired pattern, colour or motif. On
large tiles the removed layer grows to 1.0-1.2 mm (on account of curvature). To
calculate how much material needs to be removed note that where flatness varia-
tions are in the order of +/- 0.5 mm it is necessary, in order to create a perfectly
flat surface, to remove 0.5 × 2 = 1 mm plus at least another 0.2 mm.
Grain size ranges from 50-60 mesh on the first stations to 140-180 mesh on the
last. In terms of final product quality and line productivity this stage is the most
critical. Line speed is 6-7 m/min.
New, more efficient rough flattening systems eliminate roller replacement at the
product change-over stage: more recent machines, in fact, can be used with all tiles
in the 300 × 300 - 600 × 600 mm range and even those measuring 300 × 600, 450 ×
900 mm etc. without having to change the diamond-tipped tools.
Rough flattening rollers (figs. 1 and 2b) have spiral, diamond-tipped abrasive
ridges; initially about 1 cm thick, they wear down completely after rough flattening

276
Polishing

Fig. 1. Flattening-edge grinding machine and close-up of diamond-tipped roller.

some 80,000 – 100,000 m². New diamond-tipped rims are provided by specialist
suppliers and old ones can be regenerated.
The latest machines allow the abrasive tools to be changed and maintained safely
without stopping production since all zones in each roller station are independent
and have a system which raises the chucks well clear of the tiles.
The above is true for all lines up to and including fine polishing: hence they are
usually equipped with several heads more than are strictly necessary; alternatively
the machine work programs feature machine speed adjustment mechanisms that
calculate current machine requirements and optimise the qualitative-quantitative
efficiency of the system.
Because there is a gap of 2-3 mm between the ends of the rollers and the outer
tile edge parallel to the direction of product feed (this clearance is necessary be-
cause if the roller were the same width as or wider than the tile it would wear
unevenly and inevitably chip the tile) it is necessary to flatten the two strips of tile
at the edges parallel to the direction of product feed. This can be done by: a) rota-
ting the tile 90° on a turntable after the first few rollers and then continuing through
the second group or b) inserting a coarse grinding disc head between the roller sta-
tions (see fig. 2a). Solution a), given the same number of rough flattening stations,
takes up more space.
A rough flattening machine producing 1200 m²/shift normally consists of:
– 3 diamond-tipped coarse grinding rollers
– 1-2 diamond-tipped flat plane satellites
– 3 diamond-tipped finishing rollers.

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Fig. 2a. Rough flattening with/without tile rotation.

COARSE GRINDING-POLISHING
A combined system of flat plane satellites or conical heads + tangential heads
(fig. 3).
The aim of coarse grinding/polishing is to eliminate any surface roughness that
may have been caused by rough flattening.

After rough flattening After coarse surface grinding

The polishing heads must be perpendicular to the tile surface. Flat plane rota-
ting disc units (from 5 to 7) oscillate slightly, allowing them to adapt to irregulari-
ties without exerting excessive pressure or working at the wrong angle; they are
thus not perfectly perpendicular but may tilt by 0.5° - 1° vertically and to a same or
different degree horizontally.
Each tool traces a different concentric area with respect to the vertical above-
tile axis and so only a portion of each tool is in contact with the surface at any one
time.
This helps keep it clean and stops it being clogged by the removed material.
To ensure that homogeneous removal also takes place at the sides parallel to the
direction of feed the support or, rather, the upper tool-holder beam, must oscillate
across the path of the tiles.
Where heads with diamond-tipped tools are used, the first coarse grinding sta-
tions are in the order of 50/60, 60/80, 80/100 mesh. If, instead, abrasive SiC tool
heads are used the coarse grinding grain may start at 46 mesh.
Generally speaking, coarse grinding-polishing ends with a grain size sequence
of 120, 150, 220 mesh.
Feed rates range from 5 to 10 m/min, depending on the material, the thickness
of the removed layer, tile size and line type.
A coarse grinding-polishing station with an output of 1200 m²/shift usually
consists of:
– 2-3 flat plane rotary discs
– 9-10 tangential heads.

278
Polishing

Fig. 2b. Transverse roller grinder.

Fig. 3. Machine for coarse grinding and polishing followed by fine polishing; the figure below illu-
strates different types of head (tangential, cylindrical and satellite).

POLISHING
Polishing employs tangential heads to give the tile a mirror-like finish without
any scratches, shadows or signs of machining.
Tangential heads are similar to those used for coarse grinding, but the abrasive
material is of much finer grain size (starting at 400 mesh and ending with an ex-
tremely fine 1200-1500 mesh; the polishing tools are usually made of composite
mortar based on sintered oxides).
Polishing is generally performed in the second section of the coarse grinding-
polishing machine. As in the initial section, the support top or tool-holder beam
oscillates transversely to the direction of product feed.
Tiles are fed through the machine at a speed of about 6-7 m/min.

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SQUARING - BEVELLING (or SIZING-CHAMFERING)


A combined system of tangential rough flattening grinders, frontal rough flatte-
ning grinders (fig. 4) and tilted chamfering grinders (fig. 5) with diamond-tipped
tools.
Tangential grinders carry out rough flattening, removing up to 3-4 mm on each
side (6-8 mm total), while frontal grinders are used to smooth the roughness gene-
rated by the former. Chamfering units (angled edge grinders) eliminate the very
sharp corners on the face of the tile. On porcelain tiles they operate at 45°.
Because all four sides of the tile need to be ground, machines (fig. 6) generally
feature a turntable between two sets of grinding machines.
The intensity of the machining process requires a particularly effective piece
holding system. Dual push-pull belt sets both above and below the tile are generally
used. Similarly, the need for tight squareness and parallel side tolerances calls for
very accurate tile alignment, usually provided by a pusher device.

Product feed may be as fast as 10-15 m/min.


A squaring-chamfering section with an output of 1200 m²/shift normally consi-
sts (on each grinding side) of:
– 2 rough tangential grinding wheels
– 2 fine grinding wheels
– 1 chamfering unit.

Fig. 4. Tangential and frontal edge grinder.

280
Polishing

Fig. 5. Angled edge grinding machine for chamfers.

Fig. 6. Squaring machine.

DIAMOND-TIPPED ABRASIVE, GRAIN SIZE – ANSI B74 16 – 1971)


SIEVE
SETACCIO 99.9% Aperture
Apertura Max%
Max. Aperture
Apertura Min
Min.% %Max %
Max. 2% Max.
2% max
USA
USA FEPA
FEPA passing
Passante retained
% sup. retained passing
% sup. passante passing
passante
20/30 D852 1270• 920• 8 600• 90 8 429•
30/40 D602 920• 650• 8 429• 90 8 302•
(35/40) D501 770• 541• 8 429• 90 8 302•
40/50 D427 650• 455 8 302 90 8 213
50/60 D301 455 322 8 255 90 8 181
60/80 D252 384 271 8 181 90 8 127
80/100 D181 271 197 10 151 87 10 107
100/120 D151 227 165 10 127 87 10 90
120/140 D126 197 139 10 107 87 10 75
140/170 D107 165 116 11 90 85 11 65
170/200 D 91 139 97 11 75 85 11 57
200/230 D76 116 85 11 65 85 11 49
230/270 D64 97 75 11 57 85 11 41
270/325 D54 85 65 15 49 80 15 –
325/400 D46 75 57 15 41 80 15 –
(35/40)non
(35/40) is not an
è uno APERTURE
APERTUREIN(IN
MICROMETRI
MICRONS)
ANSI standard
standard ANSI

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Applied Ceramic Technology

Glazed wall tile squaring lines

Main characteristics:
– high quantities of material removed from the sides (sometimes more than 1 cm
per side, thus reducing overall size by 2 cm)
– squaring with diagonal tolerances of 0.1-0.2 mm
– perfect side finishing (no glaze chipping)
– small, adjustable-angle chamfer
– high productivity (tile feed 22-24 m/min, output greater than 5000-5500 m² per
20 h day)
– versatility (number and type of grinding wheels can be varied).

Initially, attempts were made to perform this task with cutting machines but
poor results led to the introduction of more powerful squaring machines, concep-
tually similar to those used for porcelain tiles.
Standard configuration for each grinding side:
– 3 diamond-tipped tangential grinding wheels for the removal of large quantities
of material
– 1 diamond-tipped frontal grinding wheel
– 1 diamond-tipped resinoid grinding wheel
– 1 chamfer grinding wheel, capable of following surface irregularities and adjust-
able so that shallow, almost horizontal chamfers can be made without removing
the entire glaze layer.

Polishing - satin finish - semipolishing lines for glazed, unglazed and


third firing ceramic

These machines have been designed for small (10 × 30 cm) and medium (60 × 60
cm) tile production lines with output rates higher than 600 m²/shift. They carry
out:
– mirror-like POLISHING of the relief on third fire glazed materials. Individual
(not flat-plane disc) frontal heads, featuring shock absorption and SiC or dia-
mond-tipped tools with diameters of 150-180 mm are used. Polishing requires
the upstream presence of diamond-tipped rough flattening heads.
– SEMIPOLISHING: consists of small imperfectly flat movable polishing heads
as opposed to mirror-like polishing of glazed, unglazed and especially relief
surfaces: the frontal SiC or diamond-tipped tools oscillate to adapt to the surface
outline.
– SATIN FINISH-LAPPING of unglazed porcelain tiles and non-gloss glazed
materials: this technique enhances lustre by reducing surface roughness, but does
not provide a mirror-like finish. The frontal heads mount semi-rigid rubber bru-
shes impregnated with SiC.

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Polishing

While these lines aim to provide flexibility, both in terms of performance and
tile size, they are generally less productive than their porcelain tile counterparts.
Designed to partially process (i.e. lap or mirror polish only a portion of the
surface area) medium-large tiles (60 × 60 cm); output rates are not high enough to
allow full-tile polishing of medium sizes (30 × 30 cm).

Appendices

To illustrate the above concepts, there follows a description of a standard rough


flattening-polishing-cutting line for large porcelain tiles (1200 × 1800 mm).

Output 800 m²/shift, fired tile dimensions 1200 × 1800 mm:


– ROUGH FLATTENING:
• 3 diamond-tipped coarse grinding rollers
• 2 flat plane satellite heads with diamond-tipped tools
• 3 diamond-tipped finishing rollers.
– COARSE GRINDING-POLISHING-FINE POLISHING: 18-head machine
with:
• 2-3 flat plane satellite heads
• 15-16 tangential heads.
– LONGITUDINAL AND TRANSVERSE CUTTING: completely automatic,
multi-disc cutting machines to divide slabs up into smaller elements (for panel-
ling/kitchen tops/bathroom tops).
– SQUARING/SIZING (on each grinding side):
• 2 frontal (finishing) grinding wheels
• 1 chamfer grinding wheel.
– SPECIAL PROCESSES:
• Special cutting machines to make trims from polished slabs.
• Numerical control shaper to make kitchen and bathroom tops, table tops and
other items.

Water treatment and recycling

Recovery/re-utilisation of porcelain tile polishing sludge

The polishing of porcelain stoneware produces large quantities of sludge. An-


nual production in Italy alone was, in the year 2000, estimated at 70,000 tons and
that figure looks set to increase in line with rising national and international de-
mand.
At present, porcelain tile polishing sludge is temporarily stored by the ceramic
company prior to use/treatment or consignment to external enterprises that then
dispose of it in controlled dumps. As this material largely consists of valuable por-
celain tile powder, these solutions are clearly unacceptable both from an environ-

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mental and an economic viewpoint. New waste disposal legislation in Italy has re-
cently forced the ceramic industry to meet certain requirements, namely: preven-
tion and reduction of the quantity and hazardous nature of refuse, to be achieved
by using “clean” technologies, economic incentives, environmental certification, eco-
compatible products and containment of waste disposal activities, all to be carried
out in compliance with strict safety standards.

Polishing sludge

Being a “wet” process, polishing produces very large quantities of aqueous su-
spension (e.g. a line producing 70 m2/hour of 60 × 60 cm tile requires 1800 l/min).
Environmental benefits arise from reduced consumption as a result of recycling
waste water after clarification, flocculation and settling; the recycling plant is essen-
tially made up of two parts: one for purification of waste waters (clarifier) and
another for treatment and drying of sludge (filter press). During clarification the
particles in the water sediment out; this process is accelerated by the use of chemi-
cal coagulants (ferric chloride and aluminum chloride) that cause the particles to
agglomerate and flocculating agents (organic polyelectrolyte) that cause those ag-
glomerates to grow, creating flakes (or flocs) of a size that inevitably drop out of
suspension. Subsequently, the sediment is filter-pressed to reduce its moisture con-
tent to around 40% and then dried.
The sludge is a by-product of wet grinding the porcelain tile surface with abra-
sive silicon carbide elements (grinding wheels). The resulting residue consists of
dust from the tile body (quartz, mullite, zirconium silicate where used as an opaci-
fier agent) and calcite, silicon carbide and alkaline-earth oxides from the grinding
wheels themselves and wash water. The material has the consistency of mud or
slush, about 2-3 kg of sludge being produced for each square metre polished. On
account of its composition, not environmentally harmful, sludge is classified as
special inert residue.
Chemical analysis (see tab. 1) shows a composition similar to that of the tiles
themselves (note the high alumina and silica content). The high percentages of
calcium and magnesium oxides derived from the bonding agent in the polishing
wheels is accompanied by a high percentage of carbon (elementary chemical analy-
sis) thus indicating the presence of SiC. Loss on ignition is high owing to decompo-
sition of the hydroxides and the hydrated derivates of the divalent metals.
X-ray diffractometry analysis highlights the main crystalline phases. Some of
these are representative of the materials used in the porcelain tile body: particularly
evident are the peaks associated with quartz (SiO2), zirconium silicate (ZrSiO4) and
mullite (3Al2O3.2SiO2). Also evident are other crystalline phases such as silicon car-
bide (SiC), calcite (CaCO3) and soluble magnesium compounds such as magnesium
oxychloride (MgOHCl) and periclase (MgO), which can be traced to the bonding
agents in the abrasive wheels.
Mineralogical analysis (see tab. 2) highlights the presence of the compounds
associated with the bonding agent – magnesite (MgCO3), magnesium sulphate

284
Polishing

OXIDES (% weight)

Tab. 1. Chemical composition of polishing sludge.

COMPONENTI
COMPONENTS (%weight)
(% peso)
MgCO3 55
SiC 14
MgCl2 28
MgSO4 2
pomice 1
Tab. 2. Mineralogical analysis of the abrasives analysed.

(MgSO4), magnesium chloride (MgCl2) – and the actual abrasive: silicon carbide
(SiC) and pumice.
Analysis of abrasives with different grain sizes has highlighted the correlation
between grain size and binding agent chloride content. The percentage of chloride,
in fact, is inversely proportional to the size of the silicon carbide grains embedded
in the wheels (see tab. 3).

ABRASIVE Cl/kg grinding wheel (g)

Tab. 3. Chloride content in abrasive wheels as a function of grain size.

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Difficulties in using the sludge

Porcelain tile polishing sludge cannot simply be recycled into the production
cycle because it is a source of undesirable side effects:
1) increased apparent viscosity and thixotropy of slips during wet grinding on
account of the soluble salts (mostly chlorides).
2) increased fusibility and deformation during firing on account of calcium and
magnesium compounds derived from the grinding wheel binding agent (magne-
sium oxychloride cement).
3) high porosity stemming from the considerable quantities of gas generated at
1100-1150 °C following decomposition of the silicon carbide.
4) emission of volatile chlorine compounds during firing.

The presence of volatile chlorine compounds in the sludge is particularly pro-


blematic in that their release as gas during firing can cause corrosion inside the
roller kilns.
Thermogravimetric (TGA) analysis of samples subject to heating cycles ran-
ging from 20 to 1200 °C shows a significant drop in weight between 600 and 800
°C, which correlates to volatilization of the chlorine compounds and carbonates.
Confirmation of this phenomenon has come from chemical analysis of samples
treated at different temperatures in which the remaining amount of chloride is meas-
ured.
As table 4 shows, beyond 600 °C there is a significant drop in the quantity of
chlorides (74%), thus confirming the TGA results.
Summing up, then, it is impossible to recycle the polishing sludge back into the
porcelain ceramic body.
To prevent rheological problems in the slip the tiles could be extruded, thus
allowing manufacturers to skip the wet grinding stage; to prevent firing problems
the sludge could be used with materials that are highly porous, so that they conso-
lidate at temperatures lower than the combustion temperature of silicon carbide.
Once the cause of the grinding wheel chemical composition problem has been

Tab. 4. Chloride values in sludge at different temperatures.

286
Polishing

identified, it may also be possible to modify the binding agents, switching to those
with a low magnesium oxychloride content.
If it is not possible to change the type of grinding wheels it might be possible to
separate out the material produced during the first (diamond-tipped) stage of sur-
face treatment, which does not contain silicon carbide or magnesium compounds,
thus reducing the volumes in play.
Alternatively, the sludge could be used to produce low temperature refractory ma-
terials. Some research programs have focussed on the possibility of recovering this
inert sludge via heat treatment to produce new, high porosity insulating materials.

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288
The environmental impact of the ceramic industry

Appendix 1

THE ENVIRONMENTAL IMPACT OF THE CERAMIC INDUSTRY

Like all industries involved in the transformation and processing of raw mate-
rials, the ceramic industry inevitably has an effect on the surrounding environment.
In other words, a ceramic production plant is an “open” system which draws on
the environment for its supply of:
– raw materials
– water
– fuels
– electricity
and introduces the following back into it:
– finished products
– gaseous emissions
– solid and slurry waste
– waste waters
– heat energy
– noise.

An approximate illustration of this two-way flow of materials and energy is


provided in fig. 1.
It should be pointed out that a ceramic production plant has less polluting po-
tential than factories in many other industries in that a considerable proportion of
the pollutants, especially solid particles, can be efficiently filtered at relatively low
cost to avoid releasing them into the atmosphere. It also recycles a considerable
amount of its scrap and de-watered sludge and much of the waste water. Moreover,
because of the changes which take place during firing, solid residue and sludge are
generally rendered inert.
Nevertheless, the problem should certainly not be underestimated, especially
where industrialisation leads to a concentration of factories within a given area,
inhibiting the effective dispersion of pollutants, an indispensable requisite for par-
tial self-cleaning of the environment.
In Italy, the Sassuolo area is a case in point, and has provided the industry with
valuable experience as regards the pollution problems associated with the manufac-
ture of ceramic tiles resulting in enormously improved environmental protection
measures.
Thanks to prevention-oriented public health policies and increasing awareness
among the business community, pollutant emissions have been reduced significant-
ly. The results are evident: compared to 15 years ago, airborne dust concentrations
in ceramic manufacturing areas are now just a quarter of what they were, and lead
concentrations just one twentieth.

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NOISE Gaseous
emissions

FILTRATION

Raw materials

CERAMIC
TILE Finished
Water product
PRODUCTION
PROCESS

Fuel
Energy
Electricity

Filtration

Production Filtration or Waste


waste/residue separation water
of waste/residue

Fig. 1. Incoming-outgoing material and energy flows in a ceramic tile plant (from Piastrelle Ceramiche
& Ambiente - EdiCer 1995).

Technological innovation deserves much of the credit for this progress: for exam-
ple, the widespread adoption of rapid cycle roller kilns has controlled and reduced
the fluorine compound emissions associated with the firing of clayey materials. The
introduction of these kilns also led to reformulation of glazes and significantly
lower lead content in frits.
The involvement of plant engineers and colour manufacturers has resulted in a
rational subdivision of roles and responsibilities, essential if ambitious environ-
mental protection and workplace health goals are to be achieved.
Anti-pollution measures can be taken at different levels, both upstream and down-
stream from the actual process that generates the pollutants.

290
The environmental impact of the ceramic industry

“Upstream” measures include:


– use of materials with low environmental impact (e.g. reduction of boron and
other harmful components in glazes).
– rational use of fuels with high combustion efficiency and low sulphur content.
– plant engineering solutions that allow rationalisation of energy consumption
(e.g. cogeneration plants for the combined heat/electricity production).
– appropriate technologies (e.g. powder transport systems that prevent dust di-
spersion).
– responsible management of procedures and processes of high environmental
impact (e.g. mill and glazing line washing).
– frequent checking of process efficiency, especially on heat treatment units (kilns,
driers, spray driers): extensive use of information technology to control opera-
tional parameters within the various departments.

Downstream solutions include:


– installation of efficient pollutant “entrapment” and separation systems.
– incorporation of best technology available, cost-compatible abatement techno-
logies at the plant design stage.
– research into more efficient systems for dispersion of purified waste (air, water
or solid wastes) into the environment.
– research into the potential recycling of waste both internally and in other indu-
stries.

The most efficient control system remains effective monitoring and long term
recording of key pollution data:
– pollutant emission factors upstream and downstream from separation units per
unit of output.
– pollutant concentration in production process effluent.
– abatement system efficiency.

Bear in mind that a serious approach should focus not only on specific pollutants
(mainly dust, fluorine, lead and boron), but also needs to take into account problems
that affect the world as a whole (energy resources, greenhouse gases etc.).
Finally, companies would also be well advised not to underestimate the competi-
tive advantages to be gained from a serious pollution control policy, as such efforts
enhance corporate image and provide additional advertising leverage; this is espe-
cially so in fast-growing markets where customer awareness and quality perception
evolves almost daily.

Pollutants in raw materials for bodies

SILICA: found just about everywhere in the ceramic factory, as most raw mate-
rials are rich in SiO2. From a toxicological point of view silica can, where particles
of a certain size are inhaled, give rise to chronic illnesses (silicosis).

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FLUORINE: in quartz and feldspars in quantities of 0.0002-0.042%, and up to


0.3% in clays (0.05-0.17% in Italy), and up to 2% and more of micaceous materials,
such as F- (vicariant of OH-, which has similar dimensions, in the clayey lattice), F2,
HF, H2SiF6, SiF4 (reaction with SiO2 from the destroyed lattice) and/or alkaline
fluorines in particulate form.

SULPHURS: mineral sulphurs, such as Pyrite FeS2 (disassociation beyond 300


°C) and SO42- sulphates, which disassociate beyond 800 °C.

ARSENIC: 2-15 mg/kg (ppm) in porcelain tile bodies, up to 100-150 mg/kg in


some pigments.

CHLORINE: in water and clay.

ORGANIC SUBSTANCES: C and H-based, and nitrogen-containing substances


in clays (vegetable residues, humic acids).

ORGANIC ADDITIVES: used for rheological correction during body prepara-


tion (acrylates etc.).

Pollutants in glazes

FRITS: Pb, B, As (50-600 ppm and chromophor metal in some minerals).

GLAZES AND PIGMENTS: various toxic/harmful elements. Nickel, cadmium,


chromeVI, cobalt salts etc.

ORGANIC SUBSTANCES: fixers and fluidisers, vinyl resins, CMC, ...screen prin-
ting vehicles: solvents (glycols and ethylene and propylene polyglycols); thickeners (wa-
xes, glycerol starch, other starches); fluidizers (polyacrylates); fixers: (CMC, polyvinyl
alcohol, starches).

Pollutants in gaseous emissions

These vary in nature, depending on the raw materials in the body and the glaze, the
type of fuel used in the kiln and drier and the applied firing/drying curves. Fig. 2
provides a summary of their characteristics (PV = dusts). Most emissions are pro-
duced during the firing process: dispersion of most of the above substances – in the
form of gas-carried solid particles (fumes) – is possible, as is direct vaporisation of the
low-fluxing substances. Firing, of course, involves fuel combustion, and that means
emission of gaseous products such as nitrogen oxides and carbon oxides. Where natu-
ral gas is used, CO2 emissions are in the order of 0.23g/Kcal. If small quantities of
sulphur are also contained in the fuel, sulphur oxide emissions can become substantial.

292
The environmental impact of the ceramic industry

The following are also important:


Stage
Prod. Main tasks
of production

Dry grinding
Body raw mat.
Wet grinding
prep.

Spray drying

Pressing

Drying
Ceramic tiles

Glaze grinding
Glaze prep.
and glazing Glazing

Glazed tile dry-blowing

Porcelain tiles

Biscuit only
Firing
Glaze only

Single fire

Smoothing
Polishing

Fig. 2. Gaseous emission pollutants (from Piastrelle Ceramiche & Ambiente - EdiCer 1995).

BORON COMPOUNDS
Present in frits, boric acid (H3BO3) evaporates during firing. Boron compounds
can deposit in chimneys, causing encrustation.

ARSENIC COMPOUNDS
Small quantities are found in fumes separated with bag filters: they accumulate
in the solid reagent (to be disposed of) and sometimes exceed legal limits (according
to Italian legislation, this could result in separated residues being reclassified as
toxic harmful waste as opposed to special waste, thus increasing waste disposal costs
significantly).

AMMONIUM COMPOUNDS
Generated from nitrogen-containing organic substances and, it is thought, from
the NOx produced during firing. Some (e.g. NH4Cl) compounds condense and form
deposits in chimneys.

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CHLORINE COMPOUNDS
These mainly consist of the chlorines freed during firing following the decom-
position of chlorine compounds in raw materials (mostly clays).

ORGANIC SUBSTANCES
Aldehydes, benzenes, xylenes, 1,4-dioxanes, n-derivates, alcohols, ketones, esters.
The presence of organic substances in fumes, mainly introduced during glazing, is
linked to the in-kiln counterflows. Organic substances evaporate during preheating
(and may crack), mixing with the fumes without actually becoming hot enough to
burn. Such substances may be carcinogenic (aromatics) or, more often, produce an
odour that is perceived even at extremely low concentrations.

Atmospheric pollution

A ceramic plant, then, releases many different substances into the air, and in
widely varying quantities; their significance as regards environmental impact – and
thus prevention and containment – correlates closely to their degree of toxicity.
Proper evaluation of the impact these emissions have on the area surrounding the
factory requires more than just observance of the standards in force and demands
application of strict procedures. More than just simple pollutant measurements,
these procedures need to define:
1. Specific stack or chimney outflows (Nm3/kg product)
2. Temperature (for hot emissions)
3. For each of the pollutants:
MASS FLOW = mass of pollutant emitted per unit of time (g/h).
EMISSION FACTOR (EF) of a pollutant = the mass of pollutant emitted per
unit of product (kg): defined by the relationship between Mass Flow of the
pollutant (g/h) and hourly output (kg/h).

Key parameters:
UEF = Average emission factor upstream from separation plant (g/kg product).
DEF = Average emission factor downstream from separation plant (g/kg product).
i = efficiency in terms of % reduction in the separation plant.
c = concentration of pollutant in the separated emissions (mg/Nm3).

Limits for the main pollutants in gaseous emissions take into account toxicity.
Limits according to Italian law (1995) are as follows:

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The environmental impact of the ceramic industry

3
Emissions
MaxConc.
post-treatment
Max. dopoconcentration ) 3)
(mg/Nm
depuraz. (mg/Nm
Emissione Polveri
Powders Pb F
Grinding - Pressing
Macinazione-Pressatura 30 -- --
Spray-drying
Atomizzazione 30 -- --
Smaltatura
Glazing 10 -- --
Cottura
Firing 5 0.5 5
FritForni fusori
melting kilns 30 5 5

CLASSIFICAZIONE
CLASSIFICATION INQUINANTE
POLLUTANT FLUSSO
MASSDI MASSA
FLOW LIMITE (mg/Nm33))
LIMIT (mg/Nm
Be ≥ 0.5 g/h 0.1
As ≥ 5 g/h 1
Sostanze cangerogene,
Carcinogenic, teratogen, Cr6+ ≥ 5 g/h 1
teratogene
mutagene/osubstances
mutagene Co ≥ 5 g/h 1
Ni ≥ 5 g/h 1
Acrilonitrile
Acrylonitrile ≥ 25 g/h 5
Cd ≥ 1 g/h 0.2
Se ≥ 5 g/h 1
Sb ≥ 25 g/h 5
Cr3+ ≥ 25 g/h 5
Inorganic substances
Sostanze inorganiche
mainly in powder form Mn ≥ 25 g/h 5
presenti prevalentemente
come polveri
Pb ≥ 25 g/h 5
Cu ≥ 25 g/h 5
Sn ≥ 25 g/h 5
V ≥ 25 g/h 5
F ≥ 50 g/h 5
Sostanze substances
Inorganic inorganichein NH3 ≥ 2 Kg/h 250
presenti
gaseoussotto forma diform
or vapour gas o NOx ≥ 5 Kg/h 500
vapori SOx ≥ 5 Kg/h 500
Acetaldeide
Acetal ≥ 0.1 Kg/h 20
Formaldehyde
Formaldeide ≥ 0.1 Kg/h 20
Sostanze organiche Acreoline
Acreolina ≥ 0.1 Kg/h 20
Organic substances
Propionaldeide
Propionaldehyde ≥ 2 Kg/h 150
Methyl alcohol
Alcol metilico ≥ 2 Kg/h 150
Acetone ≥ 4 Kg/h 600
PolveriTotal
totali powders ≥ 0.5 Kg/h 50
≥ 0.1 Kg/h < 0.5 150

Emissions limits (as per Italian law): the above limits are minimums; maximum values are double that
figure. For carcinogenic substances etc. the indicated limits represent both minimums and maximums.

Prevention and separation

Preventing the emission of dust and gaseous effluents into the atmosphere be-
gins with proper selection of raw materials and plant engineering solutions. Both
should be chosen so as to minimise environmental impact, contain pollutant disper-
sion and optimise the exhaustion of gasses in a way compatible with workplace
health/safety and optimal energy consumption.
Production plants should therefore feature closed conveying/transfer and
exhaust systems, specially designed and built to minimise dust dispersion, and
kilns specifically designed to reduce fuel consumption (and thus combustion emis-

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sions) to a minimum: where necessary, kilns should also have systems for the re-
covery/combustion of the vapours released during preheating etc.
Of course, in a competitive industrial context, these goals are not easily achieved:
hence the use of filtration plants is inevitable.
Gaseous emission filtration systems are designed to:
– abate dust
– purify fumes
– abate the organic substances produced by combustion.

While a detailed description of the machines used to achieve these goals is beyond
the scope of this book, a summary of the main working principles behind them is
undoubtedly useful; for example, in dust abatement it is possible to use:

Dust abatement

SYSTEM OPERATING SETTLING


PRINCIPLE
Cyclones Agglomeration via Centrifugal force
turbulence
Venturi separators Agglomeration via Inertial impact and
turbulence diffusion
Electrostatic units Agglomeration Electrostatic attraction
Bag filters Separation Inertial impact
+interception

Bag filters

Given their versatility, they are used extensively by the ceramic industry: they
can also be used at quite high temperatures (about 170 °C).
With bag filters, one of the most important parameters is the inevitable drop in
filtered vapour flow rate, caused by the increasing resistance opposed by the filtration
element. That resistance has two components: the resistance of the fabric itself (con-
stant) and the resistance offered by the layer of dust that gradually builds up on the
bag interior. To ensure proper filter performance that layer is periodically removed
using mechanical shakers, flow inverters, compressed air etc.
Bag filter sizing/performance is summarised in the following table:

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The environmental impact of the ceramic industry

Parametro di Unità di misura Valori tipici


Sizing parameter Unit of measure Standard values
dimensionamento
m/min 0.8 ÷
– 1.2
Velocità di filtrazione m/s 0.01 ÷
– 0.02
Filtration speed
m/min 1.8 ÷
– 2.4
m/s 0.03 ÷
– 0.04
Perdite di carico Kpa
kPa 1.5 ÷
– 3.8
Flow rate loss
mm H2O 150 ÷– 300

Fume filtration

This includes filtration plants capable of trapping both the gaseous (e.g. fluori-
ne) and solid particulate (e.g. lead, dust) pollutants contained in industrial gaseous
emissions. The latter are treated as per the above-described dust abatement metho-
ds while gaseous pollutants are generally treated in systems that ensure their wet
or dry absorption in an active reagent (sometimes just water).
The contact reactor may take the form of a nebulisation tower, a dynamic Ventu-
ri-type system, a plate tower or other system in which fumes exiting the stack are
scrubbed with water (to which suitable reactive absorbents are often added); such
systems should have as extensive an exchange surface area as possible and prevent
the spray or liquid particulate exiting the filtration unit itself being drawn in. In
dry systems the gas exiting the stack is passed between suitably sized particles of
chemical absorbent, or through filters of extensive surface area (honeycomb struc-
tures or similar) that react intensely with the gaseous pollutant.
A typical example of this is entrapment of fluorine via dry or wet calcium
hydroxide/calcium carbonate absorbents (the absorbent “outnumbering” the pol-
lutant by a ratio of at least 3:1).

2HF + Ca(OH)2 → CaF2 + 2 H2O

2HF + CaCO3 → CaF2 + H2O + CO2

The main problem with these filtration methods, whether wet or dry, lies in
difficult control of the reaction products (calcium hydroxides or calcium carbonates
enriched with calcium fluoride); recycling them back into ceramic bodies is difficult
because of rheological side effects and the presence of calcium carbonate, which
alters the fusibility characteristics of the body.

Abatement of organic substances

As seen, a considerable quantity of organic substances at the kiln inlet is com-


monplace, especially with glazed tiles; in addition to those contained in the raw

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Applied Ceramic Technology

materials, normally kept to a minimum through careful selection in order to elimi-


nate black core defects, many organic substances are added during the production
process in the form of rheological additives (during grinding), screen printing vehi-
cles, thickeners and fixers etc.
During firing, all raw materials are subject to reactions: these range from simple
evaporation to oxidative dissociation and varying degrees of pyrolysis, depending
on the complexity of the polymeric chain making up the molecules. While reactions
differ in complexity, it can safely be said that carbon-based substances rarely give
rise to the simple combustion reaction:

CH4 +2 O2 → CO2 + 2H2O.

Instead, because of the extremely high heating rate inside ceramic kilns, the
combustion process forms a series of organic compounds that, on account of their
toxicity or because they have an easily perceived unpleasant smell, need to be trap-
ped and eliminated.
Entrapment can usually be carried out using a dry-bed or fluid-bed process via
absorbent (or active) carbon, or by way of chemical reactant aqueous solutions in
scrubbers, in which the vapours to be purified meet a counter-flow water surface.
However, these absorption systems provide low performance and are too complex
to be used effectively by the ceramic industry.
Post-combustion is a much more efficient method of pollutant removal, yet is
complicated from a plant engineering viewpoint on account of the high fume flow
rate and is costly. It involves capturing the fumes to be treated (or, at least, a part of
them) and burning them at high temperature so as to cause complete combustion of
any remaining organic substances. A part of the heat energy used in this process
can nearly always be recovered and used for other purposes. While abatement is
never perfect, efficiency ratings of 85-95% can be achieved, depending on the orga-
nic substance in question. This does not, of course, guarantee the complete de-
struction of odorous substances, which can still be perceived at the parts per billion
(ppb) level and even lower.
Generally speaking, where the problem of organic pollutants is a pressing one
(e.g. bricks lightened with polystyrene or wood chippings), a reduction in the pollu-
tant content of the fumes is best achieved via careful kiln design: the vapours rele-
ased during preheating (400-600 °C) should be partially recuperated and directed to
the actual firing zone where they dissociate completely.

Water pollution

Obviously, the tile manufacturing process:


a) uses the greatest amount of water during the wet grinding of raw materials and
the preparation and application of glazes.
b) waste water emissions are almost exclusively associated with glaze preparation
and application.

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The environmental impact of the ceramic industry

Both the composition and flow rate of such water emissions are extremely varia-
ble, being influenced by the quantity/type of output, glaze type, glaze application
system and other difficult-to-quantify factors (organisation of production, depart-
mental layout, extent of automation in washing etc.).
This explains why there is no linear correlation between specific water consump-
tion and output type and/or potential. Water inflow/outflow balances are, rather,
influenced by the type of production technology, especially as regards raw material
grinding.
Fig. 3 shows a hypothetical water inflow/outflow balance for a generic produc-
tion cycle, while fig. 4 is more specific and shows how water is used in a ceramic
production plant.
Note how waste waters can largely be traced back to glaze preparation and ap-
plication, as the waste waters from the raw material wet grinding mill (and spray
drier) and press cooling water are already fully recycled.
The evident economic and ecological advantages of recycling are highlighted by
comparing filtration water flow rates and overall factory water requirements. Full-
scale recycling reduces water supply requirements by 86% in double fire processes
and 48% in single fire ones. In the latter, nearly all companies use recycled water,
even where only partially filtered, for wet grinding of bodies.
In double firing with dry grinding, recycled water is used to wet the raw mate-
rials and, above all, to wash glazing lines. In this case, though, the percentage of
companies making use of full-scale water recycling is lower.
Before waste waters from the various stages of the production process can be
discharged into the environment surrounding the factory (streams, rivers etc.) or
re-utilised, they must be clarified.
Observation of the parameters determining discharge acceptability (maximum
concentration in the effluent) (tab. 1) provides information as to the pollutants that
need to be removed by such treatment.

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KEY
Gaseous
effluent The W symbols
indicate specific flow
rates in m3/1000 m2 of
tile for a production
Water process:
requirement
WT: water requirement.
Outgoing
Water Water used both as
material
raw material and
process fluid.
Production process WMi: water contained in
incoming material.
WG: water formed by
Incoming chemical reactions
material Water during the production
for production process.
WV: outgoing water, as
vapour in gaseous
effluents or dispersed
as vapour in work-
Waste place.
water WMu: outgoing water
contained in finished
product.
Ws: Waste waters.
Water balance in a production process:

Fig. 3. Water inflow/outflow in a manufacturing cycle for ceramic tiles and glaze products (from Pia-
strelle Ceramiche & Ambiente - EdiCer 1995).

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The environmental impact of the ceramic industry

Water Water
used as: released as:

Vapour in
Raw Process Waste
Prod. Phase Main operations gaseous
material fluid waters
effluent

Dry grinding -
Wetting
Body raw Wet grinding W
material prep.
Spray drying W

Pressing C

Drying
Ceramic tiles

Glaze grinding W
Glaze prep. and
application Glazing W

Tile blowing

Porcelain tiles

Biscuit only
Firing
Glaze only

Single fire

Smoothing
W C
Polishing
Products for glazes

Frit production W
(from glaze
suppliers)

Colorant and Oxide grinding C

compound
prod. Spray dying C

Fig. 4. How water is used and recycled in the ceramic tile production process (W = washing, C =
cooling. From Piastrelle Ceramiche & Ambiente - EdiCer 1995).

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Type Parameter/element In surface In sewage


water systems

Chemical-physical pH
parameters

Coarse materials Absent Absent

Dispersed solid Sedimentable materials (ml/l)


substances
80-200 < 40% of
Total materials in suspension
value upstream
(mg/l)
from system

Aluminium, Al (mg/l)

Boron, B (mg/l)
Cadmium, Cd (mg/l)
Chromium III, Cr (mg/l)
Chromium VI, Cr (mg/l)
Iron, Fe (mg/l)
Manganese, Mn (mg/l)
Metals and non-metals
Nickel, Ni (mg/l)
is solution
and suspension Lead, Pb (mg/l)
Copper, Cu (mg/l)

Selenium, (mg/l)
Tin, Sn (mg/l)
Zinc, Zn (mg/l)
Fluorines in solution, F (mg/l)
Chlorines in solution, CI (mg/l)

Sulphates in solution, SO4= (mg/l)

40-250 < 70% of


BOD5 (mg/l) value upstream
from system
Organic substances
160-500 < 70% of
COD (mg/l) value upstream
from system

Tab. 1. Parameters determining discharge acceptability (maximum concentration in effluent).

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The environmental impact of the ceramic industry

Water treatment (separation)

Fig. 5 illustrates a standard separation plant.


Here, effluent undergoes chemical-physical treatment via the use of reactive alka-
lines (normally soda in aqueous solutions), inorganic flocculants [for the most part
FeCl3, AlCl3 or Al2(SO4)3] and organic coagulants (anionic polyelectrolytes of high
molecular weight).
Initial clarification takes place in the sedimentation tanks, efficacy depending on
particle size and density (see table below).

Sedimentation rate Time required for


Particle size Type
(m/s) sediment to drop 1 m

Gravel 1 second
Coarse sand 10 seconds
19 seconds
8 minutes
Fine sand 2 hour
Bacteria 8 day
Clay 2 years
Colloidal substances 200 years

Grating
Waste Accumulation
waters

Pre-sedimentation

Homogenisation
Sludge

Purified waters

Claro-flocculation

REAGENTS:
1. Neutriliser [Ca(OH)2]
2. Coagulant (e.g. FeCI 3)
3. Flocculant Sludge

Fig. 5. Water treatment plant.

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Applied Ceramic Technology

In the claro-flocculation section the flakes grow and settle out from the ascen-
ding water current; this process is aided by the filtration effect of the sludge layer
that forms beneath because the water slows down as it rises until it equals the
sedimentation speed of the larger suspended particles; these thus reach a dyna-
mic equilibrium and form a filtrating layer capable of withholding the smaller
particles too.
The thus-purified water exits the upper section of the settling tank (normally by
way of a drop spillway); sludge, instead, is periodically removed from the bottom of
the separator and may be reintroduced into accumulation tanks where it can thicken
further.
The type of plant shown in the figure is the most widespread type, although
many others exist.
Such plants generally provide manufacturers with relatively good heavy metal
separation performance.
However, given the high incoming concentrations, that performance does not
always guarantee compliance with legal limits.
The parameter which seems to have the greatest effect on heavy metal separa-
tion efficiency is pH (in addition, of course, to retention time, which depends on the
size of the plant).
In 90% of cases, infeed pH oscillates between 7.5 and 8.5, owing to the basic
hydrolysis of the raw materials contained in the water. The pH is carefully regula-
ted by adding reactants so as to control concentration of, for example, lead and zinc
in the filtered waters.
As pH increases, Zn (OH)2, present as precipitate, tends to re-dissolve, passing
into solution as a zincate anion, while for acid-level pH solubilisation of the Zn salts
with formation of Zn2+ occurs.
Lead behaves similarly: in acid environments it is in solution as a cation, while
for decidedly basic pH values re-dissolution of the precipitated lead hydroxide oc-
curs and plumbites form.
Optimum pH levels for precipitation of Pb and Zn lie between 8 and 9, especially
with regard to zinc. Where pH values are higher than 9 undesirable post-reactions
can occur, and where higher than 10 the re-dissolution of precipitates becomes
commonplace.
The main technical limit in this sort of plant is an almost total ineffectiveness
against boron and its compounds.
Boron control is a tricky problem in that separation systems specifically desi-
gned to tackle this pollutant, such as those which use ionic exchange resins, are
difficult to apply to the ceramic production process and would not, in any case,
provide cost-effective reliability or duration.
In addition to high investment and running costs, utilisation of such systems is
hampered by the need to install resin regeneration equipment and dispose of the
eluates containing high concentrations of boron. As an alternative, it may be possible
to use easily removable ionic exchange units, which can be regenerated by specialist
enterprises, although the usual “disposal” method for boron-containing waste water is
to use it for wet grinding of the body.

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The environmental impact of the ceramic industry

Porcelain tiles

Over recent years, management and purification of waste waters has been made
even more difficult by the increasingly common practices of polishing and edge-
rectifying the fired tile. These operations require considerable quantities of water
(800-1000 m3 of water/m2) and the sludge separated from the resulting effluent is
difficult to reuse in that it contains a lot of fired, very hard ceramic material, and
large quantities of abrasive granules (artificial diamond, corundum, SiC) and mate-
rials from the abrasive blocks (metal or MgCl2-based), all in quantities ranging from
2.5 to over 10 g/l.
Moreover, demand for surface smoothing/polishing of glazed products is on the
increase, thus complicating re-utilisation of sludge and recycling of purified water
even further (see Chapter 8, “Water treatment and recycling”).

Solid waste and residues

Solid waste, whether associated directly with manufacturing operations or the


filtration of gaseous/water emissions, is produced at just about every stage of the
ceramic tile production cycle. Such waste may be classified as illustrated in table 2.
A better understanding of the situation can be provided by taking a look at the
changes that occurred between the 80s and the late 90s, when internal recycling
became far more common.
Over that time enormous improvements were made regarding the amount of
waste introduced back into the environment. Waste output in the Sassuolo area
was, in past years, about 40,000 tons/year of which about 50% was directed to
landfills.
The amount being dumped has now been slashed to about 2000 ton/year: this
improvement is even more impressive when one considers that total sludge output
doubled over the same period on account of increased ceramic production.
The current situation as regards recycling of individual solid waste categories is
more or less as follows:
– BODY PREPARATION powders total recycling
– PRESSING powder and scrap total recycling
– DRYING powders and scrap total recycling
– GLAZING line sludge
[Average production of (dry) sludge = 12% of applied glaze] 68%
– Fired material chamotte (grog) 85%
– Exhausted depuration calcium hydroxide 40%
– Fired material smoothing/polishing sludge almost 0%
– Concentrated boron solutions (from ionic resin exchange) none

Re-utilisation capacity, as with the waters, depends on how separation of the


recovered solid is carried out, and thus the extent to which salts, chromophor com-
ponents or hard materials have accumulated.

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Refuse/residue

Prod. Phase Production Depuration

Body raw Powders (sludge) trapped by


material prep. gaseous emissions filtration systems

Pressing Unglazed, unfired scrap Powders trapped by gaseous


emissions filtration systems

Drying Unglazed, unfired scrap

Unfired/unfired scrap Powders (sludge) trapped by


(unfired glaze on unfired body) gaseous emissions filtration systems
Ceramic tiles

Glaze prep. and Unfired/fired scrap Water depuration sludge (chemical-


appl. (unfired glaze on fired body) physical plant)

Frit, glaze leftovers and scrap etc. Concentrated boron solutions from
water filtration (ionic exchange
Glaze trimmings/scrapings process eluates, concentrated by
membrane processes)

Firing Fired scrap (*) Exhausted calcium hydroxide from


fume filtration

Powder (sludge) trapped by gaseous


Smoothing - emissions filtration systems
Fired scrap (*)
Polishing
Water filtered sludge (chemical-
physical plant)
Glaze products

Frit production Water filtered sludge (chemical-


(from glaze
suppliers)

physical plant)
Production leftovers
Exhausted calcium hydroxide from
Colorant and fume filtration
compound prod.

(*) includes pieces rejected during subsequent sorting stage.

Tab. 2. Classification of refuse by stage of production cycle (from Piastrelle Ceramiche & Ambiente -
EdiCer 1995).

This is important because the latter have a marked effect on the rheology of the
suspensions into which they are introduced, on body and glaze colour, on surface
appearance and body vitrification curves.
Outsourced recycling, while complicated by strict standards governing the han-
dling and transport of toxic-harmful waste, may be worthwhile: however, outsourcing
is more commonplace in the production of brick (where recycled waste accounts for

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The environmental impact of the ceramic industry

5-20% of the body), expanded clay (60-90%) and cement (not more than 2% but
total quantities are very high).
Where recycling – internal or external – is impossible, refuse and solid waste
must be disposed of properly in a dump. Where such waste does not contain toxic
substances it is stocked directly, yet where, as is more likely, it contains more than
the allowed amount of toxins, it undergoes stabilisation/solidification treatment;
this consists of acid digestion followed by mixing with cement, which fixes the
components in a sort of chemical-mechanical bond via a gradual crystallisation and
polymerisation process.
The flow diagram below provides an indicative illustration of the solid waste
treatment cycle:

CERAMIC
TILE
PRODUCTION
PROCESS Recycled
back into
the
production
process
Refuse/residue

Controls

Storage

Refuse Residue

Pre-treatment

Transport

Rendered inert Re-utilisation


(toxic and
in other
harmful wastes)
products
Dump /processes

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308
The environmental impact of the ceramic industry

Appendix 2

PRODUCTION CONTROLS

Volume I underlined the importance of proper ceramic body formulation, illust-


rating key analysis techniques.
Where such techniques are applied and interpreted properly, they provide a good
understanding of each raw material vis-à-vis the desired technological characteri-
stics of the body.
Additionally, once selected, all raw materials, whether plastic or non-plastic, need
to undergo suitable quality control procedures in order to routinely monitor their
technological characteristics.
A description of the main quality controls follows: this list should be taken as a
general guideline, actual tests being applied on a case by case basis that depends on
the degree of sample homogeneity.

Controls on raw materials or bodies

Pre-analysis preparation of raw material samples should include the following:


– wet grinding in laboratory mills and evaluation of the quantity of water needed
to produce a slip of a standard, set viscosity. Grinding should always be control-
led according to the residue on 63 or 45 micron screens.
– sieving of slip through a 1000-1600 mesh/cm2 screen.
– drying of the suspension.
– breaking up of the dried material in hammer mills or manually in a mortar and
pestle.
– wetting of the powders and sieving at 90 mesh/cm2.
– ageing to homogenise the moisture.
– pressing of the powders in a 4-ton hydraulic laboratory press, with a specific
pressure of at least 300 kg/cm2, preferably with a cylindrical die, ∅ 50-70 mm,
or, if rectangular, at least 50 × 100 mm.

With non-plastic materials samples can be prepared by mixing them with a stan-
dard quantity (e.g. 30%) of a standardised illite clay: this is sometimes preferable to
the practice of adding an organic binder (usually CMC in wetting water) to the
non-plastic material.

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Applied Ceramic Technology

Sample tiles are tested to establish the following:

1a) Post-pressing expansion (%)


A side of the pressed sample tile is measured with a gauge accurate to 0.01 mm,
giving (L2). The difference between the latter and the die measurement (L1) multi-
plied by 100 then divided by L1 gives post-pressing expansion:

L2 - L1
% E = —————— × 100
L1

where
E = Post-pressing expansion
Expansion is considered to be low when less than 0.4%, medium between 0.4 and
0.7% and high above 0.8%.

1b) Pressed tile bending strength (MOR)


Bending strength is expressed in kg/cm2, or, rather, in N/mm2. Tests are carried
out on samples of at least 50 × 100 mm using 3-point testers (see fig. 1).The fol-
lowing formula is applied:

3×P×L
BS = ——————
2 × h2 × b

where
BS = bending strength (N/mm2)
P = reading on scale (N)

Fig. 1. Apparatus for measurement of bending strength.

310
Production controls

h = minimum sample thickness (mm)


L = distance between the two blades supporting the sample (mm)
b = sample width at the point of breakage (mm).

Results are generally evaluated as follows (kg/cm2) = 10.2 × N/mm2

LOW MEDIUM HIGH


Green BS <6 6-12 >12
Dry BS <20 20-30 >30

Samples dried at 110 °C in laboratory ovens are tested for the following:

1c) Drying size variation (usually shrinkage) (%)


A gauge accurate to 0.01 mm is used to measure the just-pressed sample (L2)
and the dried piece (L3). The difference between the two measurements multiplied
by 100 then divided by the pressed sample size (L2) gives drying shrinkage; the
usual reference is the pressed tile size:

L3 -L2
% Re = ————— × 100
L2

where
Re = Drying size variation

1d) Dried tile bending strength


Procedure as per 1b).

The dried samples are then fired in (electric muffle) kilns at various tempera-
tures (1060°-1220 °C) or in a gradient kiln at one hour cycles at suitable tempera-
tures (e.g. 1100-1150-1200 °C).

Tests on fired samples are carried out to evaluate the following:

1e) Loss on ignition (%)


The sample is fired at 1060 °C and weighed. The difference between dried tile
weight (P1) and fired tile weight (P2) is multiplied by 100 and divided by (P1) to
give L.O.I. (%):

P1-P2
% PF = ———— × 100
P1

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Applied Ceramic Technology

1f) Colour and aspect of tile surface


Variations in shade at different firing temperatures are recorded and a descrip-
tion of any impurities, specks, cratering etc. on the surface of the material is made.

1g) Firing size variation (usually shrinkage) (%)


A side of the fired sample is measured with a gauge accurate to 0.01 mm (L4).
The corresponding size of the die cavity (L1) is also measured and the difference
between the two measurements is divided by L1 and multiplied by 100:

L4 - L1
% R = —————— × 100
L1

where
R = Firing size variation

1h) Water absorption (%)


Samples fired at various temperatures are weighed (P1) and then placed in a
water bath and boiled for a given time. They are then left to cool to ambient tempe-
rature, excess water is wiped off the surface of the tile and they are weighed again
(P2). Absorption (WA%) is calculated by way of the following formula:

P2 - P1
% WA = ————— × 100
P1

where
WA = water absorption

The results of all the above tests are then summarised on the raw material re-
port cards. These should be filed carefully and updated as necessary (via periodic
structural, chemical, particle size distribution, thermal analyses etc. effected by ex-
ternal facilities).
Non-plastic raw materials, instead, are put through routine chemical analysis
and sometimes X-ray diffractometry, softening point and heating microscope mel-
ting behaviour tests (see tab. 1 - tab. 8).
The record cards illustrated on the following pages summarise the main physical
and mechanical characteristics of the plastic and hard materials used to produce
ceramic tiles.
Of course, attaining consistency in terms of product characteristics, plant effi-
ciency, product performance and in-depth understanding of the technical character-
istics of the raw materials will require (in the factory test lab or in external facilities)
a routine programme of regularly performed controls on all semi-finished items at
every stage of the production cycle.

312
Production controls

SACMI (laboratory)
PLASTIC CLAY

RAW MATERIAL SPECIFICATIONS

Tab. 1. Red firing plastic clay, with incipient fusibility characteristics.

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Applied Ceramic Technology

SACMI (laboratory)

RAW MATERIAL SPECIFICATIONS

Tab. 2. White firing plastic clay, with fairly refractory firing characteristics.

314
Production controls

MEDIUM PLASTICITY CLAY

RAW MATERIAL SPECIFICATIONS

Tab. 3. Clays with good unfired characteristics. Vitrification is gradual without sudden melting.

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Applied Ceramic Technology

LOW PLASTICITY CLAY

RAW MATERIAL SPECIFICATIONS

Tab. 4. Clay with limited plastic properties. Low unfired bending strength. Refractory during firing.

316
Production controls

FELDSPATHIC SAND

RAW MATERIAL SPECIFICATIONS

Tab. 5. Non-plastic materials, with medium potassium and sodium oxide values.

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Applied Ceramic Technology

POTASSIUM FELDSPAR

RAW MATERIAL SPECIFICATIONS

Tab. 6. Non-plastic materials, with high potassium oxide content (feldspathic rock with a high ortho-
clase concentration).

318
Production controls

SODIUM FELDSPAR

RAW MATERIAL SPECIFICATIONS

Tab. 7. Non-plastic material with high sodium oxide content (feldspathic rock with a high albite con-
centration).

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Applied Ceramic Technology

QUARTZ

RAW MATERIAL SPECIFICATIONS

Tab. 8. Non-plastic refractory material, with a very high SiO2 content.

320
Production controls

The most important of these are described below.


Note that the quantities to be controlled (i.e. moisture, density etc.) can be changed
in accordance with the precision of the measuring instrument (i.e. scales).

Body preparation department controls

To maximise plant efficiency and optimise output the Quality Control staff should
carry out regular checks and tests in the body preparation department.

• Controls on slips at the mill outlet or slips in secondary holding tanks:

2a) Residue
Two hundred g of slip is sieved at 10,000 mesh/cm2 (equal to 63 µm or even
finer for glazes, using 16.000 mesh/cm2, equal to 45 µm). The residue is dried to
constant weight, then weighed:

Dry residual weight in g


Residue % = —————————— × 100
dry weight in slip

Control frequency: every mill load.

2b) Slip density = weight/volume


One hundred cc of suspension is sampled with a calibrated cylinder or container:

D. (g/l) = weight in grams × 10

Control frequency: every mill load.

2c) Slip water content (%)


One hundred g of slip is sampled and dried at 110 °C to constant weight.
The dry weight is subtracted from 100 to give the percentage of water in the slip.
Automatic thermobalances, which need only about 10 g of slip, can also be used.
Control frequency: every mill load.

2d) Viscosity
For information on the rheological properties of aqueous suspensions such as
viscosity, shear stress, thixotropy etc., refer to Chapter 6 in Volume 1. Note that
comparison between different outflow viscosity measurements can be affected by
thixotropy.
For production line controls a Gallenkamp or Engler viscometer should be used;
this is used to calculate the ratio between the time it takes the slip to flow out of a
high precision outflow funnel/cup (fig. 2) via a calibrated hole (usually 4 mm) and
fill a 100 cm3 graduated cylinder and the time it takes for water to do the same:

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Applied Ceramic Technology

Fig. 2. Viscosity measuring apparatus (Ford Cup: can be used to measure Engler viscosity).

°E = T1 / T2
where
°E = viscosity in degrees Engler
T1 = slip outflow time, in seconds (this value is equal to Ford cup viscosity and
used for glazes)
T2 = water outflow time, in seconds.

Control frequency: every mill load.

Spray dried powder controls

3a) Moisture content


Calculation is similar to that described in 2c), the sample being dried in an
oven. Testing is done approximately every 4 hours. “Speedy” devices, consisting
of a metal bottle with seal plug, pressure gauge and weighing scales are generally
used. The scales are used to measure the quantity of powder to be placed in the
bottle-reactor; a quantity of calcium carbide is placed inside the bottle with the
sample (this must not be mixed with the powder until the bottle has been hermeti-
cally sealed). The bottle is then shaken. The % moisture content can be read off
directly as it is directly proportional to the pressure created in the bottle by the
release of acetylene:

2H2O+ CaC2 → C2H2+ Ca (OH)2

Other instruments are available: for example special weighing scales with fast
infrared or microwave heaters allow the moisture content of spray dried powder

322
Production controls

samples (taken from the feeder belt or press hopper) to be measured in just a few
minutes. IR or MW technology also allows use of continuous control, contact-free
instruments.
Control frequency: every half hour.

3b) Bulk density


One litre of spray dried powder is weighed: bulk density is expressed in g/cm3.
Control frequency: once a day.

3c) Particle size distribution


A sample of spray dried powder is dried to constant weight. Then 200 g of dry
product is weighed out and passed through a system for measuring particle size
distribution by sieve analysis (fig. 3) on 600-125 µm screens.
Control frequency: every day on an average sample.

Fig. 3. System for measuring particle size distribution by sieve analysis.

Press department controls

Maintenance of optimum plant efficiency and output requires that press depart-
ment staff carry out the following controls:

• Powder controls

4a) Moisture content (as described in 3a)


Calculated using a SPEEDY device (fig. 4)
Control frequency: every 2 hours.

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4b) Soft powder filling


Evaluated by measuring the distance between the first fall punch (deepest posi-
tion) and the level of the die.
Control frequency: once per day per press.

It is then necessary to re-check the particle size distribution of the body using the
vibrating set of sieves (as this may have altered during silo storage, sieving or tran-
sport on conveyor belts).

• Tile controls

4c) Thickness
A gauge is used to measure thickness on all 4 sides (marked A, B, C, D) of all the
tiles from a pressing cycle. Comparison gives information on die cavity filling and
punch settling performance. If defects are detected more accurate controls can be
carried out with the aid of a penetrometer.
Control frequency: once every two hours.

4d) Penetrometer measurement


The instrument illustrated in fig. 5 applies a standard load (about 3-4 kg) on a
cylindrical needle of selected cross-sectional area. It records the extent of penetra-
tion into various parts of the pressed tile using an electronic or mechanical micro-
meter. The greater the number of control points the better the overall picture of
pressing consistency: the minimum requisite is that readings be taken at the four
corners and in the middle of the tile. They should not be taken any closer than 15
mm to the edge. More accurate pressed tile bulk density checks can be made using
a mercury density measuring system (fig. 6).

Fig. 4. “Speedy” moisture content measuring device.

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Production controls

4e) Weight of tiles from every press cavity


All the tiles from a press cycle are collected, marked and weighed separately.
Weight comparison provides useful information for the optimisation of die fil-
ling.
Control frequency: every 2 hours.

4f) Green bending strength (MOR)


Bending strength is calculated using the apparatus illustrated in fig. 1. All the
tiles in a pressing cycle are analysed (see 1b).
Together with other parameters such as moisture content, tile thickness, pene-
trometer readings and weight, this parameter provides useful information for the
optimisation of die filling.
Control frequency: every 2 hours.

4g) Post-pressing tile dimensions


All four sides of all the tiles from a pressing cycle are measured and the average
size is calculated.
The results provide data for the calculation of post-pressing expansion and are
indispensable for calculating drying shrinkage.
Control frequency: every 2 hours.

4h) Compression ratio


This is the ratio between the thickness of the powder fill and that of the pressed
tile.
Control frequency: once per press per day.

Fig. 5. Penetrometer. Fig. 6. Mercury density measuring system.

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Controls on dried tiles

Dried tiles need to be tested as follows:

• Controls at the drier inlet

5a) Moisture content at inlet


A representative batch of tiles from a car (double fire) or a batch corresponding
to a press cycle is weighed at the drier inlet (P2); it is weighed again after being
dried to constant weight in an oven (P1). The difference between the two weights
divided by the initial weight and multiplied by 100 gives the average moisture con-
tent (%) of tiles being fed into the drier.

P2-P1
% MC = ————— × 100
P2

Control frequency: twice per shift.

• Controls at the drier outlet

5b) Average weight of dry tile


A set of tiles is dried to constant weight, then weighed; that weight is divided by
the number of tiles in the set to give average dry tile weight.
Control frequency: twice per shift.

5c) Moisture content at outlet


Procedure as per 5a), using tiles exiting the drier. The dried tile can be taken
only if the sample drying cycle has been working properly.
Control frequency: twice per shift.

5d) Dry bending strength (MOR)


Bending strength is calculated by using the apparatus and methods described
above on a set of cold, dried tiles (see 1b).
Control frequency: twice per shift.

5e) Drying shrinkage


A set of tiles representative of either a drier cross-section or a pressing cycle is
sampled. All their sides are measured before and after with a gauge accurate to 0.01
mm and average tile size is calculated. Then the following formula is applied:

D1-D2
% Re = ————— × 100
D1

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Production controls

where
Re = Drying shrinkage
D1 = post-pressing size
D2 = post-drying size.

Controls on the biscuit (double fire only)

The following controls must be carried out:

6a) Average weight


Two sets of tiles representative of the kiln cross-section are sampled then wei-
ghed. The obtained weight divided by the overall number of tiles in the sample
gives average tile weight.
Control frequency: once a day.

6b) Water absorption (%)


The above samples are weighed separately (P1) then boiled for 2 hours and left
to cool to ambient temperature. Excess H2O is wiped off with a cloth and the tiles
are re-weighed (P2): WA is given by the formula:

P2 - P1
% WA = ————— × 100
P1

Control frequency: once a day.

6c) Bending strength


Bending strength is calculated by using the above-mentioned apparatus and
methods with sample sets taken as per 6a (see 1b).
Control frequency: once a day.

6d) Size variation %


The size of each tile (L2) is measured with a gauge: size variation (%) with
respect to the original die cavity dimension (L1) is given by:

L2 - L1
% R = —————— × 100
L1

Control frequency: once a day.

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Fig. 7. Dilatometer for thermal expansion measurements.

6e) Biscuit thermal expansion coefficient


Calculated with the aid of a dilatometer (fig. 7): periodically used to check for
proper glaze-body match.

Controls in the glazing department

Control Laboratory staff should carry out periodic checks to maintain plant
efficiency and optimise production.

• Controls to be carried out on the glazing line.

7a) Glaze density and Ford cup viscosity (as described above in 2b and 2d).

7b) Applied weight


Several tiles are sampled downstream from each glaze application unit. With
double fire products the glaze used to be scraped off and weighed; a faster and more
reliable method is now used (with double and single firing) in which the pre and
post-application weight difference is calculated.
An efficient alternative is to use stainless steel trays exactly the same size as the
tiles to collect and then weigh the glaze (or engobe) directly as it is applied on the
line. The weights applied by each individual application unit are then compared
with production standards to ensure that glazing remains within acceptable para-
meters.

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Production controls

Controls on the finished product

Finished products should undergo the following checks:

8a) Average weight


Two sets of tiles representative of the kiln cross-section are weighed.
Total weight divided by the number of tiles in the sample gives average tile
weight.
Control frequency: once a day.

8b) Water absorption (%)


Samples are take as per 8a) and boiled for 2 hours and left to cool under water to
ambient temperature. Excess H2O is wiped off with a cloth and the tiles are re-
weighed (P2): WA is calculated as per the formula given in 6b).
Control frequency: once a day.

8c) Size variation %


The dimensions of each tile and the corresponding die cavity dimensions are
measured with a gauge. Size variation is calculated as per the formula in 6d).
Control frequency: once a day.

8d) Bending strength


Method as described previously. The test is carried out on a set of samples re-
presentative of the kiln cross-section.
Once a day.

8e) Crazing resistance


One or more sets of tiles representative of the kiln cross-section are taken.
All the samples are placed in an autoclave and subject to pressure/temperature
increase checks as per international standards. The tiles are then removed and
checked for crazing by spreading special inks or methylene blue over the glazed
surface.
Control frequency: at least once a day.

8f) Resistance to acid/alkaline aggression


Chemical aggression tests are carried out on several samples of each product,
taken from stocks and the kiln, as per international standards.
Control frequency: weekly.

8g) Abrasion resistance (for floor tiles)


Abrasion resistance tests are carried out on several samples of each product,
taken from stocks and the kiln.
Control frequency: weekly.

The results of the above controls, carried out at various stages of the production

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cycle, are generally recorded monthly and filed by the Technological Laboratory for
reference purposes.

Laboratory controls on raw materials for frits and colours

All the controls described below must be carried out in parallel and under the
same conditions with a standard laboratory sample. The laboratory must therefore
have a comprehensive sample set consisting of all currently used materials.

9a) Viscous or low fusibility frits


The fastest control method is to produce a “tablet” and measure its fusibility and
to glaze a tile so as to reveal surface characteristics such as glossiness, transparency,
opacification, matting, pin holes.
Where available, utilisation of a colorimetric analysis spectroscope with rele-
vant software (e.g. CIE Lab), is advisable. The control is carried out by grinding
100 g of frit in parallel with a standard sample, under the same residue and density
conditions. A tile is then glazed and the remaining quantity used for the tablet test
using the same weight.
The samples are then fired in parallel, according to the cycle and maximum tem-
perature deemed optimum for the standard frit.

9b) Fluxing frits


As above, the most important control is the tablet (or button) test which demon-
strates fusibility; the tile glazing test is less important as behaviours diverge less in
this regard.
With these materials it may be useful to evaluate fusibility in numerical terms
and this can be done empirically by applying the following formula:

Length × Button Width


Fusibility (relative index) = ——————————————
Length × Standard Button Width

With both viscous and fluxing frits it is advisable to carry out controls on seve-
ral samples from several bags in proportion with supplied amounts.
If, instead, frits are produced internally by the ceramic company, constant con-
trols (every 2-4 cycles for rotary melting kilns or every 4-6 hours for continuous
tank melting kilns with a capacity of 2-3 tons) are advisable. If considerable diffe-
rences, visible to the naked eye, are found it may be necessary to increase control
frequency.

9c) Colorant (calcined pigments and natural oxides)


There are several colorant control methods. The most practical, reliable ones
are:

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Production controls

1 - Introduce the pigment in a percentage of 1% in a glossy zirconium opaque


glaze. Then glaze the tile (always in parallel with the standard sample), fire and run
a visual check on the results.
2 - Introduce the pigment in a percentage of 3% in a glossy transparent glaze.
Then proceed as described above (1).

9d) Quartz and feldspars


Introduce the raw material being analysed into a glossy viscous transparent or
opaque frit in quantities of 15-20%. Glaze a tile, fire and run a visual check on
hardening power.
Example:
Parts Parts
Standard quartz 20 –
Quartz being analysed – 20
Standard kaolin 5 5
Standard opaque glossy frit 75 75

The percentage of the raw material to be introduced into the frit depends on the
employed frit, firing temperature and firing cycle.
This value must be sufficient to bring the frit to the gloss-matt hardening tran-
sition point and allow evaluation of the contaminants of the raw material.

9e) Wollastonite
Wollastonite (calcium silicate) is a low temperature matting agent. It is this mat-
ting property which needs to be controlled. This test is effected by introducing
Wollastonite into a zirconium opacified glossy frit in percentages of 20-25% (mini-
mum value in which it starts to matt, sufficient to evaluate contaminants).

9f) Kaolin
Two types of control are recommended for this material:
– 1st test: suspending power test. Methodology: introduce 5% of kaolin into a frit,
grind and empty into a graduated cylinder. Agitate and check sedimentation
every 15 minutes.
– 2nd test: particle size distribution and purity test. Methodology: screen 200 g of
kaolin (dispersed in about 1 litre of water) at 16,000 mesh/cm2, run a visual
check for impurities, dry and weigh the residue.

9g) Zirconium silicates


The aim of this test is to control opacifying power, an essential characteristic of
this raw material.
Percentages are established on a case by case basis as the minimum values
needed for good opacification (usually 10% in a transparent glaze).

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9h) Calcined or anhydrous alumina


Two checks need to be run on this raw material:
– 1st test: particle size distribution control on different screens.
– 2nd test: hardening power test: introduce alumina into a zirconium opacified vis-
cous frit in percentages of 15-20%.

9i) Corundum and Sands(Zirconium-Rutile-Quartz)


The main control concerns particle size distribution, which must always be in
line with optimal standard values. A test with 20-25% in the glaze is useful for
contaminant evaluation.

9l) Carbonates: Ca - Mg - Ba - Sr
Checks on these raw materials require measurement of the quantity of CO2. A
test using 15-20% of the tested material in an opaque glossy glaze is useful to verify
the presence of contaminants.

9m) Tin – Cerium – Titanium oxides


Control their opacifying power by introducing them in percentages of around 5-
10% in a glossy viscous transparent frit.

9n) Zinc oxide


Check its matting power by introducing it into a medium-fluxing frit in percen-
tages of 20-25%.

9o) Raw materials soluble in water or in any case used only in melting
These materials are checked by means of grain size distribution or a melting
test. Two laboratory melting cycles are carried out: in the first all the raw materials
are standard and in the other all the raw materials except those being tested are
standard. The thus-obtained frits are used to glaze two tiles. Check results visually.

General criteria for quality control tests on raw materials for glazes

All the above tests should be carried out ensuring that:


– the glaze composition should be sensitive to variations in the product being
analysed.
– melting, grinding, application and firing conditions must be consistent.
– all results should be recorded on analysis charts (one per raw material), to be
filed in chronological order of supply.

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Defects

Appendix 3

DEFECTS

All production processes are interlinked. Items carry with them a “history” from
earlier processes which will influence their subsequent performance.
In this sense, firing, being the last of a series of processes (edge grinding and
polishing aside) and the one in which key physical, chemical and structural changes
take place, highlights both earlier latent defects as well as those induced by firing
itself.
Being able to recognise a defect, at any stage of the production process, and
knowing how to identify its causes are skills that are largely acquired by experience:
they depend on extensive hands-on experience and a capacity to see the whole pro-
duction line – from raw material storage to sorting – as a single “organism” and
require both global and specific knowledge of the production plant and a truly
wide-spectrum understanding of ceramics.
Acquisition of such abilities is essential to the rapid elimination of production
problems; identification of a defect and rapid deduction of its origin allows manu-
facturers to act fast through carefully targeted machine adjustments and thus limit
the costs associated with product rejection or declassing.
In general (especially on fired tiles), defects are of the following sort:
• structural: flatness, orthogonality, cracks, laminations
• surface: wrinkles, holes, bubbles, particles, flakes, crazing
• aesthetic: stains, shade or decoration defects
• process: defects associated more with the handling and flow of materials than the
product itself - overlapping tiles, chipping, sticking, jamming etc.

While any defect can usually be traced to a specific stage of the production
process, it generally has a series of concomitant causes, which, beginning with the
choice of raw materials, contribute to its emergence.
A rough summary of how such causes are interlinked is given in the following
table (tab.1).

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DEFECT CAUSE
PREPARATION Black core Low grinding residue
Size Incorrect particle size distribution
(grinding residue)
High H2O absorption Low Grinding too coarse, insufficient
bending strength moisture
Stains, cratering, specks Screening or iron removal errors
PRESSING Black core Pressure too high or not
homogeneous
Small side cracks Ejection too fast or imbalanced
Size Incorrect filling
Dimensional defects Incorrect press settings
Low bending strength Low pressing force. Low moisture
content
Explosions at kiln inlet Pressing force too high, lamination
DRYING Cracks Incorrect regulation, high
temperature
Explosions at kiln inlet Residual moisture content high,
incorrect regulation
Glaze defects Incorrect drier outlet temperature
Soluble salt stains Unsuitable drying cycle
GLAZING Cracks Unsuitable temperatures, tiles
knocked along line
Explosions at kiln inlet Excessive wetting
Cracks in middle of tile Unfired tile stored too long
Stains, holes, cratering Incorrect application, glaze not
aged correctly
Planarity defects Poor glaze-body thermal expansion
match
Colour, surface defects Engobe of poor quality
FIRING Side cracks Pre-heating too fast
Side cracks – cooling cracks Cooling too fast
Explosions at kiln inlet High kiln inlet temperature
Planarity defects Poor temperature control
Black heart, glaze defects Unsuitable cycle, erroneous
atmosphere
Size Incorrect temperature distribution
Surface stains Accumulations of glaze condensate
Craters, holes etc. Preheating temperature too high

Tab. 1. Possible links between defect and production department.

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Defects

To help understand the causes and effects in the above table the following pages
provide a more in-depth explanation of defects and how they correlate with the
various stages of the production process.

Defects associated with raw materials

Defects attributable to the presence of impurities in the raw materials can be


split into three main groups:
– Specks caused by the presence of impurities, usually particles of carbonacious mine-
rals, pyrite, pyrolusite, carbon and mica.
– Specks caused by impurities absorbed during the manufacturing process such as parti-
cles of iron, drops of oil or grease or small fragments of rubber.
– More widespread defects caused by the presence of other kinds of impurities, such
as organic matter and efflorescences.
– Carbonate particles (calcite and/or dolomite).

With monoporosa products the presence of coarse particles of calcite and/or


dolomite may lead to craters or “holes”. The larger the particles, the more extensive
these defects.
With single fire tiles, the defect depends not only on the presence and size of the
such particles but also the melting point of the glaze. Those with low melting
points tend to enhance the defect (fig. 1).

Fig. 1. Surface defect caused by coarse grains, degassing during firing.

The decomposition of minerals like calcite during firing is illustrated by the


following reaction:

CaCO3 ——> CaO+CO2 á

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This reaction occurs at approximately 800-900 °C, depending on particle size.


When particles are small, decomposition is complete and calcium oxide reacts
with the other components to form calcium silicates or aluminosilicates (ghelenite,
wollastonite, anorthite) of varying complexity.
If, instead, particles are coarse, carbonate decomposition may be incomplete or,
rather, the reaction of calcium with silica and alumina may remain incomplete.
The post-firing presence of free calcium oxide may lead to expansion phenome-
na when the material comes into contact with moisture (expansion is caused by
body components that have not reacted with CaO).
The reaction is:
CaO + H2O ——> Ca(OH)2

This phenomenon, where concentrated and localized, may form a hole of a very
distinctive shape (fig. 2).
When, instead, the defect is more generalized and diffused, latent tile expansion
can cause adhesion failure of the tile after laying.

Fig. 2.

After grinding, it is possible to check for the presence of coarse calcite and/or
dolomite particles by screening (e.g. via a 200 micron mesh) and then analysing the
washed residue under a microscope.
Adding a drop of diluted hydrochloric acid can also confirm the presence of
carbonates. The exact nature of the particles can be determined precisely by analy-
sing the area with an electron microprobe (SEM) or using more traditional chemi-
cal analyses.
In this case, the exact nature of the elements in the agglomerate can be identi-
fied and the mineral can be identified.
To eliminate or reduce the frequency and presence of such defects, it is good
practice to minimize the percentage of calcite and/or dolomite particles larger than
120 microns.
Using a suitable engobe as an interface between the tile body and the glaze may
also be very effective.

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Defects

– Pyrite particles
Pyrite, an iron sulphide, may be present as an impurity in some types of clayey
materials.
The most probable defect associated with coarse particles of this mineral is speck-
like colouring of the body and/or glaze (fig. 3).
The decomposition reaction of pyrite during firing is:

2FeS + 7/2 O2 ——> 2SO2 + Fe2O3

Fig. 3.

Where thermal gradients are shallow, decomposition occurs between 400 and
500 °C.
Where, instead, firing cycles are rapid, and if there is insufficient oxygen in the
firing atmosphere, oxidation remains incomplete and different reactions may occur.
In both slow traditional firing and fast single-firing, the defects associated with
the presence of coarse pyrite particles take the form of atypical coloured specks.
If, in the case of fast firing, the oxidation reactions remain incomplete, or if the
formed sulphur dioxide causes condensate inside the kiln, problems may be caused
by the gas attacking the vitreous surface of the tiles (brightness loss).
This problem does not, though, depend on the morphology (size) of the pyrite
particles but the total amount of pyrite and conditions inside the kiln.
As with carbonate particles, coarse particles of this mineral can be identified by
washing the grinding residue left on a 80 mesh (approx. 180 micron) screen and
analysing it.
In most cases, this defect can be prevented by lowering the size of the pyrite
particles to below 180 micron through use of suitable slip preparation sieves.
As above, an intervening layer of engobe between tile body and glaze may be
effective in solving the problem.

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– Pyrolusite particles
Pyrolusite (manganese dioxide) and goethite (iron hydroxide), when present as
coarse grains, lead to the formation of spots on the surface of the glaze (fig. 4).
As above, the particles can be identified with a microscope after screening and
washing, again on a 80 mesh sieve. Final results can, as with the above minerals, be
improved by using suitable slip screening sieves (i.e. those able to separate 180 mi-
cron particles). A layer of engobe between tile body and glaze may be effective in
reducing the severity and frequency of this problem.

Fig. 4.

– Carbon particles
Coarse particles of carbon in the post-grinding residue can cause concentrated
specks similar to those caused by carbonates.
These defects stem from combustion of the carbon during firing and the forma-
tion of CO2 or CO as per the following reactions:

C + ½ O ——> CO
CO + ½ O2 ——> CO2
Fe2O3 + C ——> 2FeO + CO

The carbon monoxide formed reduces the iron minerals in the composition and
produces, together with silica and alumina, dark coloured glasses (fig. 5).
In fast double firing, the defect may be arise from incomplete combustion of the
largest carbon particles, which could finish burning during the second fire and so
produce cratering or small dark holes.
Identification of the carbon particles that cause the above defects involves washing
and screening the grinding residue (at 230 mesh/63 micron) for consistency and
then observing it under a microscope.

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Defects

Fig. 5.

An approximate weight percentage of carbon particles can be obtained via calci-


nation of the residue after washing (after removal of carbonates by acid, e.g. CaCO3).
If it is not possible to replace the raw materials that are the source of the defect,
it may be better to grind it finer and sieve it through finer screens up to 120 mesh
(2400 mesh/cm2 equal to 125 microns).
An intervening layer of engobe between body and glaze may also be useful in
limiting the problem.

Specks caused by impurities absorbed during the manufacturing process

– Iron and/or iron oxide particles


Iron and/or ferrous oxides can contaminate raw materials during extraction or
during the subsequent mechanical handling.
Body contamination is also possible during preparation processes and can occur
in mills, storage silos, transfer elevators and cooling systems etc.
The defect itself usually takes the form of a spot or agglomerate on the
surface.
A useful problem identification feature is the texture (“softness” or “roughness”)
of both these defects. A metallic particle, partially dissolved in the glaze, with a
surface that is rough to the touch, probably comes from the kiln cooling zone; a
metallic particle enveloped in the body or glaze-body interlayer will definitely have
other origins (fig. 6).
If, after macroscopic analysis and evaluation of the different characteristics of
the defect (position, colour, surface appearance) the causes are still unidentified,
microscopic analysis of samples removed from the defective areas is carried out.
Analysing the spot with an electron microprobe provides comprehensive infor-
mation as to the chemical nature of the sample, without which it is virtually impos-
sible to identify which part of the production cycle is responsible.

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Fig. 6.

However, attention should focus on the following:


• cleaning and tidiness (this can help identify contaminants)
• preventive maintenance
• preventive replacement of old plant components.

– Other impurities
Other types of contaminant such as paint, grease, oil, wood or rubber particles
can occur throughout the process (fig. 7).

Where spray dried powders contain traces of unburned fuel (naphtha), the appe-
arance of a defect, consisting of raised dots (some mm in diameter) over a certain
area of the tile, is likely (fig. 8).
This defect becomes more evident when fluxing glazes and firing cycles with
very brief preheating times are used.
As above, there are no general solutions to these problems, which will have to be
analysed and the appropriate action taken.

Fig. 7.

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Defects

Fig. 8.

More widespread defects caused by the presence of other kinds of impurities, such as
organic matter and soluble salts.

– Organic material
Clayey materials may contain various percentages of organic matter up to 5% or
more.
When ceramic tiles with compositions containing a significant percentage of
organic matter are fired, a dark centre known as “black core” may appear (fig. 9).
In single fire floor (and wall) tiles this defect often occurs when very fast firing
cycles or very high pressing pressures are used.

Fig. 9.

Silk-screen printing can augment the defect as it involves the use of organic-
based vehicles (glycols or polyglycols), thus increasing the amount of organic mat-
ter.
As stated above, black core problems depend both on the firing cycle and the
characteristics of the raw materials. This chapter mainly focuses on how the pro-
blem is influenced by the nature of the raw materials and the impurities contained
in them.
The black core problem results in a multitude of effects:
• tile swelling (bubbles in the interior)
• pyroplastic deformation
• deterioration of the technical and aesthetic characteristics of glazes
• shade changes in the body and glaze.

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– Tile swelling
Depending on its severity the defect is either localised or present right across
the tile (fig. 10).
It mostly affects vitrified materials and is caused by the low temperature forma-
tion of vitreous phases in the body such as the reduction of ferric to ferrous oxide
in red firing materials or surface melting, which prevents the escape of the gases
that develop inside the piece (CO2 and CO), and areas of the surface are deformed.

Fig. 10.

If these organic materials oxidize prior to formation of the vitreous phase, the
defect is not seen.
With white firing materials, instead, where there is little iron in the body (< 1%),
deformation is largely caused by the presence of gases (CO2 and CO) that are una-
ble to escape because of melting at the surface (or the use of glazes with a low
melting point).
In addition to swelling, trapped gases inside the tile may form reduced phases
close to the glaze surface grey or black in colour.

– Pyroplastic deformation
Shows up as both tile geometry and flatness deformations of varying severity.
As mentioned above, black core defects derive from the joint presence of a liquid
phase and trapped gasses.
It can also be said that in areas where black core appears the percentage of liquid
phase is higher and viscosity is lower than in other areas of the tile.
For that reason, pyroplastic deformation occurs more often in vitrified products
where porosity is lower than 3%.

– Deterioration of the technical and aesthetic characteristics of glazes


A phenomenon that frequently accompanies black core is the appearance of a
considerable quantity of gas bubbles in the glaze layer (fig. 11).
This considerably reduces abrasion and stain resistance on account of wide-
spread microporosity in the glaze and worsens pin holing.
These gas bubbles are caused by gases (CO, CO2, H2) in the glaze layer that
were generated by the oxidation reactions of organic matter originally present in
the tile.

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Defects

Fig. 11.

– Shade changes in the body and glaze


Where the firing environment is not oxidising enough, the formation of black
core may, in both floor and wall tiles, alter the colour of the product.
Colour changes stem from the reduction of the iron oxide in the body composi-
tion, shifting the red shades, typical of this oxide, towards green or brown.
With wall tiles containing a high percentage of calcium, however the colour
changes from burnished orange to greenish beige.
With single fire tiles the change in colour may stem from different degrees of
oxidation of any copper, manganese and iron in the glazes, causing a shift towards
duller shades.

– Dynamics of black core formation


Black core defects are usually attributed to the presence of carbon residues from
thermal decomposition of organic matter in the 300-800 °C temperature range.
Some researchers have suggested that it is the presence of reduced iron in the
grey and black zones of the tile centre that characterizes the defect.
Moreover, they have recently come to the conclusion that the components which
cause black core are elements such as reduced carbon and iron oxides (FeO and
Fe3O4).
The former is formed by pyrolysis of organic matter, the latter by reduction,
mainly of the carbon, from Fe2O3, present in the initial clay compositions.

The chemical reactions, as well as the sequential dynamics of the black core
formation are as follows:
• Loss of clay crystallization water
Hydroxyl (OH) groups, which are freed at different temperatures depending on
the kind of clayey mineral, can act as reducers.

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• Thermal decomposition and reaction of organic materials


As stated earlier, the organic matter dispersed in clays mainly consists of humic
acids and carbon.
When these materials are heated CO2 develops (below 500 °C) as the molecule is
split by the following reactions:

R-COOH ———> RH + CO2 (g)


R-OH ——> R’H + H2O (g)

where
R-COOH = organic molecule with carboxyl functional group
R-OH = organic molecule with hydroxyl functional group
RH = product of the decomposition reaction
g = gaseous substance.

If heating continues, the resulting solid residue (coke-like coal) reacts vigorou-
sly between 500 and 700 °C and produces a nuclei polycondensation reaction.
Above 700 °C the following reactions may occur:

2 (R-H) ———> R-R + H2(g)


R-H ———> R + H2 (g)

where
R-H = is the result of the initial decomposition reactions
R-R = is the result of the dehydrogenation reaction.

The clayey materials are essentially aluminosilicates capable of initiating a ca-


talysis which aids the pyrolysis reaction that occurs in the 400-500 °C range.
Hence the following reactions between carbon oxide produced by decomposition
of the organic matter and any other available gases:

C(s) + H2O (g) —> CO (g) + H2 (g)


CmH2m+2 —> mC (s) + H2 (g)

where
CmH2m+2 = a hydrocarbon formed from the decomposition reactions
s = solid material.

Without oxygen, the steam generated by previous reactions may combine with
hydrocarbons or the existing free carbon.
Oxidation temperature and rate will depend on the type of carbon and on the
organic matters in the clayey raw materials.
As a consequence of the above reactions, when clayey mixtures containing orga-
nic impurities are progressively heated, first the clay crystallisation lattice water

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Defects

and then, starting from 550-600 °C, a mixture of gases made up of H2O, CO2, CO
and H2 are released.

• Reduction of iron oxide


Iron is usually contained in clayey materials as hematite (Fe2O3) and less fre-
quently as goethite [FeO (OH)], limonite or carbonate.
Iron carbonate decomposes at 460 °C as per the following reaction:

FeCO3 (s) —> FeO (s) + CO2 (g)

At approximately 400 °C iron hydroxide changes into ferric oxide, which is sta-
ble in an oxidizing atmosphere (assuming the partial pressure of oxygen to be hi-
gher than its decomposition pressure).
Without oxygen, hematite can, instead, progressively decompose and lose oxy-
gen:

Fe2O3—> Fe3O4—> FeO—> Fe (7)


hematite magnetite wustite metallic iron

On the other hand, Fe2O3 iron oxide, with carbon oxide and hydrogen (CO and
H2) can be reduced even further at temperatures above 550 °C.

– Working conditions that help eliminate black core problems


Back core problems can be reduced by:
• Avoiding the use of high percentages of raw materials (clays) containing orga-
nic substances and/or inorganic compounds such as (bivalent) Fe.
There is no clear-cut upper limit for these materials as development of black
core depends on many factors (firing cycle, tile size and thickness, pressing pres-
sure, type of glaze used).
• Formulating compositions that give the ceramic tile sufficient permeability to
improve oxidation reactions during the pre-heating phase.

In this case too, coming up with specific solutions that aid the development of
high permeability lattices – and thus the escape of reaction gases – is no easy task.
Nevertheless, the production process must adopt all those measures, where compa-
tible with other parameters, that help bring about this situation.

• Optimisation of the firing curve


Last but not least come in-kiln firing conditions.
With some materials the prevention of black core requires that the firing curve
includes a zone of constant or slowly rising temperature between 300 and 700 °C.
This aids decomposition and oxidation and also facilitates outflow of gases befo-
re the glaze melts and traps them.
Bear in mind that the above temperature ranges may shift depending on body
characteristics and the glaze softening point.

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• Modification of the kiln atmosphere in the pre-heating zone


It has been demonstrated that increasing the partial pressure of oxygen in the
pre-heating zone reduces or even eliminates black core; this can be done by increa-
sing the volumes of primary combustion air being fed to the burners.

– Efflorescences
Efflorescences are salt concentrations which appear on the surface of fired tiles
when more than a certain percentage of soluble salts is present in the body.
High concentrations are caused by migration of salty solutions through the po-
rous lattice of the tile, causing their accumulation, over-saturation and precipita-
tion in areas where water evaporation is fastest.
Soluble salt concentrations remaining equal, the problem is more evident on
tiles with more permeable bodies.
Soluble salts have various origins: they may be an intrinsic element in the raw
materials or form during firing as chemical reactions take place among the different
components or between the latter and the combustion gases surrounding the tiles.
Generally speaking, the soluble salts that cause efflorescences are already pre-
sent in the clayey raw materials or originate from:
• gases produced by combustion (SO3)
• water used in production (sulphides, chlorides, nitrates).

In addition to the most soluble sulphates and chlorides in the raw materials, even
low-solubility sulphates such as Ca and Mg and others can cause efflorescences.
Manufacturing defects attributable to the presence of soluble salts appear as
yellow-brownish stains, holes or bubbles on the surface of the glaze or, in some
cases, as detachments of the glaze from the body (fig. 12).
Yellow-brownish staining may be caused by the presence of iron and manganese
soluble salts.

Fig. 12.

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Defects

Sometimes the above defects also depend on:


• hygrometric state of the ambient air: high levels of humidity and high ambient
temperatures tend to concentrate the salts on the perimeter or the corners of
the tile.
• firing conditions: the in-kiln dynamics of air volumes and combustion air turn-
over are critical factors in eliminating/limiting aggression on the glaze.

The importance of eliminating or minimising the raw materials containing the-


se salts is self-evident.
If this is not possible corrections may be attempted as follows:
• try to precipitate the soluble salts in the form of insoluble salts with double
exchange reactions. In the case of sulphates the addition of barium carbonate
during grinding may produce good results. Added amounts of these salts must
be batched stoichiometrically vis-à-vis the percentages of the already present
salts so as not to worsen the situation.
• in double firing: fire the biscuit at higher temperatures to aid fixing of SO3, Cl
ions in the ceramic body (this can reduce efflorescence but sometimes worsen
glaze defects).
• vice versa, reducing the biscuit firing temperature can, in some cases, increase its
porosity. This greatly reduces glazed tile defects because, as the water evapora-
tes, the soluble salts are concentrated inside the biscuit and do not affect the
glaze surface.

Problems attributable to the technological characteristics of the body

A proper treatise of this complex subject is beyond the scope of this volume:
problems associated with technological aspects of the body differ widely depending
on the product (floor or wall tiles) and the employed technology (double or single-
firing).
Nevertheless, the following pages summarise some of the more general con-
cepts associated with the various product families below:
A) White firing vitrified floor tiles
B) Red firing vitrified floor tiles
C) Porcelain floor tiles
D) White firing porous wall tiles
E) Red firing porous wall tiles.

Product families A, B and C are generally obtained through single fire techno-
logy.
Families, D and E can, instead, be produced using either double or single fire
processes; the problems will differ.
The most frequent problems affecting the different body types are:

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• Body deflocculation problems


Deflocculation difficulties, with all product families, may necessitate the use of
higher percentages of water at the body grinding stage.
Such problems may be caused by:
– the nature of the minerals in the clays
– very fine particle-size distribution of clayey particles
– organic materials (humic acids or other) in excessive percentages
– high percentages of soluble salts.

• Pressing problems
Affecting all groups.
While actual defects may be different their technological causes are generally
similar:
– mineralogical origin of the clays making up the bodies
– excessively fine particle-size distribution of the clays or other minerals
– particles flat (two dimensional), acicular or fibrous
– plasticity” or non-plasticity of the body

causing:
– lamination or peeling
– low bending strength values
– dirty moulds.

Lamination involves powder stratification, which prevents the release of the air
contained in the powders themselves and therefore inhibits pressing performance.
Low post-pressing bending strength results in frequent tile breakages in both double
and single fire plants. Excessively dirty moulds result in costly cleaning-related stop-
pages, common with steel dies but relatively rare with rubber-lined or resin ones.

• Drying problems
These differ depending on production technology (single or traditional double
firing).
However, their causes are generally to be found in:
– the nature of the clayey minerals
– the excessively fine particle-size distribution of the clays
– atypical behaviour of pressed tiles during the drying phase (high expansion and low
bending strength).

These aspects or conditions of the raw materials making up the body may lead
to the following production problems:
– excessive shrinkage during drying
– low post-drying bending strength.

The defect is more evident where single fire technology is used as the tile is
exposed to more mechanical stress, especially on the glazing lines.

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Defects

Generally, the bending strength of a ceramic product after drying should be


higher than 25 kg/cm2.
Other defects are influenced by:
– drier management (drying curve)
– moisture content of tiles entering the drier
– hygrometric / general conditions of air.

Problems associated with the nature of the raw materials that appear
after firing

Like much of the previous subject matter, an in-depth treatise of these problems
would require a book in itself. The variables that depend on sintering or vitrifica-
tion are many and their interaction is highly complex. Hence only a general de-
scription is given. Good vitrification or sintering of the body evidently depends on
the quality of the raw materials, their ratios and reactivity among the different
components (oxides). It is obvious the characteristics such as:
– high bending strengths
– low shrinkage
– product-compatible porosity
– wide firing range
– mainly depend on the origin of the raw materials and their reactivity.

Low dimensional stability during the firing process is, without doubt, more fre-
quent in vitrified materials (groups A, B, C) where dimensional variations are more
evident. The associated problems are ones of geometry (orthogonality), dimensio-
nal variation, sides (squareness) etc.
The narrower the firing range, the more evident the defects.
While the origin of the problem may also lie in the production process (pressing,
firing etc.), it is the nature of the raw materials (i.e. the organic content and clay
particle size) – and thus body composition – that play the key role.
The stability of a vitrifiable composition is, in fact, regulated by the extent of the
vitreous flows being formed and their viscosity. It is known that white firing bodies
have wider stability ranges than red firing ones because of the nature of the glasses
being formed and their higher viscosity. The phenomena is highly complex and de-
pendent on many interlinked chemical-physical factors. Body composition or, rather,
the nature of the raw materials, has much influence on the severity of the defect.

Other defects associated with raw materials

a) Excessive drying shrinkage


This usually causes several small edge cracks some 1 to 1.5 cm long, many usual-
ly appearing on each side. This defect is typical of many high-plasticity clays and
generally appears because the low bending strength of the green product is unable

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to withstand the mechanical stress caused by shrinkage. For most pressed tiles the
dry shrinkage limit is around 0.25-0.30%.
This defect may result from clays extracted from different parts of a quarry or
from their insufficient homogenisation. Shrinkage can be checked via simple labora-
tory tests.

b) Low green tile bending strength


This defect tends to cause frequent breakages in both single and double fire
products either when tiles are turned over or loaded into the rapid driers. However,
the resulting unfired waste can be reintroduced into the mill and is fully recyclable.
To obviate this problem bending strength should be no lower than 0.7-0.8 N/mm2.

c) Low dried tile bending strength


Causes frequent breakages at critical stress points on glazing and conveying
lines.
Dry bending strength should normally be no lower than 1.8-2.5 N/mm2. The
defect has its origins in the clay percentage or low plasticity.

d) Excessive free quartz


An increase in the percentage of free quartz in a body formula increases its
expansion coefficient, the alpha-beta inversion at 575 °C and the corresponding
mechanical stress.
Dilatometric analysis will identify quartz variations.
If the quartz does not react (and change into silicate) during firing, cooling-
induced “creep” can also occur.

e) Low fired bending strength


Results in inferior finished product resistance and customer complaints of wast-
age during tile laying.
Insufficient reaction and sintering of the clay and non-clay components in the
body lie at the heart of this problem, which may arise because of changes in either
percentage or particle size distribution.
As with the above defects, routine checks on technological characteristics gener-
ally prevent this problem.

Body preparation defects

a) Insufficient grinding
The effects of insufficient grinding differ depending on whether the body has a
single component or is an actual compound.
In the former case there is a slight change in surface appearance and reduced
bending strength, in many cases only slight and difficult to detect.
The latter case is a more serious affair, with coarser particles delaying important
reactions (i.e. carbonate degassing).

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Defects

The usual outcome is that the tile falls outside required physical-mechanical to-
lerances.
Prevention and correction of this defect generally involves checking slip sieving
residues and, when possible, the particle size distribution pattern.

b) Inconsistent moisture content in powders to be pressed


This defect usually occurs when the powder to be pressed has not been mixed in
draining it from the various silos or stored long enough for moisture content to
homogenise throughout the silo. The phenomenon is more frequent in dry grinding
processes. The first effect is a tendency towards lamination; green and dry bending
strengths are also found to be inconsistent.
With spray-dried powders the problem is less serious because the moisture is
concentrated inside, not outside, the particles.
Moisture control is usually performed on powders sampled from different points
of the conveyor belt over a time span of approximately one minute.
Differences in moisture content can be reduced by storing spray dried products
for at least 24 hours and dry ground wetted ones for 36-40 hours.

c) Excessive moisture content in powders to be pressed


The first effect of excess moisture is that the powder tends to stick to the die,
thus requiring more frequent mould cleaning.
Note that in fast fire processes excess powder moisture causes, indirectly, black
core.

d) Low moisture content in powders to be pressed


Low moisture content makes pressing more difficult and can lead to lamination
and de-moulding problems.
Note that powders with a low moisture content tend to have higher pressing
expansion. This increased expansion results in greater friction against the die li-
ners when the lower punch ejects the tile. It can also cause low green bending
strength and subsequent breakage later on in production.

e) Excessively fine particle size of the powder to be pressed


Causes lamination defects as a result of the low bulk density of the powder and
the considerable air that needs to be expelled.

f) Excessively coarse particle size


This gives a rough tile surface with a granular appearance.
Further troubles include frequent dirtying of the dies.

g) Particle size separation


Particularly seen in the production of porcelain tile, this problem occurs where
particle segregation in the press hopper causes the outer die cavities to be filled
with grains coarser than those in the inner cavities. The defect is extremely detri-
mental when various coloured powders are mixed (e.g. salt and pepper).

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Generally speaking, it is necessary to use spray-dried powders of uniform parti-


cle size distribution (in the 0.3-0.5 mm range).

h) Encrustation lumps
These appear because condensate forms in the storage silos, the elevators and
the hoppers. As moisture content and density in these lumps differ from those in the
rest of the powder, their firing behaviour is also different.
In the most evident cases, small cracks form around the lump on account of
shrinkage differences. In less evident cases small depressions form on the surface of
the glaze because of lower absorption in the areas affected by the lumps.
To eliminate the defect the powder is passed through finer mesh sieves prior to
the press feed point and efforts are made to prevent the lumps forming in the first
place.

Pressing defects

– Dirty dies
The problem shows up as surface defects on the just-pressed product and can
remain after glazing and firing (fig. 13, left). The quality of the die surface is highly
important as any wear-induced roughness causes powder to stick to the die more
easily. Rubber-coated dies help prevent this problem and can drastically reduce the
frequency with which cleaning needs to be carried out.

Fig. 13.

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Defects

– Lamination
The defect consists of foliated stratification of the material that can sometimes
be seen only after glazing and firing (fig. 14).

Fig. 14.

It has several possible causes:


1) When the first entry speed of the punch is excessive and does not allow air to
escape from the powder.
2) When the punch lifting time between the first and the second entry is too brief
to allow escape of the air.
3) When die construction is erroneous and clearances (which should take into ac-
count the working temperature of the die) between the liners and punches are
too narrow.

– Defects caused by ejection difficulties


This defect usually appears as:
– cracks running from the sides to the middle of the tile, but without necessarily
affecting the edges themselves (fig. 15).
– planarity defects.

There are various causes:


1) The upper punch moves too fast during ejection.
2) The die liners are not properly tapered, thus preventing normal expansion of
the piece.
3) The interval between the end of pressing and the beginning of ejection is too
long.
4) Excessive mould wear.
5) Unsuitable back pattern.

– Flash on tile edges (residues compacted between liners and punch)


This defect is generally observed at the end of the brushing and fettling opera-

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tions carried out on the collecting station. It can occur on both the face and back of
the tile. The cause lies in excessive mould wear.
The flash that forms during pressing on the edges of the surface to be glazed is
usually removed by brushes, while the larger flashes on the back of the tile are
removed by scrapers.
Small bits of flash sticking on the surface to be glazed can cause visual defects
and selection losses (fig. 13, right).

– Filling defects
Non-uniformity of filling depends on filler box regulation and causes different
densities at different points on the tile usually detected by thickness checks and bulk
density measurements with either a penetrometer or mercury densometer.

Fig. 15.

– Excessive pressure
In the fast single fire process excessive pressure can cause black core.
The particles are packed so tightly that the gas produced by the (sometimes
incomplete) combustion of the organic substances is unable to escape.

Glaze and glazing defects

There follows a description of the most commonly encountered defects.

Defects caused by the glaze

a) Excessive or insufficient grinding


Over-grinding has a negative effect on glazes with very high surface tension
such as zircon whites where shrinkage causes cuts or cracks to appear on the glaze
before melting.
The effects of unusual particle size distribution are many. For example, an over-
ground rustic corundum glaze will have a non-vitrified surface on account of excess-
ive refractoriness, while excessive grinding of a glaze to which zircon sand materials
have been added also produces cracks that do not close during melting.

354
Defects

Considerable changes in surface appearance aside, excessive grinding always


produces a glaze of higher water absorption capacity, thus causing drying prob-
lems. When glaze grinding residue is too high (materials ground for a short time)
the glaze is difficult to sieve and normally has low viscosity and settles easily.
Problems can be avoided by screening and checking residue at all mills before
the material is used in production.

b) Lack of plasticity
“Plasticity”, where it refers to a glaze, is an improper term, yet one widely used
to indicate its capacity to adhere to a tile body.
The problem is often difficult to detect on the green tile as it generally appears
during the initial stages of firing, when the glaze first starts to shrink and then
melt; because it does not stick to the body properly, it tends to “crawl” away from
the body.
In single-firing, adhesives of the C.M.C. type often need to be used.
This adhesive is also useful in resolving glaze detachment problems in the dou-
ble fire process.
Plasticity can also be improved by using ball clays, kaolins (these can be added in
percentages of 8-10%) and bentonites (up to maximum 2%).
The above materials, in addition to exerting a plasticising action, also play an
important role as suspension agents. Proper suspension is important in that it en-
sures consistent application density and prevents separation of the larger particles
by settling.

c) Poor firing stability


Some glazes are highly unstable, sensitive to very small temperature or firing
environment changes. This sensitivity often results in tiles of different shades.

d) Excessive fusibility
The origin of this problem lies in the composition of the glaze itself.
Excess fusibility can cause surface bubbling (pin holes) at the tile sides or where
the glaze layer is thinner.

e) Incomplete frit melting


A problem that clearly has its origins in the frit and normally causes two types
of defect:
1) surface bubbles and other surface defects caused by the escape of gaseous pro-
ducts that have not fully decomposed during melting.
2) partial solubility of components that have not chemically bonded completely.

It is thus important that the supplied frit be subject to in-factory quality control
checks.

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Application defects

a) Glaze detachment
The fired tile has areas of varying size where the glaze has crawled away from
the surface during firing. These zones are generally surrounded by a rounded, thick-
ened border. Such glaze movements can sometimes appear on the sides or edges of
the tile; in other cases they take the form of extensive, thickened “slicks” in the
midst of unglazed zones or may appear as circular holes of varying dimensions.
Factors in preventing this problem include the quantity of plastic material in the
glaze, application thickness, glaze-body adhesion, low grinding times and the un-
fired strength of the glaze.

b) Glaze shrinkage
Tensions between ceramic body and glaze may generate small fractures in the
latter.
Subsequently, where the melted glaze is highly viscous, these fractures are not
sealed; typical of majolica with a high zirconium silicate content, the problem is
much less frequent in most lead compound glazes.
Moreover, where melted glaze surface tension is high, the glaze shrinkage pro-
blem is proportionately high.
Glaze shrinkage (by way of surface tension) is attributable to:
– improper type or quantity of plastic material
– inclusion of special components.

The presence of materials such as zinc oxide, talc, magnesium carbonate, mar-
ble, aluminium hydrate, all characterised by extensive drying and firing shrinkage,
may be the source of such defects. These materials hold significant quantities of
water and influence glaze viscosity.

– Over-grinding
Excessive grinding increases glaze shrinkage and causes loss of adhesion.

– Presence of soluble salts


The use of frits or raw materials of marked solubility can lead to phenomena
similar to those described earlier. The defect tends to appear when manufacturers
use very fine-ground glazes that have been left in slip form for some time.

– Overlapping applications
Glazes not normally subject to shrinkage may produce this problem when:
• the base glaze is dusty or prevents the subsequently applied glaze adhering pro-
perly.
• the second application re-wets the just-dried first layer and causes it to lift off
the body.
• the two glazes are incompatible on account of surface tension and viscosity du-
ring firing.

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Defects

c) Interaction with production processes


Note that these defects often have joint causes and may originate from a combi-
nation of several factors independent of the glaze in itself.

Poor glaze-body match

Incompatibility between body and glaze expansion coefficients can cause serious
defects.
During cooling molten glaze interacts with the body; if the thermal expansion
coefficients of body and glaze differ considerably tensions may arise, causing cracks
in the now hardened glaze (crazing-flaking).

a) Crazing and flaking


If the thermal expansion coefficient of the glaze is higher than that of the body,
the glaze, as it cools below the transformation point, contracts to a relatively grea-
ter extent and thus stretches. If the resulting tension is higher than the modulus of
elasticity of the glaze, breakage occurs. Known as crazing, this defect appears as
hairline fractures.
Vice versa (i.e. when, during cooling, the thermal expansion coefficient of the body
is higher than that of the glaze), the glaze is compressed. This causes it to fracture
into numerous flakes that detach from the tile along the fracture lines, hence the term
“flaking”.
Flaking, nevertheless, is a relatively infrequent phenomenon as compression re-
sistance is some ten times greater than tensile strength.
Experience has shown that it is actually preferable to have glazes that are slightly
compressed as this helps contain any increase in body volume caused by moisture
absorption prior to, during and after laying.
Quite often, crazing appears as a series of localised fractures of circular shape,
mainly at the sides of the tile.

b) Glaze-body interaction
Also deserving of mention are the expansion phenomena caused by interaction
between body and glaze. Acceptable reactivity between body, engobe and glaze is
indispensable if they are to adhere to each other properly and avoid separation due
to edge impact, more frequent with double fire than single fire tiles on account of
their lower reactivity.

Glazed surface defects

Tile surface defects take a multitude of forms.


They rarely have one clearly definable cause but generally stem from a number
of interacting negative factors. These defects rarely affect the functionality of the
tile but can seriously compromise its appearance.

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a) Pin holes on the glaze


These are a frequent problem – and one of the most difficult to eliminate –
characterised by post-firing minute holes, hollows or craters scattered across the
surface in varying concentrations. The holes are created during firing by gaseous
bubbles bursting through the surface tension of the molten glaze.
Under certain conditions this phenomenon does not have any lasting effects as
the molten glaze automatically flows back into the pit and neatly seals it. The key
“gas escape” factors are viscosity and surface tension.
Glaze viscosity at its maturing temperature is an important characteristic as it
determines the capacity of the glaze to spread over the body and form a uniform
layer. More fluid glazes allow more complete, faster evacuation of the gasses entrai-
ned in the vitreous mass. Firing conditions being equal, high viscosity glazes are far
more susceptible to large-size pin holing.
Surface tension also pays a key role: higher tensions tend to aid re-absorption of
residual bubbles during cooling.

Nature and formation of gaseous emissions

a1) Defective fritting


Some glaze constituents do not react perfectly during preparation of the frit
(especially at the melting point) and thus retain a certain instability, re-interacting
with the other constituents of the vitreous mass during the second fire and genera-
ting gas.
Frit instability or heterogeneity is particularly deleterious in rapid firing cycles
as the available reaction times during the second fire are very short indeed. Conse-
quently, gasses may generate defects on the molten surface that do not disappear at
the cooling stage.

a2) Additions in the mill


With rapid firing cycles and where materials need to be added to the mill, it is
important not to use raw materials with degassing or reactivity characteristics that
clash with firing duration and/or temperature. Failure to observe this rule can lead
to dot-like craters, holes and pin holes etc.

a3) Over-firing
Over-firing of the glaze can cause pin holing.
Glazes with a high alkaline or boron oxide content are particularly susceptible to
this defect. These oxides, in fact, tend to volatilise if over-fired, thus giving rise to
the offending bubbles.

a4) Salts
These are usually sulphates and carbonates (especially soluble ones), which can
originate from the body, the grinding water, the pigments, additives or the glaze
itself, and can cause pin holing.

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Defects

Specks in the glaze may have accidental causes such as:


• Contamination of the glaze during the production cycle
• Air retention during application
• Imperfect drying
• Incomplete firing.

b) Depressions (dimples)
Glossy glazes, especially zirconium whites, often have their surface appearance
marred by evident dimples. Appearing as a shallow circular hollow, the defect is
rarely more than 5-6 mm in diameter.
Such imperfections may have their origins in frit grains of large particle size,
usually the result of imperfect sieving.
During melting these grains behave differently from the rest of the vitreous
mass.
On double fire tiles depressions may also be caused by significant variations of
water absorption in the body.

c) Relief grains
Grains standing out from the surface of the glaze are frequently a consequence
of contamination that occurs during the production process.
The defect may also stem from an in-mill addition of zirconium silicate or other
hard materials that have not been suitably ground. In this case the defect is cha-
racterised by easily visible, small, white, protruding specks.

d) Loss of gloss or mattness


Finished tiles sometimes lack the intended shine; instead, their glossiness varies
from one part the tile to another. In other cases the problem appears as variations in
intensity or shade of colour.
Where a highly fusible glaze is applied on a particularly porous body (especially
where the latter is highly siliceous) it can react so intensely with the body that
nearly all of it is absorbed.
This aesthetically weakens the vitreous phase in the glaze to the extent that the
final appearance is significantly altered.
Concentration of those non-vitreous, low-reactivity compounds in the glaze usual-
ly gives rise to opaque and matt surfaces. This defect is frequently accompanied by
the appearance of numerous tiny holes on the surface of the glaze, giving it a spon-
ge-like texture.
We have seen how an excessive tendency toward volatilisation of the alkaline
oxides can cause dots to form.
Glazes sometimes have undissolved phases, usually made up of silica or oxides
(calcium, barium, aluminium, magnesium, tin or chromium) as well as spinels.
If these usually opalescent phases are present on the surface or just beneath it,
the glaze may occasionally be characterised by pseudo-mattness.
Devitrification is a rather complex process and often creates problems. Surfaces
intended to be uniformly matt may have relatively glossy patches or, vice versa,

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glossy glazes may be marred by duller areas. Earlier on we stated that devitrifica-
tion, while dependent on glaze composition, is also heavily influenced by the firing
cycle and, even more so, the cooling pattern.
Generally speaking, where manufacturers using conventional cycles intend to
prevent devitrification, the ratio between the SiO2 and basic oxides in the glaze
should be 3:1. Nevertheless, even where this ratio is maintained (and even where
ratios theoretically more efficient in preventing devitrification are used) the pro-
blem can still arise. This is because not all basic oxides behave the same way. Exces-
sive calcium, magnesium or zinc oxide contents are notorious causes of devitrifica-
tion.
Moreover, the behaviour of the various devitrifying oxides during cooling dif-
fers enormously. Alumina matt glazes, for instance, are highly sensitive to tempera-
ture differences at this stage. Hence these glazes – or those with high ZnO, CaO or
TiO2 contents – have a tendency, under certain conditions, towards non-uniform
surface mattness or glossiness. The most common scenario is where the matt finish
varies from one tile to another, an occurrence largely due to variation of the firing
curve in different sections of the kiln.
Slower cooling, in fact, gives complete devitrification while higher firing tempe-
ratures can increase shininess. This explains why gloss, satin and matt glazes all
appear sensitive to devitrification phenomena when firing cycles are unsuitable.
Other phenomena are closely correlated with devitrification problems. One of
the most common is found in single layer rapid firing kilns where the leading edge
of the tile has a markedly different appearance compared to the rest of it; with matt
or crystallised glazes it looks shiny or bubbled. While evidently connected to coo-
ling – especially direct cooling – this defect stems from the extreme sensitivity of
these glazes vis-à-vis variable cooling temperatures.
In such cases the thermal inertia of the kiln walls or even the tile mass itself
may be sufficient to cause that non-uniformity. Depending on circumstances, these
differences can then give rise to an overly rapid increase in viscosity with conse-
quent bubbling, lack of devitrification and the appearance of shiny areas on the tile.

e) Sulphur
The damaging effects of sulphates contained in the tile body, the raw materials,
the grinding water or the sulphur compounds in kiln fumes give rise to a whole
series of finished tile defects. The most common are opalescence, surface halos, pin
holes, bubbling, devitrification and creasing (wrinkling) at the sides.
These defects usually appear more frequently when highly alkaline compositions
are used.
The alkali are usually introduced into the glaze as frits. Nevertheless, when the-
se frits are insufficiently rich in silica, boric oxide or alumina, or if they have a
certain reactivity due to incomplete fritting, the alkali may remain open to attack by
any sulphur oxides.
Reactions of the above type (i.e. determined by sulphur in the composition or the
kiln fumes) are also likely to occur during fritting, although tests have yet to con-
firm this hypothesis.

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Defects

The amount of sulphuric and sulphurous oxide contained in the combustion


fumes varies depending on firing conditions. Oxidising atmospheres, particularly
during the initial stages of firing, tend to accentuate sulphuric oxide production.
The concomitant presence of high quantities of water vapour (from removal of
water from the tiles and decomposition of hydrates) can form sulphuric acid.
This attacks any basic components of the glaze (especially lead, calcium, magne-
sium) not securely bonded to the silica or other acid components of the glaze.
Sulphates – extremely damaging as they do not decompose easily at high tempe-
ratures – thus form. These salts generally tend to form thin films on the surface of
the tile, giving rise to devitrified areas. When these compounds are concentrated
(e.g. at the edges), creasing or bubbling occurs.
The phenomena described thus far could be detrimental in rapid double firing.

The influence of stains

The introduction of colouring oxides can generate defects on the surface of


the glaze after firing. Such phenomena can generally be traced to unsuitable or
incomplete pigment preparation, or interaction of the latter with some glaze com-
ponents.
A description of the most common production plant problems follows.

a) Volatilisation
Some colouring oxides are subject to volatilisation phenomena, giving rise to
numerous defects on the tile surface during firing.
Chromium oxides, for example, are used extensively in ceramics on account of
their excellent colouring power and relative stability. Nevertheless, pure chromium
oxide has a strong tendency to generate halos because of the sheer intensity of its
colouring power, despite the fact that its vapour pressure is low and its volatilisation
ratio not particularly high.
Halos can be eliminated via calcination and subsequent oxide washing.

b) Calcination
Calcination is a key phase in the pigment preparation, its purpose differing accord-
ing to the raw materials in question and the final product type. Generally speaking, it
can be said that, in its simplest form, calcination aims to decompose the constituent
components of a colour at high temperature, causing them to release gas. If non-
calcinated colours are used in glazes they inevitably cause numerous defects such as
specks, bubbling, halos etc.
Where combined with the formation of crystalline lattices, the calcination func-
tion is a much more complex one. These lattices are the product of well mixed raw
materials; during calcination the latter give rise (with the aid of catalysts) to cry-
stalline neo-structures inside which chromophore ions are present by way of ionic
exchange.
The calcination process can also be used to obtain solid oxide solutions with

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improved characteristics as regards the original, individual components. A typical


example of this is calcination of chromium oxide and aluminium hydrate to obtain
a solid solution of the two oxides; this improves stability and reduces volatilisation
of the chromium, especially at high temperatures.

c) Washing
After calcination the colour may still contain a certain quantity of salts subject
to volatilisation. To eliminate these the finely ground oxide is washed, using water
and additives that aid leaching of the soluble compounds. In the above-described
case washing removes that part of the chromium oxide which would otherwise fail
to enter into formation of the solid solution and would be water-soluble, its diffu-
sion subsequently causing halos.
Washing is also indispensable when calcination aims to create a crystalline struc-
ture and uses excess amounts of catalyst and chromophore salts.
The production of zirconates is a classic example. With, for instance, turquoise
zirconate, the process begins with zirconium oxide, quartz, vanadium pentoxide
and catalysing agents.
At the end of calcination the crystalline zircon lattice forms, with ionic diffusion
of vanadium ions. This is usually achieved by introducing an excess of vanadium
pentoxide. This, together with the catalysts only, needs to be washed out after calci-
nation. If the catalysts are not removed they can reduce the colouring power of the
oxide and, because they are usually soluble salts, can cause the relevant defects when
added to the glazes as described above.
Equally detrimental are vanadium salts that have failed to bond inside the lattice.
As vanadium is a powerful fluxing agent, concentration of its salts during drying
generates aggregation zones; when fired, the latter have different fusibility cha-
racteristics compared to the surrounding vitreous mass. Hence glazes with a high
percentage of colours containing vanadium salts may be damaged by post-firing
dimples and non-uniform colour. If the surface is screen printed reactivity is accen-
tuated and some zones may be poorly coloured.

d) Reactions with contaminants


While colouring oxides generally have a certain inertia vis-à-vis the glazes in
which they are dispersed, their sensitivity to the chemical composition of the glaze
is far from negligible. This tends to highlight defects caused by colours reacting
with glaze components or, more frequently, contaminants.
The behaviour of red-pink oxides with a SnO2 - CaO - SiO2 - Cr2O3 composition
is a classic example. These oxides are extremely sensitive to reduction. The pre-
sence of reducing contaminants such as carbon, iron or other metallic particles can
cause alterations to the colouring lattice; the chromium chromophore ion is separa-
ted from the crystalline matrix by the reducers, thus freeing the tin oxide contained
in the lattice. Consequently, the contaminated area is completely de-coloured.
The surface of the finished tile is thus dotted with small white specks caused by
the opacifying action of the tin oxide.
Where the contaminant particle is quite large a dark spot appears at the centre

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Defects

of the affected zone. These defects are usually caused by inefficient removal of iron
from the glaze. Use of magnets and the addition, in small percentages, of oxidants
such as cerium oxide usually resolve the problem.

Glaze application defects

a) Drops falling on tiles


One of the most evident and frequent defects where glaze is applied in disc or
spray gun booths, it is caused by the fall of drops of glaze condensate; these can
form at any point on the inner wall of the booth, often because the air exhaust
suction is insufficient and the pulverised glaze thus condenses on its inner walls.
The defect can occur even where pressure is very low.
Likewise, with discs, the defect may be caused by condensate forming directly in
the disc unit because of imperfect atomisation. The problems may also be caused by
incorrect positioning of the protective screens, which, instead of channelling the
glaze, allow it to splash and form drops that inevitably fall onto transiting tiles.
Vibration transferred to the booth by other items of machinery contributes to the
problem. Wet drops can generally be reduced or eliminated by increasing suction
rates and by keeping all exhaust ducts and filters clean so as to maintain efficiency.

b) Glaze clots (dry agglomerates)


Clots, like drops, are caused by anomalous booth exhaust rates.
Glaze settles on the inner surface of the booth and forms clots that subsequently
detach from the wall and fall onto the surface of the transiting tiles.
The defect appears when exhaust rates are excessive and the glaze hitting the
walls tends to dry and encrust.
Glazes with a high percentage of plastic components are particularly suscepti-
ble to drying, especially where applied at high density. Engobes, owing to their high
plastic component, also tend to cause this defect.
Vibration obviously accentuates this inconvenience as it shakes the crust off the
wall.
The simplest way to prevent this problem is to wash the booths according to a
suitable schedule. Excessive suction or vibration, should, of course, also be elimina-
ted.

c) Stripes and waves with waterfall and bell units


“Stripes” originate from imperfect sieving of the glaze and can appear as imper-
ceptible lines or scratches or even unglazed streaks.
In the first case the defect will probably escape the attention of glazing line
inspectors and only become noticeable on the finished product; in the second case
the defect is evident and the tile is rejected immediately.
The cause is usually a clot or grain that has formed in the orifice, thus modifying
glaze flow at that particular point or even blocking it altogether. In the latter case a
“tear” is seen in the waterfall or veil.

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This defect can be eliminated, or at least limited, by properly sieving the glaze on
the feed line and that recycled from recovery trays. Glaze containers should also be
covered to ensure no contaminants get in.
A similar problem is “waves” on the glaze surface, straight with the waterfalls
and slightly curved with bell units.
They may be-caused by:
• low glaze density or viscosity
• drop speed too high for tile transit speed
• glazing machine frame or floor vibration.

Air bubbles in the glaze tear the veil and cause oval-shaped voids.
With highly plastic glazes washing needs to be carried out at least twice a day to
eliminate the crusts that form on ducts and sieves.

d) Irregular disc application


Applying the glaze by atomising it with centrifugal discs is perhaps the most
commonly used technique in ceramics.
Unfortunately this equipment is often troublesome, especially with larger tiles.
To begin with, glaze application on the right and left hand sides of the tile is asym-
metrical, a problem usually resolved by using two sets of discs that rotate in oppo-
site directions, each applying 50% of the required glaze.
Another defect caused by the discs, especially on large tiles, is the appearance of
so-called stripes, caused by the glaze being deposited in alternating strips of diffe-
rent thickness.
These problems generally stem from poor balancing of the disc unit, thus causing
it to oscillate rhythmically and produce stripes. This explains the trend towards discs
of smaller diameter and precision disc machining to ensure fine-tuned balance. Glaz-
ing machine manufacturers are currently engaged in intensive research activities
aimed at solving both streak and droplet problems.
Following the recent shift towards very large tiles with smooth, uniform sur-
faces, waterfall and bell units are making something of a comeback as they do not
produce the above problems and in any case produce smoother surfaces than disc
units.

e) Non-uniform cup application


This application device is almost no longer used but certain problems/solutions
may be relevant to other devices.
The main defects caused by this type of application unit are:
1) More glaze is deposited on edges parallel to the direction of transit than else-
where. especially on large tiles. The problem can be resolved by increasing cup
rotation speed or increasing the clearance between cup and tiles.
2) Excess glaze is deposited on one side parallel to the direction of transit. In this
case the manufacturer should check that the cup axis is perpendicular and that
both cup and tile are horizontal. The cup also needs to be centred over the tile
flow perfectly, and glaze feed should also be perfectly central.

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Defects

3) If a low density glaze is used less glaze may be deposited on the leading and
trailing edges of the tile. To get round this problem the tiles can be arranged as
a continuous “carpet” under the cup drop device.
4) Slightly arched streaks may be noticed crosswise to the direction of tile transit.
This usually occurs either because the cup is not perfectly centred or because tile
transit speed is excessive with respect to cup rotation speed. Decreasing transit
speed or increasing cup rotation speed and adjusting weight usually solves the
problem, although this does slightly alter the shape of the drop.
5) Drops parallel to tile motion. Mainly caused by too acute an angle of on-tile
drop impact; reducing rotation speed, lifting the cup or inserting diaphragms
along the drop fall trajectory usually resolves the problem.
6) If preparation glazes with intense colours are used or silk-screen printing is
carried out prior to application of a very liquid glaze (scorza), application should
be carried out at considerable distances so that it dries well and avoids any con-
tamination of the glaze used for the cup. Moreover, consistent application of the
glazed requires that absorption be kept constant before it is actually applied.

f) Glaze on back of tile (dirtying)


This defect is caused by glaze sticking to the support items (refractory slabs,
rollers etc.).
Problems can stem from incorrect adjustment of a waterfall orifice or bell (exces-
sively fluid glaze, low tile conveying speed, violent fall of the glaze etc.) or may be
associated with the application method itself, as with cup glazing where “cloudy”
effects require very low density glazes.
Where the problem depends on the glaze application method, the glaze can be
removed from the back of the tile by brushes. Cleaning of fast single firing pro-
ducts is particularly difficult because using dry wire brushes wears the still soft tile
and wet brushes cause water absorption.
In this case engobes are applied after glazing to form a refractory layer between
roller and tile (applications of water repellent before glazing are rarely used).
This problem can drastically reduce the output capacity of a fast single firing
plant. Not only that, it can also raise maintenance costs considerably on account of
high roller replacement rates.

g) Inefficient side fettling or cleaning


Very frequent with both single firing and double firing.
The problem is generally caused by incorrect adjustment of guides and fettling
devices, or because the glaze is not yet dry enough.
The defect can also damage the entire length of the tile side where fettlers are
improperly regulated.
Guides should have only a limited piece alignment effect and should be angled so
as to only contact the bottom edges of the tiles.
Lining the guides with Teflon generally gives good results: Teflon has water-
repellent properties and limits glaze adhesion.

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h) Glaze removal on unfired tiles


Tiles may often collide with one another as they pass through the glazing line;
these knocks tend to detach or chip the glaze and the defect then shows up during
firing as glaze shrinkage.
The situation is critical where gap-free tile “carpets” form (i.e. when the tiles
“bunch up” as conveyor speeds slow).
Generally speaking, this occurs before the silk-screen printing machines and before
the single layer kiln loading or line compensators.
Glaze detachment problems can at least partially be solved by augmenting body-
glaze adhesion with glues while mechanical impacts can be reduced by minimising
speed differences from one conveyor section to the next.

i) Shade differences caused by non-uniform glaze weight


Inconsistent glaze weight/spread performance give rise to differences in colour
and surface appearance, thus making sorting necessary. Such differences do not, in
themselves, necessarily constitute defects. However, incorrect sorting does constitu-
te a defect, and an excessive number of shades makes proper sorting extremely
difficult.
Shade differences that originate on the glazing line may be caused by variations
in glaze density, absorption, body temperature or partial clogging of the glaze ducts.
Density can be kept constant by checking it at fixed intervals; a density check is also
compulsory whenever new glaze is added to the feed tank.
Glaze application weight needs to be closely monitored when absorption time
changes.
Partial clogging of the glaze ducts is especially frequent in nozzles and holed
tubes.
Such problems are best prevented by proper sieving of the glaze and scheduled
washing of the equipment and ducts through which it flows.

l) Too much/little water


This affects density and thus causes some of the defects described above. Note
that too little water, especially with disc glazing, leads to a very grainy, rough sur-
face of poor spreading performance during firing. The outcome is a glaze with a
“hammered” look.
Vice versa, an excessive amount of water causes small craters; cuts on the edges
may also be noticed, especially where multiple glaze coats are applied.
This inconvenience is particularly frequent in on-glaze flame effects, because the
spray gun colour requires a perfectly dry attachment base. On a wet surface it tends
to move and produce the above-mentioned defects.
Another technique often affected by excessive amounts of water is waterfall
washing after application of repellent and glaze, thus resulting in high water quan-
tities being absorbed by the biscuit.

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Defects

Decoration defects

Recent years have seen intense development of screen printing techniques, with
associated ink preparation problems and difficulties in finding suitable vehicles for
machines that have very different operating principles.
A whole subset of defects is linked to these difficulties. The main ones, for flat
screen printing, are:

a) White line on tile side closest to worker


This defect is caused by the lack of screen printing paste on the side of the tile
closest to the operator and parallel to the direction of tile transport.
The screen can be cleaned but the defect often reappears just a few tiles later. If
paste residue is within the proper range and no dry areas are observed on the screen,
proceed as follows:
• Check that the screen is not too close to the tile
• Check that the squeegee is aligned properly
• Check that tile height is aligned with belt support guide
• Check for proper squeegee pressure.

b) White line on tile on side opposite worker (as above)


• Check that the home position of the squeegee is high enough; it must not press the screen
against the tile edge when the tile exits (if it does adjust the shuttle cam)
• Check synchronism of movement between belt and shuttle.

c) Accumulation of glaze at corners


This defect is usually caused by an excessive screen-tile gap.
• Check that the tile is properly aligned between belt and support guide
• Lower the screen over the corner where inconsistent accumulation is observed.

d) Pattern/motif not centred properly


• Check that the screen is positioned and secured properly
• Check that the belts grip the piece firmly.

e) Tile sticks to screen


• Check fixative application is working properly
• Check height of screen above tile.

N.B. Above-tile screen clearance is usually set to 4-5 mm but this can vary as a
function of:
• Screen tension
• Screen fabric
• Screen printing paste viscosity.

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f) Screen breaks and/or splits


This usually occurs over tile edges or corners and is caused by:
• Excessive on-screen squeegee pressure
• Excessive glaze residue
• Screen with poorly “catalysed” gelatine (emulsion).
A well made screen usually has a working life of some 2000-2500 m2 (depending
on tile size).

Firing defects with effects on the glaze

a) Temperature differences
Usually associated with tunnel kilns, but can easily occur on other kiln types.
The result is differences in tile shade or, sometimes, variations in glaze surfaces.
The problem is a serious one because it causes almost imperceptible shade diffe-
rences between adjoining tiles.
This makes sorting particularly difficult.

b) Lack of oxidation
This does not mean that ambient air in the kiln is completely reducing, but,
rather, that there is not enough excess kiln air to ensure so-called scrubbing (air
washing). Hence fume passage zones form, often sufficiently concentrated to cause a
defect; this generally consists of “eggshell” or bubbles on tile corners.
There may also be zones where the air stagnates and is full of glaze vapours.
This nearly always causes surface opacity, sometimes accompanied by pinholes. In
both cases the defect can be corrected by increasing air turbulence and volumes,
thus increasing stack exhaust rates and, consequently, air intake.

c) Incorrect fume flow


Normally appears as surface opacity and can degenerate into “eggshell”. Origi-
nates from improperly regulated pressures that cause some of the fumes from firing
zones to follow the tiles towards the outlet instead of immediately being drawn
towards the stack.
When these tiles cool, condensate can deposit on the surface of the still molten
glaze and thus be incorporated in it.
This problem can be controlled by:
– increasing the air aspirated towards the stack
– increasing counter-flow fume speed to stack
– increasing the volume of direct cooling air.

d) Over/Under-firing of glazes
Excess and insufficient firing often generate similar outcomes (as with fusible and
refractory glazes); the former generates an outer cordon characterised by bubbles or
other defects while the latter can lead to the formation of matt or hammered-looking
surfaces.

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Defects

With floor tile glazes, the matter may be more complex as it is not always possi-
ble to establish whether the tile has been fired too much or too little. For a single
firing glaze with a high percentage of added coarse material and a highly fusible
vitreous base, for example, excessive firing can cause separation of the added mate-
rial, (which remains on the surface) from the glaze (absorbed by the body). The
result is a rough, hard surface, that initially brings to mind an under-firing defect.
In such cases a good understanding of glaze types and firing behaviour is requi-
red.

e) Cycles too fast or too slow for the glazes


Like bodies, glazes may also be affected by fast firing cycles; these can stop the
glass maturing or halt development of desired colour and/or texture.
With simple glazes like transparent or zircon white frits, a hammered appear-
ance may be noticed because the glaze has no time to spread properly.
Floor tile glazes nearly always maintain the same surface area as when they are
unfired; when disc-applied they are consequently never smooth enough.
Despite the cost, manufacturers usually prefer to correct these defects by in-
creasing glaze meltability rather than extend firing cycles.
The latest bell application techniques give green materials a smoother surface
without manufacturers having to use the fluxing agents that, in fast single firing,
affect the geometry of the body.
“Eggshell’ and opacity often occur – especially with highly fusible glazes – on
the edges because of sublimation of components that are then missing from the
composition of the glaze itself. Since the cycle cannot be shortened, the amplitude
of the firing curve is reduced and the duration of maximum temperature is limited.

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Firing defects

Tile bursts in the pre-kiln (explosions)

Abrupt evaporation of water can cause tiles to explode. The problem originates
from excessive water content, be it residual after drying/glazing or reabsorbed du-
ring green tile storage. Firing with water contents above 2% is inadmissible; if
necessary, drying should be extended. As a guideline, drying temperatures in the
250-300 °C range are appropriate. However, such a degree of caution is only re-
quired in critical situations: pre-kiln temperatures are usually in the order of 350-
500 °C. To contain temperatures, which rise significantly when gaps appear in pro-
duction, the air intakes in the pre-kiln channel (through which the fan draws am-
bient air) can be opened.
The occasional explosions of just-glazed tiles with a high concentration of strati-
fied water just below the glaze is not particularly significant here, nor is the bursting
of pieces with de-airing defects (flaking or peeling).

Breakage during preheating

Characterised by fracture lines with ragged edges running from the outer zones
of the tile towards its centre; the glaze tends to penetrate the fracture and round its
edges (fig. 16).
Breakage is caused by the cracking that occurs when edges heat up and shrink
faster than the rest of the tile.
Single fire breakages of this sort are relatively rare and are usually associated
with extreme thermal gradients.
The problem may also appear as cracks some 20-30 mm long; these are nearly
always multiple and never appear at the corners.
They tend to occur at points on the kiln cross-section where temperature in-
creases occur first. The critical range lies between 700 and 900 °C. Very hot flames
under the rollers are the most common cause.
Reducing the temperature of the first/second under-roller burner set by 20-30
°C usually resolves the problem; increasing air flow towards the burners also helps
as this cools the flame.

Fig. 16.

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Defects

Small, almost imperceptible cracks can also appear on lower tile edges at the sides
of the kiln load. These are usually the forerunner of much more evident cracking
during cooling. Pre-heating breakages can also occur at around 800-900 °C because
the load comes into direct contact with cold air. This happens when burners have been
shut down or when rollers have been removed and apertures inadvertently left open.
To all intents and purposes these are actually cooling breakages on already-stiff pie-
ces that have just passed through a critical temperature range.
Preheating damage may also take the form of multiple, tightly packed, short
cracks on the upper edges (fig. 17), sometimes almost covered by the glaze. This
defect sometimes involves the leading edge only (i.e. the part of the tile most ex-
posed to the flow of gasses towards the stack).

Fig. 17.

The problem lies in preheating gradients that are too steep for pieces already
made susceptible to such defects by sharp or ragged, poorly compacted edges, high
stratified moisture contents beneath the glaze and low body plasticity. Worn press
punches can also contribute to the problem, as can intense kiln reagulation for con-
cave deformation at the preheating stage.
Broken corners can also occur during preheating; the line of fracture often gives
the detached corner a characteristic “pistol” shape (fig. 18).
The point at which this defect occurs can be identified simply by inspecting the
bottom of the firing channel: a heap of broken pieces usually indicates where the
trouble lies. Lowering temperature a few tens of degrees usually solves the pro-
blem. Increasing air flow to the burners may also help as this cools the flame.
The broken pieces must be dropped to the kiln hearth through a trap to stop
them obstructing the load.

Fig. 18.

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Other defects – also characterised by ragged fracture lines and rounded edge
glaze – are often mistaken for preheating faults; their true cause, however, is gene-
rally found upstream from the firing process.

a) Long, curving, occasional cracks occurring randomly across the load (fig. 19).

Fig. 19.

Caused by mechanical stress: crucial checkpoints include screen printing, row


accumulation units, conveyors in general and unfired tile box loading/unloading
units.

b) Cracks some 10-30 mm long at the corners, occurring randomly across the load.
Usually caused by inter-tile collisions during row formation. An accumulation
of shards and corner chippings on the floor usually identifies the critical conveyor
point.

c) Cracks in the glaze, parallel to one or more sides of the tile (fig. 20).

d) Similarly, fissures may form inside the piece, again parallel to the sides (fig. 21).
Caused at the pressing stage during ejection of the piece from the die cavity.

e) Slightly divaricated cracks some 20-30 mm long, not localized at any particular
point of the kiln cross-section. Their emergence depends on how long the unfi-
red tiles have been stored. Often seen together with the longitudinal fissures
described in d) (fig. 22).

Fig. 20.

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Defects

Fig. 21.

Fig. 22.

The origin lies in longitudinal breakage that occurs during ejection from the die;
excess water applied during glazing stratifies in the longitudinal fissure and cracks
on the glazed surface then appear during the initial stages of preheating.

f) Small cracks on the glazed surface, often so small as to be confused with pin
holes or on-glaze depressions (fig. 23).
The cause lies in defective ejection from the press die cavity or, more frequently,
application of excess water during glazing.

Fig. 23.

g) So-called “chicken claw” crack (fig. 24).


If the crack does not go all the way through the tile it is most likely the result of
a de-airing fault at the pressing stage (e.g. lamination). Vice versa, where the crack

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Fig. 24.

penetrates the full thickness of the tile, it may have been caused by an impact re-
ceived from below during conveying: for example a pulley with an overly small belt
will jolt against the underside of the tile as it passes over.

h) Laminations causing detachment or even explosion of large plaques from the


surface of the body and consequent crumbling of the piece (fig. 25).

Fig. 25.

This stems from poor de-airing during pressing.

i) Cracks that look just like the preheating cracks described earlier (fig. 16). Where
they can all be traced to the same press cavity, the real cause lies in pressing.
Such defects do not correlate with any particular part of the kiln load but are
generally found on the same area of each tile. Check that the die cavity and/or
punch are in good condition.

Similar cracks can also be produced at the drying stage: they do not appear on
any particular zone of the kiln load but they are consistently localised on a specific
zone of the drier load. In this case the cracks can often be highlighted at the drier
outlet with liquid colorants (e.g. kerosene).
In second fire, complete tile breakage can occur; where this is at random across
the load and seen to intensify at certain moments, it is attributable to existing
lesions in the body that compromise resistance to the tensions generated during
preheating.

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Defects

Cooling breakage (or “cooling cracks”)

This damage originates from excessive tensions generated by non-uniform di-


mensional variations. It is usually associated with the very high cooling ratios that
accompany the inversion of quartz at about 573 °C and results in markedly diffe-
rent temperatures from one area of the tile to another.
Damage risk is higher where the body contains significant quantities of free
quartz, tiles are thick and large, and cooling cycles are rapid.
Rapid cooling gradients or changes in gradient caused by discontinuous tile feed
also increase the likelihood of damage.
The cracks themselves tend to be curved with sharp, clear-cut edges, as with
broken glass. Fissures are never open and are, in fact, often difficult to spot without
a coloured liquid; they always run from the outer edge of the tile towards its centre.
In non-porous products the fracture has a smooth, shiny, conchoid look. Tapping
the tile produces a dull, muffled noise.
Cooling is a three-stage process and takes place in three different kiln sections.
– Initial RAPID COOLING lowers piece temperature to 650-700 °C.
– Subsequent SLOW COOLING gradually cools tiles to at least 550-500 °C.
– A third FINAL COOLING stage cools them to the point where they can be
handled at the kiln outlet.

Any attempt to correct cooling problems should take into account the following:
1 Temperatures detected by thermocouples in the firing kiln are much lower than
the actual temperature of the moving tiles.
2 Pieces at the outsides of the load cool down much faster than pieces in its middle:
this difference is accentuated by steep cooling gradients.
3 Temperatures at the sides of the tile are lower than in its middle; this difference,
accentuated by steeper cooling gradients, is the true cause of tile breakage.
4 Barriers (chicanes) separating firing and cooling zones must be intact; efficient
zone separation is essential for stable regulation of both firing and cooling.

Identifying the point of tile failure

If cooling breakages occur repeatedly in specific zones of the load and specific
situations the manufacturer is provided with useful information on the regulation
error being made.

a) Breakages are localised at one or both extremities of the roller conveyor.


This indicates that damage is occurring in rapid cooling, which is either too
intense or extended.
Correction involves raising the in-zone temperature and closing off one or more
blowers so that each tile spends less time directly under the air jets.
Reducing the stack aperture and thus increasing hot air intake can also help. A
further measure consists of closing the first heat diffuser segment in slow cooling.

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The above-roller thermocouple in the fast cooling zone usually gives a tempera-
ture reading of around 570-600 °C, temperatures being lower where cycles are
faster.
Tiles exiting rapid cooling can be checked for proper temperature with the aid
of a portable thermocouple; this is inserted inside the last roller of the zone. A
reading of 600-620 °C is ideal.

b) Breakages are mainly localised at the centre of the kiln.


Indicative of problems at the start of the final cooling zone: centrally positioned
tiles cool more slowly and may pass under final cooling jets before their temperatu-
re has dropped below 573 °C.
The problem can be corrected by enhancing cooling performance in the first two
cooling stages and/or delaying final cooling.
The dissipators should be opened wider. A moderate increase in stack draught is
also useful, as is reduced hot air intake (especially the initial intake) and closure of
the initial cold air blower in final cooling. The temperature of the last thermo-
couple in the slow cooling zone should be around 480-500 °C.

c) Breakages occur on the first tiles to enter the kiln after a significant gap in pro-
duct flow and persist for several minutes.
Gaps cause cooling temperatures to drop: a reduction of just 50-70 °C can cause
problems.
– Check that, with the air modulation valve in the rapid cooling section closed, the
blowers are not excessively pressurised.
– It may be necessary to reduce heat exchanger efficiency by partially opening the
by-pass valve.
– Check the slow cooling section and make sure the heat dissipator modulating
valve closes completely when temperature drops.
– Generally speaking, it is best to modify kiln volumes by aspirating large volumes
of hot air.
– Check that the thermoregulators in rapid and slow cooling are working proper-
ly.

d) Breakages occur after significant load gaps, not on the first tiles but those fol-
lowing on some minutes after. The problem is usually transitory.
As per c). It is especially important to limit maximum air pressure in rapid cool-
ing.

Crazing

Similar in aspect but very different in origin and nature, crazing is often confu-
sed with cooling cracks. It takes the form of sharp-edged fracturing of the glaze
only and often shows up only with the aid of marker dyes or certain lighting condi-
tions.

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Defects

Crazing is not necessarily evident at the kiln outlet either; it can appear at a
much later stage during long-term de-tensioning, or during re-hydration of the
hygroscopic body. Crazing fracture patterns are highly distinctive: lines do not ne-
cessarily run from edge to middle and tile edges are often unmarred.
The cause of crazing lies not in cooling errors but a poor glaze-body expansion
match that “stretches” the glaze.
Tests can be carried out by putting samples through repeated autoclave cycles
according to a specific protocol. A more empirical way of identifying susceptibility
to crazing is to lay tiles with cement: if the glaze-body match is incorrect crazing
will appear. However, the test can take a long time and is not well controlled.

Uniformity of shrinkage over the kiln cross-section

Attainment of uniform firing is especially difficult where kilns have wide inlets
and are used to produce large tiles. The extent of shrinkage and, more importantly,
the body vitrification range, are crucial in highlighting the effects of even small
temperature differences across the firing channel.
Temperature differences can be quantified and pinpointed by measuring pieces
pressed in the same die cavity and fired in different load positions (all tiles must be
oriented the same way with respect to the press outlet). After marking the tiles to
indicate their position (fig. 26) all the right and then all the left side pieces are
compared.

Fig. 26.

An example is evaluated as follows:


+ 0.5 mm on left side of kiln with respect to middle tile
+ 0.2 mm on right side of kiln with respect to middle tile.

An indistinct comparison between right and left sides includes pressing errors
(0.4 mm on right-hand side of piece).
When checking the tile dimensions comparisons should be made between tiles
all across the kiln section and care should be taken to note any effect resulting from
pressing errors which overlap with firing variations.

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a) The most frequent occurrence is larger tiles in the cooler areas nearer to the
outside edges of the kiln cross-section. Several causes combine to create the
problem (fig. 27):

Fig. 27.

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Defects

– Flame temperature at the nozzle is lower than further away where combustion is
complete.
– Re-circulation of colder ambient air on account of the Venturi effect generated
by flame speed.
– Fumes move more slowly near the walls than in the middle of the channel be-
cause of friction (flow towards chimney).
– Stronger irradiation of centre of the load by perpendicular walls.
– Outward dispersion of roller heat by conduction.
– Aspiration of cold air via improperly plugged roller seats in the firing zone.
– Low-speed cold air blow movement, especially above rollers.

The problem can be corrected on several fronts (fig. 28).

Fig. 28.

– Kiln pressure (see relevant paragraph) must be positive in the firing zone (at
roller height) so as to prevent cold air infiltration; however, pressure should not
be too high.
– Insertion of one or more deflectors at the beginning and inside the firing zone
diverts more fumes towards the tiles near the walls.
– Using a suitable number of burners with semi-radial dispersion above and be-
low the rollers is a tried and tested system that compensates for colder flame
areas near burner nozzles and any intake of colder ambient air.

To fine-tune, air can be dosed to the burners to modify flame temperature and
length.
– Flame deflector screens can also be positioned in front of firing zone burners
beneath the rollers (fig. 29).

b) Irregular shrinkage across the cross-section (known as “candy paper”).


Characterised by shorter tile sides 60-70 cm from the walls and longer ones
adjacent to them (fig. 30).

Here, despite the similarities with case a), erroneous flame geometry (especially
on burners above the rollers) is usually the culprit. Considerable modifications to

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Fig. 29.

Fig. 30.

flame speed and geometry are usually required. An easy and often effective solution
is to shut down a burner in those sets that markedly influence size; alternatively, the
flow of burner air can be modified.

c) Other, differently configured, irregularities can also occur; depending on the si-
tuation, their solution may require use of the above solutions or even their direct
opposites.

Glaze brilliance and shade

In terms of shine, satin effects, opacity, spread and shade the final outcome of
glazing essentially depends on the high temperature firing stage. Higher tempera-
tures or extended firing time results in more compact vitrification of the glaze and
thus improves shine. Longer times at relatively lower temperatures give a satin look
and better (flatter) spread. Much, of course, depends on the nature of the glaze, the
limitations of which are inevitably highlighted by pin holes and micro-bubbles if
temperatures are too high. The appearance of satiny effects (clouding of the glaze
at certain points of the load) indicates a combustion defect on one or more burners
in the high temperature zone; a check on (and possible increase in) the flow of
combustion air is generally required.
Shade changes across the load are the result of temperature gradients. “Lustre”

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Defects

applications, for instance, are particularly sensitive to overheating and can easily
vanish.
Where strongly reactive colouring oxides are used (iron, selenium etc.), longer
firing is known to disturb colour development. Hence iron oxide veers towards
green where firing lasts longer and red where firing is shorter and sharper.

Pin holes - holes - bubbles in the glaze

These are caused by small gas bubbles that expand in the glaze and burst, leaving
a small crater on the surface. Gas bubbles have numerous causes.
Sectioning a defective tile and taking a close look at its interior can provide
valuable information. Using a magnifying glass or pocket microscope, it is good
practice to observe the glaze along the line of fracture, paying special attention to
the nature of the trapped bubbles.

– Bubbles are very small, densely packed and close to the surface.
This defect stems from very low melting viscosity or over-firing, causing the
glaze to boil. Generally attributable to overly hot flames on the last above-roller
burners or, more simply, too high a firing temperature (fig. 31).

Fig. 31.

– Bubbles observed in body of glaze only; bubbles that are forming, incomplete or
touching the body are not observed (fig. 32).

Fig. 32.

Indicative of high melting viscosity or low quality glaze containing impurities.


May also indicate a glaze preparation (milling) or application (bubbling) error. The
problem cannot be solved by adjusting the kiln.
This defect also occurs when glaze is applied to an excessively hot body, thus
causing water vapour to form between body, engobe and glaze.

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– In addition to those in the glaze, other bubbles are seen to be forming in the body
and rising off it (fig. 33).

Fig. 33.

The most likely cause in this case is incomplete degassing prior to glaze soften-
ing:
– black core, especially if it is stratified near the glaze or takes the form of specks
scattered through the body.
– carbonate degassing problems, an eventuality more or less limited to monoporo-
sa products: the defects are larger than pin holes and the underlying engobe is
frequently exposed.
– pyrite degassing with SO2 emission: in this case the tiles need to be held at 1040-
1050 °C for several minutes (frequently solved by fine sieving of the body slip).

Confirmation that degassing is involved in the pin holing problem is usually


provided by a simple double fire test:
– some unglazed pieces are sampled at the drier outlet and then fired to fully degas
them. They are then passed through the glazing stations, ensuring that each
inter-station time lapse is long enough to let water be absorbed or evaporate.

The samples are then re-fired: absence of bubbles in the glaze confirms that
body degassing was the cause.
There may also be larger holes in the glaze. These have various causes:
– late degassing of body carbonates, especially where their particles are quite co-
arse. In this event the 920-980 °C firing time needs to be extended. Body grin-
ding and composition must be checked.
– thin, compacted flakes of body, especially from the sides of the die box, work
their way into the tile body or flakes/powder stick to its surface at the time of
ejection from the press: in the kiln this causes micro-peeling.

The only solution is to ensure that dies are kept clean by suction/blower devices.
Pin holes, holes and bubbles in the glaze may also be caused by defects in the
glaze or its application:
– grinding and sieving
– viscosity and rheology
– CMC deterioration
– incompatible glaze-engobe melting points

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Defects

– high screen print stickiness compromises adhesion of glaze to underlying en-


gobe or body
– glazing on excessively hot body
– inadequate spacing between glazing units
– poor glaze-body adhesion
– overlaying of incompatible glazes.

In some cases extending the firing time towards 500-600 °C may be useful; it
will, in any case, be necessary to eliminate the cause of the problem by correcting
glaze and glazing technology.

Degassing

All ceramic bodies lose a considerable amount of weight during firing.


Mainly by the loss of residual process water and the water in the clays. The rest
is attributable to gasses and vapours produced by the combustion of organic conta-
minants, the decomposition of carbonates (especially CaCO3) and sulphur compounds
etc. Gas generation occurs during “preheating”, a stage that ends with the forma-
tion of the first vitreous phases, which rapidly reduce permeability. This generally
occurs at 980-1000 °C in single fire operations and around 1100 °C with porcelain
tiles.
High temperatures also generate vapours (fluorine, chlorine etc.); while they do
not necessarily cause product defects, they often attack the refractory and steel parts
of the kiln structure.
Other vapours released by the glaze (lead, boron compounds etc.) can easily con-
dense on the kiln walls and roof, resulting in the fall of droplets and damage to
transiting tiles.
The theory behind degassing is a simple one: the aim is to raise the material to a
temperature at which gasses and vapours develop as quickly as possible and then
hold the temperature for as long as it takes for all the gasses to escape. The “best”
temperature is the highest possible (but, of course, still below the body and glaze
vitrification point).
Degassing problems depend on several factors:
– composition, purity and particle size of raw materials
– thickness, density and moisture content of pressed tile
– fusibility of glaze and frit
– characteristics and quantities of screen printing inks and their media (vehicles).

The prevailing opinion is that a richly oxygenated preheating environment aids


degassing; this is true only in part and in any case needs further explanation. For
instance, the flow of exiting gas may stop ambient oxygen penetrating the piece.
However, it is true that burners fed with excess air supply all the required ener-
gy and high volumes at “low” temperature: this makes overheating – and thus early
development of the vitreous phase and reduced permeability – less likely.

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Similarly, good fume draught is helpful. The first degassing benefit is not the
draught-induced vacuum, which might erroneously be thought of as “sucking” the
gases out of the tile, but the considerable quantities of hot volumes drawn in from
the firing zone; these allow a reduction in gas flow to the pre-heating burners (and
thus lower flame temperatures).

Degassing in double fire processes

Since the biscuit has already been fired once the second fire is usually free from
degassing problems. Nevertheless, problems may arise with biscuits that have been
put through rapid firing cycles and then left “on hold” for some time after application
of the glaze. The problem may be caused by water (from glaze, or absorbed by hygro-
scopy) reacting with calcium oxide (CaO) residues left over from the first fire (in long-
term storage it could transform into CaCO3 again). The resulting defects take the
form of evident, foamy bubbles and bare sections of body, often confused with glaze
adhesion problems. In this event it is good practice to extend the preheating time
below 550-950 °C both by easing the temperature gradient and slowing the cycle.

Black core

This defect has already been dealt with in the section on defects associated with
raw materials (see Appendix 3: Defects, Organic material).
It takes the form of a halo, ranging in colour from yellow-green to grey or black,
in the tile interior. The problem can also appear as simple black specks dispersed
throughout the body. Black core is caused by incomplete combustion of organic
residues in the body or by subtraction of oxygen from iron oxides: in any case, it is
always a reduction phenomenon.
Black core would not, in itself, constitute a problem (often normal in extruded
products) were it not associated with other defects such as:
– pin holes and bubbles in the glaze
– glaze porosity and its stain resistance
– differently shaded halos and spots
– appearance of back pattern on the face of the tile
– dimensional and planarity defects.

The most suitable firing range for elimination of black core generally lies between
880 and 960 °C. While the bulk of good quality glazes have a softening point of
around 980-1000 °C, note that a few low-fluxing glazes seal pores at just 680-700 °C;
where the latter are used the firing cycle will need to be slowed down considerably.
High-temperature glazes and bodies allow preheating to be extended towards
1100 °C. No less important than optimal temperature is duration of exposure to
effective degassing temperatures. Maximum efficiency is obtained by keeping tem-
peratures high at the start of preheating and low in the approach to the firing zone:

384
Defects

here, it may be useful to blow air through switched off burners (taking care not to
generate significant temperature differences above and below the rollers as these
can change tile planarity).
Good degassing requires abundant volumes, both from the firing and cooling
zones and the burners. Hence any cooling adjustment that exhausts a lot of hot air
(cooling stack) is to be avoided.
Degassing problems also raise energy costs. The use of more refined raw ma-
terials and tile technology should thus be attentively evaluated.

Black core can appear as:


– a localised halo in the “core” of the tile or as scattered specks (fig. 34)
– an under-glaze halo that fades towards the centre of the tile (fig. 35).

Glaze reaches its softening point too quickly and prevents degassing of the body.

Fig. 34.

Fig. 35.

– A localised halo at the core of the tile that fades towards the glaze (fig. 36).

Fig. 36.

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High temperature preheating time too brief or under-roller temperature at end of


preheating is too high.
– Halos limited to areas of lenticular cross-section (fig. 37).

Fig. 37.

Highlights non-uniform pressed piece density caused by a die filling defect or


accumulation of fine powder.
Where intensity is low the defect can generally be resolved by holding the opti-
mum degassing temperature long enough.
– Rather than halos, there may be evident swelling of small, circumscribed areas.
Such cases are generally sporadic (see fig. 38).

Fig. 38.

The intensity of the phenomenon means that it cannot be resolved via kiln adjust-
ment. Swelling is usually caused by drops of machine oil, carbon particles formed
by poor spray drier combustion or other body contaminants (even very wet or high
density grains).

Planarity defects

Precise diagnosis of planarity problems requires in-depth observation of the


defects. Deformation profiles, small differences between one area of the load and
another, variations caused by specific events and circumstances and links with other
problems are all, in the light of product characteristics, essential if a reasonable
hypothesis is to be developed and then tested.
Planarity defects are not necessarily caused by malfunctioning or incorrectly
adjusted kilns; more properly, it should be said that the kiln is often unable to elimi-
nate errors that occurred upstream from it. A poor dilatometric (thermal expan-

386
Defects

sion) match between body, glaze and engobe is a frequent cause; alternatively, the
problem may be associated with heterogeneous tile density or the low structural
strength of very molten, very thin or specially shaped pieces.
However, that is certainly not to say that proper kiln adjustment never solves the
problem: it often does. Sometimes it merely attenuates the defect and sometimes it
has no effect at all: in any case, close collaboration between kiln operators and tech-
nologists is essential if an effective plan of action is to be developed.
Controlling tile planarity largely involves control of the consequences of linear
shrinkage during firing.
– Imagine a tile cross-section: if the face of the tile is subject to higher temperatu-
res than the back then it will shrink more, causing the tile to bend and become
concave; vice versa, if the underside of the tile is exposed to more heat, the back
of the tile contracts more and makes the tile convex.
– Only a small area of a convex/concave tile actually rests on the rollers. Once the
body reaches its softening point, the unsupported part of the tile, tends to col-
lapse under its own weight: this secondary deformation works in the opposite
direction to the initial one caused by temperature differences.

Because it takes time for the tile to soften and collapse, this secondary effect
takes place at the same time as the curvature effects of thermal expansions occur at
the beginning-middle of the firing zone.
– Because the edges of the tile heat up faster than the middle, an appreciable tem-
perature difference during the brief final firing stage can accentuate concavity
or convexity at the corners.

Planarity problems can also result from non-uniform cooling of tile face and
back: this changes both the moment in which the glaze “locks” to the body and
influences the relationship between glaze and thermal body expansion.
Smooth, clean, straight rollers are essential for orderly in-kiln movement of
tiles and the prevention of mechanically-induced warping and planarity deforma-
tions. There follows a description of the most common planarity defects.

Downturned corners

All four tile corners droop (usually the outermost 3 cm or so); the rest of the
surface is essentially flat or slightly convex (fig. 39).
The defect is distributed throughout the load and is constant; deformation is
slightly reduced at the ends of the loaded tiles (head and tail).
Corrections should be made in the final firing zone by raising temperature above
the roller plane and reducing temperature below it.
Diagnosis should be effected with care as it is easy to confuse this defect with
others, different in nature, that are similar at first glance but quite different when
observed more closely (figs. 40-41).

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Fig. 39.

Fig. 40.

Fig. 41.

Upturned corners

All the tile corners are upturned (outermost 3 cm); the rest of the surface is
essentially flat or slightly concave (fig. 42).

Fig. 42.

The defect is distributed evenly throughout the load and is constant; deforma-
tion is slightly reduced at the ends of the loaded tiles.
Corrections should be made in the final firing zone, where it will be necessary to
lower the temperature above the roller plane and increase temperature below it.
Diagnosis requires caution as it is easy to confuse this defect with others, different
in nature, that are similar at first glance (figs. 43-44).

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Defects

Fig. 43.

Fig. 44.

Convexity

Homogeneous downward bending of all tiles, with similar deformation profiles


on all four sides (fig. 45).

Fig. 45.

One of the most frequent and difficult planarity problems as the defect stems
from glaze-body expansion incompatibility. Factors such as engobe, glaze-body thick-
ness ratio, tile density, tile size, degree of vitrification, back pattern and others all
influence this problem. The temperature curve in itself rarely causes convexity:
only a central-final firing zone characterised by higher below-roller temperatures is
capable of doing this.
However, this is not to say that kiln adjustment cannot provide solutions; in many
cases results are rather good. Nevertheless not all products respond to adjustment
the same way, hence the need to distinguish between different product types. For
instance, with single fire floor tile we can hypothesise:

a) Correction in Rapid Cooling Zone


Below-roller direct blowing is intensified at the start of rapid cooling. This re-
duces convexity throughout the piece, especially on sides parallel to the rollers. By
cooling the body earlier the latter contracts before the glaze “locks” and opposes it.
This difference between sides parallel to the rollers and those at right angles
to them may be explained by the fact that they undergo different cooling pro-
cesses. Parallel sides (leading and trailing tile sides) are cooled “all in one go”

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while sides at right angles to them are cooled “from one end to the other” as the
tile advances (fig. 46).

Fig. 46.

Meaningful correction results can only be achieved with properly designed final
cooling zones: there should be a fair concentration of blowers beneath the roller
planes, especially in the first section, and each blower must have a certain output
rate; it should also be possible to shut off corresponding above-roller blowers.
Additionally, more hot air can be aspirated into the cooling area; this air stratifies
above the rollers and keeps the glaze hot for longer, thus delaying its attachment to the
body. Removing the rollers immediately above the bottom blowers also helps. Avoid
overly dense packing of tiles in rapid cooling (i.e. maintain space between lines).
Similar results are also attainable with unglazed porcelain tiles, especially large
ones. However, no discernable advantages have been observed with porous pro-
ducts (monoporosa, biscuit, glazed double firing).
Considerable temperature differences (hot tiles on top of the rollers and cold air
under) can cause evident roller deformation. This, in turn, generates asymmetry
and overlapping of tiles. The only way out of this quandary is to use specially
designed rollers with high heat transmission coefficients.

b) Correction in the Firing Zone


Takes the form of a firing curve structured to give higher below-roller tempera-
tures in the initial section, from 1050 °C to just beyond peak temperature. The
difference is usually 20-30 °C, but may require peaks of 50-60 °C. Convexity cor-
rection is always slightly more marked on sides at right angles to the rollers than on
those parallel to them (fig. 47).

Fig. 47.

The dynamics of correction may be illustrated as follows:

Stage 1
Higher temperatures beneath the roller cause the bottom of the tile to shrink
faster than the top: the piece thus becomes convex (fig. 48).

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Defects

- t°
– SHRINKAGE
+ SHRINKAGE
+ t°
Fig. 48.

As the tile shrinks it also becomes soft.

Stage 2
In passing from one roller to another the convex tile rests on its leading and
trailing edges (black areas): the central section is suspended (fig. 49).

Convex tile rests on leading and


trailing edges only (black area).

Fig. 49.

The whole of the weight rests on the points of contact (fig. 50).

~8cm

– SHRINKAGE
+ SHRINKAGE

Support zones

Fig. 50.

Gravity causes the tile to flex and droop.

Stage 3
Firing continues: the face of the tile is now exposed to temperatures and shrinka-
ges similar to those on the back, thus causing concavity (fig. 51).
= t°
= SHRINKAGE

= t°
Fig. 51.

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Sides parallel to the rollers are rather more uniformly supported (or suspended)
and anti-convexity correction is visibly modest.

Over-correction can produce a defect characterised by upturned leading and trail-


ing edges affecting sections some 8 cm long (fig. 52)

~8 cm

~8 cm

Fig. 52.

or the “priest hat” deformation (fig. 53).

Fig. 53.

Higher above-roller temperatures in the final firing and/or maximum tempera-


ture zone may also prove useful, possibly involving shutdown of burners below the
rollers.

Excessive correction in this sense can, however, produce the “priest hat” effect
and produce upturned corners (fig. 54).

Fig. 54.

Concavity

Homogeneous upward curving of all tiles with similar deformation profiles on


all four sides (fig. 55).

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Defects

Fig. 55.

A somewhat rare defect: if it were caused by an erroneous glaze-body expansion


match the glaze would be “stretched” and crazing would result. Concave deforma-
tion is often transitory in nature, being caused by accidental kiln shutdown or ma-
croscopic errors in the firing curve.

Correction at the start of the firing zone


Takes the form of a firing curve structured to give higher above-roller tempe-
ratures in the first section, from 1050 °C to just beyond peak temperature. The
temperature difference may be as high as 50-60 °C.

The resultant correction is spread uniformly over the four sides.

The dynamics of concavity correction are similar to those for convexity.

Stage 1
Higher temperatures above the roller plane cause the face of the tile to shrink
sooner than the back: the piece thus becomes concave (fig. 56).

+ T°

Fig. 56. - T°

Shrinkage is accompanied by softening.

Stage 2
In passing from one roller to another, the concave tile rests on its middle; the
remaining peripheral areas are suspended (fig. 57).

Constantly suspended
part of tile (black areas)

Fig. 57.

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The whole weight of the tile is supported on the central part in contact with the
rollers (fig. 58).

Suspended areas

Fig. 58.

As the suspended areas press down the tile tends to flex and flatten out (fig. 59).

+ shrinkage %

– shrinkage %

Fig. 59.

Stage 3
Firing continues: the back of the tile is now exposed to temperatures and shrink-
ages similar to those on the face, thus causing convexity (fig. 60).

= T°
= shrinkage %

= T°
Fig. 60.

Exaggerated corrective action can produce a central asymmetric hump between


the leading and trailing edges (fig. 61) (i.e. only central part of tile is convex).

Fig. 61.

Correction at the end of firing


Higher below-roller temperatures in final firing and in the maximum tempera-
ture range are also useful; this may involve the shutdown of burners above the
rollers.

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Defects

Excessive correction in this sense can, however, produce deformation (fig. 62).

downturned edges

roller effect (porpoising)

Fig. 62.

Correction in the rapid cooling zone


Concentrating blown air above the rollers at the start of the zone is useful.
Maximum efficiency is obtained by pointing the blowers not at the tiles but to-
wards the kiln roof and “bunching” the tile rows as close together as possible by
decreasing rapid cooling zone roller speed.
This accelerates hardening/locking of the glaze, thus increasing the effect of
glaze-body thermal expansion coefficient differences.

Roller effect

A classic single-fire defect (fig. 63).


8 cm

3 cm

Fig. 63.

The defect only involves the sides of the tile at right angles to the rollers; the
two sides parallel to them are perfectly straight or only slightly convex.
A central area, generally flat or slightly concave, is bracketed by evidently upwar-
dly bent strips, some 8 cm wide, on the leading and trailing edges. The last 3 cm of
those strips curve downwards.

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This deformation has a number of possible causes:

1. Below-roller heating in the firing zone (or at least in its central and final sec-
tion) is excessive. The piece thus becomes convex on account of relatively
more intense underside shrinkage; as the tile advances only its leading and
trailing edges are supported by the rollers (fig. 64).

Fig. 64.

The now decidedly soft piece is unable to sustain its own weight and the central
section of the tile collapses.
If this is the case deformation is resolved by increasing temperature above the
rollers and decreasing temperature to the same extent below them: correction
should begin at the end of the firing zone and then “retreat” back towards its
beginning.

2. Greater below-roller heating at the start of the firing zone causes relatively great-
er shrinkage of the tile underside, thus making it convex (fig. 65).

- T°

SHRINKAGE
+ T°
Fig. 65.

Shrinking is accompanied by softening. Because only the leading and trailing


edges of the tile rest on the rollers the piece deforms as described in the CON-
VEXITY paragraph and on exiting the kiln will be concave, but with a tighter
radius over the outermost 8 cm of the leading and trailing edges (fig. 66). Such
defects are easily confused with others (CONCAVITY or UPTURNED CORNERS)
and often erroneously “corrected” by increasing below-roller temperatures in the
final firing zone (fig. 67).

8 cm 8 cm
Fig. 66.

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Defects

3 cm
Fig. 67.

Because the tiles remain in this section for only a short period “correction” in-
fluences the corners only, thus causing the outermost 3 cm of the leading and trai-
ling edges to become convex.

In this event deformation can be resolved by:


– FIRST: increasing the temperature above the rollers at the end of the firing
zone and then lowering it to the same extent below them.

The resulting deformation is as illustrated in fig. 66.


– THEN: increasing the temperature above the rollers at the start of the firing
zone and lowering it to the same extent below them.

3. There is a somewhat rarer third scenario, limited to products fired at very high
temperatures. Known also as the ROLLER EFFECT, it is fairly evident but has
gentler curves (fig. 68).

Fig. 68.

Solving this sort of problem requires an altogether different kind of approach.


Temperatures below the rollers need to be increased considerably and temperatures
above them reduced: this needs to be done from the beginning of firing onwards
and inevitably involves an intermediate “priest hat” stage.

Priest hat

Frequently observed where glaze and body expansion coefficients are significantly
different (i.e. mainly with glossy glazes and grains, especially where applied thickly,
in monoporosa and floor tile).
Characterised by a central convex area with a peak at the geometric centre of
the tile and upturned extremities, particularly over the last 3-4 cm at right angles to
the rollers (fig. 69).

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Fig. 69.

Where the defect is mild the ends appear flattened. The radius of the central,
convex curve remains unchanged (fig. 70).

Fig. 70.

Priest hat can also be caused by an attempt to resolve convexity (by increasing
above-roller temperatures at the end or in the central section of the firing zone).
In this event bringing the temperature differences back within more acceptable
limits and applying a more suitable anti-convexity stratagem will usually suffice.
May also be caused by excess temperatures below the rollers in the initial firing
zone. There are two possible approaches:
– bring temperature differences back within more acceptable limits.
– force the existing adjustment by increasing the temperature differential, exten-
ding it into the central firing zone and, if necessary, into the final firing zone
with higher below rollers temperatures.

Note that where such adjustment is performed on products without any particu-
lar expansion match problems, the end result is the “roller effect” (fig. 71).

which represents the exact


opposite of “priest hat”

Fig. 71.

Where “priest hat” develops at the start of firing there often follows asymmetric
warping caused by irregular feed, pieces bumping into each other and overlapping.
These secondary deformations tend to mask the “priest hat” itself and can delay its
identification.
Problem solving thus needs to be prioritised: first “priest hat”, then warping.
Given their associations, the two are often eliminated simultaneously.

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Defects

Asymmetric deformation or warping

Irregular deformation, mostly occurring on sides at right angles to the rollers


and corresponding to specific positions on the load (fig. 72).

Fig. 72.

The appearance of tiles like those in the illustrations should be taken as a warn-
ing sign that the rollers need cleaning: this is, in any case, always the first measure
that needs to be taken.
This defect always stems from tiles which are not lying flat on the rollers.

There are two possible causes:


1. Evident heat-induced tile deformation destabilises the tiles, causing them to pitch,
roll and rotate around their centre and advance or retreat with respect to the other
tiles in the row (fig. 73).

Fig. 73.

They thus tend to overrun the inter-tile gap (spacer) and bump into each other
or overlap.
The best approach is to adjust the temperature curve and eliminate or attenuate
the differences that caused tile deformation in the first place.

2. The quality and characteristics of rollers in the firing zone.


Ceramic rollers, now commonplace, must meet certain dimensional requisites
(inter-roller gap, temperature range, load bearing capacity, geometric uniformity)
and have certain qualitative characteristics (hot bending strength, modulus of ela-
sticity etc.).
Observation of any kiln shows that rollers flex constantly under the weight of
the tiles.
However, because load density is never fully homogeneous or continuous, gaps
between rows and poor tile alignment sometimes allow rollers to straighten out
momentarily.

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It thus follows that where properly arranged, aligned, straight tiles “jump” from
a flexed or bent roller to a straight one and vice versa, asymmetric non-identical
deformations can result.
The problem is intensified by worn, dirty rollers and the random mixing of
rollers of different quality.

Solutions:
– Adjust tile feed density so as to minimise inter-row gaps: a “compact” load makes
it harder for individual tiles to leave the formation and thus re-arrange it.
– Depending on planarity priorities, use temperature settings that prevent conca-
vity in preheating, and avoid tiles moving around and becoming disordered or
out of line.
– Use specially shaped rollers that are thicker in the middle: these correct and
compensate for the arch-shaped rows that stem from relatively higher speeds at
the sides of the kiln. A number of these rollers, properly distributed, can impro-
ve the situation considerably.
– In the rapid cooling zone, the beginning of which is especially critical, the often
evident roller deformation produced by temperature differences between the he-
ated part of the load and the simultaneously cooled part can be disastrous. The
solution lies in reducing roller blowing to a minimum. Stability and reliability
can also be increased by using rollers of high thermal conductivity (in silicon
carbide or blends of silicon carbide and refractory) that deform little if at all.
– Sometimes, the only answer is to replace a number of rollers with others of
better quality, especially in the firing zone (less bending under load).

Such defects have no easy diagnosis or solution. The best approach is to analyse
the situation from several angles and apply a “blend” of possible solutions.
Other deformations regard only porcelain tile manufacture. Well-defined strips
that droop at the leading and trailing ends (fig. 74) is one such example. This pro-
blem is more frequent with thin, highly vitrified products.

Fig. 74.

This defect is caused by intense softening and inter-roller distance: as the tile pas-
ses from one roller to the next, overhanging portions droop under their own weight.
– The only solution is to drastically reduce below-roller temperature at the end of
the firing zone; this may involve shutdown of some burners and/or use of blown
air. Vitrification is affected only slightly.
– A wide variety of evident, widespread warping is more likely to be seen on double

400
Defects

filling products (even where pressing results seem good); the problem, however, is
also seen with traditional die filling.

Rapid cooling, with abundant quantities of air blown through above-roller tubes
only, sometimes provides an effective solution.
Directing air jets upwards and compacting the load by slowing down roller speeds
increases the effectiveness of this adjustment.
Nevertheless, in other cases it may be useful to use only blowers below the rollers
and direct the jets upwards at the tiles.
Hard and fast rules are elusive and manufacturers will need to evaluate problems
and take action on a case by case basis.

Monoporosa

The complexities of the monoporosa firing process have yet to be fully under-
stood and are still a cause of much debate.
However, attentive observation in a variety of situations has already produced a
wealth of experience that allows the monoporosa technician to solve at least the
most common problems.

Convex planarity (Monoporosa)

Convex planarity occurs during cooling. It is particularly evident during the


allotropic β→α quartz conversion at around 573 °C. This phenomenon is easily
observed by removing a tile via an inspection hatch near the rapid cooling zone:
hold the piece with a pair of tongs and it bends before your eyes.
The extent of deformation largely depends on the tensions generated by the diffe-
rent expansion coefficients of body, glaze and engobe, their relative thickness, the
extent of back pattern protrusion, pressed tile density, ambient moisture content and
tile ageing etc. The role played by individual parameters varies from product to pro-
duct. Fig. 75 shows how expansion varies over the firing range. It goes without saying
that quality tiles are only obtained where such parameters are optimised.
As long as tile “design error” remains within “reasonable” limits there are seve-
ral ways of nullifying it via kiln adjustment.
Bear in mind that the porous nature of the body leads to absorption of atmo-
spheric moisture and, consequently, moisture expansion. If that expansion over-
stretches the glaze the end result is crazing. Hence “reasonable error” means that
the tile body must still contract more than the glaze during cooling, thus ensuring
that latter is compressed, albeit minimally, under all circumstances.
Because porous bodies can expand on absorbing moisture, the tile must leave the
kiln with its glaze under sufficient compression so that it always remains so through-
out the life of the tile. Otherwise crazing results when the glaze comes under
tension.

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EXPANSION %

Fig. 75.

Correction in Preheating
The term PREHEATING usually refers to the low temperature zone in which
degassing occurs, as opposed to the high temperature zone where melting, shrink-
age and thus planarity control take place. With monoporosa that distinction is no
longer applicable because, between 920 and 1020 °C calcium carbonate decomposes
and generates considerable CO2 outflow and, at the same time, the most important
expansion event of the entire firing process takes place.
Anti-convexity measures generally involve application of higher temperatures
below the rollers, a measure that is most effective from 950 °C onwards.
Similar measures are often taken at lower “preheating” temperatures; rarely suc-
cessful on their own, they do provide considerable benefits in conjunction with other
adjustments. Planarity differences on sides parallel to the rollers are minimal, if
they exist at all. No substantial differences in results have been observed by in-
creasing/decreasing burner air volumes or increasing/decreasing flame speed.
However, a gradual approach towards 950-960 °C has proved moderately bene-
ficial.
Under such temperature conditions direct in-kiln observation shows that the
convex tiles pitch on the rollers (fig. 76).

Fig. 76.

402
Defects

Excessive temperature differences above and below the rollers can cause unac-
ceptable deformities; if they are excessive the tile will be deformed at the kiln outlet
as illustrated in fig. 77:

Fig. 77.

Temperature differences between above and below-roller areas may be extended


as far as the 1000-1080 °C range.
In this case marked concavity will probably be observed on sides parallel to the
rollers and the trailing edge is always more concave than the leading edge (fig. 78):
the reason for this is not yet known.

Fig. 78.

Immediately after CONVEX deformation the tile becomes visibly concave, a 30-
40 mm strip all the way round the perimeter of the tile appearing raised; the middle
of the tile is affected to a far lesser extent.

Correction in firing
Anti-convexity action here generally involves application of higher tempera-
tures above the rollers, a measure that essentially becomes effective after 1100 °C.
Temperature differences between the upper and lower kiln areas are in the order of
5-30 °C.
Results are fairly uniform over the four sides of the tile but a little less so over
the load cross-section. Applying these temperature differences influences the part
of shrinkage produced by high temperature sintering (fig. 79):

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EXPANSION %

Fig. 79.

As with floor tiles, the top of the tile receives more heat and shrinks more, thus
making the piece concave (fig. 80):

+ Temperature
+ Shrinkage

– Temperature
– Shrinkage
Fig. 80.

Excessive temperature differences between the above and below-roller areas thus
causes exiting tiles to have the defect illustrated in fig. 81.

Fig. 81.

Correction at the end of the firing zone


The tail end of the firing zone (usually the last 2-4 m and, more rarely, the last 6
m) provides excellent convexity correction opportunities; results are usually homo-
geneous, within the required limits, and do not generate the deformation seen in fig.
82.

404
Defects

Fig. 82.

Correction usually involves shutting down pairs of burners (left-right) below


the rollers, 1-4 or at most 6, and then feeding large volumes of air through them (up
to 40-50 m3/h).
Rather than following the logic of “temperature difference = shrinking differ-
ence”, this correction attenuates the effect of the body expansion on the relatively
lower glaze expansion, thus delaying the moment in which the glaze adheres to the
body. With the body incandescent (over 1100 °C) and the glaze molten (i.e. liquid),
cooling of the body from beneath is begun in advance. The body starts to contract
as per its expansion curve and the liquid glaze follows it without offering any re-
sistance. Correction ends when the glaze stiffens (cools) and starts to follow its own
expansion curve.
This technique allows a part of body expansion to occur before glaze adhesion,
the practical equivalent of a better glaze-body expansion match.
It is not, of course, a system that allows for any increase in glaze heating (i.e. no
increase in above-roller temperature allowed). If this were the case the higher temp-
erature = greater shrinkage rule would apply, resulting in the deformation illustrated
below (fig. 83).

Fig. 83.

An identical technique can be applied with floor tiles, but later, during rapid
cooling.

Non-uniform planarity across the kiln load in monoporosa

Less efficient anti-convexity correction near the kiln walls is a common problem:
the more marked the corrective adjustments the more evident this drop in efficiency
becomes.
This is explained by the fact that, in preheating, temperature differences be-
tween the above and below-roller areas are attenuated by the empty spaces that
form near the walls (between tile load and wall) and, in the above-roller part of the
firing zone, by the fact that it is physically impossible for the burners to heat the

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area near the walls in exactly the same way as they heat the central zone. The sum
of these two phenomena thus reduces correction efficiency.

Solutions
a) Fairly high kiln pressures should always be maintained; ideal firing zone pressu-
res at burner level in the above-roller part of the firing zone are around 0.3-0.4
mm (water column). Note that this pressure must be generated by damping the
exhaust fume flow, not by limiting hot air intake in the cooling zone. In other
words, the solution works if there is an albeit modest flow from firing to cooling,
not vice versa.
b) Appropriate use of the chicanes fitted on the roof can improve matters; these
need to be in good condition and no higher than 80-100 mm. It is essential that
high temperature zones where higher above-roller temperatures have been set
be defined by lowered chicanes. Conversely, any transverse walls below the rol-
lers at the start of or inside the firing zone need to be eliminated.
c) Installing semi-radial burner units above the rollers in the firing zone also helps;
these must be arranged and adjusted so as not to compromise glazing results.
d) Generally speaking, “gradual” rapid cooling settings, with blowers emitting no
more air than is strictly necessary, are to be preferred.

The above also applies to double fire processes (first fire and second glost fire).

Non-uniform planarity over time (Monoporosa)

Small planarity variations caused by small or difficult-to-monitor changes in pro-


duction parameters and/or raw materials are, over a period of hours and days, quite
normal: for the kiln operator, the resultant corrections are all in a day’s work.
Macro alterations at the front of a load following a gap in production are an
altogether different matter.
The alterations that take place in an empty kiln (or, more correctly, one in which
the carpet of tiles that physically separates the above and below-roller zones is
absent) are easily understood.
The burners under the rollers produce more heat than usual and the ones above
them less. The newly introduced load thus enters a kiln in which energy distribu-
tion has been radically altered and effects on planarity are inevitable.
Active adjustment of specific burner gas flow valves has been seen to reduce
deformation, the downside being that the problem then seems to last longer.
It is, perhaps, best to accept this inconvenience as inevitable, leaving gas modula-
tion valves to operate freely, keeping deformation within as narrow a time span as
possible; rejection of the first 10-20 rows following a significant gap in production
is also routine practice.
If post-gap tile deformation persists well beyond those first 10-20 rows, thermo-
regulator and gas modulating valve reaction times need to be speeded up.

406
Defects

Non-uniformity of size across the load cross-section in monoporosa

While monoporosa is characterised by firing shrinkages of around 1%, hetero-


geneous shrinkages of considerable magnitude are far from rare, especially with
large tiles. As with floor tiles, the defect takes the form of increased size at the sides
of the kiln load.
However, the dynamics behind the defect are quite different: with floor tiles the
root cause is lower temperatures near the firing zone walls. With monoporosa, in-
stead, the problem lies in overly-fast heating of the load sides within the 950-1000
°C range, during the fast contraction that correlates with carbonate decomposition,
and the way in which expansion and shrinkage overlap and interfere with each other
(fig. 84).

temperature expansion –
temperature +
shrinkage +

Edge shrinkage is obstructed by


expansion of the centre:
= the edge shrinks less than it should

Edge expansion is
boosted by greater
residual expansion
SHRINKAGE

of centre
= the edge remains
EXPANSION
EXPANSION larger.

Fig. 84.

There is no clear-cut solution to this problem.


Experience has shown that spacing the tile rows apart helps as it homogenises
the “gap situation” at the sides of the load.
This evens out the size variation by bringing all the tiles towards the larger end
of the range.
Some success has also been obtained by adjusting pre-heating burners to reduce
temperatures at the load sides. Surer results, however, are to be had by reducing
temperatures beneath the rollers, especially in the 950-1000 °C range (if planarity
control so allows).

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It has yet to be understood why size defects are a constant with certain body
formulations and completely absent with others (fig. 85).

Fig. 85.

Comparison of expansion curves for problematic and problem-free bodies high-


lights that:
– The problem is common where bodies have a high percentage of calcium carbo-
nate.
– Size problems exist where the contraction associated with carbonate decomposi-
tion is more marked.
– Further, marked expansion following carbonate decomposition is decidedly
negative.

Production contamination

Cases vary considerably and tracing the cause of the defect is no easy task.
Analysis of the circumstances under which the phenomenon is more marked,
frequency and distribution across the load, glaze depth at which contamination is
found, size, shape and colour all provide useful clues. A small microscope will prove
indispensable.
In-kiln contamination may be sub-divided into the following groups.
a) Vitreous contamination
b) Ceramic contamination
c) Ferrous metal contamination
d) Non-ferrous metal contamination
e) Carbon contamination.

Note that a contaminant particle produced by the kiln can never sink below the
thickness of the glaze. Its exact position is found by sectioning the tile and exami-
ning the cross-section under the microscope. Contamination by grinding wheels,
welding machines and debris near the production line during assembly and mainte-
nance work is an altogether different matter.

408
Defects

a) Vitreous contamination
Appears as round blotches (drops) of considerable size (1-40 mm in diameter),
mostly yellow, green or brown. The phenomenon initially appears occasionally and
then becomes more frequent with each passing day. Increases in intensity following
significant gaps in the tile feed and substantial variations in the final preheating
zone.
Dependent on the presence of strong contaminants (mainly lead and boron) in
glazes and frits. The vapour from the frits condenses on the roof and walls of the
kiln at temperatures between 850 and 1000 °C.
Excessive accumulation or lower viscosity caused by high temperatures causes it
to drip onto the material in transit: the blotches have an evidently “vitreous” appear-
ance. Note that condensate formation cannot be prevented by kiln adjustment: signifi-
cantly increasing flow rates gives some improvement, but the practical benefits are
limited and the resultant increase in energy consumption is considerable. When vi-
treous contamination begins to compromise sorting yield, the roof must be cleaned.
The rate of condensate accumulation is sometimes high and frequent cooling of
the kiln for cleaning purposes (done by chiselling and scraping) is infeasible. The
alternative is to raise temperature (by 100-150 degrees C) in the 900-1000 degree
°C area for about 2 hours. This sharply decreases viscosity of the condensate, cau-
sing it to run off in large quantities. Needless to say, the underlying rollers must be
protected from the inevitable fouling and must thus be removed beforehand. How-
ever, if the rollers are in poor condition removal is inadvisable: in this event they
should be protected by a ballast (i.e. unglazed tiles) and the rollers should be moved
backward and forward for the entire cleaning period.
Be careful to switch the forward/backward movement on and off frequently enou-
gh to prevent activation of the relevant safety device that shuts off the gas valves.
To facilitate the increase in temperature, keep the “final cooling” fan running and, if
effective, stop the “hot air suction” fan. Monitor the kiln carefully, especially the
inlet where, because of the increase in pressure, there is a risk of damage (photo-
cells, cables, rubber rollers etc.). In any event, cleaning the roof by raising tempera-
ture is an expedient that should be used sparingly. In the long run, repeated heating
can compromise insulation because the refractory material becomes impregnated
(note that the refractory must be cleaned with the kiln cold and that impregnation
reduces cleaning efficiency).
In the long run, the only proper solution to the condensate problem is an intelli-
gent selection of compatible glazes.
Condensates of a powdery aspect may also be observed at low temperatures in
the pre-kiln and in preheating. Here, roof and walls can be cleaned with a jet of
compressed air passed through a metal tube: the latter is inserted through the side
wall hatches under the roof. Combining water with compressed air provides a more
efficient “car-wash” spray clean. Kiln cooling and roller extraction are unnecessary.

b) Ceramic contamination
Ceramic contamination appears as a relatively glossy, small, rounded “dark spot”,
perceptible when scratched with a fingernail.

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Observation with a microscope reveals an aggregate-like aspect typical of cera-


mic material and no halo: cavities are absent.
This is the fine dust that accumulates as “dunes” anywhere there is turbulence
and then detaches as small flakes because of excessive accumulation, vibration or
thermo-dimensional variations.
Flakes may also be produced by overly compact loads (tiles pitching against each
other as they move over the rollers).
Always keep the area around the kiln clean to prevent circulation of dust, bear-
ing in mind that the kiln interior is a low pressure area in which air currents from
all directions converge; this is because large volumes are aspirated by fans and dis-
charged from the chimneys and because of ascending currents produced by the hot
mass of the kiln.
Installing good filters at the combustion air and rapid cooling fan inlets is an
effective preventive measure; these filters must be kept scrupulously clean.

The kiln areas involved in this problem are:


Kiln inlet
– Loading machine structures and guards above the tiles, where dust collects.
– Blowing of the material, especially where autonomous fans are used: fit fans
with filters and periodically clean blower tubes.

Pre-kiln
– Kiln inlet door, above the load: brush and vacuum-clean.
– Roof, fume outlets and walls above the roller plane should be cleaned with com-
pressed air (via a metal tube inserted through special hatches).
– Edges of the ambient air intake in the roof at the end of the pre-kiln: brush and
vacuum-clean.

Burner
Only burners above the roller plane are involved. However, those below the rol-
lers still require regular cleaning to ensure their efficiency. Sand the heater and
electrodes and blow with compressed air.
Clean burner casing with compressed air, tap the air valve and the flex hose
fitting and clean with compressed air.

Rapid cooling
Where contamination originates here it is rigid or just partly molten, rough to
the touch and always on the surface.
Clean the blowers periodically: blow air through them simply by detaching the
flex hose from one side and knock them to detach contamination.
Blow air through the air regulation valve and the flex hose.
Directing the below-roller blowers downwards can lift dust and waste which ine-
vitably settles on the back of the tiles. However, such contamination ends immediate-
ly after the blowers are re-oriented.
In rare cases, and only in double fire operations, the unscraped, under-tile flash

410
Defects

produced by presses with worn punches tears off during the rapid cooling phase
and falls onto the still soft glaze.
This type of contamination takes the form of fragments of elongated shape
with ragged edges sticking to the still molten glaze.
Debris from exploded tiles and the waste produced when workers walk over the
kiln roof or adjust the chicanes and tube valves can also cause problems (but only
occasionally).
Blowing in final cooling is never a source of contamination as this area of the
kiln is already a long way from any molten glaze.

c) Ferrous metal contamination


Appears as a black speck characterized by a small brown ring around a black
nucleus, clearly visible with the microscope; quite frequent but very rarely pro-
duced by the kiln.
To identify the cause section the tile and identify where the problem lies. If the
contamination is produced by the kiln, the defect will always be superficial and poorly
amalgamated with the glaze.
Possible sources of contamination:
– The kiln inlet door (above the rollers) and the piping above it.
– Fume outlets in the kiln, especially where the system is subject to frequent
power failures that cause formation and stagnation of acid condensate and
moisture.

Rub down and brush the door. Pierce the piping insulation at several points and
tap with a hammer and chisel so that any unstable encrusting breaks off.
The rare event of oxidation inside the rapid cooling piping should be monitored
by placing special filters at the consumption points and inspecting pipes internally.
It is inadvisable to direct the above-roller blowers at tiles directly as contamina-
tion does not sink into the glaze and remains very rough to the touch.

d) Non-ferrous metal contamination


Shows up well under microscopic observation on account of its glossy crystal-
line appearance, reminiscent of cast iron fragments, and the absence of the brown
ring produced by partial oxidation of the iron. Possible sources of contamination
include all the exposed stainless steel and refractory parts in the firing channel
above the load and therefore:
– Fibre plate anchors in the pre-kiln roof.

Generally small particles which include body and condensate, these increase
markedly in intensity and density in post-gap loads as a consequence of the in-
crease in pre-kiln temperature.
Clean with compressed air, using a metal tube inserted through the doors.
As soon as the kiln cools brush thoroughly.

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Burners
Particularly heavy duty working conditions can cause the heater to overheat and
deteriorate or “wear out”. Contamination produced in this manner is then put into
circulation by the fast flame.
Contaminant particles are always small and round, their frequency and diffusion
remaining constant and uniform.
The same applies to excessively long starting electrodes: in this case shortening
the electrodes, thus eliminating the part that shows signs of carbonisation, usually
suffices.

Rapid cooling blowers


These produce very small powder-like black specks; contamination increases
sharply following gaps in tile feed.
These metal specks remain on the surface of the tiles and are rough to the touch.
Contamination is caused by deterioration of the blowers above the roller surface,
usually the 2 or 3 closest to the firing section.
Blower deterioration is caused by overheating of the steel: where cooling is
poorly adjusted deterioration can happen quickly.
– Regulate rapid cooling so as to ensure minimum blower cooling when the blown
air modulation valve is open to “minimum”: set pressure no lower than 10 mm
approx (water column).
– Under no circumstances should rapid cooling fan be stopped during the transi-
tory phases of kiln heating or when there are gaps in the load.
– Avoid exposing blowers to fumes in the firing section by adjusting chicane
height between firing and cooling accordingly: inspect chicanes regularly to
make sure they are intact.
– Avoid cooling settings that suck firing fumes towards the rapid cooling zone.

If blower degradation is within reasonable limits, detaching the flexible pipe


from one side and blowing out the accumulated waste will suffice. For more pro-
nounced degradation, remove the blowers, brush them and knock them.
Beyond a certain limit, especially if blowers are evidently deformed, their repla-
cement becomes absolutely necessary.
Lining those blowers most at risk with ceramic fibre prevents contamination
with waste produced on the surface exposed to the firing channel.
Today, silicon carbide blowers are often used. While costly, this material avoids
the above problems.
Blower tubes made of refractory alumino-silicates can be broken by thermal
shock: when breakage occurs jamming of the tiles is inevitably involved.

Heat exchanger
Only rarely a source of contamination, usually because of the care and attention
involved in its design. This type of contamination can easily be identified by the
shape of the metal flakes: lamellar with sharp edges. In this event it is necessary to
brush down the exchanger (with the kiln cold, of course).

412
Defects

e) Carbon contamination
Infrequent and limited to cases where use of fuels such as L.P.G. or liquid fuels
results in poor combustion and thus formation of carbon in the burners.
Appears as small black specks, opaque and ringless (without halo).
Regular cleaning of the burners is essential, as is monitoring and correction of
air-fuel regulation.

413
Printed September 2002
by Tipografia Moderna di Ravenna
for Editrice La Mandragora of Imola

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