Waste Management 30 (2010) 17141719

Contents lists available at ScienceDirect

Waste Management
journal homepage: www.elsevier.com/locate/wasman

Review

Recycling of steel slag and glass cullet from energy saving lamps by fast
ring production of ceramics
E. Furlani *, G. Tonello, S. Maschio
Universit di Udine, Dipartimento di Scienze e Tecnologie Chimiche, Via del Cotonicio 108, 33100 Udine, Italy

a r t i c l e

i n f o

a b s t r a c t

Article history:
Received 20 October 2009
Accepted 23 March 2010
Available online 18 April 2010

The paper reports on some experimental results obtained from the production of ceramics containing
steel slag and glass cullet from exhaust energy saving lamps mixed in different proportions. Blending
of components was done by attrition milling. Pressed powders were fast red (50 min, cold to cold) in
air up to several temperatures in the range 10001140 C. The sintering behaviour was studied by shrinkage and water absorption measurements. Density, strength and hardness of the red bodies were determined and XRD were examined. The red samples were nally tested in acidic environment in order to
evaluate their elution behaviour and consequently their possible environmental compatibility. It is
observed that the composition containing 60 wt.% of steel slag and 40 wt.% of glass cullet displayed
the best overall behaviour.
2010 Elsevier Ltd. All rights reserved.

Contents
1.
2.
3.
4.

Introduction . . . . . . . . .
Materials and methods
Results and discussion .
Concluding remarks . . .
Acknowledgement . . . .
References . . . . . . . . . .

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1. Introduction
Steelmaking slag (SS), one of the most common industrial
waste, is a by-product of steel production. One ton of steel implies
the production of 130200 kg of slag, depending on the composition of the steel and on the steel production process. Slag often appear as granulated materials containing large clusters, coarse and
very ne particles; they have high softening temperature and
two different phenomena are noticeable due to the large amounts
of lime and silica the slag contains: the rst phenomenon occurs as
a consequence of the reaction between the silica and lime which
form, at high temperatures, together with other phases, 2CaOSiO2
which is polymorph and transforms the slag, on cooling, into a
phase having a larger specic volume (Barnes et al., 1980); the second phenomenon is due to the presence of free lime particles in the
slag which cause grain swelling. Both the above phenomena cause

* Corresponding author. Tel.: +39 432558877; fax: +39 432558803.

E-mail addresses: erika.furlani@uniud.it (E. Furlani), gabriele.tonello@uniud.it
(G. Tonello), stef.maschio@uniud.it (S. Maschio).
0956-053X/$ - see front matter 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.wasman.2010.03.030

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1714
1715
1715
1719
1719
1719

volumetric instabilities which are a great disadvantage when slag

is used, without any additional treatment, as raw materials for
most of recycling processes. In order to limit such volumetric instabilities, various methods have been proposed such as long term
weathering, treatment of the liquid slag by injecting oxygen and
silica, autoclaving of the slag in slag baskets (Tossavainen and Liud,
2008) conversion into hot metals or useful mineral products
through high temperature smelting reduction (Fleischander et al.,
2004; Fleischander and Daum, 2006) and others (Geiseler, 1996;
Shi and Hu, 2003). Nevertheless, the great amount of SS produced
all over the world implies that their recycling is presently necessary not only due to the rising cost of their landll disposal which,
in turn, is reected on the cost of the steel produced, but also as a
consequence of the zero-waste objective which must be the nal
goal of all future human activities.
The use of SS in cements and/or concrete manufacturing is presently considered the most promising way for recycling as it is proposed by several authors (Altun and Ylmaz, 2002; Chen et al.,
2007; Kourounis et al., 2007; Lun et al., 2008; Manso et al., 2005;
Monshi and Asgarani, 1999; Qasrawi et al., 2009; Shoaib et al.,

1715

E. Furlani et al. / Waste Management 30 (2010) 17141719

2000) even if alternative options such as the production of ceramics or more in detail wall tiles have been proposed (Favoni et al.,
2005; Fiori and Brusa, 1983; Marcis et al., 2005; Porreca et al.,
2007).
Glass cullet (GC), recycled from waste bottles or windows, is
classied, in the European Waste Catalogue, as a non-dangerous
waste. Presently it is recycled and is commonly used, for example,
as additive in glass reforming due to its low softening temperature.
Conversely, GC from exhaust energy saving lamps often contains
mercury vapours and, before an eventual landll disposal or recycling, mercury must be removed by a specic washing. This type of
GC mainly derive from industrial buildings and represents a little
fraction of the total production of GC, but most of existing waste
ofcial norms establish that this type of GC cannot be recycled
by glass production. It follows that, in order to propose some easy
and environmental friendly ways for the recycling, alternative
methods to landll disposal are now under study. The present paper suggests the use, in mixture with steel slag, as raw materials
for the production of ceramics. More in particular it is evaluated
if some mixtures of the above two components displays properties
which make them suitable for the industrial production of tiles.
The aim of the paper is to demonstrate that, proper mixtures of
waste materials can compensate one the chemical composition of
the other and, consequently, be used to substitute natural materials in existing industrial implants, with limited changes in the processing parameters, for the production of tiles that satisfy the
ofcial standards for production. For this purpose, in the present
research, some processing parameters, namely pressing and sintering conditions, were the same as to those used by the industry for
the production of tiles.

2. Materials and methods

The SS was a by-product of a Basic Oxygen Furnace obtained
from the production of a high manganese steel; before the use it
was previously naturally weathered for 5 months outside the foundry and transformed into a coarse powder by a mortar in our laboratory. The GC used in the present work was an Hg free product,
containing SiO2, B2O3, CaO, Na2O and Al2O3 as most abundant components and minimal fractions of P2O5, TiO2, MgO, K2O and Fe2O3.
It was received by a society responsible for waste collection and it
was handly transformed into a coarse powder by a mortar.
The composition of the above powdered materials, obtained by
a Spectro Mass 2000 Induced Coupled Plasma (ICP) mass spectrometer, is reported, in terms of oxides, in Table 1.
The present work refers to materials obtained by mixing SS with
10, 20, 30 and 40 wt.% of GC, their symbolic names being respectively SG1, SG2, SG3 and SG4.
Each blend was homogenized by attrition milling for 3 h using a
home made attritor mill with high density nylon container and
high alumina balls. The attrition milling time was set at 3 h on
the basis of results obtained by the particles size distribution
(PSD) measurements performed by an Horiba LA950 laser scattering particle size distribution analyzer: analyses were made in
water and, before their analysis, all powders were sonicated for
3 min. In the present paper, the PSD curve of the milled SG2 powder is represented with logarithmic abscissa.
After milling, slurries were dried in an oven at 80 C and dried
powders had a residual H2O content of 4 wt.%. After drying, powders were sieved (300 lm sieve) and uniaxially pressed at
30 MPa into parallelepipedal tiles (50  70  7 mm).
Green samples were sintered in air, by an electric gradient kiln,
at temperatures ranging from 1000 to 1140 C using fast ring cycles with a heating rate of 50 C/min, a cooling rate of 60 C/min
and a D-well time of 10 min.

Table 1
Composition, expressed as oxide wt.%, of GC and granulated SS; undetermined
indicates the cumulative quantity of all oxides determined in quantity lower than
0.01 wt.%.
Component

GC

SS

SiO2
Al2O3
CaO
MgO
SrO
BaO
Na2O
K2O
B2O3
Fe2O3
ZrO2
Cr2O3
TiO2
MnO2
P2O5
CuO
SnO2
V2O5
PbO
SO@
4
Cl
Undetermined

63.40
6.42
3.66
1.03
0.02
0.19
5.44
1.65
11.36
0.76
0.01
<0.01
1.19
<0.01
2.03
<0.01
0.28
<0.01
0.74
<0.01
<0.01
1.82

13.26
7.79
37.88
11.63
<0.01
0.17
<0.01
<0.01
<0.01
9.75
0.33
0.91
<0.01
13.42
1.24
0.59
0.05
0.20
<0.01
0.04
<0.01
2.78

Shrinkage on ring was evaluated along the longest sample

dimension by a caliper using the ratio (h0  h1)/h0 (subscripts 0
and 1 referring to sample dimensions before and after the
sintering).
Water absorption was determined following the norm EN99. In
line with this procedure, sintered samples were rst weighed in air
(W1), then placed into a covered beaker and boiled in water for 2 h.
After boiling, samples were cooled in water to room temperature,
dried with a cloth and weighed again (W2). Water absorption
was evaluated using the formula: W (%) = [(W2  W1)/W1]100.
Concerning materials apparent density, specimens volume was
determined by a caliper and mass by an analytical balance. Such
methods imply measurements errors which generally do not exceed 5% of the real value. In the present research we have observed
data variation always below 2% which was considered not signicant and therefore not discussed.
Mechanical properties were measured only on tiles red at
1040 C. Rupture strength (r) was evaluated by 4-point bending
with a crosshead speed of 0.2 mm  min1 using Shimadzu AG10
equipment whereas Vickers hardness (Hv) was determined by a
100 N load with a Zwick indenter on polished surfaces (6 lm diamond paste). Strength and hardness data reported in the present
paper are all averaged over 10 measurements.
Crystal phases were investigated between 20 and 80 by X-ray
diffraction (XRD) analysis which was carried out on a Panalytical
Xpert Pro Detector Xcelerator using monochromated CuKa1 radiation (40 kV, 40 mA).
In order to test materials leaching resistance, crushed red samples with granules size in the range 0.52 mm were aged by H2O/
HCl solutions at a constant pH = 4 for 30 d at 60 C (pH value was
adjusted daily); a weight ratio 80% of liquid and 20% of solid was
used. Leachate was analyzed by ICP.
3. Results and discussion
Table 1 shows the chemical composition of GC, and SS powders
in terms of oxides percentages. It is displayed that, as expected,
SiO2 is the major component of GC which also contains relevant
quantities of B2O3, CaO, Na2O and Al2O3. On the other hand, the
major component of SS is CaO, but also SiO2, MnO2, Fe2O3 and

1716

E. Furlani et al. / Waste Management 30 (2010) 17141719

Fig. 1. X-ray diffraction pattern, between 20 and 80, of the SS material. The symbols used to identify the phases are as follows: () = portlandite; (4) = glaucochroite;
(h) = iron manganese oxide; (N) = calcite; (j) = magnetite; (s) = calcium silicate.

Al2O3 are largely present. The large amount of manganese and iron
oxide is highlighted by the dark grey colour of the SS powder used.
Even now, it is possible to observe that the great amount of CaO,
present in the SS, is progressively diluted by the increasing additions of GC in the prepared compositions. The absence of relevant
quantities of toxic compounds can be remarked as well as the low
level of Cl and SO@
4 ions.
Fig. 1 shows the X-ray diffraction pattern of the SS powder. It is
observed that glaucochroite ((CaMn)2SiO4 PDF 00-014-0376) is
the main phase of SS which also contains portlandite (Ca(OH)2
PDF 01-087-0674), calcite (CaCO3 PDF 01-081-2027), iron manganese oxide (FeO0.198MnO0.802 PDF 01-077-2361) magnetite
(Fe3O4 PDF 01-089-0950) and calcium silicate (Ca2SiO4 PDF
01-087-1256); other phases are also present in small amounts,
but it was not possible to identify them unambiguously.
The as received granulated SS contains ne particles (around
1 lm) as well as large agglomerates with dimension of several millimetres whereas the original GC consisted of particles with
dimensions in the range 210 mm. In order to obtain powders suitable for an easy pressing procedure, all the mixtures were homogenized by attrition milling. After some tests, the milling time was
set to 3 h since it was observed that, after a 3 h milling, the amount
of particles with a size larger than 10 lm is low and powders properties are not greatly affected by longer milling times. Fig. 2 shows,
as an example, the PSD curve of the blend SG2 after the milling
process; PSD curves very similar to the one reported in the paper
were obtained on the other compositions, but they are not reported in the paper. It can be observed that powders display a

Fig. 2. PSD curve of the blend SG2 after attrition milling.

Fig. 3. Water absorption versus sintering temperature of the materials produced.

monomodal distribution of particles displaying a single peak with

maximum around 10 lm. Such a ne powders PSD which is coupled with the residual H2O content allow an easy manual pressing
of the powders into parallelepipedal shaped samples.
Water absorption, directly related to the open residual porosity,
and linear shrinkage are essential parameters normally acquired to
build up the sintering curves; these are then used for ring cycles
optimization. Fig. 3 reports water absorption versus ring temperature of the compositions tested. It can be observed that composition SG1 displays high water absorption (>15%) at all temperatures.
Addition of 20 wt.% of GC (material SG2) permits to reduce water
absorption after the cycles at 1100, 1120 and 1140 C; lower sintering temperatures lead to materials with high water absorption
values. It follows ring cycles up to 1140 C are not sufcient to
display a stable sintering process for the above two compositions,
but higher temperatures could lead to products with better performances. However, the maximum temperature of 1140 C was chosen in order to conform to standard industrial productions.
Materials SG3 and SG4 display water absorption trends much more
at than SG1 and SG2 have, but both them melt between 1080 and
1120 C. The presence of small bubbles was observed on the free
surfaces of the samples with these compositions after the sintering
cycle at 1100 C: water absorption data (as well as the corresponding shrinkage values reported below) at higher temperatures were
not measured and consequently not reported. Composition SG3
displays a high water absorption decrease in the range 1000
1060 C after what remains below 1%. Conversely, composition
SG4 shows a great change below 1000 C, but, above that temperature, remains below the value of 1%. Water absorption values
below 10% meet the Italian requirements for the production of
red stoneware and monoporosa (Manfredini and Pellacani,

E. Furlani et al. / Waste Management 30 (2010) 17141719

1992). It can be therefore assessed that materials SG2, SG3 and SG4
red at temperatures superior to 1040 C, satisfy the Italian ofcial
norms for production; only composition SG1 does not reach adequate water absorption level for any examined sintering cycle.
Fig. 4 shows shrinkage reported versus ring temperature of the
materials produced. It can be observed that materials SG1 and SG2
have a similar trend even if SG2 displays a little bit greater shrinkage between 1100 and 1140 C with respect to SG1. It follows that
small changes of ring temperature cause, in materials with composition SG2, greater properties variability than for those with
composition SG1. Composition SG3 shows a growing shrinkage
trend up to 1080 C, then it slightly decreases (i.e. specimens
expansion before melting) due to the formation of voids (bubbles).
Conversely, composition SG4 displays a at trend before the melting, being the measured values between 8% and 12% in all the
range 10001100 C. The evolution of the linear shrinkage, as well
as of the water absorption, well ts with the sintering behaviour of
ceramics affected by the formation of a transitory liquid phase
which improves densication of the green body as it was rst described by Kingery (1976). Some apparent inconsistencies between
Figs. 3, 4 and Table 2 (density) depend on the physical dimension
of data displayed: water absorption and density are volumetric values whereas shrinkage is linear.
It can be concluded that all the compositions show limited
shrinkage values at all the examined temperatures: their behaviour is therefore in line with the Italian requirements for the industrial production of stoneware and red monoporosa (Manfredini
and Pellacani, 1992) and may be considered suitable for a possible
industrial production. It should be pointed out that water absorption and shrinkage are interdependent, so that to the lower water
absorption correspond the greater linear shrinkage. However small
differences in sintering temperature, always possible using fast ring cycles, or in chemical composition, likely starting from waste
materials, could lead to materials with a not negligible variability
of mechanical properties.
Concluding the above investigation, it can be stated that the
mixtures SG4 could be suitable for the industrial production of

1717

tiles, provided that the sintering temperature is not so high to induce the presence of a great amount of liquid phase. Such composition should also tolerate the unavoidable variability of the waste
which shall then be reected in higher or lower optimal sintering
temperature of the materials. On the other hand, if compositions
SG2 and SG3 are considered, the properties of the corresponding
materials are much more affected by small variations of chemical
compositions or ring temperature.
Fig. 5 reports the X-ray diffraction patterns acquired on the free
surfaces of the materials red at 1040 C. Such temperature was
arbitrary selected in order to test materials red at a same temperature, possibly far enough from their softening temperature, but
simultaneously containing a not exaggerated residual porosity. In
fact, in compositions SG3 and SG4, ring temperatures higher than
1040 C cause the presence of a great amount of glassy phase as a
consequence of a high quantity of liquid during sintering. The presence of vitreous phase was observed in all the samples red at
1040 C or above by the Scanning Electron Microscope (SEM) analysis as it is conrmed by Fig. 6a and b which shows the SEM micrographs of the as red (1040 C) surfaces of compositions SG2 and
SG4. The two SEM images are here included in order to demonstrate the presence of the vitreous phase; not to describe materials
densication degree that was previously done by the sintering
curves.
On the other hand, compositions SG1 and SG2 display relatively
high water absorption (high residual porosity) when red at temperatures lower than 1040 C. It is observed that material SG1
mainly contains CaMnSiO7 (PDF 010-040-0054) which is partially
and progressively replaced, with increasing the addition of GC
(i.e. on compositions SG2, SG3 and SG4), by diopside (PDF 01071-1495) (Aloisi et al., 2004; Torres and Alarcn, 2005). It must
be remarked that, in the present research, it was decided to label
only phases that were identied by a minimum of four representative peaks in line with the Powders Diffraction Files (PDF). The
presence of small amounts of other phases was also revealed, but
it was not possible to identify them unambiguously.
The colour of the materials fast red at 1040 C ranges from
brown (SG1) to grey (SG4) being function not only of the dark colour of the SS, but also of the residual porosity of the materials after
sintering: the lower the residual porosity, the darker the materials
colour is. An image of specimens red at 1040 C is reported in
Fig. 7. In order to explain this trend, it is necessary to remind that
SS contains a great amount of Fe and Mn oxides. These compounds
can undergo oxi-reduction during high temperature treatments. In
fact they transform from the oxidized (light colour) to the reduced
(dark colour) form on heating and, conversely, from reduced to oxi-

Fig. 4. Shrinkage as a function of ring temperature of the materials produced.

Table 2
Density (q = g/cm3), Vickers hardness (Hv = GPa) and bend strength (r = MPa) of the
materials red at 1040 C with fast cycle.
Composition

Hv

SG1
SG2
SG3
SG4

2.38
2.45
2.62
2.76

1.9 0.5
3.1 0.6
5.3 0.3
6.5 0.2

18 2
23 1
51 4
62 2

Fig. 5. X-ray diffraction patterns, between 20 and 55, acquired on the free
surfaces of the materials red at 1040 C. Phases are labelled as follows: (4)
Ca2.32Mn0.68Si2O7 (PDF 00-040-0054), (N) diopside (PDF 01-071-1495).

1718

E. Furlani et al. / Waste Management 30 (2010) 17141719

Fig. 6. SEM micrographs showing the as red surface of samples SG2 (a) and SG4
(b).

Fig. 7. Photographic image of the specimens red at 1040 C.

in the thermal interval considered. Consequently, differences of

few degrees in ring temperature could signicantly affect variations of other properties too. However, it can be observed that all
the properties follow water absorption of the materials, i.e., as
water absorption decreases, density, hardness and strength are improved. It can be also observed that the presence of different
phases seems to have little inuence on materials properties. It
must be nally pointed out that only composition SG3 and SG4
reach the level established by the Italian ofcial norms for the
industrial production of oor tiles, whereas all composition are
in line with those of wall tiles (Manfredini and Pellacani, 1992).
Similar physico-mechanical properties were measured by other
authors who proposed the use of SS in the ceramic industry (Favoni
et al., 2005; Fiori and Brusa, 1983; Marcis et al., 2005; Shih et al.,
2004). However it can be pointed out that in the present research
the properties reported in Table 2 have been measured after the
fast ring cycle at 1040 C which is a low temperature if compared
to those reported in the other cited researches. Such difference
could be due to the chemical composition of the added GC which
contains a quite high amount of B2O3 and allows production of
materials with low water absorption (low open porosity) after fast
sintering at relatively low temperature.
Table 3 displays the elution data obtained from samples red at
1040 C: in accordance with the work of other researchers (Baruzzo et al., 2006; Porreca et al., 2007; van der Sloot et al., 2001;
Wang et al., 2001) it is shown that the elution of hazardous elements, although affected by the open porosity, is low. In fact it is
higher from samples with high open porosity if compared to those
with low open porosity. Some non hazardous elements, such as
Mg, Ca, Si are present in relatively high amount in all the eluted
solutions, but their presence cannot be considered important by
most of the standard release tests for waste materials. Such a
low leachability is reasonably due to the microstructure of the
materials here described which consists of a polycrystalline framework surrounded by a vitreous phase. As reported by literature,
chemical resistance is high in vitreous materials (Cheeseman
et al., 2003) or in polycrystalline products containing pyroxenetype compounds (Bernstein et al., 2002; Cheng, 2003; Favoni
et al., 2005; Reich et al., 2002). Such phases were, as well, identied
in the materials prepared in the present research. As a consequence
of the leaching tests, all materials suffer of a certain mass loss
which was measured as 2.5 wt.% for SG1, 2.1 wt.% for SG2,
1.2 wt.% for SG3 and 0.8 wt.% for SG4, respectively. The elution
Table 3
Release, in ppb (mg/kg), of the main metal elements from the red specimens, after
ageing by H2O/HCl solutions at a constant pH = 4 for 30 d at 60 C. Elements not
reported in the table were determined in quantity lower than 25 ppb.
Element

dized on cooling. In an open structure, the reduced form can recover oxygen and return to the oxidized form; in a close structure,
moreover in a vitreous network, as it is the one which surrounds
the polycrystalline structure of our materials, re-oxidation is difcult and the reduced form remains down to the room temperature.
It follows that materials containing a high amount of GC, red to a
low residual porosity display darker colour than those containing
higher residual porosity and lower amount of GC.
Table 2 reports apparent density, hardness and bending rupture
strength of the materials after fast ring at 1040 C. For each composition, strength variability is limited being always below 10% of
the average value. Moreover variability seems to be not affected by
materials composition. On the other hand, hardness suffers of
greater variations with respect to strength as it is high for compositions containing small amount of GC and low for the others. However they all must be red with caution, since the properties
measured on fast red materials may show a great variability with-

Si
Mn
Al
Zn
Mg
Ca
Cr
B
Ba
Na
K
Sr
Ti
V
Fe
Ni
P
Zr

Release (lg/kg)
SG1

SG2

SG3

SG4

16,100
3555
2340
207
250,715
78,968
289
3714
188
1296
2836
38
263
67
2942
83
417
223

13,316
2856
1533
139
228,876
62,051
156
2854
143
1110
2043
<25
182
<25
2520
<25
322
199

9668
1789
832
88
16,126
53,730
<25
1692
93
749
1627
<25
90
<25
1193
<25
254
50

6211
1480
306
<25
12,517
40,208
<25
1117
<25
397
1344
<25
67
<25
873
<25
209
<25

E. Furlani et al. / Waste Management 30 (2010) 17141719

release data reported in the present paper are not the result of a
codied test because elution tests for red ceramics are presently
not codied. However they are indicative of the possible environmental compatibility of the ceramics eventually produced using
steelmaking slag and GC from exhaust energy saving lamps. In fact,
it is known that sintered ceramics are leach resistance materials. If
codied release tests are used the leachate is often present in very
low quantity. As a consequence, in the present work, we have
tested our materials under strong leaching conditions, similar to
those proposed by Obermann and Cremer (1991) in their pHstat-test which is recommended as a worst-case elution test in
the Federal State of North Rhein-Westfalia.
4. Concluding remarks
In the present work, ceramics containing steel slag and glass
cullet from energy saving lamps in different proportions were prepared by attrition milling, pressing and fast ring at several temperatures in the range 10001140 C. The red samples were
characterized by water absorption shrinkage, apparent density,
X-rays diffraction, exural strength, hardness. It is demonstrated
that, although all the compositions prepared display good sintering
behaviour, only two of them showed physico-mechanical properties in line with the ofcial standard for tiles production, but only
one, namely the one containing 60 wt.% of steel slag and 40 wt.% of
glass cullet, looks suitable for the industrial production of oor
tiles. Elution release tests, in accordance with literature data, conrmed the environmental compatibility of the materials produced.
The possibility of glazing the products still remain to be tested and,
for this goal, work is presently in progress. In the present research
a waste containing great quantities of CaO, MgO, Fe2O3 and MnO2
has been coupled with another containing great amounts of SiO2
and B2O3, but low quantities of other oxides. A similar approach
could be followed also coupling different typologies of waste containing inorganic oxides provided they have a complementary
chemical composition.
Acknowledgement
The Italian region Friuli Venezia Giulia is gratefully acknowledged for nancial support.
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