tribology in industry ISSN 0354-8996

VOLUME 38
DECEMBER 2016. 4
 Vol. 38, N 4 (2016)

Tribology in Industry
Journal of the Serbian Tribology Society

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EDITOR-IN-CHIEF: S. MITROVIC, Faculty of Engineering, University of Kragujevac, Serbia

FOUNDING EDITOR: B. IVKOVIC, Faculty of Engineering, University of Kragujevac, Serbia

EDITORIAL BOARD: M. BABIC, Faculty of Engineering, University of Kragujevac, Serbia

B. BHUSHAN, The Ohio State University, Columbus, USA
K.-D. BOUZAKIS, Aristotle University of Thessaloniki, Thessaloniki, Greece
M.D. BRYANT, The University of Texas at Austin, Austin, USA
M.A. CHOWDHURY, Dhaka University of Engineering & Technology, Gazipur, Bangladesh
L. DELEANU, University Dunarea de Jos of Galati, Machine Design and Graphics
Department, Galati, Romania
M. KANDEVA, Technical University of Sofia, Sofia, Bulgaria
G. MANIVASAGAM, VIT University, Vellore, India
N. MANOLOV, Technical University of Sofia, Sofia, Bulgaria
M. MILOSAVLJEVIC, Vinc a Institute of Nuclear Sciences, Belgrade, Serbia
N. MYSHKIN, Metal-Polymer Research Institute of National Academy of Sciences of
Belarus, Gomel, Belarus
S. PYTKO, AGH University of Science and Technology, Krakow, Poland
A. RAC, Faculty of Mechanical Engineering, University of Belgrade, Serbia
S. SEKULIC, Faculty of Technical Sciences, University of Novi Sad, Serbia
A.I. SVIRIDENOK, The Research Center of Resources Saving Problems of the National
Academy of Sciences of Belarus, Grodno, Belarus
A. TUDOR, University Politehnica of Bucharest, Bucharest, Romania
A. VENCL, Faculty of Mechanical Engineering, University of Belgrade, Serbia
. VUKELIC, Faculty of Technical Sciences, University of Novi Sad, Serbia

TECHNICAL EDITOR: M. PANTIC, Faculty of Engineering, University of Kragujevac, Serbia

EDITORIAL ASSISTANT: D. DZUNIC, Faculty of Engineering, University of Kragujevac, Serbia

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 www.tribology.fink.rs

Vol. 38, N 4 (2016)

Tribology in Industry
Contents
a
RESEARCH C. FRAGASSA, L. GIORGINI, A. PAVLOVIC, G. ZATTINI: Acid Aging Effects on Surfaces of PTFE
Gaskets Investigated by Thermal Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 435

S. KUMAR, A. MUKHOPADHYAY: Effect of Microstructure on the Wear Behavior of Heat Treated

SS-304 Stainless Steel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 445

M. RADOVIC: Multi-objective Optimization of Process Performances when Cutting Carbon Steel

with Abrasive Water Jet . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 454

A. ANAND, K. VOHRA, M.I. UL HAQ, A. RAINA, M.F. WANI: Tribological Considerations of Cutting
Fluids in Machining Environment: A Review . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 463

A. ELHADI, A. BOUCHOUCHA, W. JOMAA, Y. ZEDAN, T. SCHMITT, P. BOCHER: Study of Surface

Wear and Damage Induced by Dry Sliding of Tempered AISI 4140 Steel against Hardened AISI
1055 Steel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 475

S. GUPTA, A. KHANDELWAL, A.K. GHOSE, I. CHAKRABARTY: Slurry Erosion Behavior of 5

Destabilized and Deep Cryogenically Treated Cr-Mn-Cu White Cast Irons . . . . . . . . . . . . . . . . . . . 486

V.N. DURADJI, D.E. KAPUTKIN, A. DURADJI: Tribological Studies of Antiwear Antifriction

Composition and its Application . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 496

S. PORIA, G. SUTRADHAR, P. SAHOO: Wear and Friction Behavior of Stir Cast Al-TiB2 Metal Matrix
Composites with Various Lubricants . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 508
5
I. PEKO, B. NEDIC, A. OREVIC, D. DZUNIC, M. JANKOVIC, I. VEZA: Modeling of Surface
Roughness in Plasma Jet Cutting Process of Thick Structural Steel . . . . . . . . . . . . . . . . . . . . . . . . . . . 522

S.H. DIN, M.A. SHAH, N.A. SHEIKH: Effect of CVD-Diamond on the Tribological and Mechanical
Performance of Titanium Alloy (Ti6Al4V) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 530

B.T. PRAYOGA, S. SUYITNO, R. DHARMASTITI: The Wear behavior of UHMWPE against Surface
Modified CP-Titanium by Thermal Oxidation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 543

H. RAJAEI, I. MOBASHERPOUR, M. FARVIZI, M. ZAKERI: Effect of Composition on Mechanical

Properties of Mullite-WC Nano Composites Prepared by Spark Plasma Sintering . . . . . . . . . . . . . 552

A. KHURSHID, Z. KHAN, V. CHACKO, A. GHAFOOR, M.A. MALIK, Y. AYAZ: Modelling and

Simulation of a Manipulator with Stable Viscoelastic Grasping Incorporating Friction . . . . . . . . . 559

K. MEHALA, N. BENDAOUD, A. YOUCEFI: Numerical Analyses of the Non-Newtonian Flow

Performance and Thermal Effect on a Bearing Coated with a High Tin Content . . . . . . . . . . . . . . 575

M. ZIVKOVIC, M. MATEJIC, D. MILJANIC, LJ. BRZAKOVIC, V. KOCOVIC: Influence of the Previous

Preheating Temperature on the Static Coefficient of Friction with Lubrication . . . . . . . . . . . . . . . . 585
tribology in industry
ISSN 0354-8996
VOLUME 33
2011. 3
 Mi Vol. 38, No. 4 (2016) 435-444

Tribology in Industry

RESEARCH
www.tribology.fink.rs

Acid Aging Effects on Surfaces of PTFE Gaskets

Investigated by Thermal Analysis

C. Fragassa a,c, L. Giorgini b,c, A. Pavlovic c, G. Zattinib,c

a Department of Industrial Engineering, University of Bologna, viale Risorgimento, 2, Bologna, Italy,
b Department of Industrial Chemistry "Toso Montanari", University of Bologna, viale Risorgimento 4, Bologna, Italy,
c InterDept. of Industrial Research on Advanced Mechanics and Materials, University of Bologna, via Terracini 22,

Bologna, Italy.

Keywords: ABSTRACT
Polymeric materials
This paper investigates the effect of a prolonged acid attack on the
PTFE
surface of PTFE by Thermogravimetric Analysis (TGA) and Differential
Gaskets
Scanning Calorimetry (DSC). PTFE is very non-reactive, partly because of
Ultrasonic cleaning process
the strength of carbonfluorine bonds and for its high crystallinity, and,
Surface Degradation
as a consequence, it is often used in containers and pipework with
TGA
reactive and corrosive chemicals. The PTFE under analysis is
DSC
commercialized by two alternative producers in form of Teflon tapes.
These tapes are adopted, as gaskets, in process plants where tires moulds
Corresponding author: are cleaned by acid solutions inside a multistage ultrasonic process. In
Cristiano Fragassa this case, PTFE shows, in a relatively short operation time, inexplicably
Department of Industrial Engineering, phenomena of surface degradation, which could be related, in general
University of Bologna, terms, to an acid attack. But, even considering the combined effect of
viale Risorgimento 2, ultrasonic waves, temperature, humidity and acid attack, the PTFE
Bologna, Italy. properties of resistance nominally exclude the risk of the extreme erosion
E-mail: cristiano.fragassa@unibo.it phenomena as observed.
The present experimental research aim at investigating this
contradiction. A possible explanation could be related to the presence in
the cleaning solution of unexpected fluorides, able to produce
fluorinating agents and, thus, degrade carbon-fluorine bonds.
Considering more the 300 chemical elements a tire compound consists in,
it is really complex to preserve the original chemical composition of the
cleaning solution. In this research PTFE samples have been treated with
different mixtures of acids with the aim at investigating the different
aging effects. The thermal analysis has permitted the experimental
characterization of PTFE surface properties after acid attack, providing
evidence of the degradation phenomena. In particular, the different acid
treatments adopted for accelerating the aging of gaskets have
highlighted the different behaviour of the PTFE matrix, but also
differences between manufacturers.
2016 Published by Faculty of Engineering

435
 C. Fragassa et al., Tribology in Industry Vol. 38, No. 4 (2016) 435-444
1. INTRODUCTION
This experimental study is part of a larger
investigation aiming at improving the process
efficiency in the case of innovative production
plants used for the surface treatment and
cleaning of tires moulds. Mould cleaning and
maintenance are of major concern for the tire
industry. Cleaning process has to remove fouling
and residues of rubber from sensitive surfaces of
mould avoiding wear or damage effects (Fig. 1).
Fig. 1. Effects of the cleaning processes on moulds.
Several technologies are used, each one with
specific advantages and limits in applications. A
comparative assessment of tire mould cleaning
solutions is presented in [1], detailing aspects as
productivity, cost effectiveness, quality finishing,
eco-sustainability, safety, etc.
It is also reported that the so called Mould
Ultrasonic Cleaning Systems (UMCS) represents a
preferable choice in terms of efficiency and
flexibility especially in the presence of very
complex and fragile geometries.
The UMCS technology consists in a cleaning
process where ultrasonic waves, in combination
with temperature and acids, remove rubber
scraps and other physical residuals from
interstices of the moulds. Tire moulds and their
parts are immersed in a sequence of washing
baths, where chemical compounds attack the
residues, cleaning the mould surfaces.
Useful information referring this technology,
including several technical details regarding the
proper way to manage UMCS plants are available
in [2]. In particular, the guideline emphasises the
attention to be focused by final users toward a
constant monitoring of the chemical solutions.
436
Even if this document represents the guideline
for a specific UMCS, similarities emerge with
other plant manufactures. It depends on the fact
that a precise chemical composition for
solutions seems to be a relevant aspect in
cleaning efficiency. On the contrary, it results
evident that a residue from treatments tends to
accumulate as sediments on the bottom of the
basin [3].
Other investigations suggest that specific
elements from this leftover could be dissociated
in the cleaning solution modifying its chemical
compositions and properties. This aspect has
been always considered by manufacturers in
terms of loss in process efficiency or quality.
And, for this reason, a periodical action of
renovation for basins and solutions is regulated.
Nevertheless, recently, minor failures, as drops
of solution from washing basins in relatively
new plants, highlighted an unexpected
deterioration of seals. In particular, Teflon tapes,
used as gaskets in the most concentrated acid
basins, exhibits degradation theoretically
incompatible with normal conditions of use [3].
In fact, according to the material datasheets
[4,5] or independent researchers [6-9], Teflon,
better identified as Polytetrafluoroethylene
(PTFE), reveals a deep thermal and chemical
stability that make this material a valid choice
in a large number of challenging applications,
including UMCS. Referring to [10-12], it is
stated that only under very uncommon
circumstances PTFE degrades.
The existence of unexpected fluorides [13] in the
washing solution, emerging from the breakdown
of tire compound and/or used as lubricants or
processing aids, just after few weeks of plant
operations times, could be the major reason for
this quick PTFE degradation. It is noteworthy
that, inside a tire compound more than 300
chemical elements could be present [14]. On the
contrary, a consolidate know-how [12] reported
how carbon-fluorine bonds in the PTFE can be
effected by alkali metals (i.e. zinc oxide, present
in 1-2 weight % in the rubber as vulcanization
activator [15]) and fluorinating agents. With the
aim of investigate this relatively unknown
aspect, an intense research activity has been
developed. A first comparative analysis was
performed on PTFE gaskets before and after the
 C. Fragassa et al., Tribology in Industry Vol. 38, No. 4 (2016) 435-444
use in UMCS by means of mechanical tests and
micrographs. It showed a not negligible
difference between the two situations [16].
Table 1. Acid compositions (in accordance with
accelerated aging procedure detailed in [17]).
H2O Sol. I Sol. II
#
%wt
1 50 40 10
2 90 10 0
3 80 20 0
4 87.5 10 2.5
5 77.5 20 2.5
6 67.5 30 2.5
7 85 10 5 attacks have been investigated (#6, #9). A
8 75 20 5 comparison with new, untreated samples (#0)
9 65 30 5 have been also implemented (Table 2). These
10 70 30 0
Then, a comparative study on the PTFE surface
properties, after accelerated aging in controlled
environment was also realized and detailed in
[17-19]. In particular, it [17] describes the
aggravated conditions of heat, acid attack (with
an almost pH 1 solution composed by a mixture
of sulfamic, hydrochloric and hydrofluoric acids,
and, simultaneously, a temperature between 70
and 80 C) used to speed up the normal aging
processes of PTFE gaskets in the way to
correctly represent their utilisation inside the
UMCS plants. Besides, [18] describes the effects
of aging on PTFE chemical surfaces by Fourier
Transform Infrared Spectroscopy (FT-IR)
permitting preliminary considerations regarding
the use of PTFE in UMCS conditions and its aging
mechanisms. The current research intends to
merge further experimental results by useful
thermal analysis. With the aim at allowing a
quick comparison with the previous results, all
conditions used in the former experiments (e.g.
for accelerating the PTFE chemical surface
degradation), are maintained and summarized
in Table 1.
2. MATERIAL AND METHODS
In Table 1 are reported the different chemical
compositions used to speed up the aging
processes by acid attack. Different combinations
for Sol. I (sulfamic acid 15%wt, hydrochloric acid
0.1%wt) and Sol. II (hydrofluoric acid 1%wt)
have been evaluated with the aim to compare the
effects of the two solutions in different ratios. For
each of these combinations, PTFE specimens by
two different manufacturers, one Italian (IT) and
one Chinese (CH), have been investigated.
Specimens have been immersed in the solution
and maintained in oven at 80 C for 1.500 hr. This
approach was intended to reproduce the worst
process situation represented in the process line
by the most aggressive acid bath, with almost pH
1 solution of sulfamic, hydrochloric and
hydrofluoric acids and, simultaneously, a
temperature between 70 and 80 C.
With the aim at reducing the number of
experiments, two specific combinations of acid
samples have been selected representing
respectively the most and least aggressive
treatment as preliminary identified by the
microscopic observations performed by a Hirox
3D Multifocal Microscope Model HX7700 (Fig.
2) and by the Fourier Transform Infrared
Spectroscopy (FT-IR) investigation [18].
Table 2. List of samples analysed by TGA and DSC.
Treatment
Sample Label
# Sol.I Sol.II
A - - Chinese-New
0
B - - Italian-New
G 30 % 2.5 % Chinese-6
H
6
30 % 2.5 % Italian-6
I 30 % 5% Chinese-9
9
J 30 % 5% Italian-9
At the end of the aging treatment, the specimens
were extracted from oven, cleaned, dried and
investigated by Thermogravimetric Analysis (TGA)
and Differential Scanning Calorimetry (DSC).
Changes in physical and chemical properties of
the polymers have been measured by TGA as a
function of increasing temperature (considering
a constant heating rate) [20-22]. This technique
has permitted to investigate physical and
chemical phenomena, such as degradation
temperatures and absorption of low molecular
weight moieties. In particular, in the present
work, TGA has allowed the characterization of
materials through the analysis of characteristic
decomposition patterns and the evaluation of
degradation mechanisms and reaction kinetics.
By TGA, it has been also possible to verify the
presence (or absence) of organic/inorganic
contents.
437
 C. Fragassa et al., Tribology in Industry Vol. 38, No. 4 (2016) 435-444

a) b)

c) d)
Fig. 2. Examples of micrographs used for a preliminary selection of treatments and samples under investigation:
a) Italian #6; b) Italian #9; c) Chinese #6; d) Chinese #9.

This information has been useful for completing
the chemical analysis and corroborating
alternative hypothesis on the material
structures.
By Differential Scanning Calorimetry (DSC), it is
possible to analyse the difference in the amount
of heat required to increase the temperature of
samples and references (as a function of
temperature). By observing this difference, it has
been possible to measure the amount of heat
absorbed during thermodynamic transitions,
investigating subtle physical changes (phase
changes, melting) [23-25].
atmosphere has been switched to air in order to
oxidize any eventual organic residue [26].
The choice of the inert atmosphere has been
made to avoid the introduction of thermo-
oxidative phenomena during the analysis. DSC
has also performed under nitrogen atmosphere,
on 4-5 mg of polymeric material, using a TA
Q2000 instrument, set to run two heating scans
from -80 C to 360 C at a heating rate of 10
C/min. Only experimental results from the
second scan have been used for the purposes of
this work [27].

The untreated and treated gaskets have been 3. RESULTS

sampled both on the surface and in the core. TGA
has been performed on 6-8 mg of material, using
a TA Q600 instrument, set to a heating rate of 10
C/min, from room temperature to 800 C.
Analyses have been realized in inert atmosphere
(N2, 100 mL/min) until 750 C, and then the
3.1 Untreated samples (#0)
A sample purchased by the two manufacturers
performs similarly, with just few TGA and DSC
differences. Italian sample seems to undergo

438
 C. Fragassa et al., Tribology in Industry Vol. 38, No. 4 (2016) 435-444

thermal decomposition to a slightly higher melting), that could be associated with a slightly
temperature (Fig. 3a), according to the DTG higher degree of crystallinity. In fact,
(Derivative Thermogravimetric Analysis) curves crystallization and melting enthalpy in PTFE are
obtained (expressed as maximum degradation rate supposed to be directly proportional [31].
temperatures). A DSC result also shows a very
similar behaviour between the two materials (Fig. Table 3. Thermal analyses results of new samples.
3b). Both the samples exhibit two partly Chinese Italian
Manufacturer
overlapped crystalline phase transitions, typical of A (#0) B (#0)
PTFE at atmospheric pressure centred at 21/22 C Decomposition T
C, peak 571 576
and 30 C, in agreement with literature [28,29]. C, onset 543 551

TGA
Weight Loss %wt 100.0 99.5
3.5 Residue @ 750 C %wt 0.00 0.87
100 Onset T C 15 16

transitio
3.0 1st peak T C 21 22

Phase
90

ns
80
Italian New 2nd peak T C 30 30
Chinese New 2.5

DSC
70
H J/g 8.4 7.9

Deriv. Weight (%/C)

2.0 Onset T C 319 321

Melti
60
Weight (%)

Peak T C 327 327

ng
50 1.5 H J/g 34.2 32.2
40
1.0
30 Results obtained by thermal analyses of the new
20
0.5
untreated gaskets are reported in Table 3.
10 0.0
0 3.2 Treated samples (#6, #9)
-0.5
0 200 400 600 800
Temperature (C)
Samples subjected to acid treatment #6 and #9
a)
were analysed both at the surface and in the
0.8
Chinese New core of the gaskets. TGA thermograms (Fig. 4
Italian New
and Table 4) show four different weight losses,
with the first three that could be probably
0.6
attributed to compositional changes due to the
acid treatments. The last one is, instead, due to
Heat Flow (W/g)

0.4
the complete pyrolytic decomposition of the
PTFE chain, via depolymerisation at monomers.
In Table 4, TGA analysis results are summarized.
0.2 The first three weight losses show different
trends depending on the acid treatment applied.

0.0
-50 0 50 100 150
Temperature (C)
b)
Fig. 3. TGA (a) and DSC (b) thermograms of Chinese
and Italian untreated samples (#0) (exo-down).
In Table 3, onset temperature and total enthalpy
change are reported considering the two
thermal transitions as a single event. The second
thermal event observed in both manufacturers
samples, centred at 327 C, is the main melting
of PTFE according with literature [30]. The
difference in the onset melting temperature
could be considered negligible.
Chinese sample shows a fairly higher enthalpy
value for both events (phase transitions and
200 250 300 350
Amongst samples subjected to treatment #6 (#G
and #H), the surface samples behave in a very
similar manner, both in weight losses
temperatures and entities. The Italian core and
surface samples show the same weight loss
temperatures, but their entities are generally
slightly lower (Figs. 4a and 4b). The principal
observation regards the core of the Chinese
sample subjected to treatment #6, which
undergo one single weight loss, in the same
manner to what happens to the related Chinese
new untreated sample. This fact is consistent
with the FT-IR analysis previously executed,
which have highlighted the simultaneous
presence of highly degraded surface as well as
nearly unmodified areas in the core of Chinese
sample subjected to treatment #6.

439
 C. Fragassa et al., Tribology in Industry Vol. 38, No. 4 (2016) 435-444

Samples subjected to treatment #9 (#I and #J)
show a similar trend. The core samples exhibit
lower weight loss entities which occur at slightly
lower temperatures when compared to the
surface samples. Comparing Chinese and Italian
samples, the weight loss temperatures of
Chinese core sample are higher than the Italian
one, while the entities do not seem to have a
particular trend (Figs. 4c and 4d).
The last and more abundant weight loss,
attributable to the depolymerisation of PTFE at
its monomer, varies in entity from 81.9 to 100
%wt according to the previously three weight
losses. Residue at 750 C also varies between 0
and 4,78 %wt.
Samples treated with acid attack #6 do not
exhibit a precise trend (Figs. 4a and 4b). Chinese
core sample behave similarly to the related
untreated sample, and exhibits lower residue
than the surface sample. The Italian core and
surface samples show instead similar behaviour.
Temperatures of this main weight loss are quite
consistent between core and surface but differs
of 7 to 15 C between Chinese (lower T) and
Italian (higher T). In any case, both onset and
peak temperature measured are generally
higher than those of new samples.
Samples subjected to treatment #9 show coherent
values for Chinese and Italian samples, both in
entities and temperatures (peak and onset) of the
weight loss, which are all very similar between the
two manufacturers (Figs. 4c and 4d). Even in this
case, all the degradation temperatures measured
are higher than those of untreated samples.
The simultaneous higher residue and lower
entity of the last weight loss (related to the PTFE
decomposition) exhibited by the samples
subjected at #9 treatment, seems to indicate that
the aforementioned acid attack resulted in a
more aggressive aging rather than #6 treatment.

100 100
90 Chinese New 90 Italian New
Chinese 6, Surface
80 80 Italian 6, Surface
Chinese 6, Core Italian 6, Core
70 70

60 60
Weight (%)

Weight (%)

50 50

40 40

30 30

20 20

10 10

0 0
0 100 200 300 400 500 600 700 800 0 100 200 300 400 500 600 700 800
Temperature (C) Temperature (C)

a) b)
100 100

90 90
Chinese New Italian New
80 80
Chinese 9, Surface Italian 9, Surface
70 Chinese 9, Core 70 Italian 9, Core

60 60
Weight (%)
Weight (%)

50 50

40 40

30 30

20 20

10 10

0 0
0 100 200 300 400 500 600 700 800 0 100 200 300 400 500 600 700 800
Temperature (C) Temperature (C)

c) d)
Fig. 4. TGA thermograms of Chinese samples (left) and Italian samples (right), subject to treatment #6 (upper)
and #9 (lower). New untreated, Surface and Core thermal traces are reported.

440
 C. Fragassa et al., Tribology in Industry Vol. 38, No. 4 (2016) 435-444

Tab. 4. Summary of TGA and DTG results for both treated and new samples.
1 2 3 4
Position Residue
Sample Weight Loss T Weight Loss T Weight Loss T Weight Loss T Onset T
Sampled
(%) (C) (%) (C) (%) (C) (%) (C) (C) (%)
A Chinese #0 Core - - - - - - 100.0 571 543 0.00
B Italian #0 Core - - - - - - 99.2 576 551 0.87
Surface 1.66 100 1.61 212 2.24 261 92.6 571 541 1.69
G Chinese #6
Core - - - - - - 100.0 575 548 0.00
Surface 1.24 105 1.64 213 2.74 269 93.9 586 556 0.01
H Italian #6
Core 0.97 109 1.92 219 1.45 264 90.5 583 557 4.64
Surface 3.90 117 4.96 225 5.44 278 81.9 575 550 3.57
I Chinese #9
Core 1.04 112 2.35 215 3.90 275 90.2 584 552 2.02
Surface 4.55 118 4.98 226 3.77 273 85.2 574 548 1.34
J Italian #9
Core 1.25 102 1.69 210 2.56 271 89.7 585 550 4.78

Tab. 5. DSC results of new untreated and treated samples.

1 (phase transitions) 2 (melting)
Sample Position T peak T onset H T peak T onset H
(C) (C) (J/g) (C) (C) (J/g)
A Chinese #0 Core 21 15 8.4 327 319 34.2
B Italian #0 Core 22 16 7.9 327 321 32.2
Surface 21 15 6.4 326 319 25.6
G Chinese #6
Core 22 16 6.9 328 319 31.4
Surface 22 16 7.1 327 321 29.8
H Italian #6
Core 21 15 7.1 326 321 31.0
Surface 21 16 7.0 327 319 28.1
I Chinese #9
Core 21 15 8.0 327 317 33.0
Surface 22 16 7.6 327 321 28.0
J Italian #9
Core 22 16 7.5 327 321 29.3

0,8 0,8
Chinese New Italian New
34,2 J/g 32,2 J/g
0,6 0,6

0,4 0,4

0,2 0,2
Heat Flow (W/g)

Heat Flow (W/g)

0,8 Chinese 6, Surface 0,8 Italian 6, Surface

25,6 J/g 29,8 J/g
0,6 0,6

0,4 0,4

0,2 0,2

0,8 0,8
Chinese 6, Core Italian 6, Core
31,4 J/g 31,0 J/g
0,6 0,6

0,4 0,4

0,2 0,2

-50 0 50 100 150 200 250 300 350 -50 0 50 100 150 200 250 300 350

Temperature (C) Temperature (C)

a) b)
0,8 0,8
Chinese New Italian New
34,2 J/g 32,2 J/g
0,6 0,6

0,4 0,4

0,2 0,2
Heat Flow (W/g)

0,8
Heat Flow (W/g)

0,8 Chinese 9, Surface Italian 9, Surface

28,1 J/g 28,0 J/g
0,6 0,6

0,4 0,4

0,2 0,2

0,8 0,8
Chinese 9, Core Italian 9, Core
33,0 J/g 29,3 J/g
0,6 0,6

0,4 0,4

0,2 0,2

-50 0 50 100 150 200 250 300 350 -50 0 50 100 150 200 250 300 350

Temperature (C) Temperature (C)

c) d)
Fig. 1. DSC thermograms of Chinese (left) and Italian (right) samples subject to treatment #6 (upper) and #9
(lower). New Untreated, Surface and Core thermal traces are reported (exo-down).

441
 C. Fragassa et al., Tribology in Industry Vol. 38, No. 4 (2016) 435-444
DSC analyses of treated samples show the same
pattern recorded by new samples, with the
presence of crystalline phase transitions peaks
located at the same temperatures (both peak
and onset), with significant variations in the
enthalpies (H) of both the 1st and 2nd thermal
events (Table 5 and Fig. 5). A decrease in these
melting enthalpy values is related to a reduced
crystallinity of the PTFE, which in turn could be
the result of the presence of defects in the
polymer chain due to degradation. The results
reported in Table 5 show a relative pronounced
variation in the phase transitions enthalpy of
Chinese samples centred at around 21-22 C,
highlighting also a higher decrease in both
surface samples enthalpy (treatment #6 and #9)
with respect to the corresponding core samples.
Instead, Italian surface samples exhibit H
similar to their corresponding core samples.
Furthermore, treated samples show slightly
lower values of H when compared with the
corresponding new samples.
Finally, the lower H associated to the first
phase transition has been measured for both
Chinese and Italian samples subjected to
treatment #6.
The measured melting enthalpies are much
more variable in entity amongst the samples, but
the trends are quite similar to those observed
for the previously discussed phase transitions
(Fig. 5). Melting enthalpies variation of the
treated samples, with respect to the
correspondent new untreated samples, are
slightly higher for Chinese samples (1-7 J/g, Fig.
5, left) rather than for Italian ones (2-4 J/g, Fig.
5, right). However, a little difference could be
pointed out in the behaviours exhibited by the
samples of the two manufacturers in relation to
the treatment: a Chinese sample seems to be
more susceptible to treatment #6 (i.e. lower
enthalpies), while Italian samples show slight
lower H values after treatment #9.
Finally, as general trend, all samples exhibit
melting H of the surfaces lower than that of the
cores.
4. CONCLUSIONS
This paper investigates the surface and core
degradation of PTFE (Teflon) gaskets exposed to
442
different acid attacks. In particular, different
combinations for Sol.I (sulfamic acid 15%wt,
hydrochloric acid 0.1%wt) and Sol.II
(hydrofluoric acid 1%wt) have been considered
as accelerating aging factors with the aim to
compare the effects of the two solutions in
different ratios. Experimental measures have
been performed by Thermogravimetric Analysis
(TGA) and Differential Scanning Calorimetry
(DSC). Two series of PTFE gaskets, produced by
two different manufacturers (one from Italy and
other from China) have been treated and
compared with new untreated samples. The
samples have been analysed to evaluate
different behaviours in response of the various
acid treatments. Experimental TGA and DSC data
have highlighted different behaviours for the
PTFE matrix (core and surface), but also
differences between Teflon manufacturers.
These results denote a rather clear evidence of
progressive degradation of PTFE by chemical
attack. Specifically, thermogravimetric analysis
(TGA) data seems to indicate a slightly higher
amount of degradation in samples subjected to
aging treatment labelled as #9, especially in the
case of the Italian samples. DSC analysis shows
that the treatment #6 is responsible of a
generally higher decrease in phase transitions
enthalpies, as well as of the melting enthalpies,
particularly in the case of Chinese samples. In
fact, the lower enthalpies exhibited by treated
samples are sign of a more marked reduction of
their crystallinity degree. This fact could be a
consequence of a greater presence of defects in
the polymer chains, possibly induced or
enhanced by the chemical attack. These results
are generally in accordance with those
previously obtained by FT-IR analysis on
samples treated in the same manner [18].
However, regarding the superficial and internal
homogeneity, our experimental data suggest
that in all cases Chinese samples exhibit a
slightly inhomogeneous degradation after the
treatments.
Acknowledgement
This research is part of a larger investigation
aiming at improving the design in the case of
innovative production plants used for cleaning
tires moulds. These plants are produced and
commercialized worldwide by Keymical Group.
 C. Fragassa et al., Tribology in Industry Vol. 38, No. 4 (2016) 435-444
REFERENCES
[1] C. Fragassa and M. Ippoliti, Technology
assessment of tire mould cleaning systems and
quality finishing, International Journal for Quality
Research, vol. 10, no. 3, pp. 523-546, 2016.
[2] Keymical, U.M.C.S. Keymical Ultrasonic Mould
Cleaning System (Model UMCS-&-PCR). Cleaning
Process Handbook Chemical Maintenance
Management, 2015.
[3] C. Fragassa and M. Ippoliti, Failure Mode Effects
and Criticality Analysis (FMECA) as a quality tool
to plan improvements in Ultrasonic Mould
Cleaning Systems, International Journal for Quality
Research, vol. 10, no. 4, pp. 847-870, 2016.
[4] About Teflon (DuPont) available at:
http://web.archive.org/web/20080229143203
/http://www2.dupont.com/PFOA/en_US/about
_teflon/, accessed: 01.05.2016.
[5] Polytetrafluoroethylene, available at:
https://en.wikipedia.org/wiki/Polytetrafluoroe
thylene, accessed: 01.05.2016.
[6] J. Bickford, Gaskets and gasketed joints. CRC
Press, 1997.
[7] N.K. Myshkin, S.S. Pesetskiiand and A.Ya.
Grigoriev, Polymer Tribology: Current and
Applications, Tribology in Industry, vol. 37, no.
3, pp. 284-290, 2015.
[8] D. Stamenkovic, M. Nikolic, M. Milosevic, M.
Banic, A. Miltenovicand and M. Mijajlovic,
Tribological Aspect of Rubber Based Parts used
in Engineering, Tribology in Industry, vol. 36, no.
1, pp. 9-16, 2014.
[9] P. Rae and D. Dattelbaum, The properties of
poly (tetrafluoroethylene) (PTFE) in
compression, Polymer, vol. 45, no. 22, pp. 7615
25, 2004.
[10] K. Lunkwitz, U. Lappanand and D. Lehmann,
Modification of fluoropolymers by means of
electron beam irradiation, Radiation Physics
and Chemistry, vol. 57, no. 3, pp. 373-376, 2000.
[11] A. Palova, H. Fujiib, Yu. Mankelevicha, T.
Rakhimovaaand and M. Baklanovc, Modelling
degradation of PTFE under electron irradiation,
Polymer Degradation and Stability, vol. 97, no. 5,
pp. 802809, 2012.
[12] Du Pont, Teflon PTFE fluoropolymer resin
Proprieties Handbook. US., 2006. Available at:
http://www.rjchase.com/ptfe_handbook.pdf
[13] F. Capelli, Relazione Tecnica Peritale Causa
Civile Keymical 2rsm Vs Ecotecne Srl. Tribunale
Di Padova Sezione Seconda Civile. Protocollo
N. 12110/2014 r.g., 10/2015.
[14] Evans A. & R., The Composition of a Tyre: Typical
Components. In The Waste & Resources Action
Programme, England, Banbury, 2006.
[15] L. Giorgini, T. Benelli, C. Leonardi, L.
Mazzocchetti, G. Zattini, M. Cavazzoni, I.
Montanari and C. Tosi, Efficient recovery of
non-shredded tires via pyrolysis in an
innovative pilot plant, Environmental
Engineering and Management Journal, vol. 14,
no. 7, pp. 1611-1622, 2015.
[16] M.C. Bignozzi, A. Saccani and C. Fragassa,
Experimental Evaluation of the Surface
Alteration of Gasket Samples under Operative
Conditions, Tribology in Industry, vol. 37, no. 4,
pp. 482-490, 2015.
[17] C. Fragassa, Investigations into the degradation
of PTFE surface properties by accelerated aging
tests, Tribology in Industry, vol. 38, no. 2, pp
241-248, 2016.
[18] L. Giorgini, C. Fragassa, G. Zattini and A.
Pavlovic, Acid aging effects on surfaces of PTFE
gaskets investigated by Fourier Transform
Infrared Spectroscopy, Tribology in Industry,
vol. 38, no. 3, pp. 286-296, 2016.
[19] G. Zattini, A. Pavlovic, C. Fragassa and L.
Giorgini, Characterization of solid residues
emerging during ultrasonic cleaning treatments
of tyre moulds, FME Transaction, vol. 45, no. 2,
pp. 203-213, 2017.
[20] A.W. Coats and J.P. Redfern, Thermogravimetric
Analysis: A Review, Analyst, vol. 88, pp. 906
924, 1963.
[21] E. Bicciocchi, Y.K. Chong, L. Giorgini, G. Moad, E.
Rizzardo and S.H. Thang, Substituent effects on
RAFT polymerization with benzyl aryl
trithiocarbonates, Macromolecular Chemistry
and Physics, vol. 211, pp. 529-538, 2010.
[22] E. Poodts, G. Minak, L. Mazzocchetti and L.
Giorgini, Fabrication, process simulation and
testing of a thick CFRP component using the
RTM process, Composites: Part B, vol. 56, pp.
673680, 2014.
[23] H.W. Li, R, Termine, L, Angiolini, L, Giorgini, F.
Mauriello and A. Golemme, High T-g, Nonpoled
Photorefractive Polymers, Chemistry of
Materials, vol. 21, pp. 2403-2409, 2009.
[24] L. Angiolini, L. Giorgini, R. Bozio and D. Pedron,
Reversible chirality inversion of photochromic
methacrylic polymers upon irradiation with
one-handed circularly polarized light, Synthetic
Metals, vol. 138, pp. 375-379, 2003.
[25] C. Samor, F. Abbondanzi, P. Galletti, L. Giorgini,
L. Mazzocchetti, C. Torri and E. Tagliavini,
Dimethyl carbonate and switchable anionic
443
 C. Fragassa et al., Tribology in Industry Vol. 38, No. 4 (2016) 435-444

surfactants: two effective tools for the transition of polytetrafluoroethylene, Chinese

extraction of polyhydroxyalkanoates from Journal of Polymer Science, vol. 4, 1986.
microbial biomass, Green Chemistry, vol. 17, pp.
[29] J. Blumm, A. Lindemann, M. Meyer and C.
1047-1056, 2015.
Strasser, Characterization of PTFE Using
[26] A. Bellusci, M. Ghedini, L. Giorgini, F. Gozzo, E.I. Advanced Thermal Analysis Techniques,
Szerb, A. Crispini and D. Pucci, 'Anion dependent International Journal of Thermophysics, vol. 31,
mesomorphism in coordination networks based pp. 1919-1927, 2008.
on 2,2-bipyridine silver(I) complexes, Dalton
[30] Y.P. Khanna, The melting temperature of
Transaction, vol. 36, pp. 7381-7389, 2009.
polytetrafluoroethylene, Journal of Materials
[27] M.J. O'Neill, The Analysis of a Temperature- Science Letters, vol. 7, pp. 817-818, 1988.
Controlled Scanning Calorimeter. Anal. Chem.,
[31] X. Huang, J. MartinezVega and D. Malec,
vol. 36, no. 7, pp. 12381245, 1964.
Morphological evolution of polytetrafluoroethylene
[28] Fu, Z. Mo, P. Han, Y. Qi, S. Wu and D. Chen, in extreme temperature conditions for aerospace
CStudy on factors affecting room temperature applications, Journal of Applied Polymer Science, vol.
131, no. 3, pp. 1-6, 2014.

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Tribology in Industry

RESEARCH
www.tribology.fink.rs

Effect of Microstructure on the Wear Behavior of

Heat Treated SS-304 Stainless Steel

S. Kumar a, A. Mukhopadhyay a
a Mechanical Engineering Department, Jadavpur University, Kolkata- 700032, India.

Keywords: ABSTRACT
Wear Sliding wear characteristics of some heat treated SS-304 stainless steel
Heat treatment against EN-8 steel in dry condition have been studied in the present
Micro hardness experimental work. Samples of SS-304 stainless steel have been heated in
Feritscope a muffle furnace in desired temperature and allowed to dwell for two
Tribo testing hours. The heated specimen are then cooled in different media namely
inside the furnace, open air, cutting grade oil (grade 44) and water at
Corresponding author: room temperature to obtain different grades of heat treatment.
Microstructures and corresponding micro hardness of the samples have
Abhijit Mukhopadhyay been measured along with Feritscopic studies. Wear characteristics have
Mechanical ngineering Department, been studied in a multi tribo-tester (Ducom) in dry sliding condition
Jadavpur University, against EN-8 steel roller. Speed, load on job and duration of test run have
Kolkata - 700032, India. been considered as the experimental parameters. The wear of the samples
E-mail: m_obiji@yahoo.com have been obtained directly from Winducom 2006 software. Mass loss of
the samples before and after operation has also been considered as the
measure of wear in the present study. All the samples have been slid
against EN-8 steel roller with fixed experimental parameters. The data
have been plotted, compared and analyzed. Effect of microstructures as
well as micro hardness on the wear behavior has been studied and
concluded accordingly.
2016 Published by Faculty of Engineering

1. INTRODUCTION For the functional reliability of any component it

Study of friction and wear Study of friction, wear
and associated lubrication in case of interacting
surfaces under relative motion is the purview of
tribology. Wear determines the useful life of a
part/product. Product quality as well as
reliability also depends on wear. Hence the
study of friction, wear and their control plays an
important role in different engineering
applications [1,2,28].
is very important to control the friction and
wear in case of sliding contact. A fundamental
knowledge base is helpful to achieve the control.
Friction and wear are system dependent
properties [3]. There are several research based
models and formulations in the field of friction
and wear. However, majority of them are not
suitable to predict the tribological behavior in a
particular work situation. This practical
limitation necessitates the iteration of friction
and wear data through practical

445
 S. Kumar and A. Mukhopadhyay, Tribology in industry Vol. 38, No. 4 (2016) 445-453
experimentation in a particular situation and for
a particular tool-work materials combination.
Present work has been carried out to compare
the sliding wear behavior of different heat
treated SS-304 stainless steel against EN-8
stainless steel in dry working condition. The
microstructures and micro hardness of the heat
treated samples have also been studied and
attempt has been made to find out the relation, if
any, on the wear at large.
Stainless steel is a major component for
industrial, commercial and consumer products.
SS-304 stainless steel is an austenitic iron-
nickel-chromium alloy and cant be heat treated
for hardening purpose. However, annealing is
possible and annealed SS-304 stainless steel has
several use in industries like chemical,
refrigeration, paper and food processing,
beverage, screws, machinery parts, car headers,
architecture and many more [27]. This may also
be used for bellows, flexible metal hose,
spinning, tubing and numerous other stainless
applications. Study of friction and wear behavior
is thus important in the characterization of
annealed SS-304 stainless steel along with the
evaluation of other mechanical properties.
Block-on-roller configuration of a multi
tribotester TR-25 (DUCOM, India) has been
utilized for the experimental evaluation of wear
[17]. Normal load on the sample, sliding speed
(rpm) of the wheel and duration of the test run
have been considered as the design factors for
the evaluation of tribo characteristics. The
experiments have been conducted in dry
condition, that is, without any lubricants.
2. EXPERIMENTAL
AISI SS-304 stainless steel has been selected as
test material for the present experimental work.
The material has been procured directly from
the market. Samples of size 20 20 8 have
been prepared as per the dimension
requirement for the experiments in tribo tester.
The chemical composition of the as received
material has been indicated in Table 1.
Table 1. Chemical composition of AISI SS-304 stainless steel.
Constituents C Si Mn
Percentage 0.08 1.00 2.00
446
2.1 Heat treatment
Heat treatment of the samples has been done in
a microprocessor controlled electric muffle
furnace [make: N.R. Scientific Kolkata]. The
dimension of the furnace is 250 127 127
with a maximum temperature limit of 1100C.
The set up is shown in Fig. 1. It is not out of place
to mention here that stainless steel SS-304 cant
be hardened by heat treatment as no phase
changes occur on heating and subsequent
cooling. However, softening is possible. Several
ways of softening processes have been discussed
by different researchers in their research studies
[4-14, 30]. Based on the feasibility of studies in
the laboratory some basic heat treatment
processes have been selected. These operations
have been discussed in the following sub-
sections.
Fig. 1. Photographic view of muffle furnace.
For sensitization, samples have been heated at
660 C and allowed to dwell for 30 minutes at
that temperature inside the furnace. Samples
have been cooled in an open environment, that
is, air cooling.
For annealing some samples have been heated
from room temperature to 950 C and allowed to
dwell for 2 hours at that temperature inside the
furnace. At the end of the operation the furnace
has been switched off and the samples have
been allowed to cool inside the furnace, that is,
furnace cooling.
P S Ni Cr Fe
0.04 0.03 8.00-10.50 18.00-20.00 Balance
 S. Kumar and A. Mukhopadhyay, Tribology in industry Vol. 38, No. 4 (2016) 445-453

Some test specimens have been heated from
room temperature of approximately 30 C up to
a temperature of 950 C and allowed to dwell at
that temperature for 2 hours (soaking time).
Rate of increment of temperature has been
selected as 10 per minute for all the cases. At
the end of the operation specimens have been
taken out of the furnace and allowed to cool in
open air to attain room temperature. This is the
process of normalizing.
Sudden cooling from elevated temperature is
known as quenching. This has been
accomplished by dipping the heated samples in
an oil bath maintained at room temperature.
Samples have been heated up to a temperature
of 950 C with a dwelling time of 2 hours as
before and then dipped immediately inside an
oil bath maintained at room temperature.
Cutting grade oil (grade 44) has been used as the
quenching medium in this case.
microscopic observation as well as for the
measurement of micro hardness.
2.3 Micro hardness measurement
Micro hardness of the samples has been
measured in a micro hardness tester LM 248
AT (LECO, serial no. XM8 116, Michigan).
Included angle of the pyramid shaped diamond
indenter is 136. All the tests have been
conducted at a magnification of 500X, test load
of 100 gf and dwell time of 10 sec. Two
indentations have been made at two different
points on each sample and the average value has
been considered as the representative micro
hardness. Figure 2 shows the set up for micro
hardness measurement.

For solution annealing some sensitized samples

are reheated at temperature of 1040 C with a
soaking time of 30 minutes and then allowed to
cool rapidly in water maintained at room
temperature. This is, however, completely
opposite to martensitic steels where this type
of heat treatment would harden the steel
instead of softening. Solution annealing of SS-
304 dissolves any precipitated carbide phase at
high temperature resulting a homogenous Fig. 2. Set up of the micro hardness measurement.
microstructure with a minor content of -
ferrite [13]. 2.4 Determination of delta ferrite

2.2 Observation of microstructure Amount of delta ferrite on the base material has
been de by magneto inductive testing equipment
Physical properties and mechanical behaviour, Fischer Feritscope FMP 30 (Finland) as shown
in particular, of a material depends on the in Fig. 3. A feritscope is used to measure the
microstructure. An optical or electron ferrite content in austenitic and duplex steel.
microscope can be used to reveal the
microstructure. In the present study a trinocular
microscope (Radical) has been used for the
purpose. The surface of each sample has been
polished using five grades of emery papers,
courser to finer. Finally a felt polishing machine
has been used to polish the surface with aqueous
aluminium oxide (Al2O3) solution to give a
shinny, smooth and mirror like appearance of
the surface of the sample. The surface roughness
has not been measured in the present work.
Standard nital solution, a mixture of 3 % nitric Fig. 3. Feritscope FMP 30 (Finland) with probe.
acid and 97 % ethyl alcohol, has been used to Magnetic induction method is the basis of such
etch the polished surface of the samples for measurement [15,16,26]. Proportions of delta

447
 S. Kumar and A. Mukhopadhyay, Tribology in industry Vol. 38, No. 4 (2016) 445-453

ferrite, strain induced martensite and any other
ferrite phases can be measured by this method.
Testing has been done on heat treated samples of
size 20 20 8. Ten readings have been taken in
ten different places on the surface of each sample
and the average value represents the
corresponding reading. This test is based on the
fact that the austenite is nonmagnetic and the
delta ferrite is magnetic.
1800 sec of the said parameters have been
selected for the wear test. Weights of all the
specimens have been measured before and after
the wear test using an electronic analytical and
precision balance (Sartorius BSA 223S, Germany;
maximum range is 220 gm with a readability of
0.001gm). Difference of the two values indicates
the weight loss of the specimen due to wear [23].

2.5 Friction and wear test 3. RESULTS AND DISCUSSION

Friction and wear tests of the samples have been
carried out in a multi tribo tester TR-25
(DUCOM, India) supported with Winducom
2006 software. Block-on-Roller configuration of
the tester has been utilized for this purpose. The
samples have been slid against EN-8 stainless
steel roller of 50 mm diameter and hardness of
55HRC. Wear is measured in terms of
displacements in microns with the help of a linear
voltage resistance transducer in this set up [17].
All the tests have been carried out at an average
room temperature of 30 C and humidity of
approximately 85-90%. All the samples have
been cleaned thoroughly with acetone to remove
any trace of oil, grease, dirt or dust. Based on
different research studies [3, 18-22 and
references there in] rotational speed of the wheel
(rpm), load on job (N) and duration of test run
(sec) have been identified as the most important
parameters for the wear test in multi tribo tester
and corresponding values of 375 rpm, 25 N and
Micro hardness values of the heat treated
samples at different matrix or region have been
furnished in Table 2. The values of the micro
hardness indicate the probable microstructures
of the particular region. This is further supported
by corresponding micrographs. The micrographs
of all the heat treated samples at two
magnifications namely 500 and 400 have been
furnished in Fig. 4 (a) (j).
It is well known that AISI 304 stailess steel
undergoes a martensitic transformation under
cyclic loading conditions [16,24,25]. There are
three prominent matrix or zone in the
microstructures namely white, black and mixture
of white and black. Micro hardness values have
measured in those zones or regions. Comparing
the micrographs and corresponding micro
hardness values, as tabulated in Table 2,
following analysis can be made:

Table 2. Micro hardness at different matrix of heat treated samples.

Heat Treatment Matrix Type Microstructure D1 (m) D2 (m) HV (H) Avg. HV
White Martensite 24.72 m 21.64 m 345.1
331.6
White Martensite 25.37 m 22.92 m 318.1
Sensitized
Black Martensite 21.24 m 19.96 m 437.0
432.3
Black Martensite 20.37 m 21.28 m 427.6
White Austenite 30.48 m 32.16 m 189.0
202.1
Solution White Austenite 29.87 m 29.87 m 215.2
Annealed Black Ferrite 23.50 m 29.29 m 266.2
270.8
Black Ferrite 24.88 m 27.02 m 275.4
White Austenite 28.51 m 28.35 m 229.4
223.1
White Austenite 30.84 m 27.65 m 216.8
Oil Quenched
Black Ferrite Band 26.66 m 25.45 m 273.2 273.2
Black Carbide(CrC) 16.28 m 14.04 m 806.9 806.9
White Carbide(CrC) 15.88 m 16.63 m 701.8
734.6
White Carbide(CrC) 15.16 m 15.93 m 767.4
Annealed
Black Ferrite 25.36 m 25.44 m 287.4
291.3
Black Ferrite 24.99 m 25.14 m 295.2
White Austenite 29.54 m 29.30 m 214.8 214.8
White Ferrite 26.14 m 27.23 m 257.8 257.8
Normalized
Black Carbide(CrC) 16.55 m 16.23 m 690.3 690.3
Black Mixture of Martensite and Carbide 20.54 m 19.86 m 454.4 454.4

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 S. Kumar and A. Mukhopadhyay, Tribology in industry Vol. 38, No. 4 (2016) 445-453
Figure 4 (a) and (b) indicates the
microstructures of sensitized sample where
white and black matrix in both the figures
indicates the formation of martensite. Mixture of
martensite and carbide is present in the black
matrix or region and some part contains ferrite,
where as white matrix or region is austenite in
case of air cooled samples as indicated in Fig. 4
(c) and (d) respectively. Microstructures of
annealed samples have been depicted in Fig. 4
(e) and (f). Figure 4 (e) indicates that austenite
has been transformed into ferrite and carbide
(chromium carbide). White matrix in Fig. 4 (f)
reveals the presence of austenite within grain
(a)
(c)
(e)
boundary. Carbide deposition is also prominent
on the grain boundary. Oil quenched sample
shows the presence of ferrite as evidenced as
black band [cf. Fig. 4 (g)]. The entire black
matrix here represents carbide. Figure 4 (h)
shows the existence of austenite (white), ferrite
and carbide. In case of solution annealed
samples the existence of austenite and formation
of ferrite has been revealed from Fig. 4 (i).
Figure 4 (j), on the other hand, indicates the
formation of martensite inside the grain
boundaries. It is needless to be mentioned that
austenite already contains carbon.
(b)
(d)
(f)
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 S. Kumar and A. Mukhopadhyay, Tribology in industry Vol. 38, No. 4 (2016) 445-453

(g) (h)

(i) (j)
Fig. 4. Micrographs of different heat treated SS-304 samples showing the microstructures of (a) sensitized
sample at 500 (b) sensitized sample at 400 (c) normalized sample at 500 (d) normalized sample at 400 (e)
annealed sample at 500 (f) annealed sample at 400 (g) oil quenched sample at 500 (h) oil quenched at 400
(i) solution annealed sample at 500 and (j) solution annealed sample at 400.

Table 3. Percentage of bcc phase as obtained from Fischer Feritscope.

Heat Treatment % Reading of bcc Phase Average
Type 1 2 3 4 5 6 7 8 9 10 (bcc Phase)
Sensitized 0.25 0.15 0.14 0.26 0.25 0.12 0.17 0.16 0.24 0.18 0.192
Annealed 0.67 0.75 0.68 0.58 0.72 0.88 0.70 0.51 0.63 0.65 0.676
Oil Quenched 0.61 0.51 0.55 0.60 0.49 0.61 0.43 0.59 0.45 0.58 0.542
Annealed 1.0 0.87 0.93 0.97 1.1 0.81 0.90 1.0 0.91 0.99 0.948
Normalized 0.51 0.53 0.51 0.71 0.78 0.59 0.80 0.53 0.71 0.64 0.631

Different types of heat treated SS-304 stainless
steel contain mainly austenite (approximately
95 %), carbide, martensite (less than 1%) and -
ferrite (less than 1%). Fischer Feritscope
measures the bcc percentage in the heat treated
samples [26]. Presence of bcc structure is mainly
due to martensite and -ferrite. Table 3 indicates
the percentage of bcc phase in different heat
treated samples. Ten measurements have been
taken in ten different places on the surface of
each sample and the average values have been
considered as the representative data in this
regard. It has been revealed from the above
table that quantity of -ferrite is less than 1% in
all the cases. Thus, -ferrite has very little effect
on the hardness of heat treated samples. The
hardness of the heat treated samples may be
assumed to be affected by austenite, carbide and
martensite (very little). Hardness, again, is
related to micro hardness of ferrite austenite,
carbide and austenitic phases. Micro hardness
values have already been presented in Table 2.
Weight loss data due to wear have been
furnished in Table 4, whereas Table 5 indicates
wear (micron) data as obtained directly from
Winducom 2006 software at different time
intervals. Corresponding curves have also been
drawn in Fig. 5.

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 S. Kumar and A. Mukhopadhyay, Tribology in industry Vol. 38, No. 4 (2016) 445-453

Table 4. Weight loss of the specimens due to wear.

Weight Loss (w1-w2) in gm
Sample No.
Sensitized Furnace Cooled Air Cooled Oil Cooled Solution Annealed
I 0.076 0.069 0.057 0.098 0.092
II 0.074 0.063 0.061 0.093 0.088
Avg. 0.075 0.066 0.059 0.096 0.090

Table 5. Wear (micron) of different heat treated samples in regular time intervals.
Heat Treatment Wear (micron) in different time intervals (sec)
300 600 900 1200 1500 1800
Sensitized 86.152 94.262 107.793 125.043 151.501 164.972
Annealed 111.040 117.157 116.397 117.201 120.968 123.966
Normalized 31.712 40.092 48.325 60.933 73.133 91.218
Oil quenched 139.965 177.901 204.43 218.06 224.054 231.011
Solution annealed 134.974 168.633 189.968 199.537 205.777 210.34

Fig. 5. Comparative charts of wear (micron) against time.

From Table 2 it has been revealed that
normalized sample has good hardness owing to
the presence of austenite, carbide (CrC) and
mixture of martensite and carbide. So it has lesser
amount of wear than all other heat treated
samples. The wear follows almost a straight line
path (cf. Fig. 5). Sensitize samples contain higher
amount of martensite. Thus, more hardness is
obtained in sensitized samples resulting less
wear rate as is evidenced in Table 5. The wear is,
however, gradually increasing with time (cf. Fig.
5). On the contrary, annealed samples have more
amount of carbide. These samples also have good
amount of hardness. Initial wear is somehow
more than that of sensitized samples. But the
wear is almost stable with time and follows a
straight line path. Sensitized, annealed and
normalized samples have less amount of wear
than oil quenched and solution annealed samples
as the hardness of oil quenched and solution
annealed samples are far less than sensitized,
annealed and normalized samples. Ferrite and
austenite phases are prominent in majority of the
portions of oil quenched and solution annealed
samples. Though oil quenched sample contains
carbide (CrC) but quite likely the percentage is
very low. Hence, this sample has little resistance
against wear. Weight loss data (gm) of the worn
samples have been given in Table 4. It has been
revealed that the weight loss data and the wear
(micron), as obtained directly from the
Winducom 2006 software, are in good
agreement. Thus, it is justified to consider the
weight loss data as a measure of wear.
4. CONCLUSION
Some important findings of the present
experimental work have been furnished below:
Some important heat treatments of SS 304
stainless steel have been done utilizing in
house facilities. This is a great value
addition in conceptual learning process.
Microstructures and corresponding micro
hardness of different matrix has been
appraised and evaluated accordingly.

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 S. Kumar and A. Mukhopadhyay, Tribology in industry Vol. 38, No. 4 (2016) 445-453
Presence of - ferrite and martensite, that
is, bcc structure is less than 1% in all the
heat treated samples.
Normalized samples have minimum wear
whereas oil quenched samples have
maximum wear. Wear of normalized
samples is minimum, however there is a
gradually increasing trend.
Annealed samples show medium wear
with a stable trend.
Weight loss data are in good agreement
with wear data, as obtained directly from
Winducom 2006 software, in the present
study.
Acknowledgement
The present experimental work has been
accomplished in the frame work of the
laboratories of Mechanical engineering
department and partly in Metallurgical and
Material Sciences department of the Jadavpur
University, Kolkata, India. Any kind of assistance,
whatever little it may be, from any individual is
sincerely acknowledged by the authors.
REFERENCES
[1] P. Leroux, Stainless steel analysis using
tribology and 3D metrology, NANOVEA, pp. 1-9,
available at: http://www.nanovea.com, 2010.
[2] K.C. Ludema, Friction, Wear, Lubrication: A
Textbook in Tribology. USA: CRC Press, 1996.
[3] G.A. Fontalvo and C. Mitterer, Comparison of
the tribological properties of different cold work
steels at temperatures up to 250C, in 6th.
International Tooling Conference, Austria, p. 223.
[4] D.J. Naylor and W.T. Cook, Heat Treated
Engineering Steels, Materials Science and
Technology, vol. 7, pp. 405-538, 1992.
[5] A.K. Sinha, Ferrous Physical Metallurgy. Boston,
MA: Butterworths, 1989.
[6] M.A. Grossmann and E.C. Bain, Principles of Heat
Treatment. Metals Park, OH: American Society
for Metals, 1964.
[7] G. Krauss, Steels: Heat Treatment and Processing
Principles. Materials Park, OH: ASM
International, 1990.
452
[8] R.A. Lindberg, Processes and materials of
manufacture. New Delhi: Prentice-Hall, 1974.
[9] F. Han, G. Lin, M. Hu, S. Wang, D. Peng and Q.
Zhou, Softening interstage annealing of
austenitic stainless steel sheets for stamping
processes, Journal of Cent, South University, vol.
19, pp. 1508-1516, 2012.
[10] M. Sharma and A. Kumar, Study of effect on
mechanical properties of SS 304 at different
ranges of carburization temperature, IJCSCE,
Special issue on NCRAET-2013, pp.13-17, 2013.
[11] X. Meng, J. Zhang, J. Zhao and W. Han, Influence
of annealing treatment on microstructure and
properties of cold sprayed stainless steel
coatings, Acta Metall. Sin. (Eng. Lett.), vol. 24,
no. 2, pp. 92-100, 2011.
[12] A.K. Tanwer, Effect of various heat treatment
processes on mechanical properties of mild
steel and stainless steel, AIJRSTEM, vol. 8, no. 1,
pp. 57-68, 2014.
[13] S.A. Tukur, M.S. Dambatta, A. Ahmed and N.M.
Muaz, Effect of heat treatment temperature on
mechanical properties of the AISI 304 stainless
steel, IJIRSET, vol. 3, no. 2, pp. 9516-9520, 2014.
[14] Stress reliving heat treatments for austenitic
stainless steels, available at
http://www.bssa.org.uk/topics.php?article= 76.
[15] S.A. Gigovi-Geki, M. Oru and S.M. Goji,
Determination of the content of delta ferrite in
austenitic stainless steel nitronic 60, in 15th
International Research/Expert Conference
Trends in the Development of Machinery and
Associated Technology-TMT 2011, Prague, Czech
Republic, 2011, p. 157.
[16] H.J. Christ, U. Krupp, C. Mueller-Bollenhagen, I.
Roth and M. Zimmermann, Effect of deformation
induced martensite on the fatigue behavior of
metastable austenitic stainless steels, Personal
communication, Germany, E-mail: Hans-
Juergen.Christ@uni-siegen.de. pp. 3-4.
[17] DUCOM User Manual for safety, installation,
operation and maintenance, WO No. 305,
DUCOM, India, 2002.
[18] N.L. Parthasarathi, U. Borah and K.Sh. Albert,
Correlation between coefficient of friction and
surface roughness in dry sliding wear of AISI
316L (N) stainless steel at elevated
temperatures, Computer Modeling and New
Technologies, vol. 17, no. 1, pp. 51-63, 2013.
[19] M.A. Chowdhury, D.M. Nuruzzaman, B.K. Roy,
P.K. Dey, M.G. Mostafa, M.S. Islam and R.Md. Mia,
Experimental investigation on friction and wear
of stainless steel 304 sliding against different
 S. Kumar and A. Mukhopadhyay, Tribology in industry Vol. 38, No. 4 (2016) 445-453

pin materials, World Applied Science Journal, Influence of temperature and carbon content,
vol. 22, no. 12, pp. 1702-1710, 2013. Mater. Sci. Eng., A 481482, pp. 713-717, 2008.
[20] M.A. Chowdhury, D.M. Nuruzzaman, B.K. Roy, A. [25] M. Smaga, F. Walther and D. Eifler,
Islam, Z. Hossain and R. Md. Hasan, Deformation-induced martensitic
Experimental investigation of friction transformation in metastable austenitic steels,
coefficient and wear rate of stainless steel 202 Mater. Sci. Eng., A 483484, pp. 394-397, 2008.
sliding against smooth and rough stainless steel
[26] FERITSCOPE FMP30 Measurement of the
304 counter-faces, Friction and Wear Research,
Ferrite Content in Austenitic and Duplex Steel.
vol. 1, no. 3, pp. 34-41, 2013.
www.helmut-fischer.com- Helmut Fischer
[21] A. Mukhopadhyay, P. Mondal, R. Saha and S. GmbH Institute fur Electronic und Messtechnik
Dutta, Optimization of process parameters 71069 Sindelfingen, Germany.
during dry sliding wear of different weld zones
[27] R.A. Covert and A.H. Tuthill, Stainless steels: an
of AISI-304 SS in a block-on-roller tribotester,
introduction to their metallurgy and corrosion
in: National Conference IFMMT 2014, Manipal
resistance, Dairy, Food and Environmental
University, Jaipur, India, 2014, p. 1.
Sanitation, vol. 20, no. 7, pp. 506-517, 2000.
[22] A. Mukhopadhyay, SEM study of worn surface
[28] A. Mukhopadhyay, Some tribological
morphology of an indigenous EPDM rubber,
characterization of EPDM rubber, Tribology in
Polymer Testing (Elsevier), vol. 52, pp. 167-173,
Industry, vol. 36, no. 2, pp. 109-116, 2014.
2016.
[29] I. Sivakumaran and V. Alankaram, The wear
[23] S. Kumar and A. Mukhopadhyay, Study of dry
characteristics of heat treated manganese
sliding tribo-characteristics of heat treated SS-
phosphate coating applied to AlSi D2 steel with oil
304 stainless steel against En-8 stainless steel
lubricant, Tribology in Industry, vol. 34, no. 4,
using a multi tribo tester, in 2nd International
pp. 247-254, 2012.
Conference ICRIET-16, MAIT, Baddi, Himachal
Pradesh, India, 2016, p. 258. [30] J.O. Agunsoye and A.A. Ayeni, Effect of heat
treatment on the abrasive wear behaviour of high
[24] U. Krupp, C. West and H.J. Christ, Deformation-
chromium iron under dry sliding condition,
induced martensite formation during cyclic
Tribology in Industry, vol. 34, no. 2, pp. 82-91,
deformation of metastable austenitic steel:
2012.

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Tribology in Industry

RESEARCH
www.tribology.fink.rs

Multi-objective Optimization of Process

Performances when Cutting Carbon Steel with
Abrasive Water Jet

M. Radovanovi a
a University of Ni, Faculty of Mechanical Engineering, Aleksandra Medvedeva 14, 18000 Ni, Serbia.

Keywords: ABSTRACT
brasive water jet cutting
Multi-objective optimization of process performances (perpendicularity
ulti-objective optimization
deviation, surface roughness and productivity) when cutting carbon
Perpendicularity deviation surface
steel EN S235 with abrasive water jet is presented in this paper. Cutting
Roughness
factors (abrasive flow rate, traverse rate and standoff distance) were
Productivity
determined when perpendicularity deviation and surface roughness are
minimal and productivity is maximal. Multi-objective genetic algorithm
Corresponding author: (MOGA) was used for the determination set of nondominated optimal
Miroslav Radovanovi points, known as Pareto front.
University of Ni, 2016 Published by Faculty of Engineering
Faculty of Mechanical Engineering,
Aleksandra Medvedeva 14,
18000 Ni, Serbia.
E-mail: mirado@masfak.ni.ac.rs

1. INTRODUCTION versatility and has been proven to be an

There are some machining technologies for
contour cutting metal or non metal sheets.
Flame cutting, plasma cutting, laser cutting, wire
EDM and water jet cutting are more applicable
machining technologies for contour cutting
sheets. Abrasive water jet (AWJ) cutting is a
modern nonconventional machining technology
that enables contour cutting a wide range of
materials and thickness. AWJ cutting has
advantages over the other contour cutting
technologies such as: no thermal distortion, no
heat affected zone, small cutting force, minimum
stress on the workpiece, high flexibility, high
effective technology for machining various
engineering materials and wide range of
thickness. hickness which can be cut are 100
mm for stainless steel and 120 mm for
aluminum, for water pressure of 400 MPa. With
AWJ it is possible to cut random contours in
thick, middle and thin sheets, such as very fine
tabs and filigree structures. Tolerances of 0.1
mm can be realized in metal cutting. [1]
Process of AWJ cutting is based on material
removal from the workpiece by erosion. High
speed water jet stream accelerates abrasive
particles and those particles erode the material.

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 M. Radovanovi, Tribology in Industry Vol. 38, No. 4 (2016) 454-462
In AWJ cutting high pressure pump via
accumulator and high pressure tubing directs
the pressurized water to the cutting head. Types
of pumps and levels of pressure are classified by
water jet industry as:
Low pressure, p<10000 psi (p<690 bar,
p<69 MPa)
Medium pressure, 10000<p<15000 psi
(690<p<1030 bar, 69<p<103 MPa)
High pressure, 15000<p<40000 psi
(1030<p<2760 bar, 103<p<276 MPa)
Ultra high pressure, 40000<p<75000 psi
(2760<p<5170 bar, 276<p<517 MPa)
Hyper pressure, p>75000 psi (p>5170 bar,
p>517 MPa).
There are two types of high pressure pumps:
direct drive pumps and intensifier pumps. Direct
drive pumps generally are found in industrial
applications with pressure to 380 MPa. These
pumps use an electric motor to turn a crankshaft
that moves three or more pistons that create the
water pressure. But, the most common pumps in
industrial applications are intensifier pumps.
Intensifier pumps are called intensifiers because
they use the concept of pressure intensification
to generate the desired water pressure. These
pumps use hydraulics to apply a certain amount
of oil pressure on one side of a piston of a certain
diameter. On the water side of the pump, the
diameter of the piston is much smaller. The
difference in the surface area between the
hydraulic side and the water side gives a
multiplication factor, or intensification, to the
pressure from the oil side. Most intensifier
pumps have an intensification ratio of 20 times.
Intensifier pumps generally are found in
pressure applications to 600 MPa. With
intensifier pump can be achieved hyper
pressure. Water jet pumps are specified in either
horsepower (HP) or kilowatts (kW) to indicate
the size of the electric motor that creates the
force to pressurize the water. High pressure
pumps power range is from 15 HP (11 kW) to
200 HP (150 kW). Most common AWJ machine
tools are with power between 30 HP (22 kW)
and 100 HP (75 kW). Cutting head consists of
orifice, mixing chamber and focusing tube.
Orifice is with diameter of 0.15 to 0.35 mm and
is made of sapphire, ruby or diamond. Focusing
tube is with diameter of 0.54 to 1.1 mm, length
of 50 to 100 mm, and is made of tungsten
carbide. Water is pressed out of the orifice in
form of very thin jet at a high speed. Speed of
water jet can calculate using equation:
2p . (1)
v wj
w
where are: vwj-speed of water jet in m/s, -
correction factor (0.9-0.98), p-water pressure in
Pa, w-density of water in kg/m3.
Abrasive particles are added to water jet in
mixing chamber of the cutting head. There are
two methods to add abrasive particles to water
jet: suspension and injection. The suspension
method (direct, indirect or bypass) is used in
industry only at pressures of up to 70 MPa.
Today the injection method is mainly used for
industrial applications with operating pressures
of up to 400 MPa. The high velocity of the water
jet creates a Venturi effect or vacuum in the
mixing chamber located immediately beneath
the orifice. Abrasive particles are metered from
a mini-hopper through a plastic tube down to
the cutting head and are sucked into the water
jet stream in the mixing chamber. Abrasive
particles are accelerated with high speed water
jet. Abrasive particles are mixed with the water
jet creating abrasive water jet. Speed of abrasive
water jet can calculate using equation [2,4]:
v wj . (2)
v awj
m
1 a
mw
Where are: vawj-speed of abrasive water jet in
m/s, -momentum loss factor (0.65-0.85), vwj -
speed of water jet in m/s, ma-abrasive mass flow
rate in kg/s, mw-water mass flow rate in kg/s.
Abrasive water jet is focused by a focusing tube.
Focusing tube directs the abrasive water jet to
cut the workpiece. Abrasive water jet cuts
workpiece along the programmed contour using
CNC (computer numerical control) motion
system of the machine. Scheme of the AWJ
cutting is shown in Fig. 1. [2,3].
For evaluation of the AWJ cutting, the greatest
influence has a group of geometric characteristics
of the workpiece issued in cutting process. The
geometric characteristics are: form accuracy,
dimensional accuracy and cut quality. Cut quality
relates to form of kerf and cut surface. Terms in
AWJ cutting, according ISO/TC 44 N 1770 [5], are
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 M. Radovanovi, Tribology in Industry Vol. 38, No. 4 (2016) 454-462
shown in Fig. 2, where are: Ra-surface roughness,
f-pitch of drag line, g-burr, hf-fine cut, hr-
remaining surface, n-drag line, rk-edge radius, s-
jet direction, sb-jet affected zone, t-workpiece
thickness, u-perpendicularity or angularity
tolerance. Cut quality limits AWJ cutting
application. The perpendicularity deviation and
surface roughness of the cut are the most
significant characteristics of the cut quality.
Fig. 1. Scheme of AWJ cutting.
Fig. 2. Terms related to kerf and cut surface.
There are some studies of multi-objective
optimization of abrasive water jet machining
and multi-objective optimization using genetic
algorithms (GA). Aultrin J. and Anand D. in [6]
studied abrasive water jet cutting of aluminum
alloy 6061. They have investigated the effect of
factors (water pressure, abrasive flow rate,
orifice diameter, focusing tube diameter and
standoff distance) on performances (material
removal rate and surface roughness). using
456
Response Surface Methodology (RSM). Two
objectives (material removal rate and surface
roughness) are optimized by using Grey Relation
Analysis (GRA).
Chakravarthy P. and Babu N. in [7] studied
abrasive water jet cutting of granite. They have
investigated the effect of factors (water
pressure, traverse rate and abrasive flow rate)
on performance (depth of cut). In order to
determine the Pareto front for the multi-
objective optimization problem with three
objectives (cost of production, rate of production
and consumption of abrasives) they have
applied a new approach based on the principles
of fuzzy logic and genetic algorithm (GA).
Chaitanya M. and Krishna A. in [8] studied laser
cutting of aluminum alloy 7075. They have
investigated the effect of factors (pulse-power,
pulse frequency, pulse width and assist gas
pressure) on performances (surface roughness
and heat affected zone). In order to determine
the Pareto front for the multi-objective
optimization problem with two objectives
(surface roughness and heat affected zone) they
have applied GA based non dominated sorting
algorithm-II (NSGA-II).
Soni V. et al. in 9 studied turning of aluminum
using carbide cutting tool. They have
investigated the effect of factors (depth of cut,
feed and cutting speed) on performances
(material removal rate and surface roughness).
In order to determine the Pareto front for the
multi-objective optimization problem with two
objectives (material removal rate and surface
roughness) they have applied multi-objective
genetic algorithm (MOGA).
Bouzakis K. et al. in 10 studied milling of
aluminum alloy 2024 using cemented carbide
face milling cutting tool. They have investigated
the effect of factors (depth of cut, feed rate and
cutting speed) on performances (machining cost
and machining time). In order to determine the
Pareto front for the multi-objective optimization
problem, for rough milling with three objectives
(production cost, production time and distance
from maximum power) and for finish milling
with three objectives (production cost,
production time and cutting tool deflection),
they have applied multi-objective genetic
algorithm (MOGA).
 M. Radovanovi, Tribology in Industry Vol. 38, No. 4 (2016) 454-462

2. AWJ CUTTING FACTORS AND Factors of motion system (precision,

PERFORMANCES accuracy, stiffness, working conditions).
Factors of process (water pressure,
AWJ cutting is a complex process with many
traverse rate, abrasive flow rate, standoff
factors that determine performances.
distance, impact angle).
Mechanism of erosion depends on the level of
various process factors and is explained by
AWJ cutting performances can be classified into
multiple phenomena. AWJ cutting factors can be
five categories, Fig. 4:
classified into six categories, Fig. 3:
Process performances (orifice wear,
Factors of workpiece (material type,
focusing tube wear, temperature, noise,
thickness, chemical structure, hardness,
vibration).
toughness, grain size, tolerances,
roughness). Quality performances (form deviations,
dimension deviations, cut quality: kerf
Factors of water system (pump pressure,
depth, kerf width, perpendicularity
water flow rate, water purity, accumulator
deviation of the cut surfaces-kerf taper,
volume, high pressure tubing).
striations, burr, edge radius, jet affected
Factors of abrasive system (abrasive zone, surface roughness).
material type, abrasive hardness, abrasive
Productivity performances (machining
particle size, abrasive particle shape,
time, productivity).
abrasive particle size distribution,
abrasives input method). Economy performances (manufacturing
cost, power consumption, abrasives
Factors of cutting head (orifice diameter,
consumption, water consumption).
orifice material, focusing tube diameter,
focusing tube length, focusing tube Ecology performances (noise, pollution,
material). recycling).

Fig. 3. AWJ cutting factors.

Fig. 4. AWJ cutting performances.

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 M. Radovanovi, Tribology in Industry Vol. 38, No. 4 (2016) 454-462

Some of the most important performances in levels) with center point. Control factors are:
AWJ cutting are perpendicularity deviation, abrasive flow rate (ma), traverse rate (vf), and
surface roughness and productivity. standoff distance (h). Control factors and their
levels are shown in Table 1. [12]
Perpendicularity deviation of the cut surfaces
(kerf taper) is distance between two parallel Table 1. Control factors and levels
straight lines (tangents) between which the cut Levels
surface profile is inscribed, and within the set Code Control factors
-1 0 +1
angle (e.g. 90 in the case of vertical cuts).
A Abrasive flow rate, ma (g/min) 300 500 700
Perpendicularity deviation includes and the
flatness deviations. B Traverse rate, vf (mm/min) 50 100 150
C Standoff distance, h (mm) 1 3 5
Surface roughness is a measure of the
technological quality of the cut. Commonly Three control factors are arranged in design of
arithmetic average roughness (Ra) was used to experiment with 9 runs (8 runs are for base
describe surface roughness. Ra is defined as the design and 1 run for center point). Measured
arithmetic value of the profile from centerline performances are: perpendicularity deviation
along the sampling length. (u) and surface roughness (Ra). Perpendicularity
Productivity is defined as: deviation has measured using optical
microscope Metkon and surface roughness has
Q tvf . (3)
measured using surface measuring instrument
where are: Q (mm2/min)-productivity, t (mm)- Hommel Tester T500. Design of experiment with
material thickness, vf (mm/min)-traverse rate. factor levels and measured values of
performances, is presented in Table 2.
Productivity in contour cutting of sheets is
defined as cut surface productivity, i.e. surface of Table 2. Design of experiment and results.
the cut in unit of time. The goal in contour Control factors u Ra
cutting is to have maximum cutting length with Run
A B C (mm) (m)
minimum kerf width.
1 -1 -1 -1 0.07 4.12
2 -1 -1 1 0.11 4.50
3. EXPERIMENTAL RESEARCH 3 -1 1 -1 0.17 5.18
4 -1 1 1 0.14 5.13
Experimental research was planed and realized 5 1 -1 -1 0.20 4.23
in order to define regression equations for 6 1 -1 1 0.21 4,45
performances (perpendicularity deviation and
7 1 1 -1 0.30 4.99
surface roughness) in correlation of factors
(abrasive flow rate, traverse rate and standoff ... ... ... ... ... ...
distance). The equipment used for 9 0 0 0 0.26 4.22
experimentation was abrasive water jet cutting
machine Hydro Jet Eco 0615 with high pressure Analysis of variance (ANOVA) was carried out to
pump of 150 MPa, power of 7.5 kW and water find the relative effect of factors and interactions
flow rate of 2.4 l/min. Cutting head was on performances perpendicularity deviation and
composed of orifice made of sapphire with inner surface roughness. If p<0.05 the factors have a
diameter of 0.35 mm and focusing tube made of significant effect on performance. If p>0.10 the
tungsten carbide with inner diameter of 1.02 factors have not an effect on performance. If
mm and length of 76 mm. Jet impact angle was 0.05<p<0.10 the factors have a moderate effect
90. All experiments were conducted with water on performance. Analysis of variance for
pressure of 150 MPa. Abrasive material was perpendicularity deviation (u) is shown in Table
Garnet mesh 80 ( 177 m). Workpiece material 3. Standard F table value at 95 % confidence
was carbon steel EN S235, thickness of 6.5 mm. level is F0.05,1,3=10.13.

Design of experiment was conducted using full From Table 3 can see that factors: abrasive flow
factorial design 23 (three factors each on two rate, traverse rate and standoff distance have a

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strong (clearly statistically significant) effect on Table 4. Analysis of variance for Ra.
the perpendicularity deviation with contribution Source DF SS MS F p %
of 90.28 %. Traverse rate is the most significant Main effects 3 1.33330 0.44443 4848 0.000 65.39
factor affecting the perpendicularity deviation
A 1 0.06845 0.06845 746 0.000 3.36
with contribution of 51.04 %. Abrasive flow rate
affects with contribution of 34.70 % and B 1 1.26405 1.26405 13789 0.000 61.99
standoff distance affects with contribution of C 1 0.00080 0.00080 8.73 0.060 0.04
4.54 % on the perpendicularity deviation. Some 2-Way
3 0.03225 0.01075 117 0.001 1.58
interactions have significant effect on the Interactions
perpendicularity deviation. Interaction abrasive AB 1 0.02645 0.02645 288 0.000 1.30
flow rate-traverse rate affects with contribution AC 1 0.00080 0.00080 8.73 0.060 0.04
of 1.27 %, abrasive flow rate-standoff distance BC 1 0.00500 0.00500 54.55 0.005 0.24
affects with contribution of 5.67 % and
3-Way
interaction abrasive flow rate-traverse rate- Interaction
1 0.02000 0.02000 218 0.001 0.98
standoff distance affects with contribution of
ABC 1 0.02000 0.02000 218 0.001 0.98
1.90 % on the perpendicularity deviation.
Curvature 1 0.65340 0.65340 7128 0.000 32.04
Table 3. Analysis of variance for u. Error 3 0.00028 0.00009 - - 0.01
Source DF SS MS F p % Total 11 2.03922 - - - 100
Main effects 3 0.07184 0.02394 261.23 0.000 90.28
A 1 0.02761 0.02761 301.23 0.000 34.70
Traverse rate is the most significant factor
affecting the surface roughness with
B 1 0.04061 0.04061 443.05 0.000 51.04
contribution of 61.99 %. Abrasive flow rate
C 1 0.00361 0.00361 39.41 0.008 4.54 affects with contribution of 3.36 %. Standoff
2-Way
3 0.00584 0.00194 21.23 0.016 7.34 distance has moderate effect with contribution
Interactions of 0.04 %. Some interactions have significant
AB 1 0.00101 0.00101 11.05 0.045 1.27 effect on the surface roughness. Interaction
AC 1 0.00451 0.00451 49.23 0.006 5.67 abrasive flow rate-traverse rate affects with
BC 1 0.00031 0.00031 3.41 0.162 0.39 contribution of 1.30 %, traverse rate-standoff
3-Way distance affects with contribution of 0.24 %,
1 0.00151 0.00151 16.50 0.027 1.90 abrasive flow rate-traverse rate-standoff
Interaction
ABC 1 0.00151 0.00151 16.50 0.027 1.90 distance affects with contribution of 0.98 % on
the surface roughness. Interaction abrasive flow
Curvature 1 0.00010 0.00010 1.14 0.365 0.13
rate-standoff distance has moderate effect with
Error 3 0.00027 0.00009 - - 0.34 contribution of 0.04 % on the surface roughness.
Total 11 0.07957 - - - 100 Regression equation for surface roughness, with
DF-degree of freedom, SS-sum of square, MS-mean square, coefficient of determination of R2=99.99 %, is:
F-variance ratio, pvalue, %-percent contribution
R a 3.01125 0.0017125m a 0.015325v
Regression equation for perpendicularity 0.1325h 0.00001325m a v 0.000225m a h (5)
deviation, with coefficient of determination of 0.0015vh 0.0000025m a vh
R2=99.65%, is:
u 0.106562 0.000434375m a 0.00283125v f
0.0090625h 0.0000031875m a v f (4) 4. MULTI-OBJECTIVE OPTIMIZATION
0.000009375m a h 0.0000006875m a v f h
Procedure of multi-objective optimization has
Analysis of variance for surface roughness (Ra) is four phases. First phase is mathematical
shown in Table 4. Standard F table value at 95 % modelling of performances in correlation of the
confidence level is F0.05,1,3=10.13. factors. Second phase is determining
optimization problem. In second phase
From Table 4 can see that factors: abrasive flow objectives are selected and constraints are
rate and traverse rate have a strong (clearly defined. Third phase is selection of method for
statistically significant) effect on the surface solution of optimization problem. Fourth phase
roughness with contribution of 65.35 %. is solution of optimization problem.

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 M. Radovanovi, Tribology in Industry Vol. 38, No. 4 (2016) 454-462

Mathematical model of the multi-objective Nondominated points, generated by multi-

optimization was defined with goal to minimize objective genetic algorithm solver, have plotted
perpendicularity deviation and surface rougness in form of the Pareto front, Fig. 5.
and maximize productivity. Mathematical model
of the multi-objective optimization is:
Objective functions:
f1 min u
f 2 min R a
f 3 max Q

Constraints:
ma ,min ma ma ,max
vf ,min vf vf ,max
h min h h max

Mathematical model of the multi-objective

optimization for this study has form:
Fig. 5. Pareto front points.
Objective functions:
u 0.106562 0.000434375m a Listing of the Pareto front points obtained as

0.00283125v f 0.0090625h outcomes from the optimization process
f1 min presented in Table 6.
0.0000031875m a v f 0.000009375m a h

0.0000006875m v h
a f Table 6. Pareto front points.
R a 3.01125 0.0017125m a 0.015325v f f1 f2 f3 x1 x2 x3
Index u Ra Q ma vf h
0.1325h 0.00001325m a v f
f 2 min (mm) (m) (mm2/min) (g/min) (mm/min) (mm)
0.000225m a h 0.0015v f h
1 0.134 4.120 325.000 300.000 50.000 1.000
0.0000025m v h
a f 2 0.356 5.153 974.877 507.442 149.981 1.069
f3 min Q 6.5vf 3 0.251 4.563 588.735 339.636 90.113 1.965
4 0.590 5.121 972.039 579.961 149.545 4.711
Constraints 5 0.526 5.030 891.874 573.326 137.211 4.248
300 m a 700 6 0.353 5.153 974.757 507.461 149.963 1.016
50 v f 150 7 0.469 4.841 716.290 600.770 110.198 4.359
1 h 5 8 0.507 5.014 873.178 585.376 134.335 3.984
9 0.434 5.033 937.266 367.289 144.195 3.377
Table 5. Parameters of the multi-objective genetic
10 0.201 4.431 505.085 325.091 77.705 1.163
algorithm.
11 0.267 4.723 696.890 309.600 107.214 1.426
Population type Double vector
12 0.487 5.101 947.547 580.924 145.776 3.217
Population size 50
Creation function Constraint dependent 13 0.232 4.408 465.341 364.071 71.591 2.582
Selection function: Tournament, 14 0.382 4.913 806.165 482.089 124.025 2.598
Selection
Tournament size: 2 15 0.421 4.980 844.410 561.978 129.909 2.756
Reproduction Crossover fraction: 0.8 16 0.259 4.474 524.641 332.475 80.714 3.201
Mutation function: Constraint 17 0.333 4.865 757.053 501.921 116.470 1.747
Mutation
dependent
Crossover function:
Crosover From Table 6 it is evident that near optimal
Intermediate, Ratio: 1.0
Migration
Direction: Forward, Fraction: factor levels for rough cutting carbon steel EN
0.2, Interval: 20 S235 with abrasive water jet can be selected as:
Multiobjective Pareto front population fraction:
abrasive flow rate of ma=507.442 g/min,
problem settings 0.35
Generations: 100*number of traverse rate of vf=149.981 mm/min and
Stopping criteria standoff distance of h=1.069 mm. For these
variables
Current iteration 116 factor levels, perpendicularity deviation is

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 M. Radovanovi, Tribology in Industry Vol. 38, No. 4 (2016) 454-462
u=0.356 mm, surface roughness is Ra=5.153 m
and productivity is Q=974.877 mm2/ min.
From Table 6 it is evident that perpendicularity
deviation u is important performance for finish
cutting carbon steel EN S235 with abrasive
water jet. Surface roughness is Ra6.3 m. For
example, if tolerance of dimensions is T=0.25
mm (u0.25 mm) and Ra6.3 m, than the near
optimal factor levels can select as: abrasive flow
rate of ma=325.091 g/min, traverse rate of
vf=77.705 mm/min and standoff distance of
h=1.163 mm. For these factor levels,
perpendicularity deviation is u=0.201 mm,
surface roughness is Ra=4.431 m and
productivity is Q=505.085 mm2/ min.
5. CONCLUSION
AWJ cutting is a modern nonconventional
machining technology. Cut quality limits AWJ
cutting application. Some of the most important
performances in AWJ cutting are
perpendicularity deviation, surface roughness
and productivity. To optimize AWJ cutting
performances it is essential to have knowledge
of the perpendicularity deviation and surface
roughness in relation to process factors. When
AWJ cutting carbon steel EN S235 regression
equations for perpendicularity deviation and
surface roughness in relation of the abrasive
flow rate, traverse rate and standoff distance
have defined using experimental research. For
minimize perpendicularity deviation and surface
rougness and maximize productivity,
mathematical model of the multi-objective
optimization was defined. Multi-objective
genetic algorithm solver was selected as method
for solution of the optimization problem. For
rough cutting the near optimal factor levels can
select as: ma=507.442 g/min, vf=149.981
mm/min and h=1.069 mm. For these factor
levels perpendicularity deviation is u=0.356 mm,
surface roughness is Ra=5.153 m and
productivity is Q=974.877 mm2/min. For finish
cutting, if T=0.25 mm and Ra6.3 m, the near
optimal factor levels can select as: ma=325.091
g/min, vf=77.705 mm/min and h=1.163 mm. For
these factor levels perpendicularity deviation is
u=0.201 mm, surface roughness is Ra=4.431 m
and productivity is Q=505.085 mm2/min.
Acknowledgement
The paper is a result of the technological project
TR35034 which is supported by the Ministry of
Education, Science and Technological
Development of the Republic of Serbia.
REFERENCES
[1] M. Radovanovi and M. Madi, Optimizing
factor levels based on cost in abrasive water jet
cutting using GA, Methods and Techniques for
Industrial Development, University of Maribor,
Faculty of Mechanical Engineering, Politecnico
di Torino, Maribor, Slovenia, pp. 17-30, 2015.
[2] M. Radovanovi, Investigation of surface
roughness in abrasive water jet cutting using
Shainin method, Tribological Journal BULTRIB,
vol. 5., no. 5, pp. 105-110, 2015.
[3] M. Radovanovi and E. Herghelegiu,
Perpendicularity deviation and surface
roughness in abrasive water jet cutting of
carbon steel, Nonconventioal Technologies
Review, no. 2, pp. 39-44, 2016.
[4] B. Nedi and J. Barali, The wear of the focusing
tube and the cut-surface quality, Tribology in
Industry, vol. 32, no. 2, pp. 38-43, 2010.
[5] ISO/TC 44 N 1770, Water jet cutting-
Geometrical product specification and quality,
2010.
[6] J. Aultrin and D. Anand, Multi-objective
optimization of abrasive water jet machining of
aluminum 6061 alloy by Grey Relational
Analysis, Journal of Chemical and
Pharmaceutical Sciences, vol. 9, no. 1, pp. 410-
417, 2016.
[7] P. Chakravarthy and N. Babu, A new approach
for selection of optimal process parameters in
abrasive water jet cutting, Materials and
Manufacturing Processes, vol. 14, no. 4, pp. 581-
600, 2007.
[8] M. Chaitanya, A. Krishna, Multi-objective
optimization of laser beam cutting process,
International Journal of Research in Mechanical
Engineering & Technology - IJRMET, vol. 3, no. 2,
pp. 279-290, 2013.
[9] V. Soni, S. Mandal and B. Singh, Process
parameters optimization in turning of
aluminum using a new hybrid approach,
International Journal of Innovative Science,
Engineering & Technology - IJISET, vol. 1, no. 3,
pp. 418-423, 2014.
461
 M. Radovanovi, Tribology in Industry Vol. 38, No. 4 (2016) 454-462
[10] K. Bouzakis, R. Paraskevopoulou and G.
Giannopoulos, Multi-objective optimization of
cutting conditions in milling using genetic
algorithms, in: 3rd International Conference on
Manufacturing Engineering - ICMEN-2008, 1-3
October, Chalkidiki, Greece, pp. 763-774, 2008.
[11] E. Herghelegiu, Contributions to the
optimization of the water jet working
parameters, Dissertation, University Vasile
Alecsandri of Bacau, Romania, 2011.
[12] M. Madi, M. Radovanovi and B. Nedi,
Correlation between Surface Roughness
Characteristics in CO2 Laser Cutting of Mild
Steel, Tribology in Industry, vol. 34, no. 4, pp.
232-238, 2012.
[13] M. Radovanovi, Investigation on surface
roughness of carbon steel machined by abrasive
462
water jet using Taguchi method, Tribological
Journal BULTRIB, vol.4, pp. 47-54, 2014.
[14] P. Jankovi, M. Radovanovi, J. Barali and B.
Nedi, Prediction model of surface roughness in
abrasive water jet cutting of aluminium alloy,
Journal of the Balkan Tribological Association,
vol. 19, no 4, pp. 585-595, 2013.
[15] M. Radovanovi, P. Jankovi and M. Madi,
Predictive models of traverse rate in abrasive
water jet cutting based on RA and GA, Academic
Journal of Manufacturing Engineering, vol. 10,
no. 1, pp. 107-112, 2012.
[16] M. Radovanovi, Abrasive Waterjet Cutting
cost, Nonconventional Technologies Review, no.
1, pp. 97-102, 2007.
 Vol. 38, No. 4 (2016) 463-474

Tribology in Industry

RESEARCH
www.tribology.fink.rs

Tribological Considerations of Cutting Fluids in

Machining Environment: A Review

A. Anand a, K. Vohra a, M.I. Ul Haq a, A. Raina a, M.F. Wani b

a Department of Mechanical Engineering, SMVD University, Katra, Jammu & Kashmir, India,
b Centre for Tribology , National Institute of Technology, Srinagar, Jammu & Kashmir, India.

Keywords: ABSTRACT
Tribology The paper presents a review to highlight the tribological aspects of
Cutting fluids cutting fluids in machining environment. In this study, different
Lubrication machining processes viz. turning, grinding, drilling and milling have
Machining been considered with a special focus on grinding process. The cutting
fluids are primarily used as coolants and lubricants in the various
Corresponding author: machining processes. Different cutting fluids and the health hazards
associated with their use have also been represented in this research
A. Anand article. The paper also highlights the role of work materials and the
Department of Mechanical Engineering, cutting tool materials from tribology point of view. The literature
SMVD University, revealed that the development of biocompatible cutting fluids, recycling
Katra, J&K, India. of cutting fluids, cutting fluids for high temperature tribological
E-mail: anand.ankush13@gmail.com applications, studying the wetability characteristics with addition of
nanoparticles, etc. can be taken up as study in order to enhance the
tribological properties of the cutting fluids.
2016 Published by Faculty of Engineering

1. INTRODUCTION emphasis on the role of tribology in the areas of

In todays competitive world, manufacturers and
designers are under tremendous pressure to
make the machining processes more and more
efficient. With the development of new materials
and the recent advancements in the cutting
technologies, friction and wear are still the
major issues in a material removal environment.
However, these issues are addressed with the
use of cutting fluids, which remove the heat
generated during the machining operation and
on the other hand, lubricates the two surfaces in
order to decrease the amount of friction. The
lubrication research cell of ASME has laid
energy conservation. It has been observed that
nearly 5.5 percent of U.S. energy consumption is
used in primary metals and metal-processing
industries, out of which 0.5 percent is conserved
due to the tribological advancements made in
the recent past [1]. The recent tribological
developments during the last few years have led
to a shift in the metal cutting technology.
Tribology the science of friction, wear and
lubrication plays a significant role in the
synthesis of materials with a greater focus on
metal cutting processes [2]. This paper reviews
some of the commonly used cutting fluids and
the fluid application systems, which are in

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 A. Anand et al., Tribology in Industry Vol. 38, No. 4 (2016) 463-474
practice in a machining environment. In a metal
cutting process, the tribological aspects to be
considered in a machining process are area of
contact, stress distribution factor, interfacial
temperature, etc. Various research studies have
been carried out in the area of tribology in
machining systems [3-5]. The conventional
approach for selecting a cutting fluid in a
machining environment is actually on the basis
of performance characteristics and also the
economical factors. Various researchers have
developed different cutting fluids for machining
processes [6-9]. In these research studies, the
researchers have taken into consideration
mechanical performance and environmental
impact as the parameters for a cutting fluid.
Owing to the global environmental consciousness
among the end users and the stringent
environmental legislations machinists are in
search of cutting fluids which pose minimal
threat to the environment without compromising
the performance of these fluids [6]. Moreover the
disposability of these cutting fluids is another
challenge faced by the researchers as they
contain hazardous waste in the form of chemical
or toxic matter [10]. Hence an optimal cutting
fluid with all the attributes is the need of the
present times. This paper is structured in a
manner that it focuses on the various types of the
cutting fluids developed by researchers, work
material considerations thereof, tool material
considerations, health factors associated, non
traditional cutting fluids and minimum quantity
lubrication for various machining processes from
tribological point of view.
2. CUTTING FLUIDS IN A MACHINING
ENVIRONMENT
2.1 Role of Cutting fluids
The cutting fluids are primarily used for cooling
and lubrication purposes in a metal cutting
operation. Over the last century, water was used
mainly as a coolant due to its high thermal
stability and availability [11,12]. However, its
use is being slowly replaced due to the corrosion
aspects and also due to non-satisfactory
lubrication characteristics. The development of
cutting fluids which were oil based have also led
to the use of cutting oils (lubricants) for
machining purposes, with the addition of
464
extreme pressure (EP) additives. In the present
industry, the cutting fluids commonly used are
water based emulsifiable oils and straight
cutting oils. However, some semi-synthetic and
synthetic based cutting fluids have also been
developed to improve cooling and lubrication
characteristics in a machining environment
[13,14]. Various parameters play an important
role in the selection of cutting fluids.
Owing to the increasing manufacturing costs, the
present day designers and manufacturers are
shifting from conventional cooling systems to
new cooling systems [15,16]. However, a
thorough knowledge of tribology in a machining
environment is essential, and therefore the
designers and manufacturers need to
understand the tribo concepts in terms of heat
removal, cooling, wear reduction, lubrication
aspects, and corrosion aspects involved therein.
2.2 Types of Cutting Fluid
This section describes the various types of
cutting fluids used in a machining environment.
Straight Cutting Oils: These type of cutting
fluids are a combination oil-based extreme
pressure additives which improve the
performance characteristics of the base oil to
perform the desired cooling and lubrication
activities. Generally applied in un-diluted state,
the characteristic feature of these cutting fluids
is that they do not mix with water and therefore
do not form an emulsion with water. Apart from
exhibiting good lubrication properties, effective
anti-seizure qualities, they offer good corrosion
resistance [17]. However, at cutting speeds mist
and smoke formation has been reported. These
cutting fluids are best suitable for heavy duty
machining operations and also in some grinding
applications. The poor heat dissipation in case of
high speed cutting restricts their use. The higher
initial and disposal cost also is a limiting factor
due to which straight cutting oils find
application in the cases when other types of
fluids are not viable.
Water Emulsifiable Oils: Also known as soluble
oils, these cutting oils form an emulsion but are
not completely soluble in water. These are oil
based concentrates, which contain emulsifiers
which permit them to mix with water and form
an emulsion. To improve the lubrication
 A. Anand et al., Tribology in Industry Vol. 38, No. 4 (2016) 463-474
characteristics, additives are also added as in
case of straight cutting oils. These cutting oils
also contain some rust and corrosion inhibitors.
These fluids are characterised by the properties
of better cooling efficiency, low viscosity, non-
flammability and non-toxicity, ease of
reclamation and low initial and disposal costs.
However, they also offer low lubricity, mist
formation. These type of cutting oils are the
most commonly used oils in present day
machining scenario including grinding
operations [17-19].
Synthetic Fluids: These cutting fluids are the
chemical fluids containing synthetic water-
soluble lubricants, which provide the necessary
lubrication characteristics. These cutting fluids
also contain some rust and corrosion inhibitors,
biocides, and surfactants but do not contain any
oil. Synthetic fluids offer resistance to rancidity,
have good cooling properties, low viscosity, non-
toxicity, biodegradability, etc. However, when
used in heavy duty applications often encounter
the problem of insufficient lubricity. Various
tribological investigations have revealed that
synthetic fluids are an appropriate choice in the
future. Another issue with the application of
synthetic fluids in machining is the non-
compatibility of grinding operations in a
manufacturing system. Moreover, poor
lubrication properties are the major cause of its
non-compatibility when synthetic fluids as
coolants are used.
Semi-Synthetic Fluids: These cutting fluids
contain up to 25 % of oil which is added to the
concentrate solution. An important characteristic
of these fluids is that upon dilution with water,
they form a very fine emulsion. To improve the
lubrication characteristics, oil is added. The issues
related to the use of synthetic fluids led to the
development of semi-synthetic fluids.
Cryogenic Coolants: Another improvement in
the cutting fluid technology is the development
and use of cryogenic fluids. Apart from thermal
and environmental benefits cryogenic fluids
offer better wear reduction capabilities. Having
a temperature of the order of 196 0C, these
fluids are used primarily in difficult-to-machine
materials, chip formation and chip breaking
being the major issues associated with them
[20,21]. The use of liquid nitrogen as a cutting
fluid involves applications where it acts as a
coolant to the tool, which has internal channels
through which, liquid nitrogen is supplied under
controlled pressure.
Dhar et al. have investigated the cutting
temperature, tool wear, surface roughness in
case of machining steel by using liquid nitrogen
as the cutting fluid wherein significant
improvement in the surface finish and tool wear
has been reported [22]. Stanford et al. carried
out a similar investigation on the turning
operation of a plain carbon steel by using liquid
nitrogen as a coolant. In this study authors have
reported 55 % reduction in the flank wear [23].
The use of liquid CO2 as a cutting fluid has been
reported in various research studies [24,25]
wherein reduction in the tool wear and
oxidation wear has been observed [25]. The use
of CO2 as a coolant has resulted in doubling the
tool life in case of machining of titanium alloys
[24]. Jerold et al. have observed that the use of
liquid CO2 as a coolant results in better tool life
as compared to the liquid nitrogen [26]. It is
clear from the reviewed literature that Liquid
nitrogen and Liquid CO2 have been used as
cryogenic fluids however the studies on other
cryogenic fluids like liquid argon , liquid helium
have not been reported much.
3. WORK MATERIAL CONSIDERATIONS
An important area of concern with respect to the
role of cutting fluid is the work materials under
a given machining environment from tribology
point of view. The cutting fluid to be used must
facilitate the machining processes involved so as
to ensure its compatibility with a wide variety of
materials. From tribology point of view various
research studies have been carried out [27-30].
In case of materials like cast iron, the brittle
behaviour during machining often leads to its
breaking and formation of small chips. The
influence of friction between cutting tool and the
chip is less on account of the small size chip
formation. The use of emulsion based cutting
fluids enhances some machining characteristics
like surface finish quality and, also restricts the
formation / coagulation of foreign matter during
the machining operations [28,30]. Sulphur
added oils are used in the machining of stainless
steel materials, which lead to stains over the
machined surface [28,30-31]. Water based
cutting fluids are used in machining of heat
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 A. Anand et al., Tribology in Industry Vol. 38, No. 4 (2016) 463-474
resistant and difficult-to-cut steel alloys, due to
the involvement of higher temperature in
cutting zone area. However, sulphur based
mineral cutting oils may also be used in some
machining operations [28,32]. Easy to machine
materials like aluminium and aluminium based
alloys when subjected to machining, no major
issues on account of temperature are
encountered. The use of waterless cutting fluids,
prevent the formation of built up edge [28,32].
In the machining of copper and copper based
alloys, the emulsion based cutting fluids or thin
mineral oils are preferred, however for
machining of brass, high pressure additive
cutting oils are used [28,32].
Fig. 1. Nozzle positions [20].
For the machining of difficult-to-cut materials
such as titanium alloys, generation of high
temperature, is a matter of concern while
carrying out the selection of a cutting fluid. The
selected cutting fluid must have both cooling
and lubricating characteristics. It has been
observed that lubrication properties of selected
cutting fluids are preferred when low cutting
speeds are selected. For composite materials,
the cutting fluids influence the surface
roughness quality [33].
Patrick et al. [34] studied the effect of cutting
fluids on the mechanical properties of mild steel
in a turning operation. In this study, the authors
have used soluble oil, water and palm kernel oil
as cutting fluid for turning operation using
Tungsten carbide and HSS as cutting tools. In
this study, the researchers have reported that
palm kernel oil as a cutting fluid exhibits very
good qualities including good chip formation,
reduced heat generation and comparatively
good surface finish.
466
Hamdan et al. [35] carried out the performance
evaluation of different types of cutting fluid in
the machining of AISI 01 hardened steel using
pulsating jet minimum quantity lubrication
system. In this study, research was carried out
using three cutting fluids namely neat oil,
soluble oil and semi-synthetic cutting fluids
under minimal quantity lubrication (MQL)
system with the application of high velocity
cutting fluid in narrow pulsed jet forms. The
results clearly proved that soluble oil gave the
lowest cutting forces and does not change with
variable velocities.
Tsao [36] carried out an experimental
investigation on cutting fluid effect in milling an
aluminum alloy. The experiment shows that
adding sulfurous boric acid ester cutting fluid
reduced tool wear by 12.5 % for hard coating
tungsten carbide end mills and also decreases
the milling force by 10 %. Saravanakumar [37]
performed an experimental analysis on cutting
fluid dispersed with silver nano particles. The
research focuses on the performance of the
cutting fluid after inclusion of suitable additive,
in the form of silver nano particles, in the cutting
fluid to improve its thermal and tribological
properties. The results have shown a
considerable reduction in tool tip temperature, a
8.8 % reduction in cutting forces for the cutting
forces with the inclusion of nano particles and
7.5 % improvement in surface roughness. Hung
et al. [31] experimentally analyzed the effect of
cutting fluid on the machinability of metal
matrix composites. The effect of cutting fluid on
the machinability of aluminium-based matrix
composites reinforced with SiC or AI2O3
particles was investigated. The researchers have
concluded that pressurized and copious cutting
fluid has no effect on tool life due to effective
chip flushing and lack of lubricating film.
4. TOOL MATERIAL CONSIDERATIONS
In a machining operation like grinding, the
commonly used grinding materials are
abrasives. However, on account of the heat
generated during the grinding operation and the
presence of forces, the use of cutting fluid from
tribology point of view is very significant as it
may affect the life of the abrasives used and the
surface finish characteristics. A wide variety of
materials are available for carrying out the
 A. Anand et al., Tribology in Industry Vol. 38, No. 4 (2016) 463-474
machining processes, including the grinding
operation [39,40]. However, it becomes
necessary to choose a particular cutting fluid-
tool material combination so as to get an
optimized machining parameters. For materials
like tungsten carbide, waterless cutting fluids
are preferred [41]. It is important to consider
that in case of cutting tool materials, the cutting
fluids have a significant role to play. The
generation of high heat in the interface of cutting
tool (grinding tool) and workpiece material,
causes wear of the tool at a much higher rate
lowering the tool life and further leading to poor
surface quality [28,29]. Some typical grinding
materials like cubic boron nitrate (CBN) and
polycrystalline diamonds (PCD) may also be
used for machining operations [42]. The
economic constraints and the high temperature
associated with these materials restrict their
use. However, such materials are generally used
in finishing operations to achieve high
dimensional accuracy and surface finish
characteristics [28,29].
However, with a particular reference to grinding
process, some researchers have suggested
rankings of cutting fluids based upon their
various properties. Webstar et al. [43] have
carried out a study of four cutting fluid types as
used in a grinding process as shown in Table 1.
In this research study, the researchers have
highlighted the characteristics of these fluids.
The work carried by Bardie was a further
extension to the studies done by Gr et al. [44]. It
was observed that no such fluid can be
suggested which may act as an ideal alternative.
It was further suggested that the parameters
such as heat removal, filterability, cost and
environmental aspects may be considered
altogether. Breingsmeir et al. [45] showed that
with the increase in oil additive concentration,
there is a decrease in the grinding energy and
temperature, however the wheel life increases,
later on established and confirmed by Yoon and
Krueger [46]. These researchers have observed
that diluted synthetic fluids had a grinding ratio
(G-ratio) of 2.5 and 7.5, semi-synthetics had G-
ratios between 2.5 and 6.5, and soluble oils had
G-ratios between 4 and 12. Undiluted cutting
fluids had G-ratios between 60 and 120. Minke
[47] carried out a research study on the role of
coolants in a grinding process. In this research
study, the researcher has compared oil and
water based cutting fluids under different
grinding environments. It was observed during
this research work that water-based emulsions
have better cooling. However, it leads to
generation of higher grinding forces and is not
able to prevent damage to the workpiece.
Table 1. Grinding fluid characteristics by Webstar et
al. [31].
Semi- Soluble Straight
Characteristics Synthetics
synthetics oil oil
Heat removal 4 3 2 1
Lubricity 1 2 3 4
Maintenance 3 2 1 4
Filterability 4 3 2 1
Environmental 4 3 2 1
Cost 4 3 2 1
Ranking Scale: 1-4 where,
1-Worst , 2 Good , 3- Very Good, 4- Best
Silva et al. [48] carried out an experimental
investigation on thermal and rheological
behavior of eco-friendly metal cutting fluids The
research evaluated the thermal and rheological
performance of two chemically modified
cottonseed oils epoxidized fluid and
hydroxylated fluid, against unmodified
cottonseed oil and commercial cutting oils. The
results clearly depict that hydroxylated and
epoxidized fluids offer better thermal resistance
than commercial cutting fluid without causing
char formation, and former two fluids are more
efficient in lubricating and cooling the drill bit
and part, thus causing less wear. Another
research study carried out by Ozcelik et al. [49]
investigated the effects of vegetable-based
cutting fluids on the wear in drilling to
investigate the performances of three VBCFs
developed from crude sunflower oil, refined
sunflower oil, refined canola oil and commercial
semi-synthetic cutting fluid and compared the
tool wear, thrust force and surface roughness in
drilling operation of austenitic stainless steel
with HSSE tool. The researchers reported that
CCF (canola based cutting fluid)-II is the best
cutting fluid for drilling of AISI 304 stainless and
gives the best performance due to its higher
lubricant properties. Mayr et al. [50] performed
an experimental investigation to observe the
influence of cutting fluid on thermal behavior of
5-axis machine tools in precision machining. The
generated graphs illustrate that measured
temperatures are higher without using cutting
fluid and cutting fluids can also reduce the
chances of errors of the machine tool.
467
 A. Anand et al., Tribology in Industry Vol. 38, No. 4 (2016) 463-474
5. HEALTH FACTORS ASSOCIATED WITH
CUTTING FLUIDS
The human interaction with the cutting fluids in
a conventional machining process has forced the
researchers to carry out studies on the health
hazards involved in the use of cutting fluids. It
has been observed that some of the cutting fluids
have proved hazardous to the machine
operators [51,52]. The use of cutting fluids in
machining processes may often lead to skin
related issues. Some typical cases of skin
disorders like dermatitis are the most common
diseases caused due to frequent exposure to the
cutting fluids [53]. There are reports indicating
respiratory problems faced by the operators
who work continuously in environments where
cutting fluids are used. Dahmen et al. [54]
carried out a research investigation for
separation of debris in a grinding process. In this
research study, the researchers have developed
a process using supercritical carbon dioxide to
separate the debris and it was originally
implemented for glass grinding with high oil and
lead content.
6. NON TRADITIONAL CUTTING FLUIDS IN A
MACHINING PROCESS
Various research studies have been carried out
where solid lubricants have been used as a
cutting fluid in a machining process. Callister
[55] in his research study observed that graphite
can be used as a solid lubricant for cutting fluid
applications because it possesses weakly bonded
hexagonal plate structure. The author also
confirmed the use of molybdenum disulfide
(MoS2) as a new solid lubricant.
Ninomiya et al. [56] studied the effect of the
floating nozzle in grinding of mild steels with
vitrified CBN wheel. During his research study
the author found that by using a floating nozzle
on a CBN wheel, the wheel wear was reduced by
50 % for shallow depths of cut and low
workpiece speeds (Fig. 2). The surface finish
also improved under these conditions. When
compared with traditional coolant application,
the author observed that floating nozzle
improves the grinding performance with an
impressive one twelfth of the cutting fluid,
however when the work speeds were increased
beyond 20 m/min, there was major wheel wear.
468
Fig. 2. Schematic diagram of a floating nozzle [36].
Okuyama et al. [57] carried out an experimental
investigation of cooling action of grinding fluid
in shallow grinding. During this investigation,
the authors observed a better performance in
grinding by having 436 small grooves, 3 mm
wide and 0.5 mm deep, attributed to the rise in
heat transfer coefficient. A reason for the
elevation in the heat transfer coefficient may be
due to coolant being held and stirred by the
grooves. The researchers suggest that the
grooves have a capability of improving the
efficiency in heavy grinding with super-abrasive
wheels with no porosity as the increased
number of grooves also increases the heat
transfer coefficient.
Yui and Terashima [58] carried out a research
study for development of a coolant-less grinding
system. The authors mixed cold air (-30 C) and
vegetable oilmist (08.6 cc/h) in order to
improve upon cold air application and
concluded that the grinding ratio is higher as
compared to the traditional grinding method
with coolant oil. The investigation revealed that
that the critical depth of cut was only 6 mm.
Baheti et al. [59] carried out a research study on
environmentally conscious cooling and
lubrication for grinding. In this research study
the authors reported better results upon using
environmentally safe ester oil and air during the
straight surface grinding of carbon steels using
alumunium oxide wheels. A mathematical model
of the process was also developed to predict
with reasonable accuracy the temperature rise.
S.C. Salmon [60] carried out a research study on
the effects of hard lubricant coatings on the
performance of electro-plated super abrasive
grinding wheels. In this research study, the
author has used MoS2 as a hard lubricant and
titanium aluminum nitride (TiAlN) to resist
wear on CBN wheels. During this research study,
 A. Anand et al., Tribology in Industry Vol. 38, No. 4 (2016) 463-474
the author observed that the coated wheels do
not require added lubricity of the oil and the
CBN wheels operate satisfactorily because they
perform adequately with water-based fluids. The
author also observed that coated wheels
perform better than the traditional wheels, due
to their compatibility with the environmentally-
friendly water-based coolants.
Choi et al. [61] carried out a comparison of the
cooling effects of compressed cold air and
coolant for cylindrical grinding with a CBN
wheel. The authors reported that the
effectiveness of cold air was nearly comparable
with conventional wet-grinding for shallow
depths of cut; however, the surface roughness
would increase as the tensile surface residual
stresses would appear upon increasing the
depths of cut as a result of the lack of lubrication
through the grinding zone. Inoue and Aoyama
[62] carried out an experimental investigation
on application of air cooling technology and
minimum quantity lubrication to relief grinding
of cutting tools. The authors used cold air at -33
C with a cooling air output flow of 320 Nl/min
at a pressure of 200 kPa. The lubricant was
salad oil and was supplied at 6 m/min. The
results from this setup were compared with dry
grinding and grinding with an oil-based fluid.
During this experimental investigation, the
authors concluded that when the depth of cut
exceeded 0.1 mm, the oil-based cutting-fluid
grinding exhibited the lowest temperature rise.
It was observed that conventional oil-based
cutting-fluid grinding has an advantage over
cooling-air and minimum-quantity lubricant
application in terms of temperature rise control
for large depths of cut.
Xu et al. carried [63-67] out a research on heat
transfer characteristics in grinding contact zone
with radial water jet impinging cooling. The
authors worked with a radial cooling
mechanism. It was found that by using
perforated electroplated CBN grinding wheels
with radial jets, where the fluid is forced from
the cooling holes at high pressure, the fluid
tends to break the boundary layer. The authors
were able to improve the critical heat flux and
the cooling effect in the contact zone which
increased overall efficiency. The temperature of
the workpiece surface in the grinding zone was
steadily kept below the film boiling temperature
of 100120 C for water based coolants, even
with a high heat flux. Shaji and Radhakrishnan
[68] carried out an experimental investigation
on surface grinding using graphite as a lubricant.
The authors used graphite paste with water-
soluble oil as a lubricant in a grinding process
and compared the performance of graphite-
assisted grinding with dry grinding and
conventional wet grinding by varying the
workpiece material, dressing conditions and
cutting fluid application. In this research study
the authors observed that the tangential forces,
grinding zone temperatures and specific
energies are lower with the graphite paste when
compared to dry or coolant grinding but the
system has problems with wheel clogging and
grinding ductile materials. Yokogawa et al. [69]
carried out a research work on improving
grinding performance of BN wheels by dual-fluid
supply method. During this research study, the
authors used a dual cutting fluid method in a
cylindrical grinding operation using mineral oil
as a lubricant in the grinding zone and used
water to cool the workpiece. The experiments
were carried out with a removal rate of 1200
mm2/min, a wheel speed of 3600 m/min, and a
CBN wheel. Coolant water was applied to the
underside of the workpiece via a positional
nozzle, (Fig. 3). The results showed that surface
roughness of the workpiece dramatically
improved. With conventional cutting fluid
applications the surface roughness was
approximately 3 mm Rz but with the dual cutting
fluid application the surface roughness dropped
to under 1 mm Rz for the same removal.
Shaji and Radhakrishnan [70] carried out
another experimental investigation on the
application of solid lubricants in grinding on
graphite sandwiched grinding wheels. Slotted
wheels were used with graphite impregnated
into the slots. Three different wheels with
varying numbers of slots: 10, 15 and 20 were
used. Compared to conventional dry- and wet-
grinding, the normal forces with the graphite
slotted wheels came out to be more or less the
same or even slightly higher at low feed rates,
but at increased feed rates, these forces were
higher in most cases. The results showed that
the surface roughness, residual stresses and
hardness profiles were greatly improved with
the graphite wheels. These experiments were
performed with small depths of cut and do not
represent a considerable improvement over
more traditional cutting fluid application. Shetty
469
 A. Anand et al., Tribology in Industry Vol. 38, No. 4 (2016) 463-474
et al. [71] carried out tribological investigation
of discontinuously reinforced aluminium
composites based on the orthogonal arrays.
Fig. 3. Dual cutting fluid setup [49].
In this tribological investigation, the tests were
carried out under dry, oil and water based
emulsion and steam lubricated (cutting fluid)
conditions. Both The tool wear and surface
roughness were found to be less for steam
cutting in this investigation.
Anjaiah et al. [72] used a pressurized steam jet
approach to tool wear minimization in cutting of
metal matrix composites by full factorial design
of experiments. In this experimental analysis,
the researchers have observed that pressurized
steam jet plays a significant role on the tool
wear. Kuram et al. [73] carried out a research
study on the optimization of the cutting fluids
and parameters using taguchi and ANOVA in
milling. In this research study, the researchers
have considered two different vegetable based
cutting fluids developed from refined canola and
sunflower oil and a commercial type semi-
synthetic cutting fluid. The optimum conditions
for tool wear and forces were studied. Walter
Belluco and Leonardo De Chiffere [74] carried
out a research study on testing of vegetable
based cutting fluids by hole making operations,
using vegetable oil as cutting fluid for drilling
operations, involved drilling, tapping and
reaming operations and results indicated that
while reaming, higher cutting speeds had a
strong impact on part accuracy and at smaller
cutting speeds, the effect considerably reduced.
470
7. MINIMUM QUANTITY LUBRICATION AND
TRIBOLOGY
During the past few years, a new trend in the use
of cutting fluids technology in a machining
environment is MQL (minimum quantity
lubrication). MQL is being adopted nowadays for
high speed machining operations. This type of
advanced lubrication systems in a machining
environment plays a vital role particularly in
large cutting fluids application and dry
machining. Minimum quantity lubrication (MQL)
also known as Near Dry Machining (NDM) or
semi dry machining is an alternative to
traditional use of cutting fluids. In MQL, there is
a use of very small quantity of lubricant for
lubrication or cooling requirements. Minimum
quantity lubricants (MQL) systems generally
consists of cutting fluids (coolants and
lubricants) which are non-soluble in water.
These fluids however, reduce the health hazards
associated which may affect the health of the
machinist [75]. Some research studies have
revealed that use of MQL technique enhances
lubrication and also leads to minimum power
consumption in a grinding process (grinding
power). The wear rate of the grinding wheel also
reduces in a significant way [76].
Tawakoli et al. [77] investigated the the
performance of MQL technique in a grinding
operation. In this investigation, the researchers
have considered both hard steel 100cr6 and soft
steel 42CrMo4 for investigation. It was observed
that for LB8000 MQL oil with wheel speed 25
m/s and depth of cut 25m the improvement in
surface quality in MQL grinding is more
significant in comparison to dry and fluid
grinding. Dhar et al. [78] investigated the effect
of MQL technique to grind 16MnCr5 alloy steel
on the cutting performance compared to
completely dry cutting and flood cooling with
respect to grinding temperature, surface
roughness, chip morphology. The results
indicate that the use of minimum quantity
lubrication (MQL) by cutting oil (VG-68) leads to
lower surface roughness compared to dry and
wet environments. Silva et al. [79] investigated
the performance of MQL system to grind ABNT
4340 steel (HRC 60) with alumina wheel. It was
found that, MQL system leads to finer surface
finish and higher compressive residual stress
compared to dry and conventional cooling.
Sabahudin et al. [80] in his research study
 A. Anand et al., Tribology in Industry Vol. 38, No. 4 (2016) 463-474

broadly discussed the application of marginal Cutting Fluids and its types
amount of coolant instead of large coolant fluid
Health hazards with cutting fluids
used in machining, known as Minimum Quantity
Lubrication (MQL) machining. The study Work material considerations with cutting
revealed that the MQL machining leads to lesser fluids
cutting forces, less strain hardening and a
favourable chip formation process. Tool material considerations
Minimum quantity lubrication in grinding
systems
8. FUTURE SCOPE

The literature revealed the below mentioned REFERENCES:

gaps in the research work performed till date
and the future work should be focussed in the [1] A.P. Viktor, Tribology of metal
following areas so as to lead to the further cutting, Mechanical Tribology, New York: Marcel
developments in this area of research: Dekker, pp 307-346, 2004.

1. Development of biocompatible cutting [2] G. Wit, J. Rech and K. ak, Determination of

fluids with minimum or no toxic harm rate.
2. Recycling / reclamation of cutting fluids.
3. Development of cutting fluids for high
temperature tribological applications.
4. A system of studying the wetability
characteristics with addition of nanoparticles.
5. Development of new cooling techniques in
dry machining.
6. Development of some more nano-cutting
fluids aimed at reducing the cutting forces
and increasing the tool life with minimum
energy consumption at reduced costs.
9. CONCLUSIONS
The cutting fluids used in a grinding process
significantly improve the machining
characteristics of the process. Grinding process
is one of the important machining operations in
a manufacturing environment. Apart from
cooling the cutting fluids also perform the
lubrication at the tool-workpiece interface.
Recent developments in the cutting fluid
technology have led to rapid changes in the
design and development of various cutting
fluids, used for various grinding operations. The
concepts like minimum quantity lubrication
(MQL) in grinding operations have greatly
influenced the material removal rate (MRR) and
also the life of cutting tool. Some of the key areas
which have been considered in this research
article are:
friction in metal cutting with tool wear and flank
face effects, Wear, vol. 317, no. 1, pp. 8-16, 2014.
[3] M. Fallqvist, F. Schultheiss, R. Msaoubi, M. Olsson
and J.-E. Stahl, Influence of the tool surface
micro topography on the tribological
characteristics in metal cutting: Part I
experimental observations of contact
conditions, Wear, vol. 298, pp. 87-98, 2013.
[4] U. Durul and T. zel. Determination of tool
friction in presence of flank wear and stress
distribution based validation using finite
element simulations in machining of titanium
and nickel based alloys, Journal of Materials
Processing Technology, vol. 213, no. 12, pp.
2217-2237, 2013.
[5] P. Hendrik, F. Klocke and D. Lung, A new
experimental methodology to analyse the
friction behaviour at the tool-chip interface in
metal cutting, Production Engineering, vol. 6, no.
4-5, pp. 349-354, 2012.
[6] Y.M. Shashidhara and S.R. Jayaram, Vegetable
oils as a potential cutting fluidan
evolution, Tribology International, vol. 43.5, pp
1073-1081, 2010.
[7] S.M. Alves and J.F. Oliveira, Development of new
cutting fluid for grinding process adjusting
mechanical performance and environmental
impact, Journal of Materials Processing
Technology, vol. 179, no. 2, pp. 185-189, 2006.
[8] H.S. Abdalla, W. Baines, G. Mclntyre and C. Slade,
Development of novel sustainable neat-oil metal
working fluids for stainless steel and titanium
alloy machining, Part 1. Formulation
development, The International Journal of
Advanced Manufacturing Technology, vol. 34, no.
1-2, pp. 21-33, 2007.

471
 A. Anand et al., Tribology in Industry Vol. 38, No. 4 (2016) 463-474
[9] L. Sunday Albert, A review of application of
vegetable oil-based cutting fluids in machining
non-ferrous metals, Indian Journal of Science
and Technology, vol. 6, no. 1, pp. 3951-3956,
2013.
[10] E. Kuram, B. Ozcelik and E. Demirbas,
Environmentally friendly machining: vegetable
based cutting fluids, Green Manufacturing
Processes and Systems, Springer, Berlin,
Heidelberg, pp. 23-47, 2013.
[11] J.S McCoy, Introduction: Tracing the historical
development of metalworking fluids. In: JP Byers,
Ed. Metalworking Fluids, New York: Marcel
Dekker, pp. 1-23, 1994.
[12] A.R Machado and J. Wallbank, The effect of
extremely low lubricant volumes in machining,
Wear, vol. 210, pp. 76-82, 1997.
[13] R.C Gunderson and A.W Hard, Synthetic
Lubricants, Reinhold, New York, 1962.
[14] J.A. Schey, Metal Deformation Processes: Friction
and Lubrication, Marcel Dekker Inc, New York,
1970.
[15] P.S. Sreejith and B.K.A. Ngoi, Dry machining:
machining of the future, Journal of Materials
Processing Technology, vol. 101, pp. 287-291,
2000.
[16] L.D. Chiffre, Function of cutting fluids in
machining, Lubrication Engineering, vol. 44, pp.
514-518, 1988.
[17] V.P. Astakhov, Tribology of metal
cutting, Mechanical Tribology, New York: Marcel
Dekker, pp. 307-346, 2004.
[18] B.L. Juneja, Fundamentals of metal cutting and
machine tools, New Age International, 2003.
[19] E.M. Trent and P.K. Wright, Metal cutting.
Butterworth-Heinemann, 2000.
[20] N.R. Dhar and M. Kamruzzaman, Cutting
temperature, tool wear, surface roughness and
dimensional deviation in turning AISI-4037 steel
under cryogenic condition, International Journal
of Machine Tools and Manufacture, vol. 47, no. 5,
pp. 754-759, 2007.
[21] S.Y. Hong, Y. Ding and R.G. Ekkens, Improving
low carbon steel chip breakability by cryogenic
cooling, International Journal of Machine Tools
and Manufacture, vol. 39, pp. 1065-1085, 1999.
[22] Z.Y. Wang and K.P. Rajurkar, Cryogenic
machining of hard-to-cut materials, Wear, vol.
238, pp. 169-175, 2000.
[23] M. Stanford, P.M. Lister, C. Morgan and K.A.
Kibble, Investigation into the use of gaseous and
liquid nitrogen as a cutting fluid when turning
472
BS 970-80A15 (En32b) plain carbon steel using
WCCo uncoated tooling, Journal of Materials
Processing Technology, vol. 209, no. 2, pp. 961-
972, 2009.
[24] C. Machai and D. Biermann, Machining of -
titanium-alloy Ti10V2Fe3Al under cryogenic
conditions: Cooling with carbon dioxide snow,
Journal of Materials Processing Technology, vol.
211, no. 6, pp. 1175-1183, 2011.
[25] S. Hesterberg, Dry machining of stainless steels:
process design for turning and drilling with
indexable inserts, Vulkan-Verlag GmbH, vol. 35,
2006.
[26] B.D. Jerold and M.P. Kumar, Experimental
comparison of carbon-dioxide and liquid
nitrogen cryogenic coolants in turning of AISI
1045 steel, Cryogenics, vol. 52, no. 10, pp. 569-
574, 2012.
[27] M.A. El Baradie, Cutting Fluids, Part I:
Characterisation, Journal of Materials Processing
Technology, vol. 56, pp. 786-797, 1996.
[28] G. Avuncan, Machining Economy and Cutting
tools, Makine Takim Endstrisi Ltd. Publication,
Istanbul (in Turkish), pp. 375-403, 1998.
[29] Kavuncu, Cutting Oils In Metal Machining,
Turkish, Chambers of Mechanical Engineers
Publication, Istanbul (in Turkish).
[30] ASM Committee, Machining of titanium alloys,
Metals Handbook, ASM Publication, 499-507.
[31] E.O. Ezugwu, J. Bonney and Y. Yamane, An
overview of the machinability of aerospace
alloys, Journal of Materials Processing
Technology, vol. 134, pp. 233-253, 2003.
[32] S. Ebbrell, N.H. Woolley, Y.D. Trimidas, D.R.
Allanson and W.B. Rowe, The effects of cutting
fluid application methods on the grinding
process, International Journal of Machine Tools
and Manufacture, vol. 40, pp. 209-223, 2000.
[33] N.P. Hung, S.H. Yeo and B.E. Oon, Effect of cutting
fluid on the machinability of metal matrix
composites, Journal of Materials Processing
Technology, vol. 67, pp. 157-161, 1997.
[34] P.A.O. Adegbuyi, G. Lawal, O. Oluseye and G.
Odunaiya, Analysing the effect of cutting fluids on
the mechanical properties of mild steel in a turning
operation, American Journal of Scientific and
Industrial Research, vol. 2, no. 1, pp. 1-10, 2011.
[35] A. Hamdan and M. Fadzil, K.A. Abou-El-Hossein
and M. Hamdil, Performance evaluation of
different types of cutting fluid in the machining
of AISI 01 hardened steel using pulsed jet
minimal quantity lubrication system, pp. 1-9,
Invited Paper.
 A. Anand et al., Tribology in Industry Vol. 38, No. 4 (2016) 463-474
[36] C.C. Tsao, An experiment study of hard coating
and cutting fluid effect in milling aluminum
alloy, International Journal of Advanced
Manufacturing Technology, vol. 32, pp. 885891,
2007.
[37] N. Saravanakumar, L. Prabu, M. Karthik and A.
Rajamanickam, Experimental analysis on
cutting fluid dispersed with silver nano
particles, Journal of Mechanical Science and
Technology, vol. 28, no. 2, pp. 645-651, 2014.
[38] N.P. Hung, S.H. Yeo, B.E. Oon, Effect of cutting
fluid on the machinibility of metal matrix
composites, Journal of Material Processing
Technology, vol. 67, pp. 157-161, 1997.
[39] M.A. Shalaby, M.A. El Hakim, M.M. Abdelhameed,
J.E. Krzanowski, S.C. Veldhuis and G.K. Dosbaeva,
Wear mechanisms of several cutting tool
materials in hard turning of high carbon
chromium tool steel, Tribology
International, vol. 70, pp.148-154, 2014.
[40] T. Doi, E. Uhlmann and I.D. Marinescu eds.,
Handbook of Ceramics Grinding and Polishing.
William Andrew, 2015.
[41] O. akr, A. Yardimeden, T. Ozben and E.
Kilickap, Selection of cutting fluids in machining
processes, Journal of Achievements in materials
and Manufacturing engineering, vol. 25, no. 2,
pp. 99-102, 2007.
[42] F. Nabhani, Wear mechanisms of ultra-hard
cutting tools materials, Journal of Materials
Processing Technology, vol. 115, no. 3, pp. 402-
412, 2001.
[43] J.A. Webster, C. Cui and R.B. Mindek Jr., Grinding
fluid application system design, CIRP Annals,
vol. 44, no. 1, pp. 333338, 1995.
[44] P.Q. Ge, L. Wang, Z.Y. Luan and Z.C Liu, Study on
service performance evaluation of grinding
coolants, Key Engineering Materials, vol. 258
259, pp. 221224, 2004.
[45] E. Brinksmeir, C. Heinzel and M. Wittman,
Friction, cooling and lubrication in grinding,
Annals of the CIRP, vol. 48, no. 2, pp. 581598,
1999.
[46] S.C. Yoon and M. Krueger, Optimizing grinding
performance by the use of solgel alumina
abrasive wheels and a new type of aqueous
metalworking fluid, Machining Science and
Technology, vol. 3, no. 2, pp. 287294, 1999.
[47] E. Minke, Contribution to the role of coolants on
grinding process and work results Technical
Paper, Society of Manufacturing Engineers, MR
(MR99-227), pp. 118, 1999.
[48] F. Silva Viviane, N. Batista Luciano, 'Robertis
Eveline De, Castro Claudia S. C., Cunha Valnei S.,
Costa Marcos A. S., Thermal and rheological
behavior of ecofriendly metal cutting fluids, J
Therm Anal Calorim, DOI 10.1007/s10973-015-
4848-X.
[49] B. Ozcelik, E. Kuram, E. Dmeribas and S. Emrah,
Effects of vegetable-based cutting fluids on the
wear in drilling, Sadhana, Indian Academy of
Sciences, vol. 38, no. 4, pp. 687706, 2013.
[50] M. Josef, G. Michael, M.B. Benjamin, S. Weikert
and W. Konrad, Cutting fluid influence on
thermal behavior of 5-axis machine tools, in 6th
CIRP International Conference on High
Performance Cutting, 2014.
[51] M.L. Hoff, Cutting fluids: necessary nuisance to
productivity tool, Society of Manufacturing
Engineers, MR (MR02-302), pp. 16, 2002.
[52] C.A. Sluhan, Selecting the right cutting and
grinding fluids, Tooling and Production, vol. 60,
no. 2, pp. 1-7, 1994.
[53] H.S.E. Anon, Warnings for grinding coolants,
Metalworking Production, vol. 147, no. 5, 2003.
[54] N. Dahmen, J. Schon, H. Schmieder and K. Ebert,
Supercritical Fluid Extraction of Grinding and
Metal Cutting Waste Contaminated with Oils,
ACS Symposium Series, vol. 670, pp. 270279,
1997.
[55] W.D. Callister Jr., Materials Science and
Engineering an Introduction, Fifth ed., Wiley,
New York, 2000.
[56] S. Ninomiya, M. Iwai, T. Uematsu, K. Suzuki and
R. Mukai, Effect of the floating nozzle in grinding
of mild steels with vitrified CBN wheel, Key
Engineering Materials, vol. 257258, pp. 315
320, 2004.
[57] S. Okuyama, Y. Nakamura and S. Kawamura,
Cooling action of grinding fluid in shallow
grinding, International Journal of Machine Tools
and Manufacture, vol. 33, no. 1, pp. 1323, 1999.
[58] A. Yui and M. Terashima, Proceedings of the
Third International Conference on Abrasive
Technology, pp. 394, 1999.
[59] U. Baheti, C. Gou and S. Malkin, Environmentally
Conscious Cooling and Lubrication for Grinding,
Proceedings of the International Seminar on
Improving Machine Tool Performance, San
Sebastian, Spain, vol. 2, pp. 643654, 68 July,
1998.
[60] S.C. Salmon, The effects of hard lubricant
coatings on the performance of electro-plated
superabrasive grinding wheels, Key Engineering
Materials, vol. 238239, pp. 283288, 2003.
473
 A. Anand et al., Tribology in Industry Vol. 38, No. 4 (2016) 463-474
[61] H.Z. Choi, S.W. Lee and H.D. Jeong, A comparison
of the cooling effects of compressed cold air and
coolant for cylindrical grinding with a CBN
wheel, Journal of Materials Processing
Technology, vol. 111, pp. 265268, 2001.
[62] S. Inoue and T. Aoyama, Application of air
cooling technology and minimum quantity
lubrication to relief grinding of cutting tools,
Key Engineering Materials, vol. 257258, pp.
345350, 2004.
[63] H.J. Xu, Y.C. Fu and F.H. Sun, Research on
enhancing heat transfer in grinding contact zone
with radial water jet impinging cooling, Key
Engineering Materials, vol. 202203, pp. 5356,
2001.
[64] L. Zhen-Chang, A. Satoshi and N. Masahiro,
Influence of grinding oil viscosity on grinding
heat and burn damage in creep-feed grinding,
Lubrication Engineering, vol. 51, no. 8, pp. 647
651, 1995.
[65] W. Graham and M.G. Whiston, Some
observations of through-wheel application in
grinding, International Journal of Machine Tool
Design and Research, vol. 18, pp. 918, 1978.
[66] T. Suto, T. Waida, H. Noguchi and H. Inoue, High
performance creep feed grinding of difficult to
machine materials with new-type wheels, Japan
Society of Precision Engineering, vol. 24, no. 1, pp.
3944, 1990.
[67] S.M. Rezaei, T. Suto, T. Waida and H. Noguchi,
Creep feed grinding of advanced ceramics,
Proceedings of the Institution of Mechanical
Engineers, Part B: Journal of Engineering
Manufacture, vol. 206, B2, pp. 9399, 1992.
[68] S. Shaji and V. Radhakrishnan, An Investigation
on surface grinding using graphite as lubricant,
International Journal of Machine Tools and
Manufacture, vol. 42, pp. 733740, 2001.
[69] M. Yokogawa and K. Yokogawa, Improving
grinding performance of CBN wheels by dual-
fluid supply method, International Journal of the
Japan Society for Precision Engineering, vol. 27,
no. 1, 1993.
[70] S. Shaji and V. Radhakrishnan, Application of
solid lubricants in grinding: investigations on
graphite sandwiched grinding wheels,
Machining Science and Technology, vol. 7, no. 1,
pp. 137155, 2003.
[71] R. Shetty, R.B. Pai, S.S. Rao, Tribological studies
on discontinuously reinforced aluminium
474
composites based on the orthogonal arrays,
ARPN Journal of Engineering and Applied
Sciences, vol. 3, no. 1, pp. 94-92, 2008.
[72] D. Anjaiah, R. Shetty, R.B. Pai, M.V. Kini and S.S.
Rao, A pressured steam jet approach to tool wear
minimization in cutting of metal matrix
composites, Materials Science Forum, vol. 561-
565, pp. 643-646, 2007.
[73] E. Kuram, B.T. Simsek, B. Ozcelik, E. Demirbas
and S. Askin, Optimization of the Cutting Fluids
and Parameters Using Taguchi and ANOVA in
Milling, Proceedings of the World Congress on
Engineering, Vol II, London, U.K., 2010,
[74] W. Belluco and L. De Chiffrie, Testing of
vegetable based cutting fluids by hole making
operations, Society of Triblogists and Lubrication
Engineers at ASME Tribological Conference,
Janauary 2001.
[75] U. Heisel, D. Lutz, R. Wassmer and U. Walter,
The Minimum Quantity Lubricant Technique
and its Application in the Cutting Process,
Machines and Metals Magazine, vol. 386, pp. 22-
38, 1998.
[76] D. Hafenbraedl and S. Malkin, Technology
Environmentally Correct for Intern Cylindrical
Grinding, Machines and Metals Magazine, vol.
426, pp. 40-55, 2001.
[77] T. Tawakoli, M.J. Hadad, M.H. Sadeghi, A. Danesh,
S. Stockert and A. Rasifard, An experimental
investigation of the effects of workpiece and
grinding parameters on minimum quantity
lubricationMQL grinding, International
Journal of Machine Tools & Manufacture, vol. 49,
pp. 924932, 2009.
[78] N.R. Dhar, M. Hossain and M. Kamruzzaman,
MQL applications in grinding of 16mncr5 steel:
A comparison with wet and dry grinding,
Proceedings of the International Conference on
Mechanical Engineering, Dhaka, Bangladesh,
ICME 05-AM-33, 2005.
[79] L.R. Silva, E.C. Bianchi, R.E. Catai, R.Y. Fusse, T.V.
Franc and P.R. Aguiar, Analysis of surface
integrity for minimum quantity lubricant-MQL
in grinding, International Journal of Machine
Tools and Manufacture, vol. 47, pp. 412418,
2007.
[80] S. Ekinovic, E. Begovic, E. Ekinovic and B. Fakic,
Cutting forces and chip shape in MQL machining
of Aluminium Bronze, Journal of Trends in the
Development of Machinery and Associated
Technology, vol. 17, no. 1, p.p. 17-20, 2013.
 Vol. 38, No. 4 (2016) 475-485

Tribology in Industry

RESEARCH
www.tribology.fink.rs

Study of Surface Wear and Damage Induced by Dry

Sliding of Tempered AISI 4140 Steel against
Hardened AISI 1055 Steel

A. Elhadi a, A. Bouchoucha b, W. Jomaa c,d, Y. Zedan c, T. Schmitt e, P. Bocher c

a Departmentof Mechanical Engineering, University of Mohamed Boudiaf, Msila, Algeria,
bDepartment of Mechanical Engineering, University of Constantine, Algrie,
c Department of Mechanical Engineering, TS, Montral, Canada,
dDepartment of Mechanical Engineering Laval University, Qubec, Canada,
eDepartment of Physics Engineering, Polytechnique Montral, Montral, Canada.

Keywords: ABSTRACT
Steels
In industry, the sliding mechanical systems are subject to friction and
Hardness
wear phenomena. These phenomena can be the origin of a reduction of
Friction coefficient
the efficiency of the mechanical system even to be responsible for its
Wear rate
incapacity. Generally, the materials of the parts which are moving relative
Surface damage
(tribological couple) of these systems are low alloy steels and carbon
steels, thanks to their good mechanical and tribological properties. The
Corresponding author: present work aimed to study, the surface wear and damage induced by
Abdelmalek Elhadi dry sliding of hard carbon steel AISI 1055 (disc) against tempered low
Department of Mechanical alloy steel AISI 4140 (pin) with different hardness and applied loads was
Engineering,University of Mohamed investigated. The results revealed that the interaction between the
Boudiaf, Msila, Algeria applied load and pin hardness result in complex thermo-mechanical
E-mail: elhadimalek65@gmail.com behaviour of the worn surfaces. When a lower hardness pin is used, the
main wear mechanisms observed on the discs were abrasion, adhesion,
and oxidation. When a higher hardness pin is used, the wear of the discs is
governed by delamination, oxidation, and plastic deformation. In
particular, third-body wear occurs at high applied load resulting in higher
wear rate of high hardness pins compared to low hardness pins.
2016 Published by Faculty of Engineering

1. INTRODUCTION motion, sliding velocity, surface roughness of the

Low alloy steels are the most used material for
machines elements industry because of their
high mechanical properties [1]. It was observed
by several researchers [2,3] that the variation of
friction depends on interfacial conditions such
as normal load, geometry, relative surface
rubbing surfaces, type of material, system
rigidity, lubrication and vibration. In many metal
pairs, in the high load regime, the coefficient of
friction decreases with load [4]. Friction
coefficient and wear rate of metals and alloys
showed different behavior under different
operating conditions [5,6]. Therefore,

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addressing the wear mechanism regimes have
generated a large number of research topics in
friction and wear by sliding fields [7].
The main steel selection criteria for parts
submitted to wear is usually based on the
surface hardness of the component [8].
Many variables may affect the wear mechanism
which makes it a complex phenomenon. Among
these variables are service conditions (such as
mating partners, normal load, sliding speed,
temperature and surface finish of the couple
tribological parts), environmental parameters
(atmospheric or sea environment) and other
factors like lubrication or corrosion [1,9]. The
wear rate can also be related to other factors
such as microstructure and its features,
hardness, work hardening index, fracture, and
fatigue properties [10-13].
The difference in hardness of the mating parts
has a decisive influence on the contact surfaces
life. Several studies have investigated the effect
of hardness on the wear mechanisms of
unlubricated sliding wear of steels [14-16]. It is
well reported that sliding wear is driven by
abrasion, adhesion, and delamination processes
[17]. On one hand, the process of delamination is
caused by the nucleation of voids. Their growth
and subsequent coalescence are favoured by
strained material under severely sliding
conditions [18, 19]. On the other hand, the
abrasion and adhesion wear mechanism may be
attributed to the fragmentation of the softer
material which cause to form wear debris. It was
reported that fragment formation is the result of
the local increase of dislocation density;
consequently, fragment can be formed after
strain accumulation.
Experimental results have been reported that
the small debris particles created by plastic
deformation (abrasion, adhesion, etc.) are
trapped in the contact zone and cannot be easily
removed [17]. Thus, the situation changes from
two to three bodies contact conditions
consisting of two counterparts and the debris
[20]. The third body particles affect the
displacement in the contact zone and thus affect
the coefficient of friction [21]. Due to the energy
dissipated in the contact (mechanical and
thermal), the wear particles can oxidized and
become hard abrading oxides which thus
476
increase the wear rate, or they can isolate the
surfaces and have a protective role so that
reducing the wear rate [22]. Others [12]
attributed the change in the frictional regime to
the cyclic formation/detachment of coarse
debris in the case of low hardness/ductile
materials. It has been shown that a decrease in
the friction coefficient with an increase in
normal load can be attributed to an increase in
frictional heating of the slider and a consequent
decrease of material strength [23].
As only few studies have addressed the effect of
tempered martensite on the wear behaviour in
dry sliding conditions, the present study aims to
investigate the wear behaviour of low alloy steel
AISI 4140 against carbon steel AISI 1055, which
are commonly used in the manufacturing of the
parts of the sliding mechanism. The analyses
were made by performing pin-on-disc wear
tests, under various loads for fixed sliding speed.
Different pin (AISI4140) hardness were tested
while the disk hardness (AISI1055) was kept
harder than the pin. Such study of wear
behaviour with different heat treatment may
provide a proper selection of
typicalhardnesssteel for sliding application.
2. MATERIALS AND METHODOLOGY
2.1 Materials
The materials chosen in this investigation are
AISI 4140 and AISI 1055 steels for the pin and
disc, respectively. The chemical compositions of
both steels are displayed in Table 1. The pins
were quenched and tempered to 33HRC and
39HRC while discs were quenched and
tempered to 52HRC. The microstructures of the
pins are composed mainly by tempered
martensite for both steels with the presence of
some bainite for low hardness (33HRC) one as
shown in Fig. 1.
2.2 Methodology
Dry sliding wear tests were conducted according
to the ASTM G99-5 (2010) standard using a pin-
on-disc system (Fig. 2). The linear sliding
velocity was kept constant at 0.5 m/s for all
tests. All wear tests were carried in air at
ambient temperature and relatively humidity of
~35 %. The normal load was varied between 15
 A. Elhadi et al., Tribology in Industry Vol. 38, No. 4 (2016) 475-485

and 35 N. A sliding time of 900 s was selected for
the tests, allows reaching a steady state in
friction. Before each test, both the disk and the
pin were cleaned with acetone, and each
specimen was tested on fresh track. The test
pins were weighed initially, and at the end of
each wear test. They were wiped clear of wear
particles, degreased and re-weighed. The
difference in weights of test pin, before and after
the experiment, determines the weight loss,
which was used for calculating the volume of
material lost. The latter was studied as function
of the applied load for each steel samples. The
worn mass of the pin specimen were measured
by a precise electric-balance (10-4 mm). The
worn surfaces were analysed with 3D measuring
laser microscope (Lext OLS4100 from Olympus)
and a HITACHI S-3600N scanning electron
microscopy (SEM).
The friction coefficient was calculated as the
ratio between the friction force and the normal
load. The average value from steady state regime
was considered. The start of the steady state
regime was selected as the sliding time at which
the standard deviation of friction coefficient
became lower than the 10 % of its average value.

Table 1. Nominal chemical composition (Wt. %) of AISI 4140 and AISI 1055 steel.
Element C Cr Mo Mn Si P S
AISI 4140 0.38 - 0.43 0.80 - 1.1 0.15 - 0.25 0.75 - 1.0 0.15 - 0.30 0.035 0.040
AISI 1055 0.50 - 0.60 0.60 - 0.90 0.040 0.050

(a) (b)

20 m 20 m

Fig. 1. Optical microstructures of AISI4140 steel tempered at a hardness of (a) 33HRC and (b) 39HRC.

Fig. 2. Pin-on-disc system: (1) Pin; (2) Pin holder; (3) Test disc; (4) Support; (5) Speed reducer; (6) Normal load
(dead weight); (7) Load cell for frictional force.

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3. RESULTS AND DISCUSSION 1

3.1. Friction and wear behavior 0.8

Friction coefficient
0.6
The variation of the friction coefficient over the
sliding time can be seen in Fig. 3. The evolution 0.4
of the friction coefficient experiences a running- Pin_33HRC
in period during the first hundreds of seconds 0.2 Pin_39HRC
followed by a relatively steady state friction
regime. The duration of the running-in period is 0
10 15 20 25 30 35 40
found to vary with the applied load and the pin Applied load [N]
hardness. For the steady state period, the
Fig. 4. Effect of the applied load on the average
friction coefficient curves exhibit different
friction coefficient with relative standar deviation.
behaviours, involving low and high friction
plateaux. This is specifically true for the low
The average values of the friction coefficient,
hardness pins and applied loads of 20 N, 25 N,
measured in the steady-state condition (from 600
and 35 N (Fig. 3a). This phenomenon is observed
to 900 sliding distance) are plotted vs. applied
only at applied load of 25 N for high hardness
load in Fig. 4. The average values of the friction
pin (Fig. 3b). Moreover, the frequency of the
coefficient are in the range [0.5, 0.8] which is
transition from one regime to another over the
generally found in dry sliding friction of steels
sliding time varies with the applied load and the
[12,7]. The applied load affects the friction
pin hardness. The observed friction coefficient
coefficient in different manner and no specific
evolution with time and applied load suggests
trend was observed, particularly for low hardness
that changes in the wear mechanism and/or
pins. In fact, the high hardness pins have seen
temperature at the contact interface may be
their friction coefficients decrease with increasing
taking place for different applied load as
the applied load. Whereas the low hardness pins
suggested by [12].
have seen the opposite. Compared to the low
hardness pin, the high hardness pin produces
high friction coefficients except for the highest
applied load (35 N). Thus, SEM analysis will be
done in the next section to highlights the actual
wear mechanisms operating in the proposed
frictional systems and try to rationalize the
obtained results.

7.E-06
6.E-06 Pin_33HRC
Wear rate [mm/mm]

Pin_39HRC
5.E-06
(a) 4.E-06
3.E-06
2.E-06
1.E-06
0.E+00
10 15 20 25 30 35 40
Applied load [N]

Fig. 5. Effect of the applied load on the wear rate with

relative standar deviation.

Figure 5 shows the wear rate (per sliding

(b) distance) as a function of applied load. In
Fig. 3. Friction coefficient as function of sliding time general, the wear rate increases with the applied
for (a) Pin tempered at 33HRC, and (b) Pin tempered load. Surprisingly, the high hardness pins wear
at 39 HRC. faster for high applied load than the low

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 A. Elhadi et al., Tribology in Industry Vol. 38, No. 4 (2016) 475-485
hardness pins. This finding is in disagreement
with the classical theory of sliding wear which
postulates that the harder is the material, the
higher is its wear resistance, unless specific
wear mechanisms took place during sliding as
argued in [12,24]. Studying the wear
mechanisms of pin and disc under the tested
conditions will provide some explanations for
this behaviour.
3.2. Worn Surfaces analysis
In order to identify the wear mechanisms, worn
surface of pins and tracks have been analyzed by
optical microscopy and SEM techniques. Figure 6
displays examples of optical images of worn pins
and tracks. For the highest load (35 N), the worn
surface of the high hardness pin is larger (Fig.
6b) than the low hardness one (Fig. 6a).
Moreover, the high hardness pin experiences
high level of oxidation (Fig. 6b). The worn area
of the tracks follows the same trend depicted in
Figs. 6c and 6d. Moreover, Fig. 7 shows that the
wear track is significantly larger and deeper for
the high hardness pin than for the low hardness
one for the same loading condition of 35 N.
SEM observations allowed the identification of
typical damage features into the worn surfaces
as a function of normal load and pin hardness
(Figs. 8, 9, and 10). For low hardness pin and the
applied load (20 N), the worn profile (Fig. 8a)
presents a rough surface with damage features
constituted mainly by local adhesive scars (Fig.
8b) and particles (Fig. 8c). The presence of
chromium and molybdenum (Fig. 8d) indicates
that these particles come from the pin material.
It is suggested that these debris are the results of
the micro-chipping and fragmentation of the low
hardness pin material most likely induced by
cumulative plastic shearing as suggested in
Lepesant et al. [25]. When the highest load is
applied (35 N), the worn surface of the track
becomes smoother with abrasion marks that can
be described as micro-ploughing and relatively
narrow scars in the direction of sliding are
formed and some adhered material layers are
found (Fig. 9a). SEM micrograph (Fig. 9b)
highlights the plastic deformation on this layer
where the plastic flow lines and some micro-
cracks are visible suggesting that the surface
material has underwent high contact stresses
during sliding. Once again, EDS analysis reveals
the presence of oxygen and chromium indicating
that this layer is mainly composed of
agglomerated and compacted oxidised third
body particles of oxide from the pin material.
For high hardness pin used at applied load of 20
N, the track worn surface presents micro-
grooving and smooth surface with ploughing
marks (Fig. 10a). A close examination of the
ploughing marks indicates the presence of
severe plastic deformation and cracking (Fig.
10b) which was note visible for low hardness
pin at the same applied load. Moreover, micro-
chipping and resulting fine particles were
observed on the formed micro-grooves (Fig.
10c) attesting the high shearing and rupturing
mechanisms in agreement with a higher Youngs
modulus which will increases the contact
pressure when high hardness pins are used even
at low applied load (20 N). EDS analysis
confirmed that these particles are mainly
composed of oxidized material from the disc as
no/very few chromium element has been
detected (Fig. 10d). At applied load of 35N
induces severely damage on the track surface as
can be seen in (Fig. 11a). The main damage
features include delamination (Fig. 11b) and
severe plastic deformation (Fig. 11c). In the
micro-delamination features, small flakes of
material are pulled out from the surface (Fig.
12b). As for the load 20 N, the adhering material
for the higher applied load (35 N) is mainly
composed of the disc material as confirmed by
the EDS spectrum in Fig. 11d.
Additional EDS analyses were performed over
larger areas (~1 mm 1 mm) in the wear track
to highlights the effect of the applied load and
pin hardness on the main wear mechanisms. The
EDS spectrums give evidence of oxidative wear.
One can observe significant interaction between
the applied load and pin hardness regarding the
amount of oxygen on the wear products (Fig.
12). In fact, the oxygen content decreases when
increasing the applied load for the low hardness
pin, the inverse been true for the high hardness
pin. Figure 13 displays the effect of applied load
and pin hardness on the chromium content. It is
clear that the applied load do not affect the
chromium content. However, the high hardness
pin produces lower chromium content into the
worn track as compared to the low hardness
one.
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(a) (b)

1 mm 1 mm
(c) (d)
Fig. 6. Optical images of worn surfaces at load of 35N: (a) Worn pin tempered at 33 HRC, (b) Worn pin tempered
at 39 HRC, (c) Worn disc with pin tempered at 33 HRC, and (d) Worn disc with pin tempered at 39 HRC.
Height [m]

(a)
Height [m]

Evaluation length [m]

(b)
Fig. 7. Worn track profiles for pins at (a) Hardness of 33HRC and (b) High hardness of 39HRC.

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 A. Elhadi et al., Tribology in Industry Vol. 38, No. 4 (2016) 475-485

(a) (b)

(c) (d)
Fig. 8. (a) SEM micrographs of worn tracks with pin tempered at 33 HRC and applied load of 20 N, (b)
Delamination (zone A), (c) Adhering particle (zone B), and (d) Corresponding EDS spectrum.

+
A

(a) (b)

(c)
Fig. 9. (a) SEM micrographs of worn tracks with pin tempered at 33 HRC and applied load of 35N, (b) Adhering
layer, and (c) Corresponding EDS spectrum.

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 A. Elhadi et al., Tribology in Industry Vol. 38, No. 4 (2016) 475-485

(a) (b)

(c) (d)
Fig. 10. (a) SEM micrographs of worn tracks with pin tempered at 39 HRC and applied load of 20N, (b) Plastic
deformation (zone A), (c) Micro-chipping and fragmented debris (zone B), and (d) EDS spectrum of zone C.

A
B

(a) (b)

(c) (d)
Fig. 11. (a) SEM micrographs of worn tracks with pin tempered at 39 HRC and applied load of 35N, (b) Adhering
particles and delamination (zone A), (c) Plastic deformation (zone B), and (d) EDS spectrum of the adhering
particle (zone A).

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 A. Elhadi et al., Tribology in Industry Vol. 38, No. 4 (2016) 475-485
14.00
Load=20N
12.00
Oxygen content [%]
10.00
8.00
6.00
4.00
2.00
0.00
Pin at 33HRC
Fig. 12. Oxygen content versus pin hardness at
different applied load.
0.40
Load=20N
0.35
Chromium content [%]
0.30
0.25
0.20
0.15
0.10
0.05
0.00
Pin at 33HRC
Fig. 13. Chromium content versus pin hardness at
different applied load.
The wear mechanisms operating on the pin
surface are strongly related to those operating
on the track side and several scenarios can
operates as the interaction between the applied
load and pin hardness result in complex thermo-
mechanical behaviour of the worn surfaces. This
change of mechanisms can explain the unstable
trend of the wear rate and friction coefficient
with regard to the applied load and pin
hardness. When high load is applied (35 N), the
high hardness pin induces high level of disc
material loss in the form of small debris. These
debris, which are harder than the pin material
generate in turn high level of wear rate by
abrasion on the pin surface. The same
mechanism is applied to the low hardness pin
but with low level of generated debris volume
resulting in lower erosion rates. For the high
hardness pin, the wear mechanisms are
governed by delamination, oxidation, and plastic
deformation and fracture. In the case of low
hardness pin, the main wear mechanisms
observed were abrasion, adhesion, and
oxidation. Specifically, the oxidative wear is
Load=35N
found to be governed by the applied load for
both tempered pins used in this study.
Lepesant et al. [25] argued that, in a specific
friction conditions, compacted oxide particles
from the pin, can plastically deformed to form a
layer, referred to as a glaze layer. It is shown
that the matrix strength of the pin material has
to be considered to know whether the oxides
from the glaze layers are protective, or not,
Pin at 39HRC against wear [26]. If the matrix is strong enough,
the oxides formed during friction have a positive
influence on wear. On the contrary, if the matrix
is not strong enough, the oxides from the glaze
layer do not protect the surfaces from wear and
Load=35N they may even act as an abrasive third body. In
the present study, we suggested that the oxides
from the glaze layer plays a positive role in
improving the wear resistance of the low
hardness pin as compared to the high hardness
pin results regarding to the obtained wear rate
trends (Fig. 5).
4. CONCLUSIONS
Pin at 39HRC
The present study investigated the wear
mechanisms of tempered low alloy steel against
hardened carbon steel under dry sliding wear.
Based on the obtained results, the following
conclusions may be drawn:
In specific tribological conditions, low
hardness pin can perform better, than high
hardness pin in terms of dry sliding wear
resistance.
Wear mechanisms of the hard track
material (disc) should be considered as
three-body contact wear which is mainly
governed by the hard particles detached
from the worn disc and pin.
Under high applied loads, it is shown that
when high hardness pins are used, the disc
generates amount of particles/debris that
significantly increases the wear of the pin.
This can be avoided by using a pin with a
slightly lower hardness.
The obtained results can be considered as
a preliminary investigation for improving
the performance of the sliding mechanism.
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Acknowledgments
The authors appreciate the financial support
from the Mechanical Engineering Department of
the Faculty of technology, University of
Mohamed Boudiaf, Msila, Algeria. The authors
are also grateful for the technical support of the
Department of Mechanical Engineering, TS,
Montreal, Canada through the Laboratoire
dOptimisation des Procds de Fabrication en
Arospatiale, LOPFA.
REFERENCES
[1] N. Khanafi-Benghalem, E. Felder, K. Loucif and P.
Montmitonnet, 'Plastic deformation of 25CrMo4
steel during wear: Effect of the temperature, the
normal force, the sliding velocity and the
structural state', Wear, vol. no. 268, pp. 23-40,
2010.
[2] M.B. Peterson and W.O. Winer, Wear Theory and
Mechanisms, Wear Control Handbook. ASME,
New York, NY, pp. 35-80, 1980.
[3] B. Bhushan, Principle and Applications of Tribology.
New York: John Wiley & Sons, Inc, 1999.
[4] M.A. Chowdhury and D.M. Nuruzzaman,
'Experimental Investigation on Friction and Wear
Properties of Different Steel Materials', Tribology
in Industry, vol. 35, no. 1, pp. 42-50, 2013.
[5] M.A. Chowdhury, M.M. Helali, 'The Effect of
Relative Humidity and Roughness on the
Friction Coefficient under Horizontal Vibration',
The Open Mechanical Engineering Journal, vol. 2,
pp. 128- 135, 2008.
[6] M. Kandeva, L. Vasileva, R. Rangelov and S.
Simeonova, 'Wear-resistance of Aluminum
Matrix Microcomposite Materials', Tribology in
Industry, vol. 33, no. 2, pp. 57-62, 2011.
[7] O. Barrau, C. Boher, Gras R, Rezai-Aria F.
Analysis of the friction and wear behaviour of
hot work tool steel for forging', Wear, vol. 255,
no. 7, pp.1444-1454, 2003.
[8] J.D. Bressana, D.P. Darosa, A. Sokolowskib, R.A.
Mesquitac and C.A. Barbosad, 'Influence of
hardness on the wear resistance of 17-4 PH
stainless steel evaluated by the pin-on-disc
testing', Journal of materials processing
technology , vol. 205, pp. 353-359, 2008.
[9] H. Goto and Y. Amamoto, 'Effect of varying load
on wear resistance of carbon steel under
unlubricated conditions', Wear, vol. 254, no. 12,
pp. 1256-1266, 2003.
484
[10] V. Abouei, H. Saghafian and S. Kheirandish,
'Effect of microstructure on the oxidative wear
behavior of plain carbon steel', Wear, vol. 262,
no. 9-10, pp. 1225-1231, 2007.
[11] D. Rai, B. Singh and J.Singh, 'Characterisation of
wear behaviour of different microstructures in
NiCrMoV steel', Wear, vol. 263, no. 1-6, pp.
821-829, 2007.
[12] L. Tang, C. Gao, J. Huang, H. Zhang and W. Chang,
'Dry sliding friction and wear behaviour of
hardened AISI D2 tool steel with different
hardness levels', Tribology International, vol. 66,
pp. 165-173, 2013.
[13] K. Hokkirigawa, K. Kato and Z.Z. Li, 'The effect of
hardness on the transition of the abrasive wear
mechanism of steels', Wear, vol. 123, no. 2, pp.
241-251, 1988.
[14] CC. Vifara and A. Sinatora, 'Influence of
hardness of the harder body on wear regime
transition in a sliding pair of steels', Wear, vol.
267, no. 1, pp. 425-432, 2009.
[15] C.C. Vifara and A. Sinatora, 'Unlubricated sliding
friction and wear of steels: An evaluation of the
mechanism responsible for the T1 wear regime
transition', Wear, vol. 271, no. 9, pp. 1689-1700,
2011.
[16] V. Toppo, SB. Singh and KK. Ray, 'Wear
resistance of annealed plain carbon steels in pre-
strained condition', Wear, vol. 266, no. 9-10, pp.
907-916, 2009.
[17] V. Panin, A. Kolubaev, S. Tarasov and V. Popov,
'Subsurface layer formation during sliding
friction', Wear, vol. 249, pp. 860-867, 2002.
[18] J.R. Fleming and N.P. Suh, 'Mechanics of crack
propagation in delamination wear', Wear, vol.
44, no. 1, pp. 39-56, 1977.
[19] S. Jahanmir, N.P. Suh, 'Mechanics of subsurface
void nucleation in delamination wear', Wear, vol.
44, no. 1, pp. 17-38, 1977.
[20] Y. Berthier, 'Third body reality-Consequences
and use of the third body concept to solve a
friction and wear problems', Wear, Materials,
Mechanisms and Practice, DOI:
10.1002/9780470017029.ch12, 2005.
[21] N. Diomidis and S. Mischler, 'Third body effects
on friction and wear during fretting of steel
contacts' Tribology International, , vol. 44, no. 11,
pp. 1452-1460, 2011.
[22] S.Q. Wang, M.X. Wei and Y.T. Zhao, 'Effects of the
tribo-oxide and matrix on dry sliding wear
characteristics and mechanisms of a cast steel',
Wear, vol. 269, no. 5, pp. 424-434, 2010.
 A. Elhadi et al., Tribology in Industry Vol. 38, No. 4 (2016) 475-485
[23] S. Kumar, A. Bhattacharyya, D.K. Mondal, K.
Biswas and J. Maity, 'Dry sliding wear behaviour
of medium carbon steel against an alumina disk',
Wear, vol. 270, no. 5, pp. 413-421, 2011.
[24] Y. Wang and T. Lei, 'Wear behavior of steel 1080
with different microstructures during dry
sliding', Wear, vol. 36, no. 2, pp. 213-217, 1997.
[25] P. Lepesant, C. Boher, Y. Berthier and F. Rezai-
Aria, 'A phenomenological model of the third
body particles circulation in a high temperature
contact', Wear, vol. 298-299, pp. 66-79, 2013.
[26] S. Wang, M. Wei and Y. Zhao, 'Effects of the tribo-
oxide and matrix on dry sliding wear
characteristics and mechanisms of a cast steel',
Wear, vol. 269, no. 5-6, pp. 424-434, 2010.
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Tribology in Industry

RESEARCH
www.tribology.fink.rs

Slurry Erosion Behavior of Destabilized and Deep

Cryogenically Treated Cr-Mn-Cu White Cast Irons

S. Gupta a, A. Khandelwal a, A.K. Ghose a, I. Chakrabarty a

aDepartment of Metallurgical Engineering, Indian Institute of Technology (Banaras Hindu University), Varanasi
221005, India.

Keywords:
Alloy white cast iron
Castings
Optical microscopy
Erosive wear
Corrosion
Cryogenic treatment
Corresponding author:
I. Chakrabarty
Department of Metallurgical
Engineering, Indian Institute of
Technology (Banaras Hindu
University), Varanasi 221005 India.
E-mail: ichakraborty.met@itbhu.ac.in
ABSTRACT
The effects of destabilization treatment and destabilization followed by
cryogenic treatment have been evaluated on the microstructural
evolution and sand-water slurry erosion behavior of Cr-Mn-Cu white cast
irons. The phase transformations after the destabilization and
cryotreatment have been characterized by bulk hardness measurement,
optical and scanning electron microscopy, x-ray diffraction analysis. The
static corrosion rate has been measured in tap water (with pH=7) and the
erosion-corrosion behavior has been studied by slurry pot tester using
sand-water slurry. The test results indicate that the cryogenic treatment
has a significant effect in minimizing the as-cast retained austenite
content and transforming into martensitic and bainitic matrix embedded
with ultra-fine M7C3 alloy carbides. In contrast, by conventional
destabilization treatment retained austenite in the matrix are not fully
eliminated. The slurry erosive wear resistance has been compared with
reference to destabilized and cryotreated high chromium iron samples
which are commonly employed for such applications. The cryotreated Cr-
Mn-Cu irons have exhibited a comparable erosive wear performance to
those of high chromium irons. Higher hardness combined with improved
corrosion resistance result in better slurry erosion resistance.
2016 Published by Faculty of Engineering

1. INTRODUCTION material from corrosion are worn out by the

A combined action of electrochemical corrosion
and mechanical damage due to erosion by the
solid particles suspended in a liquid slurry
medium accelerates failure to many critical
components. The effect of this combined action
is synergistic in nature that is corrosion
accelerates wear and vice-versa. Thin
passivating surface layers that protect the
impinging eroding particles in the slurry and
further corrosion increases. Plastic deformation
of the metal surface during wear can also
generate localized high energy sites more prone
to corrosion than the unworn sites. High
chromium and nickel-chromium white cast irons
are potent materials for corrosion-erosion
applications such as in the mining, earth moving,
cement and coal industries [1-4]. The carbide

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morphology and the matrix phase are the two
influencing factors contributing to maximum
wear resistance, toughness and corrosion.
Discontinuous plate like eutectic M7C3 carbides
along with tough matrix embedded with fine
secondary alloy carbides are preferable for such
applications [5,7]. A thin passive layer is formed
on the surface due to high percentage of
chromium in the solid solution [8,9].
Beside the developments in the high
chromium and nickel-chromium irons there
has been continuing interest in the
development of substitute alloy irons to
provide either a partial or total replacement of
costly and scarce alloying elements viz. Ni, Mo
etc. A new class of chromium manganese
alloy irons has been developed with
manganese, a cheaper alloying addition to
produce a predominantly austenitic matrix in
as-cast condition by suppressing pearlitic
transformation [10-12]. Copper addition to
chromiummanganese irons reported to be
beneficial because of its partitioning tendency
to austenite phase and it enhances resistance
to aqueous corrosion [13-17].
The as-cast austenitic matrix is conventionally
destabilized by a destabilization or
destabilization treatment to transform as-cast
austenite to martensitic and/or fine bainitic
matrix embedded with fine secondary carbides
[1,2]. But even after such conventional
destabilization the retained austenite cannot be
totally transformed. Cryogenic treatment is
successfully employed especially in tool steels
[18-32] and high chromium cast irons [33-37] to
minimize the retained austenite content as far as
possible. The consequent improvement in wear
resistance has been attributed to i)
transformation of retained austenite to
martensite, ii) conditioning of martensite at low
temperature and iii) enhanced volume
percentage of refined secondary carbide
precipitation. In a recent study, Shaohong Li et.
al [31] have verified the mechanism of the
refined carbide precipitation by internal friction
method and transmission electron microscopy,
in tool steels on deep cryogenic treatment. The
high internal stress developed from austenite to
martensite transformation is responsible for
modification of carbide precipitation. The
martensite lattice contraction causes to
segregate interstitial carbon atoms at the nearly
moving dislocations. The tetragonality becomes
very low as a consequence. A strong interaction
in between the time dependent strain field of
dislocation and the segregated carbon atoms is
produced. The segregated carbon atoms form
clusters at nearby dislocations forming nuclei
for carbide precipitation during subsequent
warming up to room temperature or tempering.
These uniformly dispersed secondary carbides
are responsible for the improvement of
properties on deep cryogenic treatment.
The aim of the present article is to study the
effect of destabilization and cryogenic treatment
on the microstructural evolution and
consequent erosive wear behavior of Cr-Mn-Cu
white cast iron in sand-water slurry media.
2. EXPERIMENTAL PROCEDURE
The alloy irons were melted in a basic lined high
frequency induction furnace. Cylindrical test
bars and wear test samples were cast in sodium
silicate CO2 bonded sand moulds with a pouring
temperature of 1773K (1500 0C). For
comparison of wear behaviour high chromium
iron specimens were also cast; the chemical
compositions analysed in ARL optical emission
spectrometer are shown in Table 1.
Table 1. Chemical compositions of alloy irons cast.
Alloy irons C% Mn% Si% Cr% Cu%
a)Cr-Mn-Cu iron 2.8 4.8 1.87 9.2 3.1
b) High Cr iron 2.9 0.53 0.32 16.3 -
Optimum destabilization temperature ranges
and time for as-cast Cr-Mn-Cu irons were
selected based on isochronal and isothermal
heat treatments. Initially the as-cast samples
were subjected to isochronal heat treatment for
a fixed period of 1 hour in the temperature
range of 973K (700 0C) to 1373K (1100 0C) in
373K (100 0C) steps and followed by air cooling
to room temperature. In the optimum
temperature range thus found from the
isochronal treatment, the samples were
isothermally treated for various soaking times
and subsequently either air cooled or quenched
in liquid nitrogen bath and kept immersed for 30
minutes for the cryogenic treatment. The wear
samples were heat treated at the optimum
temperature {1023K (750 0C)} and time (9
hours) obtained from isochronal and isothermal
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treatments. High chromium irons were treatment conditions of the test alloy specimens
subjected to conventional destabilization at can be well assessed with reference to the high
1273K (1000 0C) for 9 hours and subsequently chromium iron samples under identical
cryotreated. The microstructures of the alloy conditions. Cylindrical wear specimens (10 mm.
irons observed under optical and scanning diameter x 50 mm. length) were ground with
electron microscopes. The bulk hardness at emery paper number 1000, cleaned with water
different heat treatment conditions were and acetone, dried and fitted in the holding disc
measured in Rockwell C- scale with 150 kgf load. of the test rig. Specimens with similar heat
treatment condition were placed at the
The retained austenite contents in a few selected
samples were measured by x-ray diffraction
analysis with Cu K radiations. To avoid the
effect of texture the samples were continuously
rotated. The carbide volume percentages
present in the alloys at different conditions were
measured by electrolytic extraction of carbides.
The carbide volume percentages thus
determined were computed to estimate the
retained austenite content in the matrix. A bath
with 5 % concentrated HCl in ethyl alcohol was
employed with sample as anode and a stainless
steel plate as cathode for electrolytic extraction.
The extraction was continued for about 20 hours
with a current density of 5 mA/cm2 and the
extracted carbides were collected in a glycerine
layer from the bottom of the bath. The volume
percentages of the extracted carbides were
calculated after drying at 343K (70 0C). Fig. 1. Slurry erosion test set-up.

The static corrosion rate of the alloy irons was
measured as per ASTM standard (ASTM G-1-72).
Mirror polished rectangular specimens (10x10
mm.) were cleaned with water and acetone,
dried and weighed in an electronic balance. The
samples were suspended in a glass beaker with
tap water (pH=7) for 168 hours at room
temperature. After this period of immersion, the
specimens were again cleaned thoroughly with
water and acetone, dried and reweighed. The
static corrosion rates were computed from the
expression,
Corrosion rate [ in mg/decimeter2/ day (mdd)] =
K.W /(A.T.D)
where, K= 2.4 x 106.D; W= weight loss in g
nearest to 1 mg; A= surface area in square cm
nearest to 0.01 cm2; T= duration in hours; D=
density of the material in g/cc.
The erosive wear performance was evaluated in
a slurry pot tester as shown in Fig. 1. Although
the effect of impact angle of the slurry particle
impingement cannot be evaluated by this set up,
the relative wear performance in different heat
Two diametrical opposite position at the holding
disc to avoid any biasness. The sand-water
slurry was prepared with 60 % silica sand
particles by weight in plain tap water. The
details of the silica sand eroding particles are
shown in Table 2.
Table 2. Details of silica sand used for slurry erosion
test.
Shape Average Micro-hardness,
Erodent
(Roundness)a size, m Kg/mm2
Silica sand 0.79 325 1100-1150
a according to Rittenhouse sphericity scale
The specimens were rotated in the slurry for a
total duration of 24 hours at 500 rpm which
corresponds to a linear speed of 4.5 m/s. After
every 6 hours of test run the specimens were
taken out, cleaned, dried and the mass losses
were noted. After 24 hours run the samples tips
were cut off, cleaned ultrasonically in acetone
and examined under scanning electron
microscope for worn-out surface topography.

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3. RESULTS AND DISCUSSION
3.1 Phase Transformation Behaviour
As revealed in the optical microstructure shown
in Fig. 2, the as-cast Cr-Mn-Cu iron consists of
predominantly austenitic matrix along with
discontinuous eutectic carbides. The matrix
structure is confirmed by XRD analysis, the
austenite content has been estimated to be 87.63
% and the types of eutectic carbides are detected
as M7C3 carbides (Fig. 3). The volume percent of
these carbides has been estimated as 15.4 %
from electrolytic extraction.
Fig. 2. Optical micrograph of as-cast Cr-Mn-Cu iron
showing predominantly austenitic matrix.
Fig. 3. XRD pattern of as-cast Cr-Mn-Cu alloy iron
with Cu K radiation.
The bulk hardness after isochronal treatment
temperature attains a peak at a temperature
around 1023K (7500C) and decreases with
further increase in temperature. Fig. 4 shows the
corresponding microstructural change in optical
micrographs from which it can be inferred that
as the temperature is increased initially as-cast
austenitic matrix is gradually transformed into
martensitic and/or fine bainitic matrix along
with fine alloy carbide precipitates.
Fig. 4. Optical micrographs of isochronally treated
alloy irons for 1 hour at a) 973K (700 0C), b) 1073K
(800 0C), c) 1273K (1000 0C) and d) 1373K (1100 0C).
Fig. 5. Variation in bulk hardness with isothermal
treatment time followed by a) cryotreatment and b)
air cooling.
This results in an increase in hardness. If the
treatment temperature crosses beyond the peak
temperature, it is perhaps too high above the A3
temperature of the alloy and austenite phase
becomes stabilized again. This is substantiated
by the optical micrographs. The attainment of
peak hardness can be attributed to the following
factors:
i) Initially when the alloy is held just above
the A3 temperature, the solid solubility of
carbon and other alloying elements being
the lowest possible, the austenite matrix
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gets depleted of carbon and other alloying shown in Fig. 7 and the EDS spectra obtained
elements with consequent fine alloy carbide from secondary carbides is shown in Fig. 7a.
precipitation.
ii) The martensite start temperature (Ms) of
the alloy depleted austenite matrix is raised
and during subsequent air cooling the
matrix transforms to martensite embedded
with fine carbides.
iii) On further increase in temperature, the
austenite gets stabilized again because of
the higher solid solubility and the
precipitates are also coarsened resulting in
a drop in hardness.

Fig. 7. SEM image of destabilized {1023K (750 0C) for

9 hours} and air cooled Cr-Mn-Cu alloy.

Fig. 6. Optical micrographs of isothermally treated

Cr-Mn-Cu alloy for a) 3 hours and air cooled; b)
9 hours and air cooled; c) 3 hours and cryotreated Fig. 7a. EDS spectra of secondary carbides in
and d) 9 hours and cryotreated. destabilized and air cooled alloy.

The bulk hardness versus isothermal treatment

time plot at the optimum temperature 1023K
(750 0C) obtained from isochronal treatment is
shown in Fig. 5. It is evident from the figure that
the hardness initially increasing almost linearly
with time and becomes steady at the latter stage
of treatment. A gradual conversion of austenitic
matrix into a dark matrix embedded with very
fine alloy carbides are revealed in the
corresponding optical micrographs (Fig. 6). The
actual phase present in the matrix is difficult to
be resolved under optical microscope. The as-
cast supersaturated austenite matrix tends to
attain equilibrium carbon and alloy contents Fig. 8. XRD profile of i) destabilized and cryotreated
with consequent rejection of these elements and alloy and ii) destabilized and air cooled alloy.
on subsequent cooling to room temperature the
alloy depleted austenite transforms to the dark The effect of cryotreatment following isothermal
phase. The dark matrix could be resolved under destabilization for varying soaking periods on
scanning electron microscope and it is found to the bulk hardness is shown in Fig. 5. It depicts a
be mostly fine bainite with few areas of similar trend as in the case of air cooling.
martensite embedded with fine alloy carbides. However, in case of cryotreatment, the hardness
The SEM image of the destabilized matrix is increase is significantly higher than that in air

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cooling. This trend can be justified with the
retained austenite percentage measured from
XRD analysis (Fig. 8) and the corresponding
optical and SEM micrographs in Figs. 6 and 9
respectively. The EDS spectra from secondary
carbides is shown in Fig. 9a.
Fig. 9. SEM image of destabilized {1023K (750 0C) for
9 hours} and cryotreated Cr-Mn-Cu alloy.
Fig. 9a. EDS spectra of secondary carbides formed in
destabilized and cryotreated alloy.
Table 3. Details of carbide volume% and retained
austenite content in different conditions.
Carbide Retained
Alloy conditions
volume% austenite%
1. As-cast 15.44 87.63
2. Destabilized at
1023K (750 0C) + 9 hrs. air 21.50 13.54
cooling
3. Destabilized at
1023K (750 0C) + 9 hrs. 28.32 - The cumulative wear loss versus wearing time
cryotreatment
A large dispersion of very fine secondary carbide
precipitates accounts for further increase in
hardness which has been confirmed by the
volume fraction of carbides determined by
electrolytic extraction (Table 3). The matrix also
contributes to the high hardness, a
predominantly martensitic matrix with lesser
areas of fine bainites are formed as evidenced by
the SEM.
3.2 Static corrosion rates
The static corrosion rates of destabilized and
subsequently air cooled or cryotreated Cr-Mn-
Cu and high chromium alloys in tap water (pH
=7) are shown in Fig. 10. It is evident from the
figure that cryotreated alloys are having a lower
rate of corrosion than those of destabilized and
air cooled alloys.
Fig. 10. Static aqueous corrosion rate in different
alloy conditions.
Similar improvement in corrosion resistance has
been observed by Amini K. et al. in cryotreated
tool steel [30]. The improvement in corrosion
resistance has been attributed to the more
uniform carbide distribution in association with
higher fine carbide formation in cryotreated
alloy. It is believed that, the deep cryogenic
treatment reduces the internal stress and
stabilizes the dislocation structure in steel,
consequently, decreasing the free energy of
atoms. This results in a better corrosion
resistance in steel [37,38].
3.3 Slurry-erosion behaviour
curves are shown in Fig. 11, from which it is
apparent that, the wear resistance of the
cryotreated specimens is significantly improved
compared to those in destabilized and
subsequently air cooled specimens. The wear
resistance of the as-cast alloy is least among
other tested alloys. The erosive wear resistance
of the cryotreated Cr-Mn-Cu alloys is
comparable to that of cryotreated high
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chromium alloy irons. The hardness perhaps harder phase compared to the matrix. The
plays a vital role in decreasing the wear rate. matrix regions have worn out preferentially
The corresponding microstructures obviously leaving the carbide regions to support the load
have a great influence on the wear loss. A fine of eroding particles. In all the worn out surfaces
Grained predominantly martensitic matrix with plough marks are prominent in the matrix
least amount of retained austenite embedded phases (Figs. 12a and 12b).
with fine and hard alloy carbides exhibit very
good wear resistance. The better wear
resistance of cryotreated samples can be
attributed to three factors:
I. Due to reduction of retained austenite and
its conversion to higher percentage of
martensite in the matrix. This provides
stronger support to the hard and fine
secondary alloy carbides during erosion.
II. More homogeneous precipitation with high
volume fraction of finer alloy carbides.
III. Cryotreatment produces refined martensitic
matrix causing a fine grained strengthening
effect which improves wear resistance
further.

Fig. 12. a) SEM image of worn out surface of

destabilized and air cooled alloy, b) Magnified image
showing plough mark sand lip formation in the matrix.

Fig. 11. Average cumulative wear loss vs. time plot in

slurry erosion test.

The worn out surface topography have been

studied with scanning electron microscope
(SEM). The SEM micrographs show formation of
indentation craters by ploughing mechanism as
suggested by Hutchings [39]. The round to sub-
angular shaped eroding particles impinges on
the metal surface pushing the metal in the
direction of the movement of the eroding
particles. The erosion occurs due to fracture and
detachment of this lip. The metal is displaced
also at the sides of the impact craters. The worn Fig. 13. SEM image of worn out surface of as- cast
out surface show the carbides in relief, being alloy showing micro-cracks in the matrix.

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The as-cast Cr-Mn-Cu alloy shows fine cracks
formed in the matrix. These cracks might have
led to spall formation and hence material
detachment (Fig. 13).
Fig. 14. SEM image of worn out surface of destabilized
and cryotreated alloy showing smoother surface.
It was perhaps due to excessive preferential
wear of the matrix regions for which carbides
might become unsupported and susceptible to
spalling and fracture. In contrast, cryotreated
sample surfaces are smoother which can be
attributed to their higher hardness resulting in
shallow penetration and improved aqueous
corrosion resistance hence lesser attack by
corrosion- erosion (Fig. 14).
4. CONCLUSIONS
The Cr-Mn-Cu alloy iron consists of a
predominantly austenitic matrix in as-cast
condition. This as-cast matrix can be
transformed to a hard martensitic and/or fine
bainitic matrix embedded with fine M7C3 type
secondary carbides by a destabilization
treatment, conventionally employed for most
wear resistance applications.
The retained austenite content in as-cast matrix
cannot be fully eliminated by conventional
destabilization treatment which can be almost
totally converted to martensite by a
destabilization followed by cryogenic treatment.
The consequent bulk hardness increases
significantly.
The slurry erosion resistance of the cryotreated
Cr-Mn-Cu iron is well comparable to that of
cryotreated high chromium iron. Not only higher
hardness but improved corrosion resistance
contributes to better slurry erosion property.
It is evident from the SEM images of the
worn out surfaces that, the predominant
mechanism of material removal during slurry
erosion is by ploughing. In as-cast irons cracks
are formed around the matrix leading to spall
formation. In case of cryotreated iron matrix
being harder, no preferential erosion between
matrix and carbides are occurring and hence a
smoother worn out surface is revealed.
REFERENCES
[1] J.T.H. Pearce, High chromium cast irons to resist
abrasive wear, Foundryman, vol. 95, pp. 156-
166, 2002.
[2] C.P. Tabrett, I.R. Sare and M.R. Ghomashchi,
Microstructure-property relationships in high
chromium white iron alloys, Int. Mater. Rev., vol.
41, no. 2, pp. 59-82, 1996.
[3] J. Liu and Y. Man, Development of abrasive
resistant Ni-hard 4 cast irons, Wear, vol. 162-
164, pp. 833-836, 1993.
[4] M. Salasi, G.B. Stachowiak and G.W. Stachowiak,
Three-body tribocorrosion of high chromium
cast irons in neutral and alkaline environments,
Wear, vol. 271, pp. 1385-1396, 2011.
[5] G.B. Stachowiak, G.W. Stachowiak and O. Celliers,
Ball-cratering abrasion tests of high-Cr white
cast irons, Tribol Int., vol. 38, pp. 10761087,
2005.
[6] E. Zumelzu, L. Goyos, C. Cabezas, O. Opitz and A.
Parada, Wear and corrosion behaviour of high-
chromium (14-30% Cr) cast iron alloys, J. Mater.
Process. Tech., vol. 128, pp. 250-255, 2008.
[7] J.O. Agunsoye and A.A. Ayeni, Effect of Heat
Treatment on the Abrasive Wear Behavior of
High Chromium Iron under Dry Sliding
Condition, Tribology in Industry, vol. 34, no. 2,
pp. 82-91, 2012.
[8] J.F. Flores, A. Neville, N. Kapur and A. Gnanavelu,
Erosioncorrosion degradation mechanisms of
FeCrC and WCFeCrC PTA overlays in
concentrated slurries, Wear, vol. 267, no. 11, pp.
1811-1820, 2009.
[9] H.H. Tian, G.R. Addie and R.J. Visintainer,
Erosioncorrosion performance of high-Cr cast
iron alloys in flowing liquidsolid slurries,
Wear, vol. 267, no. 11, pp. 2039-2047, 2009.
493
 S. Gupta et al., Tribology in Industry Vol. 38, No. 4 (2016) 486-495

[10] L.I. Levi et al., Wear resistant chromium- [22] M.A. Jaswin and D. Mohan Lal , Optimization of
manganese cast irons, Russ. Cast. Prod., August, the cryogenic treatment process for En 52 valve
pp. 409-412, 1967. steel using Grey-Taguchi method, Materials and
Manufacturing Processes, vol. 25, no. 8, pp. 842-
[11] A. Basak, J. Penning and J. Dilewijns, Effect of Mn
850, 2010.
on wear resistance and impact strength of 12%
Cr white cast irons, Int. Cast Met. J., vol. 6, no. 3, [23] M. Koneshlou, K.M. Asl and F. Khomamizadeh,
pp. 12-17, 1981. Effect of cryogenic treatment on microstructure,
mechanical and wear behaviors of AISI H13 hot
[12] A. Basak, J. Penning and J. Dilewijns, Effect of Ti
work tool steel, Cryogenics, vol. 51, pp. 55-61,
inoculation on wear resistance and impact
2011.
strength of Cr-Mn alloy white cast irons, Met.
Technol., vol. 9, no. 9, pp. 381-384, 1982. [24] K Amini, S. Nategh and A. Shafyei, Influence of
different cryotreatments on tribological
[13] I. Chakrabarty and A. Basak, Ausaging and
behavior of 80Cr Mo12 5 cold work tool steel,
corrosive wear behavior of Cr-Mn-Cu white cast
Mater. Des., vol. 31, pp. 4666-4675, 2010.
irons, AFS Trans., vol. 98, pp. 707-716, 1990.
[25] D. Senthilkumar and I. Rajendran, Optimization
[14] I. Chakrabarty, A. Basak and U.K. Chatterjee,
of deep cryogenic treatment to reduce wear loss
Corrosive wear behavior of Cr-Mn-Cu white cast
of 4140 steel, Materials and Manufacturing
irons in sand-water slurry media, Wear, vol.
Processes, vol. 27, pp. 567-572, 2012.
143, pp. 203-220, 1991.
[26] M. El Mehtedi, P. Ricci, L. Drudi, S. El Mohtadi, M.
[15] I. Chakrabarty, Effect of copper on the corrosion
Cabibbo and S. Spigarelli, Analysis of the effect
resistance behavior of as-cast and destabilized
of deep cryogenic treatment on the hardness
Cr-Mn white cast irons, AFS Int. J. Metal Cast.,
and microstructure of X30 Cr Mo N15 1 steel,
vol. 5, no. 1, pp. 49-56, 2011.
Mater. Des, vol. 33, pp. 136-144, 2012.
[16] P.N.V.R.S.S.V Prasada Rao, A.K. Patwardhan and
[27] R. Sri Siva, A. Arockia Jaswin and D. Mohan Lal,
N.C. Jain, Effect of microstructure on the
Enhancing the wear resistance of 100 Cr6 bearing
corrosion and deformation behavior of a newly
steel using cryogenic treatment, Tribology
developed 6Mn-5Cr-1.5Cu corrosion-resistant
Transactions, vol. 55, pp. 387- 393, 2012.
white iron, Metall. Mater. Trans. A, vol. 24, no. 2,
pp. 445-457, 1993. [28] M. Arockia Jaswin and D. Mohan Lal, Effect of
cryogenic treatment on the tensile behavior of
[17] A.K. Patwardhan and N.C. Jain, Modeling of the
En 52 and 21-4N valve steels at room and
corrosion behavior and its interrelation with the
elevated temperature, Mater. Des., vol. 32, pp.
deformation behavior and microstructure in a
2429-2437, 2011.
newly developed 7.5Mn-5Cr-1.5Cu alloy white
iron, Metall. Mater. Trans. A, vol. 22, no. 10, pp. [29] P. Baldissera, Deep cryogenic treatment of AISI
2319-2325, 1991. 302 stainless steel: Part I- hardness and tensile
properties, Mater. Des., vol. 31, pp. 4725-4730,
[18] D. Das, A.K Dutta, V. Toppo and K.K. Ray, Effect
2010.
of deep cryogenic treatment on the carbidic
precipitation and tribological behavior of D2 [30] K. Amini, A. Akhbarizadeh and S. Javadpour,
steel, Materials and Manufacturing Processes, Investigating the effect of the quench
vol. 22, pp. 474-480, 2007. environment on the final microstructure and
wear behavior of 1.2080 tool steel after deep
[19] D. Das, R. Sarkar, A.K Dutta and K.K. Ray,
cryogenic heat treatment, Mater. Des, vol. 45, pp.
Influence of sub-zero treatments on fracture
316-322, 2013.
toughness of AISI D2 steel, Mater. Sci. Eng. A,
vol. 528, pp. 589-603, 2010. [31] Shaohong Li, Na Min, Junwan Li, Xiaochun Wu,
Chenhui Li and Leilei Tang, Experimental
[20] A.J. Vimal, A. Bensely, D. Mohan Lal and K.
verification of segregation of carbon and
Srinivasan, Deep cryogenic treatment improves
precipitation of carbides due to deep cryogenic
wear resistance of En 31 steel, Materials and
treatment for tool steel by internal friction
manufacturing Processes, vol. 23, no. 4, pp. 369-
method, Mater. Sci. Eng. A, vol. 575, pp. 51-60,
376, 2008.
2013.
[21] N.S. Kalsi, R. Sehgal and V.S. Sharma, Cryogenic
[32] V.G. Gavriljuk, W. Theisen, V.V. Sirosh, E.V.
treatment of tool materials: A Review, Materials
Polsin, A.Kortmann, G.S. Mogilny, Yu.N. Petrov
and Manufacturing Processes, vol. 25, no. 10, pp.
and Ye. V. Tarusin, Low temperature
1077-1100, 2010.
martensitic transformation in tool steels in

494
 S. Gupta et al., Tribology in Industry Vol. 38, No. 4 (2016) 486-495
relation to their deep cryogenic treatment, Acta
Mater., vol. 61, pp. 1705-1715, 2013.
[33] Hong- Shan Yang, Jun Wang, Bao-Luo Shan, Hao-
huai Liu, Sheng-Ji Gao and Si-Jiu Huang, Effect of
cryogenic treatment on the matrix structure and
abrasion resistance of white cast iron subjected
to destabilization treatment, Wear, vol. 261, pp.
1150-1154, 2006.
[34] Hao-huai Liu, Jun Wang, Bao-Luo Shan, Hong-
Shan Yang, Sheng-Ji Gao and Si-Jiu Huang,
Effects of deep cryogenic treatment on property
of 3Cr13Mo1V1.5 high chromium cast iron,
Mater. Des., vol. 28, pp. 1059-1064, 2007.
[35] Hao-Huai Liu et al., Effects of cryogenic
treatment on microstructure and abrasion
resistance of CrMnB high- chromium iron
subjected to sub-critical treatment, Mater Sci.
Eng. A, vol. 478, pp. 324-328, 2008.
[36] C.P. Tabrett and I.R. Sare, Effect of high
temperature and sub-ambient treatments on the
matrix structure and abrasion resistance of a
high chromium white iron, Scripta Mater., vol.
38, no. 12, pp. 1747-1753, 1998.
[37] R.F. Barron and R.H. Thompson, Effects of
cryogenic treatment on corrosion resistance,
[Paper BP-17] in Fast RW (Ed.), International
cryogenic materials conference, New York;
Plenum Press, 1989.
[38] Xuan Fu-Zhen, Huang, Xiaoqing and Tu, Shan-
Tung, Comparison of 30Cr2Ni4MoV rotor steel
with treatments on corrosion resistance in high
temperature water, Mater. Des, vol. 29, pp.
1533, 2008.
[39] I.M. Hutchings, Tribology Friction and Wear of
Engineering Materials, Edward Arnold, 1992.
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Tribology in Industry

RESEARCH
www.tribology.fink.rs

Tribological Studies of Antiwear Antifriction

Composition and its Application

V.N. Duradji a, D.E. Kaputkin a, A. Duradji a

a National University of Science and Technology "MISiS", Leninskiy prospect 4, 119049, Moscow, Russia.

Keywords: ABSTRACT
Friction
In recent decades appeared the considerable interest in the use of the
Wear
antiwear, anticorrosion and restoration technologies in friction units,
Lubricant
including the internal combustion engines. These technologies allow
Wearless friction
reducing the friction coefficient and the wear of friction surfaces during
Servovite film
the operation without disassembly of the components and assemblies.
Coating
The present work involves the studies of the tribotechnical characteristics
Running-in
of the friction pairs when using the antiwear antifrictional (AWAF)
composition, injected in the lubricating medium. The results show, that
Corresponding author: injection of the AWAF composition in the lubricating material does not
V.N. Duradji cause the changes in the microstructure and microhardness of the surface
National University of Science and of friction pairs, friction coefficient decreases in 1.5 2 times, the amount
Technology "MISiS", Leninskiy of wear of the rubbing parts is close to zero. The obtained effect is causes
prospect 4, 119049, by the establishing of the selective transfer process (wearless friction)
Moscow, Russia with the formation of the servovite film. Application of this composition
E-mail: vnduradji@mail.ru allows to improve efficiency of machines and equipment, considerably
reduce the content of CO and CH as well as solid impurities in the engine
exhaust gases, and reduce the running-in time of the diesel engines.
2016 Published by Faculty of Engineering

1. INTRODUCTION material, decreases the mutual penetration of

The diversity of part destruction types during
the friction is associated with number of
physical-chemical and mechanical processes in
the contact area, mainly, with environment,
friction conditions and applied constructional
and lubricating materials.
For a long time the main directions of the
struggle against wear and the decreasing of
friction forces was the increasing in the friction
surface hardness. At increase in hardness of the
one surface into another, plastic deformations
and oxidation processes reduce, as well as the
abrasive action. Many methods was developed
to increase the parts hardness: cementing,
chrome plating, nitriding, surface hardening,
hard-surfacing and other, that allowed to solve
many issues associated with increasing in
lifecycle of the machines and equipment [1,2].
However, the friction pair can be considered as a
thermodynamic system, where can be the
exchange of energy and substance between the

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 V.N. Duradji et al., Tribology in Industry Vol. 38, No. 4 (2016) 496-507
friction surfaces and the external environment
(lubricant), and consequently, the formation of
new structures based on self-organizing
processes is possible [3]. Based on this
phenomenon new metalplacking additives were
developed, which are injected into the lubricating
materials, reduce the friction energy costs and
significantly improve the wear resistance of the
rubbing parts of machined and mechanisms. To
this group of substances, apparently, can be
attributed antiwear antifriction composition
based on mineral serpentine.
Antiwear antifriction technology with its
physical nature and with its impact character on
the friction surfaces is one of the varieties of
methods to improve the wear resistance of the
machine parts, based on the effect of the
wearlessness during the implementation of the
selective transfer. The selective transfer a
special kind of friction, which is caused by the
spontaneous formation in the contact area of the
thin non-oxidizing metal film with low shear
resistance and incapable to the cold work
hardening. Such a protective film with thickness
1-4 microns is called servovite.
The formation of the servovite film during the
friction process is caused by its creative nature,
defined by the intensity of energy and matter
exchange between the friction unit and external
environment, as well as the collective behavior
of metal ions. The properties of the protective
servovite film, formed during the friction
process, are other than the original metal.
It should be noted, that during the friction the
parts contact on a very small area, which is 0.01-
0.001 of the nominal area of the mating surfaces.
As a result, the actual contact areas are
experiencing a very high stress, which leads to
their mutual penetration, plastic deformation,
and consequently, to the intensive wear. In case
of the selective transfer the contract of mating
surfaces is carried out through the actual contact
area and increased tenfold.
Known the metalplacking lubricants[3-5], whose
operating principle consists in forming in areas
of actual contact of the protective films based on
a soft metals (Cu, Sn, Pb, Zn and other), which
decrease the force impact and the wear intensity
of the mating surfaces. However, these materials
have a number of disadvantages (the
dependence of the film formation efficiency on
the concentration of metals in the environment,
low resistance of the dispersions of metal
powders, high purity powders, etc.), due to
which their application is mostly limited to
plastic lubricants for the certain friction units.
It is of interest to obtain cladding layers with
natural friction geomodifiers based on
serpentinite, and establish the possibility of
their use in the form of additives for lubricants:
in oils and lubricant greases.
2. EXPERIMENTS
Antiwear antifriction composition [6,7] it is
ultradispersive, multi-component mixture of the
minerals, additives, catalysts. The main raw
materials for its production are natural
materials of serpentinite group.
The decrease in the number of particles with
high hardness is obtained due to the fact that
after preliminary crushing and grinding of the
mineral with appropriate additives (particle size
0.1 0.2 mm) particles of magnetite, pyroxene,
and silica are removed from the mixture by an
electromagnetic selection. Then the remaining
part is mechanically crushed in the planetary
centrifugal mill, resulting in ultradispersive
powder (particle size up to 40 microns) with
phase composition given in Table 1.
Table 1. Phase composition of the antiwear
antifriction powder.
The identified Content,
Chemical formula
phase wt.%
Serpentine
(chrysotile and Mg6[Si4O10](OH)8 78-85
lizardite)
Chlorite (MgAlFe)2[(Si,Al)8O20](OH)16 2-3
Magnetite Fe3O4 1-2
Amakinite (Mg,Fe)(OH)2 1-2
Amphibole Ca2(Mg,Fe)5(Si,Al)8O22(OH)6 1.5-2
Calcite CaMg(CO3)2 0.5-1.0
X-ray amorphous
9-12
phase
AWAF composition is powder with the
dispersion: from 40 microns to 10 microns 15
%; from 10 microns to 1 micron 20 %, the rest
of the composition is less than 1 micron (Fig. 1 a,
b). This composition does not dissolve in oils and
other carriers and does not enter with them into
chemical reactions; does not change the viscosity
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 V.N. Duradji et al., Tribology in Industry Vol. 38, No. 4 (2016) 496-507
of the oil, due to its very low concentration in it
(0.05-0.1 g/l); it is not an abrasive material.
Harmless both in the initial state (powder) and in
the process of the running-in.
a)
b)
Fig. 1. a) AWAF structure, b) Combined spectrogram
of 4 spectrums.
Metallographic studies of friction pair surfaces
made from different metals (steel10 steel10,
St.45-St.45, St.45-bronze, St.45- aluminium alloy,
St.45-cast iron etc.) were carried out using a
microscope MIM-8 and microhardness PMT-3
with an increase from 500 to 1200-fold. These
studies were conducted both for initial samples
and for samples tested on the friction machine
using the consistent greases (Lithol-24, Buksol,
Solidol) and industrial oil I-20A with the
addition of antiwear antifriction compositions of
various concentrations from 0.05 to 1 %.
The obtaining of the tribological characteristics of
various friction pairs for various compositions
was partially carried out by means of friction
498
machine SMC-2 and mainly by means of friction
machine MTU-01. Universal friction machine
MTU-01 is intended for testing on friction and
wear of the metallic and non-metallic materials in
terms of the various lubricants application (oils
and plastic lubricants). A special feature of the
friction machine is usage of original friction unit
block in the friction installation, which allows
keeping the parallelism of the friction surfaces
during the operation, and to use as a drive a
commercially available bench-drilling machine.
The testing time varied from 1 to 8 hours. The
pressure on the friction pair was varied in the
range 1-5 MPa, the linear speed of rotating rollers
was varied from 1 to 2 m/s (1000 RPM for
consistent greases and 600 RPM for oils). The
friction torque was determined using the load
cell. The registered parameters were recorded
and processed using a PC. The change in weight of
the samples is determined by weighing on a
laboratory scales VLE134 and electronic scales
model Sartorius 1201. The surface quality was
controlled visually (the presence of scratches,
grooves and burrs) by means of the optical
microscope at a magnification of 100 to 500-fold.
As a friction pairs were used: plates made of
brass, steel 10, st. 45, an aluminium alloy, cast
iron SCh 24 (same as DIN 1691 GG-25) and
rollers made of steel 10 or St. 45 (hardened with
a hardness of 45-47 HRC). To measure the
surface roughness of the samples and parts of
diesel engine before and after the running-in
was used a profilometer mod. 201 factory
"Kalibr".
It is known that under the same cooling
conditions the temperature of the lubricating oil
is directly dependent on the temperature of
friction surfaces. Therefore, the change in the
temperature of friction surfaces was evaluated
by the temperature of lubricating oil using the
thermocouple chromel copel, which was
mounted in a PVC tube. The thermocouple was
connected to the potentiometer KSP-4.
The test of the running-in oil M-10DM with
AWAF composition was carried out on
overhauled diesel engines D-180. The test
engines were assembled from parts that have
the same size group. The inserts and CPG parts
were installed new. Tests were carried out on
the break-in-brake stand KI-5541M, designed
for running engines of this size.
 V.N. Duradji et al., Tribology in Industry Vol. 38, No. 4 (2016) 496-507
The running-in of the engines with pure oil M-
10DM is carried out in modes in accordance with
typical technology, and with AWAF composition in
modes of the experimental technology. To register
engine parameters the analyser of the pneumatic
density and tightness of cylinders AGC 2.
The experiments were performed with a scanning
electron microscope model VEGA2 TS 5136XM
running at high and low vacuum. Scanning
electron microscopes (SEM) series TESCAN
VEGA- fully controlled via a personal computer.
3. RESULTS AND DISCUSSIONS
3.1 Tribological properties of the antiwear
antifrictional composition
In the search for means to increase the wear
resistance of the machine parts, the selective
transfer during friction was discovered [3]. The
selective transfer a special kind of friction,
which is caused by the spontaneous formation in
the contact area of the thin non-oxidizing metal
film with low shear resistance and incapable to
the cold work hardening. On a film, in its turn,
the polymer film is being formed, which creates
additional antifrictional layer.
The complexity of the selective transfer consists
in a fact that numbers of its chemical and physical
processes are not found in practice of a friction
research. These include the processes occurring
in the servovite film, when the accumulation of
dislocations during its deformation is maintained
at a low level, thereby providing the wearlessness
of the contacting surfaces. Servovite film the
protective metal film, appearing at the initial
stage of the friction as a result of the selective
dissolution of the anodic components of the
material surface layer.
For the implementation of the selective transfer
in the friction pairs steel-steel, cast iron-steel,
etc. that do not contain film-forming material,
the metalplacking lubricating materials are used.
The metalplacking lubricant the class of the
lubricating materials, containing (by weight
from 0.1 to 10 %) additives: powder of metals,
alloys and their oxides, salts and complex
compounds of metals or organometallic
compounds, that release metal during the
decomposition in the friction area. The most
widespread metalplacking lubricating materials,
which form a copper, tin or lead servovite film.
The metalplacking lubricating materials by phase
characteristic are divided into homogeneous and
heterogeneous. The first ones as an additives
contain metal compounds soluble in a base
lubricating medium, the second ones contain
metal or its oxides in form of powder. However,
these materials have a number of disadvantages
(the dependence of the film formation efficiency
on the concentration of the metals in medium,
low resistance of the dispersions of metal
powder, high purity of the powders and other)
due to which their application is limited mainly to
the plastic lubricants for certain friction units.
In recent years, a number of technical solutions
appeared [4-9], according to which the layered
natural hydro silicates (serpentinite, talc,
serpentine, jade, dolomite and other) are used as
a filler of solid-lubricant compositions. The
presence of the powder of these compounds in
the lubricant composition under certain
conditions of its manufacturing and injection
between friction surfaces and their running-in
leads to the formation on the friction metal
surfaces of the protective film, which
significantly reduces their wear. Some authors
believe that the protective layer is a servovite
film [3,5]. Strength and antifrictional
characteristics of the servovite film depend in
particular on manufacturing conditions,
composition of the lubricating material, the
running-in after its injection between the
friction surfaces and their state, etc.
However, it is possible to assume that the
establishing mechanism of the selective transfer
(ST) process and formation of the servovite film
for the metalplacking additives and for antiwear
antifrictional (AWAF) composition is different.
Mechanochemical activation of the AWAF
composition in the planetary centrifugal mill
depending on the activation time, ultimately, can
lead to the formation of the nanoparticles of
such size, which are commensurate with the
crystal lattice parameters. Further dispersing
inevitably entails restructuring (change of the
crystal lattice, amorphization) with a
corresponding change of all thermodynamic
characteristics of the substance and its
reactivity.
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The presence of x-ray amorphous component
(Table 1) indicates the content in the AWAF
composition of nanoparticles with a developed
surface, having a high catalytic ability that
promotes the accelerated and efficient formation
of the servovite film. Besides, nanoparticles of
less than 100 nm are held in the liquid
(lubricating material) by the Brownian motion
that promotes the more efficient use of the
AWAF composition, by reducing the
concentration of injected powder, since a
smaller portion is precipitated by gravitational
forces or retained in the fine filter.
It should be noted, that there is an optimal time of
the mechanical activation depending on the
number of parameters: design of the mill,
material and diameter and mass of the balls,
amount of the load, rotation frequency, the
medium, where the activatable composition
located and the like. With further increase in
processing time, the nanoparticles aggregation
starts or the substance destruction will occur
(mechanolysis, mechanical cracking, dissociation,
etc.). When the ultrafine grinding occurs, the
original mineral ceases to exist in its original
structure or chemical composition, turning into a
new substance with the different properties,
structure and even elemental composition.
The AWAF composition particles (due to the
property the perfect cleavage) are splitted as
long as do not form nanoparticles sols. This is
liquid colloidal systems with particles of the
dispersed phase freely and independently from
each other moving during the process of
Brownian motion. In the friction area under the
action of electrostatic forces, they reach the
metal surface. It can be assumed, that because of
the mechanochemical reactions at the friction
surface, the self-organizing protective layer is
formed the servovite film.
Carrying out of tribological tests for lubricant
greases using as a base: Litol-24, Solidol-G,
Vaseline etc. (made by different companies) is
complicated by the fact that all these lubricants
contain various additives, sometimes abrasive
particles, as a result the wear amount during 1-
hour testing period can range from 3-4 mg up to
100 mg. In this connection, we cant clearly
determine what the reason of the obtained
negative result is: it is a lubricant composition or
it is an added composition. Best unequivocal
500
results are obtained when using as the base
lubricating medium the natural lubricant
Soliton, which does not contain any extraneous
additives. The amount of wear of the friction
pairs in this medium is 4.0 mg for the plate (steel
10) and 6.0 mg for the roller (steel 10). The
nature of the friction coefficient change with
time under load 160 N is presented on Fig. 2.
Fig. 2. Friction coefficient oscillograms: 1 lubricant
Soliton, 2 lubricant Soliton with AWAF.
In studying the effect of concentration values of
the antiwear antifrictional composition in the
lubricant grease on the tribological
characteristics, its concentration varied from 2
to 30 %. Research show that the increase in
concentration more than 10 % leads to the
increase in wear values and when concentration
is 30 % the abrasive effect is being observed.
Possible, that in real mechanisms the
composition is not so intensely gets into a
friction area as in the friction machine and it is
possible to use such concentrations. In further,
the research was carried out with AWAF
concentration in the lubricant grease 1-5 %.
Experiments show that in case of using Soliton
as a base lubricant the friction coefficient
decreases and its value is 0.6-0.8 from the
friction coefficient of the clean lubricant (Fig. 2).
Besides, on the plate surface, apparently, the
protective coating is formed, since no wear been
observed, but stable gain of the plate within 1-
1.5 mg, i.e. of 0.8-1.3 mg/cm2, this means that
the thickness of the protective layer can be 1.5-3
microns. This effect was obtained for all
researched compositions. In work [10], on a
friction surfaces by means of the electronic
microscopy revealed the presence of the
protective film with the thickness about 6
microns having a non-metallic character.
The dependence of the mass change of friction
pairs: the rollers and the plate using lubricating
 V.N. Duradji et al., Tribology in Industry Vol. 38, No. 4 (2016) 496-507
medium oil I-20A, from the concentration of
the injected composition varying from 0.008 to
0.06 % under the load 160 N are shown on a Fig.
3. In these cases, the weight gain of the rotating
part (rollers) is observed. At that with increase
in the concentration of AWAF composition up to
0.048% the weight gain of the roller is observed,
but at further increase in the concentration the
value of the weight gain decreases, tending to
zero. For the second counter body (the plate),
the weight change with increasing concentration
of powder in oil up to 0.048 % is almost not
observed. With increasing concentration of the
AWAF composition, more than 0.05 % the value
of the plate wear begins to grow noticeably.
Fig. 3. Weight change of the roller (1) and plate (2)
depending on the concentration of the AWAF
composition (the friction pair steel10 steel10).
Fig. 4. Weight change of the roller (1) and plate (2)
depending on the processing time (the friction pair
steel10 steel10).
Fig. 5. Friction coefficient oscillograms: 1 oil I-20A;
2 oil I-20A with AWAF composition (the friction
pair steel10 steel10).
The conducted research of the wear amount
(Fig. 4) and friction coefficient (Fig. 5) from the
running time of friction pairs show that major
changes on the friction surfaces occur mainly
during the first hour of work, during which the
formation of a protective (servovite) layer occur,
and in further the weight of samples (roller and
plate) remains unchanged.
The antiwear antifrictional nanodispersed
(AWAF) composition, getting together with an
oil or lubricant grease on the friction surfaces of
parts, initiate the formation process on the
friction surfaces of the modified coating with
high wear resistance and low friction coefficient.
Thus, during the process of interaction of the
AWAF composition with friction surfaces the
value of gap between the rubbing parts
gradually stabilizes and approaches the optimal
over the entire area of contact spots.
The resulting nanoparticle of the AWAF
composition, apparently, have the enhanced
catalytic ability, the increased reactivity and the
excessive electric charge due to which they dont
leave the friction area and concentrate on the
metal surfaces of friction units.
One would assume that effect of the selective
transfer caused not by the physic-chemical
properties of the composition, but due to a size
of the particles forming the composition. Thus, if
the particles of some substance become
commensurable with nanoparticles, then this
substance could realize the process of selective
transfer. To check this assumption the
tribotechnical tests of lubricating substances
were conducted with addition of the
nanopowders (particle size less than 100 nm),
boehmite (AlOOH), talcum powder, cobalt,
carbon nanofiber and other. However, there
were not such effect of decrease in the friction
coefficient and decrease in the value of wear as
with antiwear antifrictional repair-regenerative
composition. This means that effect of the
selective transfer is caused by the unique physic-
chemical properties of this composition.
As mentioned above, modified coatings with
high wear resistance and low friction coefficient
are formed on the metal surfaces of the friction
pairs and the effect of the selective transfer is
being observed. In order to establish whether
these properties decisive in the phenomenon of
the friction coefficient reduction and the wear
amount reduction, the tribotechnical tests of the
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friction pairs were conducted in accordance with
the following scheme: 1 during 4 hours the
friction pair worked in the lubricating
environment containing antiwear antifrictional
composition; 2 then the lubricating
environment was replaced by the pure oil and
alternately every hour, keeping the friction
surface unchanged, the friction coefficient and
the amount of wear were measured. The tests
have shown that after the replacement of oil
containing AWAF composition with the pure oil
the protective (servovite) layer is retained on
the friction surfaces, the friction coefficient and
the amount of wear were slightly different from
the values they had directly after work in the
lubricating environment containing antiwear
antifrictional composition. These results are
confirmed in practice: in particular, car engines
with lubricant containing antiwear antifrictional
composition retained technical indicators for 50-
80 thousand kilometres, despite the fact that a
planned oil change was carried out every 10
thousand kilometres. It means that this
composition is not simply identical to the solid
lubricants, but related to the effect of selective
transfer (wearless friction).
It is natural, that conducted metallographic
studies of the friction surfaces and tribological
tests are not enough to create action models of
antiwear antifrictional composition. However,
the conducted research allow to make a
conclusion that with the injection of this
composition into a lubricating medium the self-
organizing protective (servovite) film specific to
the selective transfer (wearless friction) is
formed on the friction surfaces. The theory of
this process is sufficiently developed for
metalplacking additives [3,5,11-19], but for this
moment there is no such theory for the additives
based on the minerals.
3.2 Application of the AWAF composition for
the treatment of motor transport engines
In recent years, dramatically exacerbated the
problem of environmental protection, especially
in large cities, where concentrated tens of
millions of vehicles. The content of harmful
components in the exhaust gases increases
during the operation of the worn internal
combustion engines, leaking oil through the
faulty seals result in contamination of
agricultural land, decline in the quantity and
502
quality of received production, growth of
diseases of people and animals, other adverse
effects. Besides, usage of the low quality oil and
fuel leads to additional wear of the friction pairs,
power reduction, increased fuel consumption, oil
burnout, and reduction of the vehicle
exploitation efficiency as a whole.
The antifrictional additives provide guaranteed
fuel economy by reducing mechanical friction loss
and a corresponding increase in efficiency of the
motor. They are most effective when the
boundary friction mode, for example, between
the compression piston rings and cylinders close
to the upper dead points. Their advantage is their
efficiency, both at low and at high temperatures.
The protective antifrictional layer, which
formation is caused by the physic-chemical
composition of the injected additive, could have
various structures, providing the significant
decrease in the friction coefficient and the
amount of wear. At that with the increase in the
operating time of the friction unit, the friction
coefficient tends to the value 0.03 0.04 and the
amount of wear tends to zero.
However, along with these indicators the
operating results should be considered. For
example, for the metalplacking compositions it is
necessary to inject next portion after each
lubricating medium replacement. In addition,
after prolonged use occurs stripping of the
protective layer from the friction surface. It
should also be taken into account that
metalplacking compositions are deposited not
only on the friction surface, but also on the
closed cavities [4].
The polymerized substances are characterized
by the rapid onset of the effect of the friction
coefficient reduction. However, the Teflon
coating, during the process of friction unit
operation, is being saturated with fine products
of wear and works in further as an abrasive [4].
The uses of preparations based on molybdenum
disulphide significantly increase the sulphate
ash content of engine oils exceeding the
permissible limits. It should be taken into
account that the use of halogen compounds in
the lubricants promotes the formation of acids,
which increase the acid number of the base
lubricant and, hence, its corrosivity.
 V.N. Duradji et al., Tribology in Industry Vol. 38, No. 4 (2016) 496-507

Application of the antiwear antifrictional Table 3. The results of processing engine of Opel
composition [7] allows getting on the friction Astra car.
surfaces the protective layer, which persists Opel
Car
when the vehicle mileage is 50 thousand Astra
kilometres and more, i.e. during several Full mileage 106540 106632 106900 107870
replacements of oil in the internal combustion Mileage after
92 360 1330
engines. Let us consider some of the results of application
the processing of automobile engines. Oil level MAX MAX MAX-0,2 kg MAX-0,5 kg
Compression
Application of the antiwear antifrictional 1 9 14.4 14.9 14.9
composition is accomplished by direct addition 2 6.5 14.4 14.8 15.3
into the engine according to the required 3 12.5 14.4 14.8 15.2
concentration (the calculation is carried out 4 14.4 14.4 14.9 15.3
depending on the quantity of the lubricant and Exhaust
oil in the engine). Then you can immediately gases
continue the exploitation in the normal mode The gas
55 C 55 C 55 C 55 C
temperature
without any restrictions.
CO 1.2-1.7 % 0.06 % 0.06 % 0.00 %
CO2 14 % 14 % 13.70 % 14 %
Processing of the internal combustion engine
O2 0.48 % 0.25 % 1.20 % 0.51 %
with the antiwear antifriction composition was
carried out according to the scheme: - warm up
to the operating temperature, - taking of The engine processing with the antiwear
testimony of the engine parameters; - processing antifrictional composition leads not only to wear
of the engine with the repair-regenerative reduction of the parts, but also to the certain
composition; - running-in at least 500 km; taking stabilization of gaps. Especially it concerns the
of testimony of the parameters. Technical cylinder-piston group and the crank mechanism.
condition of these engines corresponds to the This in turn leads to a decrease in the impact
category of the technical condition "acceptable". intensity of the parts and, consequently, to
Measured parameters in the process of diagnosis noisiness reduction.
for several types of vehicles are shown in Tables
2 and 3. As known, one of the main sources of the engine
wear is the start-up mode, especially at low
Table 2. The values of compression in cylinders for temperatures. The engine processing with the
the engine TATRA 815 (air-cooled). antiwear antifrictional composition simplifies the
cold start conditions, due to the reduction of
Cylinder 1 2 3 4 5 6 7 8 9 10
power losses to overcome the friction forces, and
Compressio reduced start-up time. In addition, the growth of
n before
the compression also facilitates start of the
20.0
22.5

20.0

22.5

20.5

24.0
22.0
23.0
22.0

24.0

treatment,
kg/cm2 engine. This has a positive effect on reducing the
After treatment wear of all interfaces of the friction units.
Compressio
n, kg/cm 2, 3.3 Application of the AWAF composition for
running-in of the vehicle engines
25.0

23.0

25.0

23.5
24.0
25.0
25.0
24.5
24.5

25.0

mileage
2 500 km
Compressio Carrying out the running-in of the vehicle
n, kg/cm 2, aggregates, such as internal combustion engine
27.0

26.0

27.5

24.5
27.0
26.0
26.0
27.0
27.0

28.0

mileage 30 and elements of the transmission, is caused by the

000 km presence of defects in the manufacture and
Compressio assembly of parts and components leading to the
n kg/cm 2, grasp of the friction surfaces and the possible
29.0

29.0

30.0

30.0
30.0
29.0
29.0
29.0
29.0

29.3

mileage 95 appearance of burrs on them and also the need to

000 km identify possible hidden manufacturing defects.

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 V.N. Duradji et al., Tribology in Industry Vol. 38, No. 4 (2016) 496-507
It is known, that most of the vehicle dont need
the operational running-in, however, for some of
them it is mandatory process step both at
automotive factories and repair shops. The
necessity of the running-in, as a technology
operation, is caused by the fact that even when
the perfect assembly and accordance of the
waviness and roughness of working surfaces to
the drawings requirements, almost impossible in
other process steps to achieve optimal
tribological properties of the surface layers of
friction parts. Running-in largely determines the
reliability of a diesel engine, especially in the
initial period of operation and at a minimum of
the running-in and steady-state wear of the
tribological connections provides the increase of
the diesel engine resource.
For the diesel engine, the duration of running-in
is 30-40 machine hours or about 5000 km of
mileage for the vehicle. The development of
mechanical engineering indicates the need to
accelerate this process and reduce it to 2-3 min.,
necessary to control the operability of the
product and identify possible hidden defects.
When the running-in there is a change in
geometry of friction surfaces and physico-
mechanical properties of surface layers of
materials during the initial period of friction,
manifested under constant ambient conditions
and consist in reducing friction, temperature and
wear rate. Running-in of the parts is carried out at
the automotive factories and repair shops in the
process of bench testing and in households -
consumers during the operational running-in. It
should be understood that almost any
disassembly of rubbing joints leads to necessity of
carrying out operations of running-in of the
reassembled unit with loss of a part of interrepair
resource on the running-in wear. The application
of the running-in preparations will not only allow
to reach faster the normal operation mode
(reduce the running-in time) but also significantly
increase the overhaul life of machinery units
(improve the quality of running-in).
Adding the AWAF composition in the oil M-
10DM contributes to the acceleration of the
running-in and improvement of the quality of
the run-in surface, since this composition
contains the most effective components of
lubricating and plastically-deformable action -
the serpentine and magnetite. When the
504
temperature of friction surfaces increases over
473 K (hot running-in) the serpentine forms on
the friction surfaces, in places of their contact, a
thin antifriction film which is able to withstand a
higher load than the lubricating film of mineral
oil. At that, the contacting irregularities are not
cut off, but plastically deform under a film of the
serpentine. The force and temperature of
friction significantly decrease.
The presence of the hard magnetite particles in oil
should lead to the intensive wear of the friction
surfaces. However, small abrasive particles dont
intensify wear, but also inhibit to it [15]. In some
cases, the particle size of less than 5 microns is
considered safe and even beneficial. This is due to
the polishing effect. Mechanical impurities
contained in the used oil, wherein the dispersant
effect of the additives is weakened, represent
complexes, in the centre of which are located the
solid abrasive particles coated with a multilayer
colloid protection consisting of the polar-active oil
oxidation products. The positive impact of these
particles is manifested in the fact that they
intensify heat transfer between the friction
surfaces, increase the electrical conductivity of the
oil film and eliminate the roughness on the surface.
Furthermore, the micro abrasive enhances physic-
chemical processes in the friction area, causing
slight deformation of the surface layers and the
formation of new surfaces, which are active sites
for chemical reactions and diffusion processes. The
presence of the micro abrasive particles up to 1.5
% in the lubricating oil decreases the friction
coefficient, accelerates the formation of the
optimal micro relief on the entire contact area.
The quality of the running-in is estimated also
by the intensity of surface roughness change
depending on the test time. It is known, that the
initial surface roughness of the rubbing parts
becomes operational roughness. The formation
of the operational roughness is influenced by a
complex set of different kinds of mechanical,
physic-chemical, electro-chemical and other
processes occurring in the contact between two
rubbing bodies. Therefore, in the work was
studied the surface roughness of the friction pair
"piston ring - cylinder liner" using the studied
running-in oils as a lubricant. The initial
roughness of the friction surfaces of both
samples (roller, plate) Ra = 0.63 microns. Fig. 6
shows the profilograms of samples surfaces
before and after running-in.
 V.N. Duradji et al., Tribology in Industry Vol. 38, No. 4 (2016) 496-507

Before running-in:

b)
After running-in on pure oil M-10DM:
Fig. 7. a) sample surface, run-in on oil M-10DM, b)
the spectrogram of the sample surface, run-in on oil
M-10DM.

After running-in on oil M-10DM with AWAF

composition:

a)
Fig. 6. The profilograms of friction surfaces of the
parts samples.

b)
Fig. 8. a) Sample surface, run-in on oil M-10DM with
AWAF composition, b) The spectrogram of the sample
surface, run-in on oil M-10DM with AWAF composition.

The best results obtained on the oil M-10DM

with AWAF composition. Thus, the roughness
a) stabilized after a 30 minute test on the value of

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 V.N. Duradji et al., Tribology in Industry Vol. 38, No. 4 (2016) 496-507
Ra = 0.14 microns, which is 60 % less than with
pure oil M-10DM. Within 15-20 minutes of the
tests, takes place the plastic smoothing of the
roughness peaks up to the platforms, which
gives a better distribution of the load and the
reduction of the actual pressure between the
rubbing pairs. The nature of changes in these
parameters shows that the running-in process
takes place under more favourable conditions
and completes much earlier as compared to pure
operating oil, i.e. serpentine and magnetite,
which are included in the AWAF composition
allow to speed up the running-in process of
parts and get higher physical and mechanical
properties of the friction surfaces.
In studying the sample surfaces, lapped in the
oil M-10DM with AWAF composition, it was
found the presence of a metal-ceramic layer.
This fact is confirmed by the X-ray
microstructure analysis of the surface (Figs. 7
(a, b) and 8 (a, b)), which shows that the sample
surface consists of iron, magnesium, silicon,
and carbon. The presence of such elements as
magnesium and silicon indicates that the
elements of the AWAF composition bind to the
surface of the running-in sample.
4. CONCLUSION
As a result of the X-ray spectral, metallographic
analysis and tribological tests of the friction
units using the lubricating materials containing
the antiwear antifrictional composition, it is
established that no hardened layers with high
hardness is formed on the friction surfaces.
Injection of the AWAF composition in the
lubricating material does not cause changes of
the microstructure and the microhardness of the
surfaces of friction pairs, wherein the friction
coefficient is reduced in 1.5-2 times, amount of
wear of the rubbing parts is close to zero. We
consider that the resulting effect is mainly
caused by the establishment of the process of
selective transfer (wearless friction) with
formation of the servovite film.
Thus, in order to establish the process of
selective transfer (wearless friction) using the
metalplacking additives it is necessary to pick up
their composition so that the particles were in a
dissolved state, then using the antiwear
antifrictional composition based on the layered
506
silicates this requirement is eliminated and it is
possible to inject them into any lubricating
medium.
REFERENCES
[1] Thermochemical treatment of metals and alloys
/ ed. Lyakhovich L.S. M.: Metallurgy, 1981. (on
Russian)
[2] A.N. Minkevich, Thermochemical treatment of
metals and alloys. M.: Mechanical Engineering,
1965. (on Russian)
[3] D.N. Garkunov, Tribotechnology (wear and
wearless friction). M.: Publishing House of the
Moscow Agricultural Academy, 2001. (on
Russian)
[4] V.I. Balabanov, In-place recovery of rubbing joints
of the car. M.: AST. 2014. (on Russian)
[5] P.B. Aratsky and A.G. Kapsarov, 'Application of
geo modifiers of friction for metalworking tools',
Friction, wear and lubrication, no. 3, p. 73-80,
2003. (on Russian)
[6] Patent of the Russian Federation. # 2243252,
2004. (on Russian)
[7] Patent of the Russian Federation. # 2313565,
2007. (on Russian)
[8] R.G. Nigmatullin, B.Y. Sholom, L.S. Shuster and
I.M. Nigmatullin, 'Improving the efficiency of
lubricants with friction geomodificators',
Bulletin USATU, vol. 16, no. 1, . 27-32, 2012.
(on Russian)
[9] V.V. Usachev, L.I. Pogodaev, D.M. Teluh and V.N.
Kuzmin, 'Introduction to the problem of natural
layered geomodifiers in friction units', Friction
and lubrication in the machines and mechanisms,
no. 1, p. 36-42, 2010. (on Russian)
[10] V.N. Polovinkin, V.B. Lannoy and Y.G. Lavrov,
'Antifrictional antiwear additive in lubricants of
mineral origin (friction geomodifiers)', Friction,
wear and lubrication, no. 3, p. 65-72, 2003. (on
Russian)
[11] V.N. Polovinkin, Y.G. Lavrov and P.B. Aratsky,
'Application of friction geomodifiers to restore
worn-out surfaces of friction units during
operation', Friction, wear and lubrication, no. 4,
p. 55-62, 2003. (on Russian)
[12] A.A. Polyakov, 'To the question about lab testing
of materials of friction units', Friction and wear,
no. 6, . 668-674, 2000. (on Russian)
[13] A.A. Polyakov and F.I. Ruzanov, Friction based on
self-organization. M.: Science. 1992. (on Russian)
 V.N. Duradji et al., Tribology in Industry Vol. 38, No. 4 (2016) 496-507
[14] A.S. Kuzharov, 'Physic-chemical principles of
lubricating action in the regime of selective
transfer', The effect of wearless friction and
tribology, no. 2, . 3-11, 1992. (on Russian)
[15] L.I. Pogodaev, S.N. Dmitriev and V.V. Usachev,
'Basics of technology of final strengthening
processing of parts', The problems of the
mechanical engineering and reliability of
machines, no. 4, p. 79-89, 2006. (on Russian)
[16] Y.A. Radin and P.G. Suslov, Wearlessness of
machine parts during friction. L.: Mechanical
engineering, 1989. (on Russian)
[17] V.G. Volkov, K.A. Pavlov, Y.P. Toporov and other.
'Tribological modifiers based on natural
silicates', The effect of the wearless friction and
tribology, no. 2, . 46-49, 2003. (on Russian)
[18] M.A. Chowdhury and D.M. Nuruzzaman.
'Experimental Investigation on Friction and
Wear Properties of Different Steel Materials',
Tribology in Industry, vol. 35, no. 1, pp. 42-50,
2013.
[19] O.N. Tsvetkov, 'Tribology in the oils science',
Friction and lubrication in the machines and
mechanisms, no. 5, pp. 45-49, 2015. (on Russian)
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Tribology in Industry

RESEARCH
www.tribology.fink.rs

Wear and Friction Behavior of Stir Cast Al-TiB2

Metal Matrix Composites with Various Lubricants

S. Poria a,b, G. Sutradhar a, P. Sahoo a, b

a Departmentof Mechanical Engineering, Jadavpur University, Kolkata 700032, India,
bCentre of Excellence on Phase Transformation and Product Characterization, TEQIP-II, Jadavpur University,
Kolkata 700032, India.

Keywords: ABSTRACT
Al-TiB2
Al- TiB2 metal matrix composites are fabricated using stir cast method
Metal matrix composites and its tribological characterization is done using three different
Wear lubricants. Tribological studies are performed in a multi-tribotester
Coefficient of friction using block-on-roller configuration under 25-75 N loads and 400-600
Lubricant rpm rotational speeds. Four different weight percentages of TiB2 are
considered in this study. Comparison between dry condition and
Corresponding author: lubricated conditions is gleaned to differentiate wear and friction
characteristics and SEM images are taken to fortify them. Lubricated
Prasanta Sahoo conditions yield large reduction in wear and friction compared to dry
Department of Mechanical Engineering, condition.
Jadavpur University, Kolkata 700032,
India. 2016 Published by Faculty of Engineering
E-mail: psjume@gmail.com

1. INTRODUCTION industry and also in chemical and transportation

Aluminum alloy based ceramic particulates
reinforced metal matrix composites are active
area of research for last few years [1-3]. The
reason behind wide acceptance of metal matrix
composites as engineering materials is the
excellent combinations of properties which are
difficult to achieve by individual alloy phase or
particulates. Metal matrix composites are mainly
combination of two or more phases among
which base one is metallic alloy based matrix
phase and reinforcements are ceramic type
particulates or short fiber or whisker [4-6].
Applications of MMCs are established in
aerospace industry, automobile industry, marine
industries [7-8]. As one of the onerous
yardsticks in new age materials is good strength
to weight ratio combined with high wear
resistance, soul aluminum alloys are lagging
behind aluminum based metal matrix
composites in terms of industry usage focus on
materials [9-12]. Various literatures reveal that
aluminum alloy based metal matrix composites
show better hardness, Youngs modulus, yield
strength, ultimate tensile strength and wear
resistance in comparison to other alloy i.e. Mg,
Cu based metal matrix composites [13].
Considering all of these properties aluminum
based metal matrix composites are gradually
becoming potential alternative materials in

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 S. Poria et al., Tribology in Industry Vol. 38, No. 4 (2016) 508-521
connecting rods, cylinder blocks, gears, shafts
etc. [14-15].
In spite of all great potentials of metal matrix
composites, main challenge is to get proper
uniformity of the phases in composites and
accepted compatibility between matrix and
reinforcement. Thats why selection of
fabrication process and also reinforcement is
indispensable task to get proper enhancement in
the properties of MMCs. Powder metallurgy,
liquid metallurgy techniques, in-situ techniques
and chemical synthesis are the methods
normally used for synthesis of MMCs [16].
Several opinions exist on which techniques are
most preferable for fabrication of MMCs. For
selection of reinforcement, ceramic particulates
are popular as several literatures delineate the
enhancement of mechanical and tribological
properties due to incorporation of ceramic
particulates in MMCs [1, 17-18]. SiC, TiC, ZrC,
TiB2, ZrB2, AlN, Al2O3, B4C, TiC are the ceramic
particulates commonly used to intensify the
characteristics of aluminum based metal matrix
composites [1,19-20]. Thermodynamic stability
in matrix phase, solubility in molten metal, grain
boundary regime near to the metallic atoms are
the characteristics of reinforcement responsible
for determining the properties of MMCs.
TiB2 particulate is chosen in this work as
reinforcement in aluminum alloy based matrix
due to properties like high Youngs Modulus
(345-409 GPa), low specific gravity (4.5), good
hardness (3400HV), high melting point (3225
C), good thermal stability and good thermal and
electrical conductivity [21-22]. TiB2 also
enhances mechanical and tribological properties
of aluminum matrix composites in a
deterministic way [22-23]. TiB2 does not react
with aluminum which also helps not to lead to
any interface product with detrimental effect on
behavior [24]. SiC reinforced aluminum metal
matrix composites are absorbing larger
percentage of commercially available MMCs but
in this case formation of aluminum carbide
(Al4C3) reduces physical, mechanical and
chemical properties of the composites [25]. TiB2
reinforcement is free from this problem and TiB2
acts also as a nucleating agent at the grain
boundary of aluminum alloy and TiB2 grains [2].
It is widely reported in various literatures that
fabrication of Al- TiB2 MMCs through in-situ
methods are advantageous and popular due to
several reasons [22-23,26]. But agglomeration
behavior of TiB2 particles segregates the grain
boundary and weakens the inter-atomic force
which is very much detrimental in functional
output [27]. Some additives, e.g., CeO2, Mg, Zr
are used within the matrix to solve out the
problem of agglomeration [27-28]. In case of in-
situ techniques, production of reinforcement
happens by exothermic behavior which also can
be negatively effective on the grain boundary
regime of MMC [29]. To overcome these
problems and also to make the fabrication
processes more simple, flexible and economical
for commercial purpose, stir casting method is
introduced [30]. Stir-casting method is basically
an ex-situ method where reinforcement
particles are prepared externally and poured
into the molten metal. Stir casting methods are
also helpful to break the dendritic structures
already present in the molten aluminum alloy
which lead to better mechanical strength than
original alloy excepting the effect of
reinforcement. Some problems associated with
this method like non-uniform distribution of
particles and porosity can be addressed easily by
controlling stirring process, lower particle size
of TiB2, preheating of the particles and molding
techniques [7, 30]. Recent literatures on Al- TiB2
composites reveal that stir casting method has
been accepted widely as the mode of fabrication
of MMCs including Al- TiB2 MMC [7,10,31].
Al-TiB2 MMC fabricated through stir casting
method is the working material in this study. As
tribological properties are one of the important
considerations of Al- TiB2 MMCs, miscellaneous
works are found on this topic. Some works are
also available considering mechanical behaviors
of specified composites and comparison with
others [12,13]. But most of the works are based
on in-situ stir cast Al- TiB2 composites. With
increase of weight percentage of TiB2 in in-situ
composite, wear resistance increases in case of
dry wear, sliding wear, abrasive wear, and
erosive wear [22,26,32-33,]. Effect of grain
refinement, surface roughness and in-situ
reaction parameters on wear behavior of Al-
TiB2 composites are also studied [34]. How wear
trend varies in elevated temperature is also
reported [34]. Characterization of in-situ
fabricated specific composites is also available in
good numbers. But reports on characterization
and tribological trends of stir cast Al- TiB2
composites are really scanty [31]. All composites
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 S. Poria et al., Tribology in Industry Vol. 38, No. 4 (2016) 508-521
including Al- TiB2 have been studied to find out
the inclination of wear and coefficient of friction
on applied load, and weight percentage mostly
in dry condition. Characterization of composites
and other new age materials, e.g., polymide
composites, Al2O3f/SiCP/Al hybrid MMCs except
Al- TiB2 composites is also available in various
lubricated conditions. But it is difficult to find an
analysis of tribological trends of stir-cast Al- TiB2
MMC in various lubricated conditions or a
systematic approach to characterize tribological
parameters in various lubricated conditions in
comparison with dry condition.
There are many potential areas where Al- TiB2
composites can be used for sliding and rolling
applications. In that case lubricants also can be
used for bringing the tribological parameters in
favor. These tribological parameters are
definitely influenced by the nature of the
lubricant because most of the loads in contact
surface of sliding are carried out by the pressure
regime generated within lubricant film. So, it is
needed to improve the understanding of the
tribological behavior of Al- TiB2 composites under
lubricated contacts. It is reported that maximum
percentage of lubricant is based on petroleum
and they ended up in environment which leads to
increment of toxicity in nature [35]. To overcome
this issue of petroleum based lubricants on
environment, vegetable oils based lubricants are
becoming the alternative now a days [36].
Triacyglycerol structure presents in natural oil
which is an important aspect as lubricant because
it contains long chains of polar fatty acids which
adheres to metallic surfaces [37]. Length of
carbon chain present in the fatty acids also can
affect the friction nature of the contacting
surfaces [37]. Many researchers have paid their
attention to various bio-diesel based lubricants
derived from vegetable oils, e.g., rapeseed oil,
canola oil, soy oil, sunflower oil, rice bran oil [38].
As a part of the research on bio-diesel based
lubricants and additives used on it, it is also
concluded by some researchers that individual
fatty acid esters are not so much effective as
methyl esters derived from fatty acids are
effective in reducing friction [39]. Works on bio-
esters and their effects on engines as diesel and
as lubricant are going on but some clear
understandings are also needed on their
behaviors in contact surfaces of newly developed
materials to develop the potentiality of real time
applications for both the materials and the bio-
510
lubricants also [40]. Works on tribological
behaviors under various types of bio-lubricants
and on metal matrix composites are really scanty
[1]. Some works are reported on aluminum
matrix composites in air and water lubricated
condition in direction to opt out detrimental
effects of commercial lubricant on environment
[41]. Some works are also reported on in-situ Al-
TiB2 composites in hydrocarbon based synthetic
lubricated condition [42]. In case of many
practical applications it is difficult to use water as
lubricant. In this work, one commercial synthetic
petroleum based lubricant, one commercial
Chloro-fluro-Carbon free lubricant based on
petroleum oil but blended with natural oil and
one vegetable oil based bio-lubricant are used to
understand the contact surface behavior and
tribological parameters of stir cast Al- TiB2
composites in lubricated condition. Contribution
of various bio-diesel contaminated bio lubricants
on contact surface are not well studied though a
good number of works are carried out on
characterization of bio-lubricants. Other than two
commercially available lubricants, Rice bran oil
based methyl ester is chosen for development
and usage as bio-lubricant in this study due to
some advantages as the wear resistant properties
of rice bran oil is less in comparison with other
vegetable oils because of the presence of natural
anti oxidants like gamma oryzanol and
tocopherols. Rice bran oil is thermally stable at
high temperature i.e. 395 0C without any mass
degradation and also methyl esters are more
effective for reduction of friction [43].
In this work, tribological tests on stir-cast Al-
TiB2 composites are performed in Multi-
tribotester for various loads, speeds, and weight
percentages of TiB2 using three different
lubricants. SEM images are taken after
tribological tests to characterize the worn out
surfaces in lubricated contact and to compare
the tribological characteristics of Al-TiB2 MMC
under lubricated sliding from dry contact
conditions.
2. EXPERIMENTAL PROCEDURE
2.1 Sample preparation
Stir casting process is used in this study for
fabrication of Al-TiB2 composites. Average
particle size of TiB2 varies from 5 m to 40 m.
 S. Poria et al., Tribology in Industry Vol. 38, No. 4 (2016) 508-521

Base alloy used as matrix phase is LM4. Chemical layer over the particles [31]. Diagram of this
composition of LM4 alloy and TiB2 particulates total process is shown in Fig. 1. After ensuring
are given in Table 1 and Table 2. overall equal distribution of particles, the
mixture of molten metal and TiB2 particulates
Table 1. Chemical composition of LM4 alloy. poured into a fixed size metallic mould at fixed
Element Cu Si Mg Fe Mn Ni Zn Al temperature 800 C. Then it solidifies and with
wt% 3.2 6 0.05 0.6 0.4 0.2 0.15 Rest repetition of the same process four different
weight percentages (1 %, 2.5 %, 4 %, and 5.5 %)
Table 2. Chemical composition of TiB2 powder. of TiB2 reinforced composites are prepared.
Element Ti B C O N Fe
2.2 Lubricants used
wt% 67-69 29-32 0.5 0.5 0.2 0.09
Three different liquid lubricants are used in this
study. Petroleum based commercial lubricant is
SAE20W-40 procured from Indian Oil
Corporation Limited. This commercial lubricant
is based on high refined petroleum stocks with
well balanced group of additives. Similar type
lubricant is used previously by researchers to
find out boundary lubricated tribology of an
aluminumsilicon alloy sliding against steel [44].

Other commercial lubricant (Chain Lube Oil) is

collected from a Germany based company (OKS).
This liquid lubricant is based on refined
petroleum oil but blended with some additives
collected from natural mineral oil. This lubricant
is free from chloro-fluro-carbon (CFC) which is
healthy for environment in heated condition.
Similar type of lubricant has been used
previously to characterize Ni-P coatings [45].
Properties of SAE20W-40 and chain lube oil are
listed in Table 3.

Table 3. Properties of SAE20W-40 and Chain lube oil.

Viscosity Flash
Lubricant Viscosity Density
Index Point
13.5-15.5 cSt
SAE20W- 0.8-0.9
@100 0C 132 200 0C
40 g/ml
Fig. 1. Stir casting system used for fabrication. (ASTM D445)
Chain lube 300 cSt @40 0C
0.9 g/ml 320 164 0C
To get proper homogeneous distribution of oil (DIN 51 562-1)
particles over the matrix phase, an electric
stirrer controlled by speedometer is connected One bio-lubricant (Rice bran oil based TMP
with Electric Resistance Arc Furnace. LM4 ingots Ester) is formed in laboratory according to the
are first placed in the furnace and got molten. standard process [43]. The crude rice bran oil is
TiB2 particles preheated at 600 C are poured purchased from local industries in Kolkata. This
into the vortex of the molten LM4 alloy. String crude oil is first heated to a temperature 110C
speed is kept fixed at 500 rpm for 15 minutes. and then mixed with a methanolic solution
Stirring of molten LM4 alloy helps to break which is also prepared by properly mixing
dendritic structure if present inside and leads to methanol and KOH according to fixed molar
better micro-structural unity in the end. ratio [40]. The mixing of processed crude oil and
Preheating of reinforcement is necessary methanolic process is performed in a stirred
because preheating helps to create an oxide condition with the help of an electric stirrer.

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After keeping that mixture at 70 C for 1 day, two
distinct layers are formed of which upper one is
ester. This process is called trans-esterification.
Upper ester layer is separated out from that
mixture and collected and used as bio lubricant
for this study. Above steps are performed as
replication of processes published in various
research articles [38,43,46]. Properties of the
fabricated rice bran oil based ester are tabulated
in Table 4.
Table 4. Properties of Rice bran oil based TMP esters
[43,47].
Specific
Lubricant Viscosity Flash Point
gravity
Rice bran oil
4-5.5 cSt 0.877
based TMP 183 0C
@40 0C @30 0C
ester
2.3 Hardness measurement
Micro-hardness testing is done for various TiB2
weight percentage composites using Vickers
Micro Hardness Tester (Model-VMHT MOT, Sl.
No. 1002001). Average load of 3 kgf is applied
and a diamond indenter is used for indentation.
Dwell time is retained at 15 s and speed of
indentation is 50 m/s. Tests are carried out at
five different locations and the average is taken
as the hardness of the sample.
2.4 SEM study
The surface morphologies of the fabricated
composites are studied by scanning electron
microscope (SEM, INSTRUMENT JSM-6360,
Japan) to understand the basic mechanisms
happening on the wear track. Same SEM
machine is used to analyze wear track of the
composites in dry condition [31]. Before
scanning, samples are cut according to the size
of the tray of the machine. Samples are also
polished and etched using proper etchant.
2.5 Wear and friction measurement
Friction and wear tests are carried out on a
computer controlled block-on-roller Multi-
tribotester (DUCOM TR-25). Block specimen
used in this study has the size 20 mm 20 mm
8 mm. Tests for measuring wear and friction are
performed at ambient temperature (25 C)
under three different lubricated conditions.
Time duration for each test is taken as 1800
seconds to get estimation for long run
512
applications. In each experiment, specimen is
held against the counter roller. Contact surface is
flooded with lubricants at the time of
experiment. For each experiment, a fixed flow
rate of lubricant is maintained to get lubrication
regime within contact surface. Pictorial diagram
of test set-up is shown in Fig. 2.
Fig. 2. Pictorial view of tribological test apparatus.
Table 5. Test parameters for measuring wear and
friction.
Parameters Values
Constant normal load 25 N, 50 N, 75 N
Constant sliding speed 400 rpm, 500 rpm, 600 rpm
Weight percentage of
1 %, 2.5 %, 4 %, 5.5 %
TiB2 in composites
SAE20W40, Chain Lube Oil,
Lubricants Rice bran oil based TMP
Ester
EN8 stainless steel is used as the roller material
and the surface is ground with 600 grit abrasive
paper before and after each wear tests. Material
of the counter-face roller is important as it
determines hardness ratio which is defined as
ratio of the hardness of roller material to the
hardness of block material and this hardness
ratio determines also the wear rate of the
contact regime [35]. Considering hardness of
Al- TiB2 composites from previous study, EN8
steel as roller material is perfect for testing
wear and friction [31]. Wear is measured in
terms of wear depth created at the surface in
micrometer and friction is measured as friction
loads in N using load cells for measurements.
Coefficient of friction is calculated from the
value of friction load. Normally effects of
lubricants in contact surface exhibit their best
functions in boundary lubrication regime.
Pressure at contact interface is totally
 S. Poria et al., Tribology in Industry Vol. 38, No. 4 (2016) 508-521
dependent on constant normal load applied at
the time of tests which directs that normal
loads are also responsible for creating
boundary lubrication regime or mixed regime.
Thats why parameters for wear and friction
measuring tests should be chosen in such a way
so that optimal lubrication regime can be
achieved in boundary or mixed regime.
Parameters used for measuring friction and
wear are tabulated in Table 5. After performing
tests, results are analyzed and compared with
the results obtained in dry condition for same
materials under same load and speed
conditions [31].
3. RESULTS AND DISCUSSIONS
3.1 Hardness
Change in micro-hardness of Al- TiB2 composites
with amount of TiB2 particulates is shown in Fig. 3.
Fig. 3. Variation of hardness with wt% of TiB2.
It is obvious from figure that with inclusion of
TiB2 particulates, hardness is affected due to fine
particulate dispersion and higher hardness is
achieved by higher weight percentage of TiB2 in
Al-TiB2 composites. Similar observation is
reported earlier [22,31].
3.2 SEM characterization
After fabrication of composites, surface
morphology of each weight percentage
composites is observed under SEM. Distribution
of TiB2 particulates over the surface is
determined through this and also homogeneous
nature in distribution is found out from SEM
images. Detailed discussion on surface
morphology of SEM images of various weight
percentage fabricated composites is performed
elsewhere [31].
(a)
(b)
Fig. 4. SEM images of (a) 1 % TiB2 composites and (b)
5.5 % TiB2 composites.
Figure 4 shows the SEM images for composites
with highest weight percentage TiB2 and lowest
weight percentage TiB2 as reinforcement. It is
clearly noticed that nature of the distribution of
particles is uniform and presence of TiB2
particles in fabricated composites is confirmed.
3.3 Wear behavior in lubricated condition
and comparison with dry condition
Figure 5 shows the wear test results of Al- TiB2
composites using various lubricants at a
particular speed of roller i.e. 400 rpm. Figure 5a
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presents the wear results for three different
contact loads and for different weight
percentage Al-TiB2 composites including base
alloy with two lubricants, one is CFC free
commercial bio-lubricant with bio-additives
[chain lube oil] and another one is bio-lubricant
[rice bran oil TMP ester].
(a)
(b)
Fig. 5. Wear vs. weight percentages of TiB2 for three
different loads: (a) comparison of chain lube oil and
rice bran oil, (b) comparison of rice bran oil and
SAE20W-40.
514
With increase in normal loads, wear depth
increases for all TiB2 percentage composites
irrespective of the nature of lubricants and this
trend is in line with Archards wear law. Wear
depth decreases with increase in weight% of
TiB2 in composites. This is due to increase in
hardness with higher amount of TiB2 in the
composites. At a particular load and speed
combination, rice bran oil performs better than
chain lube oil in terms of wear reduction. For
same load i.e. 25 N, difference in wear depths for
5.5 % TiB2 composite is almost 4.4 % and for
base alloy it is almost 13 %. Similar trends are
observed in Fig. 5b which depicts the wear
results for different load and for different weight
percentage composites but with rice bran oil
TMP ester and commercial lubricant SAE20W-
40. In terms of the value of wear depths,
commercial SAE20W-40 is more effective as
wear resistant followed by rice bran oil TMP
ester and chain lube oil. This trend is followed in
all the cases shown in Figs. 5a and 5b except a
few. At 50 N loads and above 4 wt% of TiB2
composites, wear is slightly more in presence of
rice bran oil TMP ester than chain lube oil. At 25
N and 50N loads for 4 wt% and 5.5 wt% of TiB2
composites, wear for rice bran oil TMP ester and
for commercial SAE20W-40 are almost same. All
of these tests are carried out at a fixed sliding
speed, 400 rpm. At highest contact load i.e. 75 N
and fixed sliding speed, comparison of wear in
case of all three lubricants and all weight
percentage composites is shown in figure 6a. At
75N loads, difference in wear values for 5.5 %
TiB2 composites between highest effective
lubricant and lowest effective lubricant is almost
15 %. It is obvious from the figure that
commercial SAE20W-40 is most effective wear
resistant lubricant for composite -steel contact
interface.
Figure 6b shows wear results for different
sliding speeds with two commercial lubricants,
one with bio-additives and one with petroleum
base. Wear increases with sliding speeds and
effects of the two lubricants remain same in
nature in compliance with previous trends for all
the roller speed conditions.
Comparison of wear in dry condition and in
lubricated condition is drawn in Fig. 7. Dry
condition results and parameters are based on
previous report [31]. It is clearly seen that
differences of wear depth reduces significantly
 S. Poria et al., Tribology in Industry Vol. 38, No. 4 (2016) 508-521
in lubricated condition when compared to dry
sliding conditions. It is important to observe
here that inclination of graphs for wear depths
with respect to weight percentages of TiB2 in dry
condition is much higher than in lubricated
conditions. In dry condition, wear is mainly
dependent on nature of contact surfaces and
hardness ratios between two surfaces. But in
lubricated condition, lubricant film and its
interactions with surface layers play the main
role and the contribution of weight percentage
of TiB2 particles (i.e. hardness of the composite)
on tribological behavior becomes relatively
insignificant.
(a)
(b)
Fig. 6. Wear vs. weight percentages of TiB2 (a) For
three different lubricants at 75 N loads (b) For three
different speeds for SAE20W-40 and chain lube oil.
Fig. 7. Wear vs. weight percentages of TiB2 under dry
and lubricated conditions.
In lubricated contacts, wear is governed by the
development of lubrication film in the contact
interface between the composites and steel, and
the interaction of the surfaces with the lubricant
film. Generation of the lubrication film depends
on the composition and the nature of the
lubricant. Wear takes place due to breakage of
junctions in apparent contact area of the mating
surfaces or due to the deformation of asperities.
In dry condition, dominating mechanism is
abrasion and adhesion. In presence of lubricants,
lubricant film reduces the number of junctions or
number of asperities of the surfaces in contact.
Beside this, absorption of lubricant by the surface
helps to reduce adhesion force between two
adjacent atoms of the mating surfaces, as a result
of which mild abrasion occurs at the surface.
Cooling effect of lubricant also helps to decrease
surface temperature which leads to restrain the
adhesion transference and plastic deformation
[48]. Similar type of restraining in adhesion also
occurs in Al- TiB2 composite-steel interface in the
presence of lubricants. These facts are
responsible for reduction of wear in lubricated
conditions. In lubricated condition, wear
increases with normal loads also due to removal
of the lubricant layer between contact surfaces
and same reason is also applicable for the case of
increased rotational speed. But in dry condition,
more penetration of asperities in the contact
surface occurs with higher load which yields
more wear. But variation in wear with different
lubricants occurs due to the variation in
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capability of the lubricant film to develop

boundary lubrication or mixed lubrication or
elasto-hydrodynamic lubrication condition [48].
In boundary lubrication regime, chemical
interaction occurs between surface layers and
lubricants that influences wear. In this aspect,
SAE20W-40 and rice bran oil TMP ester is more
effective as wear resistant lubricant. Esters
present in the bio-lubricant helps to create
effective boundary lubrication condition that
influences wear in a large way though the film
thickness may not be so thick [49]. SAE20W-40 is
more effective by producing mixed regime mainly
elasto-hydrodynamic lubrication [48] as the (c)
viscosity of this lubricant is higher compared to
other two lubricants.

To observe the wear mechanisms in lubricated

contact sliding, SEM micrographs of worn
surfaces in SAE20W-40 lubricated contacts
under 25 N and 400 rpm are shown in Fig. 8. As
reported earlier [31], in dry condition, presence
of longitude grooves, partial pits, micro-cutting
and micro-ploughing indicates the contribution
of adhesion and abrasion wear mechanism both.

(d)
Fig. 8. SEM micrographs of worn surfaces of
composites: (a) 1 % TiB2, (b) 2.5 % TiB2, (c) 4 % TiB2
and (d) 5.5 % TiB2.

But in lubricated condition, other than 1 % and

2.5 % TiB2 composites, there is no sign of
ploughing or cracking. No holes or pits are
observed on the worn surfaces. Thus there is no
effect from corrosiveness of lubricants. Elastic
deformation of asperities is supposed to be an
(a) important mechanism for composite surface in
lubricated condition. Wear due to elastic
deformation creates no ploughing effects on the
surface. With higher weight percentage, hardness
of the composite increases which also increases
the chance of abrasion of the surface at the time
of sliding and this phenomena is observed in the
dry condition but in lubricated condition higher
weight percentage of TiB2 increases the number
of hard asperities at the mating surfaces resulting
in lesser possibility of plastic deformation.

In dry condition, due to plastic deformation of

asperities, hard particles are generated and laid
(b) in the surface but in lubricated condition only in

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case of lower weight percentage composites;

there is small amount of plastic deformation
yielding a comparatively rough surface.
Lubricants also help to wipe out the tips which
are procured at the time of sliding or rolling
action and that is also an important reason
behind getting smoother surfaces in lubricated
conditions. Similar type of observations is
reported elsewhere [42].

3.4 Friction behavior in lubricated condition

and comparison with dry condition

Friction behavior of Al-TiB2 composites under

lubricated condition is shown in Fig. 9. The
Figure 9a compares coefficient of friction vs. wt%
of TiB2 for rice bran oil based TMP ester and
chain lube oil. Figure 9b compares coefficient of
friction vs. wt% of TiB2 for rice bran oil based
TMP ester and SAE20W-40. It is observed that
(b)
friction decreases with increase in wt% of TiB2
and increases with normal load for all three Fig. 9. Friction vs. weight percentages of TiB2 for
lubricants. For TMP ester lubricant, friction three different loads (a) comparison of chain lube oil
and rice bran oil (b) comparison of rice bran oil and
coefficient values are in the range between0.054
SAE20W-40.
and 0.062 for 25 N loads. Change in friction
values for the same lubricant with change in
From Figs. 9a and 9b, it is seen that with loads
loads from 25 N to 75 N for base alloy is about 17
also, friction values vary more in case of ester
% for base alloy and about 20 % for 5.5 % TiB2
lubricant than other two lubricants and friction
composite. Friction values for 5.5 % weight
values are more or less lie in the same range for
percentage composites lie in the range between
other two commercial lubricants. For same load
0.077 and 0.087 for different loads in SAE20W-
and same weight percentage of composites,
40 lubricant and lie between 0.08 and 0.087 for
friction values are lower for ester lubricants and
different loads in Chain lube oil lubricant.
comparatively these are much lower in case of
higher load than in case of higher weight
percentage. Ester type lubricant appears as the
most effective lubricant on frictional behavior of
Al-TiB2 composites. Lowest value of friction
obtained within these parametric conditions is
0.0547 which is significantly low from
application point of view and the same is
obtained in presence of ester lubricant.

Comparison of friction in dry condition and

lubricated condition is shown in Fig. 10. Dry
condition results and parameters are based on
previous report [31]. It is clearly visible that the
effect of weight percentages of TiB2 on friction in
dry condition is significant, while lines are almost
parallel to axis under lubricated condition. It
means effect of lubricant is much prominent than
effect of weight percentage of TiB2 on friction. In
dry condition, friction values vary between 0.313
(a) and 0.332 with varying loads for 5.5 % TiB2

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composites while these lie between 0.077 and
0.087 for commercial lubricant. Actually friction
values are 5 times lower in lubricated condition
compared to dry condition. It is apparent that for
control of friction, lubricants play very vital role
that cant be compensated by incorporating more
TiB2 particulates in weight percentages as
reinforcement. Difference between friction
values in dry condition and lubricated condition
is also higher for ester lubricant.
Fig. 10. Friction vs. weight percentages of TiB2 under
dry and lubricated conditions.
In lubricated conditions, frictional force develops
due to generation of shear force within lubricant
film and this shear force is dependent on
characteristics of the lubricant itself. Thats why
lubricants having closed structure will be able to
give similar frictional behavior [47]. This leads to
almost same friction values of Al-TiB2 composites
under two commercial lubricants i.e. chain lube
oil and SAE20W40 though these yield different
wear values which is depicted in Fig. 5.
Lubricants which are not absorbed by the surface
show this type of effects but lubricants which can
be absorbed by the metallic surface, form a
metallic soap which resists the asperities to come
near and thus they reduce the frictional values.
This capability of reducing friction by forming
metallic soap does not depend on the contact
loads. The effect of metallic soap on surface is
more than the developed shear force within
certain parametric values. Thus frictional values
are less in presence of methyl esters on contact
518
surface as they can be absorbed to form metallic
soap [49]. However, with higher load this
condition may be destroyed and will be difficult
to achieve in presence of methyl ester type of
lubricant. In recent times, there has been
growing interest in friction and wear study of
metal matrix composites [50-54]. However, all
these studies consider only dry contact
situations. In this respect, the present study will
help in widening the use of such composites in
various lubricated conditions as well.
4. CONCLUSION
In the present study, Al-TiB2 composites are
developed through stir casting method and
tribological tests are performed in a Multi-
triobotester using three different lubricants are
chosen in this study. In lubricated contact,
mostly elastic deformation of asperities occurs
during sliding against steel surface by higher
weight percentage of TiB2-composites. It leads to
relatively smoother surface morphology of wear
tracks which is confirmed by SEM images. In
case of lower weight percentage of TiB2-
composites, little amount of ploughing and
cracking is present on the surface due to mild
wear by abrasion and less amount of plastic
deformation of asperities. Petroleum based
commercial lubricant is the most effective
lubricant as wear resistant followed by methyl
ester based lubricant and bio-additives based
lubricant. In case of frictional characteristics,
methyl ester based lubricants are the most
effective one as they are capable to make
metallic soap through absorption by surface up
to a certain extent.
REFERENCES
[1] N. Kumar, G. Gautam, R. K. Gautam, A. Mohan and
S. Mohan, Synthesis and Characterization of
TiB2 Reinforced Aluminium Matrix Composites:
A Review, Journal of Institute of Engineers India
Series D, DOI 10.1007/s40033-015-0091-7.
[2] M. Rosso, Ceramic and Metal Matrix
Composites: Routes and Properties, Journal of
Material Processing Technology, vol. 175, pp.
364-375, 2006.
[3] G. Mars, Mixed fortunes for aerospace materials,
Materials Today, vol. 3, pp. 21-25, 2000.
 S. Poria et al., Tribology in Industry Vol. 38, No. 4 (2016) 508-521
[4] S. Suresh and A. Mortensen, in Fundamentals of
Metal Matrix Composites Butterworth-
Heinemann, 1993.
[5] T. Miyajima and Y. Iwai, Effects of
reinforcements on sliding wear behavior of
aluminium matrix composites, Wear, vol. 255,
pp. 606-616, 2003.
[6] G.B.V. Kumar, C.S.P. Rao and N. Selvaraj,
Mechanical and tribological behavior of
particulate reinforced aluminium metal matrix
compositesa review, Journal of minerals and
materials characterization and engineering, vol.
10, pp-59-91, 2011.
[7] C.M.A. Partheeban, M. Rajendran, S.C. Vettivel, S.
Suresh and N.S.V. Moorthi, Mechanical behavior
and failure analysis using online acoustic
emission on nano-graphite reinforced Al6061-
10TiB2 hybrid composite using powder
metallurgy, Materials Science and Engineering
A, vol. 632, pp. 1-13, 2015.
[8] D.B. Miracle, Metal matrix composites from
science to technological significance,
Composites Science and Technology, vol. 65, pp.
2526-2540, 2005.
[9] M. Rittner, Metal matrix composites in the 21st
century: markets and opportunities, BCC, Inc.,
Norwalk, CT, 2000.
[10] K.L. Tee, L. Lu and M.O. Lai, Synthesis of in situ
AlTiB2composites using stir cast route,
Composite Structures, vol. 47, pp. 589-593, 1999.
[11] H. Nami, H. Adgi, M. Sharifitabar and H.
Shamabadi, Microstructure and mechanical
properties of friction stir welded Al/Mg2Si
metal matrix cast composite, Materials and
Design, vol. 32, pp. 976- 983, 2011.
[12] S.A. Alidokht, A. Abdollah-Zadeh, S. Soleymani
and H. Assadi, Microstructure and tribological
performance of an aluminium alloy based
hybrid composite produced by friction stir
processing, Material and Design, vol. 32, pp.
2727-2733, 2011.
[13] M.K. Akbari, H.R. Baharvandi and K.
Shirvanimoghaddam, Tensile and fracture
behavior of nano/micro TiB2 particle reinforced
casting A356 aluminum alloy composites,
Materials and Design, vol. 66, pp. 150-161, 2015.
[14] D.J. Lloyd, Particle reinforced aluminium and
magnesium matrix composites, International
Materials Reviews, vol. 39, pp. 1-23, 1994.
[15] A.M. Hassan, A. Alrashdan, M.T. Hayajneh and
A.T. Mayyas, Wear behavior of AlMgCu-based
composites containing SiC particles, Tribology
International, vol. 42, pp. 1230- 1238, 2009.
[16] H. Lu, C. Chen, H. Sun, Z. Hu and D. Yang,
Characterization of Al2O3Al nano-composite
powder prepared by a wet chemical method,
Ceramics International, vol. 32, pp. 481-485,
2005.
[17] S. Ghosh, P. Sahoo and G. Sutradhar,
Tribological performance optimization of Al-
7.5%SiCp composites using taguchi method and
grey relation analysis, Journal Composites, vol.
2013, ID 2745271, 2013.
[18] Y. Sahin, Preparation and some properties of
SiC particle reinforced aluminium alloy
composites, Materials and Design, vol. 24, pp.
671- 679, 2003.
[19] K.M. Shorowordi, T. Laoui, A.S.M.A. Haseeb, J.P
Celis and L. Froyen, Microstructure and
interface characteristics of B4C, SiC and Al2O3
reinforced Al matrix composites: a comparative
study, Journal of Material Processing
Technology, vol. 142, pp. 738-743, 2003.
[20] T. Nukami and M. C. Flemings, In situ synthesis
of TiC particulate-reinforced aluminium matrix
composites, Metallurgical and Materials
Transactions A, vol. 26, no. 7, pp. 1877-1884,
1995.
[21] S. Suresh, N.S.V. Moorthi, S.C. Vettivel and N.
Selvakumar, Effect of graphite addition on
mechanical behavior of AL6061/TiB2 hybrid
composite using acoustic emission, Materials
Science and Engineering A, vol. 612, pp. 16-27,
2014.
[22] K. Sivaprasad, S.P. Kumaresh Babu, S. Natarajan,
R. Narayanasamy, B.A. Kumar and G. Dinesh,
Study on abrasive and erosive wear behaviour
of Al 6063/TiB2in situ composites, Materials
Science and Engineering A, vol. 498, pp. 495-500,
2008.
[23] S.C. Tjong and Z.Y. Ma, Micro-structural and
mechanical characteristics of in situ metal
matrix composites, Materials Science and
Engineering A, vol. 29, pp. 49-113, 2000.
[24] L. Wang and R.J. Arsenault, Interfaces in XD
processed TiB2/NiAl composites, Metallurgical
and Materials Transactions A, vol. 22, pp. 3013-
3018, 1991.
[25] A.R. Kennedy, A.E. Karantzalis and S.M. Wyatt,
The microstructure and mechanical properties
of TiC and TiB2-reinforced cast metal matrix
composites, Journal of Materials Science, vol. 34,
pp. 933-940, 1999.
[26] K.L. Tee, L. Lu and M.O. Lai, Wear performance
of in-situ AlTiB2 composite, Wear, vol. 240, pp.
59-64, 2000.
519
 S. Poria et al., Tribology in Industry Vol. 38, No. 4 (2016) 508-521

[27] J. Xue, J. Wang, Y. Han, P. Li and B. Sun, Effects of
CeO2 additive on the microstructure and
mechanical properties of in situ TiB2/Al
composite, Journal of Alloys and Compounds,
vol. 509, pp. 1573- 1578, 2011.
[28] A. Jha and C. Dometakis, The dispersion
mechanism of TiB2 ceramic phase in molten
aluminium and its alloys, Materials and Design,
vol. 18, pp. 297-301, 1997.
[29] Y.M. Youssef, R.J. Dashwood and P.D. Lee, Effect
of clustering on particle pushing and
solidification behaviour in TiB2 reinforced
aluminium PMMCs, Composites: Part A, vol. 36,
pp. 747-763, 2005.
[30] Y. Taneoka, O. Odawara and Y. Kaieda,
Combustion Synthesis of the Titanium-
Aluminum-Boron System, Journal of the
American Ceramic Society, vol. 72, no. 2, pp.
1047-1049, 1989.
[31] S. Poria, P. Sahoo and G. Sutradhar, Tribological
Characterization of Stir-cast Aluminium-TiB2
Metal Matrix Composites, Silicon, vol. 8, pp.
591-599, 2016.
[32] K. Niranjan and P.R. Lakshminarayanan, Dry
sliding wear behavior of in-situ Al-TiB2
composites, Materials and Design, vol. 47, pp.
167-173, 2013.
[33] A. Mandal, B.S. Murty and M. Chakraborty,
Sliding wear behaviour of T6 treated A356-TiB2
in-situ composites, Wear, vol. 266, pp. 865-872,
2009.
[34] C. Mallikarjuna, S.M. Shashidhara, U.S. Mallik
and K.I. Parashivamurth,Grain refinement and
wear properties evaluation of aluminum alloy
2014 matrix-TiB2 in-situ composites, Materials
and Design, vol. 32, pp. 3554-3559, 2011.
[35] C.J. Reeves, P.L. Menezes, M.R. Lovell and T. Jen,
The Size Effect of Boron Nitride Particles on the
Tribological Performance of Biolubricants for
Energy Conservation and Sustainability,
Tribolgy Letters, pp. 437452, DOI
10.1007/s11249-013-0182-2, 2013.
[36] L.A. Quinchia, M.A. Delgado, T. Reddyhoff, C.
Gallegos and H.A. Spikes, Tribological studies of
potential vegetable oil-based lubricants
containing environmentally friendly viscosity
modifiers, Tribology International, vol. 69, pp.
110-117, 2014.
[37] N.J. Fox, B. Tyrer and G.W. Stachowiak,
Boundary lubrication performance of free fatty
acids in sunflower oil, Tribology Letters, vol. 16,
no. 4, pp. 275-281, 2004.
[38] J. Hu, Z. Du, C. Li and E. Min, Study on the
lubrication properties of biodiesel as fuel
lubricity enhancers, Fuel, vol. 84, pp. 1601-
1606, 2005.
[39] D.P. Geller and J.W. Goodrum, Effects of specific
fatty acid methyl esters on diesel fuel lubricity,
Fuel, vol. 83, pp.2351-2356, 2004.
[40] M. Mohamed Musthafa, S.P. Sivapirakasam and
M. Udayakumar, Comparative studies on fly ash
coated low heat rejection diesel engine on
performance and emission characteristics
fueled by rice bran and pongamia methyl ester
and their blend with diesel, Energy, vol. 36, pp.
2343- 2351, 2011.
[41] H. Mindivan, E.S. Kayali and H. Cimenoglu,
Tribological behavior of squeeze cast aluminum
matrix composites, Wear, vol. 265, pp. 645-654,
2008.
[42] C.A. Caracostas, W.A. Chiou, M.E. Fine and H.S.
Cheng, Tribological Properties of Aluminum
Alloy Matrix TiB2 Composite Prepared by In Situ
Processing, Metallurgical and Materials
Transactions A, vol. 28A, pp. 491-502, 1997.
[43] L. Lin, D. Ying, S. Chaitep and S. Vittayapadung,
Biodiesel production from crude rice bran oil
and properties as fuel, Applied Energy, vol. 86,
pp. 681-688, 2009.
[44] S. Das and S.K. Biswas, Boundary lubricated
tribology of an aluminiumsilicon alloy sliding
against steel, Tribology Letters, vol. 17, no. 3, pp.
623-628, 2004.
[45] A. Ramalho and J.C. Miranda, Tribological
characterization of electroless NiP coatings
lubricated with biolubricants, Wear, vol. 263,
pp. 592-597, 2007.
[46] S. Zullaikah, C.C. Lai, S.R. Vali and Y.H. Ju, A two-
step acid-catalyzed process for the production
of biodiesel from rice bran oil, Bioresource
Technology, vol. 96, pp. 1889-1896, 2005.
[47] S. Sinha, A.K. Agarwal and S. Garg, Biodiesel
development from rice bran oil: Trans-
esterification process optimization and fuel
characterization, Energy Conversion and
Management, vol. 49, pp. 1248-1257, 2008.
[48] J.H. Jia, J.M. Chen, H. Zhou, J. Wang and H. Zhou,
Friction and wear properties of bronzegraphite
composite under water lubrication, Tribology
International, vol. 37, pp. 423-429, 2004.
[49] D. Tabor, in Friction, Lubrication, and Wear,
Chapter 7, Mechanical Design Handbook.
[50] B.M. Viswanatha, M.P. Kumar, S. Basavarajappa
and T.S. Kiran, Effect of ageing on dry sliding
wear behaviour of. Al-MMC for disc brake,
Tribology in Industry, vol. 36, no. 1, pp. 40-48,
2014.

520
 S. Poria et al., Tribology in Industry Vol. 38, No. 4 (2016) 508-521
[51] J. Lakshmipathy and B. Kulendran,
Reciprocating wear behaviour of 7075Al/SiC
and 6061Al/Al2O3 composites: A study of effect
of reinforcement, stroke and load, Tribology in
Industry, vol. 36, no. 2, pp. 117126, 2014.
[52] N. Radhika and R. Raghu, Evaluation of dry
sliding wear characteristics of LM 13 Al/B4C
composites, Tribology in Industry, vol. 37, no. 1
pp. 20-28, 2015.
[53] N. Radhika, A. Vaishnavi and G.K. Chandran,
Optimisation of dry sliding wear process
parameters for aluminium hybrid metal matrix
composites, Tribology in Industry, vol. 36, No. 2
pp. 188194, 2014.
[54] S. Srivastava and S. Mohan, Study of wear and
friction of Al-Fe metal matrix composite produced
by liquid metallurgical method, Tribology in
Industry, vol. 33, No. 3, pp. 128-137, 2011.
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Tribology in Industry

RESEARCH
www.tribology.fink.rs

Modeling of Surface Roughness in Plasma Jet Cutting

Process of Thick Structural Steel

I. Peko a, B. Nedi b, A. orevi b, D. Duni b, M. Jankovi b, I. Vea a

aFaculty of Electrical Engineering, Mechanical Engineering and Naval Architecture, University of Split, Ruera
Bokovia 32, 21000 Split, Croatia,
bFaculty of Engineering, University of Kragujevac, Sestre Janji 6, 34000 Kragujevac, Serbia.

Keywords: ABSTRACT
Plasma jet cutting
Today highly competitive market and demands for obtain high surface
Surface roughness
finish and machining of complex shape geometries replace conventional
Modeling
machining processes with non-conventional. Plasma jet cutting is one of
Experiment
these non-conventional processes that primary uses a thermal energy of
Structural steel
highly ionized gas to cut specified material and blow molten metal away.
Main advantages of plasma jet cutting process are high speed of cutting,
Corresponding author: cutting different types of materials, the quality of cut and moderate to low
investment costs. This paper presents experimental results concerning the
I. Peko
surface roughness variation at plasma jet cutting of structural steel
Faculty of Electrical Engineering,
S235JRG2 plate thickness of 15 mm. Using the experimental data artificial
Mechanical Enginering and Naval
neural network (ANN) model was developed in order to predict the surface
Architecture,
roughness in terms of two input parameters, cutting current and cutting
University of Split, Ruera Bokovia
speed. After the prediction accuracy of the developed model was validated,
32, 21000 Split, Croatia
the model was used for analyzing influence of input parameters on process
E-mail: ipeko@fesb.hr
response values.
2016 Published by Faculty of Engineering

1. INTRODUCTION abrasive water jet cutting are optimal

Today, different non-conventional thermal
processes can be found in many applications in
metal processing and shipbuilding industry.
These processes include oxy fuel cutting, laser
cutting and plasma jet cutting. They can be used
for the cutting various types of materials at
various thicknesses. Plasma jet cutting process
has many advantages which can help the
modern company to survive in a turbulent
market. Main benefits that characterize this
process and position it in front of the laser and
combination of cut quality, productivity and
costs for mild steel, stainless and aluminium
cutting. Competitive investments, high
productivity, long consumables life and lower
costs per part lead this technology to become a
practical alternative to other processes such as
laser and abrasive water jet cutting.
Plasma jet cutting process was developed at the
end of 1950s. Plasma can be defined as the
fourth state of substance which is obtained by
supplying a tremendous amount of energy to gas

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 I. Peko et al., Tribology in Industry Vol. 38, No. 4 (2016) 522-529
or when a gas is subjected to a high electric field.
In this process an electric arc is generated
between the electrode and the workpiece. An
electrode acts as an anode and the workpiece as
a cathode. The plasma gas expandes with the
high velocity through the nozzle at the same
time an electric current passes through the gas
with the help of a tungsten electrode due to
which a high intensity plasma jet is generated.
This jet is able to melt or vaporize the plate
surface that should be cut and to blow the
molten metal away from the cut. The most
commonly used gases for this process are
compressed air, nitrogen, argon-hydrogen,
oxygen and their combinations. They can be
used both as a plasma and shield gases.
Main components of plasma jet cutting system
are power supply unit, an arc starting circuit and
a torch. These units provide the electrical
energy, ionization, and process control for
cutting all ellectrically conductive materials to
180 mm thickness.
Today many of plasma jet cutting systems are
supported by manufacturers recommendations.
However these recommendations usually reflect
the point of view of the manufacturers bussines
but do not lead to the optimization of all cut
quality features required by users. Because of
that various experimental researches were
conducted in order to describe and model
plasma jet cutting process and to chose the
optimal process parameters.
Kumar Das et al. [1] analyzed the influence of
three process parameters, gas pressure, arc
current and torch height on material removal
rate and surface roughness parameters. They
conducted experiments on EN31 steel
according to Taguchi L27 orthogonal array.
Parametric optimization was carried out using
grey relational analysis. Salonitis et al. [2] used
the regression analysis to describe the effect of
cutting power, cutting speed, cutting height and
plasma gas pressure process parameters on cut
quality features such as kerf taper angle, the
edge roughness and the size of the heat affected
zone. Bini et al. [3] analyzed the influence of arc
voltage, cutting speed, plasma and shield gas
flowrates on kerf position and shape in 15 mm
thick mild steel sheets cutting. They used a two-
level fractional factorial design for design
experiment and ANOVA (Analyisis of variance)
for data analysis. Chamarthi et al. [4] cut a
Hardox 400 plate thickness of 12 mm. They
varied cutting speed, plasma gas flow rate and
voltage as the process parameters in the 16
experiments and analyzed their influence on
the unevennes of cut surface. ANOVA is
performed later in order to identify the
parameters that clearly define the unevenness
quality attributes. Gullu et al. [5] investigated
material structure changes that occurred after
plasma jet cutting of AISI 304 stainless steel
and St 52 carbon steel. Gariboldi et al. [6] cut
titanium sheets using high tolerance plasma arc
cutting process. They used free feed rate range
with the adoption of oxygen and nitrogen as
plasma and shield gases and analyzed cut
quality features such as unevenness, kerf width,
angle of cut and surface roughness. Also they
conducted temperature measurements in the
regions near to the cutting edge,
microstructural investigations and
measurements of geometric and surface
atributes of the cutting edges. Adalarasan et al.
[7] assesed te quality characteristics of the cut
surface by measuring the surface roughness
and kerf width while cutting the 304L stainless
steel. Taguchi L18 orthogonal array and Grey
Taguchi based respone surface methodology
were used to design experiments and find
optimal cutting parameters. Chen et al. [8]
analyzed two process responses such as bevel
magnitude and the hole diameter deviation.
They conducted 36 experiments according to
Taguchi L9 experiment design and varied six
process parameters, tip size, feed rate, voltage,
amperage, air pressure and pierce time.
Taguchi method was used to find optimal
combination of process parameters that lead to
the smallest bevel angle and diameter deviation
of the hole. Thilak et al. [9] analyzed the
influence of arc current, gas pressure, cutting
speed and arc gap in plasma cutting of stainless
steel 316L on process responses such as
machining time, hardness and kerf width. They
used Taguchi method for design experiment
and Grey relational analysis for optimization.
Radovanovic et al. [10] conducted experiments
in which they varied three input process
parameters, cutting current, plate thickness and
cutting speed. They developed artificial neural
network model to predict the ten point height
of irregularities of cut surface (Rz) and to
identify cutting parameters values that lead to
optimal surface roughness. Kechagias et al. [11]
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also used artificial neural network approach for Table 1. Plasma jet cutting parameters.
prediction of bevel angle that appear after CNC Input parameters
plasma arc cutting of St37 mild steel sheets. No. of
Experiment Cutting current, Cutting speed, v
They conducted a L18 Taguchi orthogonal array I (A) (mm/min)
experiment. Input parameters whose influence 1 60 425
was analyzed are plate thickness, cutting speed, 2 60 530
arc current and torch standoff distance. 3 60 635
4 80 490
In the present research paper experiments were
5 80 610
conducted on structural steel S235JRG2 plate
6 80 730
thickness of 15 mm. It was analyzed the
7 80 870
influence of input process parameters, cutting
current and cutting speed on surface roughness. 8 80 1055
Artificial neural network approach was used for 9 100 530
mathematical modeling and to identify cutting 10 100 695
parameters ranges that lead to minimal surface 11 100 870
roughness values. 12 100 1055
13 120 730
14 120 870
2. EXPERIMENTAL PROCEDURE 15 120 1055
16 120 1320
Experimental work was conducted on a CNC 17 120 1585
Steel Taylor plasma cutting machine (Fig. 1).
Test specimens were cut on 15 mm thickness Table 2. Experimental results.
structural steel plate S235JRG2 with the use of
compressed air as plasma gas. Input process Measured Mean value of
No. of Measurement surface surface
parameters levels that were varied in Exp. places roughness, Ra roughness, Ra
experiments were shown in Table 1. Fixed (m) (m)
input parameters are: nozzle diameter 1.5 mm, g 10.50
gas pressure 6 bar, cutting height 5 mm. Every 1 s 17.00 19.00
experiment was conducted one time. During the d 30.70
experiments it was noticed that some
g 12.40
combinations of cutting parameters lead to not
2 s 21.30 24.70
penetrated workpieces such as those in runs
d 40.40
number 3 and 8. In Figures 2 and 3 it was
shown look of well cut specimen and one not g
penetrated. Measurements of surface 3 s Workpiece is not penetrated
roughness were performed on three places of d
cut surface: near to upper cut edge (g), in the g 17.50
middle (s) and near to lower cut edge (d) (Fig. 4 s 29.40 24.50
4). Results of measured surface roughness were d 26.60
shown in Table 2. g 15.20
5 s 35.80 24.67
d 23.00
g 14.10
6 s 24.30 21.03
d 24.70
g 14.00
7 s 41.00 36.67
d 55.00
g
8 s Workpiece is not penetrated
Fig. 1. CNC Steel Taylor plasma jet cutting machine. d

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g 35.00
9 s 19.00 28.67
d 32.00
g 13.00
10 s 13.00 11.93
d 9.80
g 12.40
11 s 8.80 11.40
d 13.00 Fig. 4. Surface roughness measurement places.
g 12.00
12 s 12.40 11.50
d 10.10 3. ARTIFICIAL NEURAL NETWORK
g 16.00 MODELING OF SURFACE ROUGHNESS
13 s 14.00 16.00
d 18.00 The Artificial Neural Network (ANN) is an
g 17.00 artificial system similar to the biological nervous
14 s 14.00 17.00 system able to intelligently process the
d 20.00
information simulating the biological
intelligence. The artificial neural networks are
g 10.30
applicable today in various areas such as process
15 s 11.00 7.10
modeling and optimization, design and
d -
simulation, classification, robotics, etc. [12-14].
g 10.80
16 s 9.90 11.20 Architecture of artificial neural networks is
d 12.90 parallel-distributed and it consists of a large
g 8.30 number of neurons distributed in several layers.
17 s 10.10 9.40 Each ANN must have at least three layers: input
d 9.80 layer, hidden layer and output layer [15-17].
Neurons of one layer are connected by specific
synapses to the neurons of their neighbouring
layers. Interconnections between particular
neurons by the layers are characterized by weights
and biases, which change during the ANN training.
By proper adjustments of weights and biases in the
training process ANN is more capable to better
describe the relationships between input process
parameters and output responses. Prior to ANN
training process optimal number of hidden layers
and the number of neurons in each of them should
be properly defined. These numbers change
Fig. 2. Look of penetrated specimen. during training and can be defined empiricaly or
by using some existing equations that take in
consideration number of input and output neurons
and training data. Training is carried out on the
exmples data usually obtained by the experiments.
This process should be repeated until the ANN is
stabilized or error is defined below a previously
defined treshold. Validation and testing process
of developed ANN are performed on data subsets
that are not included in the training data subset.
The trained, validated and tested ANN can be
used for modeling and prediction various
Fig. 3. Look of not penetrated specimen. processes [15-22].

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In this paper, the three layered feed-forward
backpropagation ANN architecture has been
selected for modeling surface roughness in
plasma jet cutting process of thick structural steel
plate. The input layer of the ANN model consists
of two neurons corrsponding to the two process
parameters that were varied in the experiments,
cutting current (I) and cutting speed (v) and the
output layer has one neuron for prediction of
surface roughness values (Fig. 5).
Fig. 5. Selected ANN architecture for modeling
surface roughness in plasma jet cutting process.
The whole experimental data set (Ntot=17) is
divided into a data subset for training, a data
subset for validation and a data subset for testing.
90 % randomly selected data of the whole
experimental data have been employed for
training, 5 % for validation and 5 % for testing.
Main problems that occure in backpropagation
ANNs are overfitting and overtraining.
Overtraining means that ANN only memorizes
the training data set and excellent learns these
data but doesnt have an ability to generalize to
new data and because of that performance of the
validation set decreases. According to this, the
goal is to find the simplest ANN model that has
the total error considerably low [23-24]. In this
paper ANN architecture with one hidden layer
and ten neurons was used for process modeling
and prediction. It was found out that this
architecture gives a minimal difference between
the predicted values and real experimental data.
Transfer functions that were used in the
network are tangent sigmoid function in the
hidden and linear function in the output layer.
Prior to ANN training the training data were
526
normalized to a range of (-1,1) and the initial
values of weights were set according to Nguyen-
Widrow method. As it was already mentioned
backpropagation algorithm with momentum
was used for ANN training.
The performance of the network was measured
by the Mean Squared Error (MSE) of the
predicted outputs with regards to the real
experimental data. The goal is to get MSE as
close as possible to zero. The zero means that
there is no error between outputs of the
network and experimental values. In this case,
ANN training was initially set to terminate after
a maximum number of epochs, but it was
stopped at 15 iterations since no further
improvement in the MSE was achieved. MSE
values obatined after training, validation and
testing of ANN are shown in Table 3.
Table 3. MSE values of ANN model.
ANN Mean Squared Error (MSE)
architecture Training Validation Testing
2-10-1 0.0218 0.0697 0.0043
Fig. 6. Correlation between predicted and
experimental data during training, validation and
testing of the developed ANN model.
Except MSE another performance measure for
ANN model is correlation coefficient (R). This is
a statistical measure of the strength of
correlation between predicted and experimental
values. A perfect correlation is obtained when
R=1. In real manufacturing processes this case is
 I. Peko et al., Tribology in Industry Vol. 38, No. 4 (2016) 522-529

very rare. A good ANN model should have the
correlation coefficient greater than 0.8.
Correlation coefficients of the developed ANN
model for all three datasets are shown in Fig. 6.
Also, it was carried out comparison of actual
data and those predicted by developed ANN
model. Results were shown in Fig. 7.
input cutting parameters, cutting current (I) and
cutting speed (v) can be expressed following the
Equation 1. In this equation X is the column
vector which contains normalized values of v
and I and Ranorm is the normalized value for the
Ra. To obtain actual values of surface roughness
it is necessary to denormalize the data:
2
Ranorm 1 wkj b k (1)
1 e2( X w ji b j )

4. RESULTS

Using Equation 1 and by varying value of both or

Fig. 7. Comparison of actual and predicted surface
roughness values.
The weights and biases of the ANN model that
were determined in training process are given in
Table 4-5.
just one parameter while the other was kept at
specified level the effects of input process
parameters on the surface roughness were
analyzed. In Figs. 8-9 were shown their individual
impacts while in Fig. 10 was shown impact of
their interaction on process response values.

Table 4. The weights wji of developed ANN model.

Weights
wji
I -3.2376 2.829 0.85764 4.8486 4.7737
I 3.0145 5.2474 -5.1114 -5.6098 2.7624
wji
II 0.46901 -1.7208 6.2266 -0.64648 3.1856
II 2.4687 3.2077 6.0504 -2.4774 -3.535

Table 5. The weights wkj and biases of developed

ANN model. Fig. 8. Influence of the arc current (I) on the surface
Weights Biases roughness (Ra).
wkj bj bk
-1.4067 5.4031 -0.13449
1.2101 -4.6788
-0.65194 3.9649
-0.73323 -0.877
0.16832 -2.7303
2.3098 1.534
-0.53875 0.83182
-2.6379 -1.9525
0.85298 -0.49454
0.077574 4.2281

Using the weights and biases from Table 4-5 and

in accordance with selected ANN architecture
the exact mathematical relationship between Fig. 9. Influence of the cutting speed (v) on the
process response, surface roughness (Ra) and surface roughness (Ra).

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Analyzing the experimental data the area of
parameters combinations within certainly
comes to sheet metal cutting was defined. This
area was shown in Figs. 8-10.
Fig. 10. Influence of the I-v interaction on the surface
roughness (Ra).
From Figs. 8-10 it can be concluded that higher
values of cutting speed (>800 mm/min) and
cutting current (>100 A) lead to smoother surface
of the cut. At lower cutting current levels cutting
speed has an inappreciable effect on the surface
roughness values. At cutting speed values to 700
mm/min better surface can be obtained if the
cutting current is set at 100-110 A.
5. CONCLUSION
In this paper a mathematical modeling of surface
roughness in plasma jet cutting of thick
structural steel was shown. This was performed
using artificial neural networks. Neural
networks have proven more suitable due to their
potential to learn nonlinear features of any
system from incomplete experimental data
regardless of external noise. Model was verified
using statistical measures such as R and MSE.
Beside that a comparison between experimental
and predicted values was conducted. These
indices showed that model is quite acceptable.
Created model was used to describe the
influence of input parameters such as cutting
current and cutting speed on analyzed process
response. According to this the plots were
created that can be used to identify cutting
conditions that lead to minimal surface
roughness values.
528
Future research will take in consideration other
cut quality responses such as kerf width, dross
width, dross height that occur during plasma jet
cutting. Their values will be included in
mathematical modelling procedure to obtain a
complete view of output process quality.
Acknowledgement
The paper has been fully supported by The
Croatian Science Foundation under the project
Innovative Smart Enterprise INSENT (1353).
REFERENCES
[1] M. Kumar Das, K. Kumar, T.K. Barman and P.
Sahu, Optimization of process parameters in
plasma arc cutting of EN31 steel based on MRR
and multiple roughness characteristics using
grey relational analysis, Procedia material
science, vol. 5, pp. 1550-1559, 2014.
[2] K. Salonitis and S. Vatousianos, Experimental
investigation of the plasma arc cutting process,
Procedia CIRP, vol. 3, pp. 287-292, 2012.
[3] R. Bini, B. M. Colosimo, A.E. Kutlu and M. Monno,
Experimental study of the features of the kerf
generated by a 200 A high tolerance plasma arc
cutting system, Journal of Materials Processing
Technology, vol. 196, pp. 345-355, 2008.
[4] S. Chamarthi, N.S. Reddy, M. K. Elipey and D.V.R.
Reddy, Investigation analysis of plasma arc
cutting parameters on the unevenness surface
of Hardox-400 material, Procedia Engineering,
vol. 64, pp. 854-861, 2013.
[5] A. Gullu and U. Atici, Investigation of the effects
of plasma arc parameters on the structure
variation of AISI 304 and St 52 steels, Materials
and Design , vol. 27, pp. 1157-1162, 2006.
[6] E. Gariboldi and B. Previtali, High tolerance
plasma arc cutting of commercially pure
titanium, Journal of Materials Processing
Technology, vol. 160, pp. 77-89, 2005.
[7] R. Adalarasan, M. Santhanakumar and M.
Rajmohan, Application of Grey Taguchi based
response surface methodology (GT-RSM) for
optimizing the plasma arc cutting parameters of
304L stainless steel, International Journal of
Advanced Manufacturing Technology, vol. 78, pp.
1161-1170, 2015.
[8] J.C. Chen, Y. Li and R.A. Cox, Taguchi based Six
Sigma approach to optimize plasma cutting
process: an industrial case study, International
 I. Peko et al., Tribology in Industry Vol. 38, No. 4 (2016) 522-529
Journal of Advanced Manufacturing Technology,
vol. 41, pp. 760-769, 2009.
[9] M. Thilak, N. Boopalan, I. Cyril Gnanaraj, A.R.
Ganesh Babu and N. Gogul, Optimization of
machining process parameters in plasma arc
machining, International Journal of Innovative
Research in Science, Engineering and Technology,
vol. 5, no. 8, pp. 229-240, 2016.
[10] M. Radovanovic and M. Madic, Modeling the
plasma arc cutting process using Ann,
Nonconventional Technologies Review, no. 4, pp.
43-48, 2011.
[11] J. Kechagias, M. Pappas, S. Karagiannis, G.
Petropoulos, V. Iakovakis and S. Maropoulos, An
ANN approach on the optimization of the
cutting parameters during CNC plasma-arc
cutting, in 10th Biennial Conference on
Engineering Systems Design and Analysis,
ESDA2010, Istanbul, Turkey, 2010.
[12] M.J. Madic and V.J. Marinkovic, Assesing the
sensitivity of the artificial neural network to
experimental noise: A case study, FME
Transactions, vol. 38, no. 4, pp. 189-195, 2010.
[13] M. Bachraty, M. Tolnay, P. Kovac and V.
Pucovsky, Neural network modeling of cutting
fluid impact on energy consumption during
turning, Tribology in Industry, vol. 38, no. 2, pp.
149-155, 2016.
[14] H. Alimam, M. Hinnawi, P. Pradhan and Y.
Alkassar, ANN & ANFIS models for prediction of
abrasive wear of 3105 aluminium alloy with
polyurethane coating, Tribology in Industry, vol.
38, no. 2, pp. 221-228, 2016.
[15] O. Eyercioglu, E. Kanca, M. Pala and E. Ozbay,
Prediction of martensite and austenite start
temperatures of the Fe-based shape memory
alloys by artificial neural networks, Journal of
Materials Processing Technology, vol. 200, pp.
146-152, 2008.
[16] K. Elangovan, C. Sathiya Narayanan and R.
Narayanasamy, Modeling and forming limit
diagram of perforated commercial pure
aluminium sheets using artificial neural
network, Computational Materials Science, vol.
47, no. 4, pp. 1072-1078, 2010.
[17] Z. Miljkovi, B. Bojovi and B. Babi, Application
of artificial neural network and fractals in
biomedical materials surface behaviour
prediction, Tehnika-Novi materijali, vol. 19, no.
4, pp. 5-14, 2010.
[18] N.K. Bose and P. Liang, Neural network
fundamentals with graphs, algorithms, and
applications. New York: McGraw-Hill, 1996.
[19] S. Haykin, Neural networks: A Comprehensive
Foundation, New York: Prentice Hall, 1998.
[20] G. Dreyfus, Neural Networks, Berlin: Springer
Verlag, 2005.
[21] Z. Miljkovic, Systems of Artificial Neural
Networks in Production Technologies. Belgrade,
Faculty of Mechanical Engineering, University of
Belgrade, 2003. (in Serbian)
[22] Z. Miljkovic and D. Aleksendric, Artificial Neural
Networks Collection of Resolved Tasks with
Excepts From the Theory. Belgrade, Faculty of
Mechanical Engineering, University of Belgrade,
2009. (in Serbian)
[23] S.G. Tzafestas, P.J. Dalianis and G. Anthopoulos,
On the overtraining phenomenon of
backpropagation neural networks, Mathematics
and Computers in Simulation, vol. 40, pp. 507-
521, 1996.
[24] L. Prechelt, Automatic early stopping using
cross validation: quantifying the criteria, Neural
Networks, vol. 11, no. 4, pp. 761-767, 1998.
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 Vol. 38, No. 4 (2016) 530-542

Tribology in Industry

RESEARCH
www.tribology.fink.rs

Effect of CVD-Diamond on the Tribological and

Mechanical Performance of Titanium Alloy
(Ti6Al4V)

S.H. Din a, M.A. Shah b, N.A. Sheikh a

aDepartment of Mechanical Engineering, National Institute of Technology Srinagar 190006, India,
bDepartment of Physics, National Institute of Technology Srinagar 190006, India.

Keywords: ABSTRACT

Hot filament CVD Nano-crystalline diamond and microcrystalline diamond films have been
Nanocrystalline separately deposited on chemically treated titanium alloy (Ti6Al4V)
Microcrystalline substrates from methane/hydrogen (CH4/H2) gas mixture, using hot
Coefficient of friction filament chemical vapor deposition technique. The coatings have
Wear track architecture of Ti6Al4V/NCD and Ti6Al4V/MCD. The as grown nano-
Tribo-layer crystalline diamond and microcrystalline diamond films were
characterized using high resolution scanning electron microscope and
Ramans spectroscopy. The residual stresses along the surface of nano-
crystalline diamond coatings and micro-crystalline diamond coatings are
compressive in nature as shown by the Raman spectroscopy.
Corresponding author: Nanoindentation tests were also conducted using Berkovich nanoindenter
Sajad Hussain Din for the purpose of measurement of hardness and elastic modulus values.
Department of Mechanical The indentation depth for microcrystalline diamond coating was 65 nm,
Engineering, National Institute of whereas for nanocrystalline diamond coating, it was 72 nm.
Technology Srinagar 190006, India. Microcrystalline diamond and nanocrystalline diamond coatings have
E-mail: sajad_08phd12@nitsri.net yielded the super-hardness of ~55 G Pa and ~38 G Pa respectively. The
average coefficient of friction of microcrystalline diamond and
nanocrystalline diamond coatings decrease from 0.305-0.27 to 0.068-
0.053, respectively, when the load is increased from 1 N to 10 N. However,
for conventional Ti6Al4V substrate the average coefficient of friction
changes from 0.625 to 0.38 under the same input conditions.
2016 Published by Faculty of Engineering

1. INTRODUCTION used in joint implants need to have a good

Many researchers are working on the deposition
of diamond coatings on metallic substrates
because of their applications in medical field [1-
5]. Among these metals titanium and its alloys
are best suited for joint implants. The materials
biocompatibility, good fixation, chemical
inertness and load transfer capacity. Titanium
and its alloys have exceptional properties such
as: good specific strength, creep resistance,
corrosion resistance and biological inertness.
Due to these properties titanium and titanium

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alloys are widely used in medicine, aeronautics,
astronautics, chemical industry, power industry
and food industry [6-10]. Titanium and its alloys
are preferred for implants and surgical devices
because of its biocompatibility, resistance and
tolerance to body fluids. The mechanical and
tribological properties of titanium alloys
combine to provide implants that are extremely
damage-tolerant. The durability and service
performance of titanium by chemical vapor
deposition can markedly be enhanced [11-14].
By altering the microstructures of the substrate
materials the gas reactants severely deteriorate
the mechanical properties [1519]. Hydrogen is
crucial to synthesize quality diamond as it
preferentially etches non diamond carbon
species. But hydrogen also readily dissolves into
titanium and induces phase transformation and
increase embrittlement. [20-25]. A new hetero-
interface is introduced which complicates the
adhesion failure models of diamond coatings.
Thus preventing the formation of an
intermediate titanium carbide layer at the early
stage of CVD processing [26,27]. For smoothing
the surface of diamond films, various methods
have been developed. Various effective tools to
improve the tribological behavior of the
diamond film and lower the surface roughness
are nanocrystalline diamond (NCD) film,
substrate pretreatment, activated hydrogen
etching on surface, diamond polishing, growth
parameters control, addition of interlayers, solid
lubrication composite coating on diamond films
and alternate deposition of poly/nanocrystalline
diamond multilayer [28-35]. With the
development of the technique of CVD diamond
films, synthesis of nanocrystalline diamond
(NCD) and microcrystalline diamond (MCD)
films have gained wide spread research interest
[36,37]. NCD films possess fine diamond crystals
with small grain sizes ranging few nanometers
[38,39]. Compared with microcrystalline
diamond (MCD) films, NCD films have lower
hardness than MCD films due to the presence of
graphitic carbon in the films. Moreover, due to
high grain boundary density the NCD coatings
show surface hardness reduction [40-46].
Further, NCD films have smoother surface and
lower friction coefficient, which makes them
ideal coatings for tribological applications. K. D.
Bouzakis et al. studied the application of inclined
impact test for evaluating the temperature
dependent fatigue strength of NCD coatings
interface [47]. Moreover, it clarified the
influence of the NCD films adhesion on wear of
NCD-coated tools in milling aluminum alloy AA
7075 T6, which is a characteristic material for
aerospace applications. The NCD coating-
substrate interface fatigue strength is a key
aspect for measuring the coated tool life in
milling. The NCD coating-interface fatigue was
probed using inclined impact tests at ambient
and elevated temperatures. The investigations of
milling AA 7075 T6 showed that the NCD film-
substrate interface strength at elevated
temperatures is a key factor for explaining the
wear behaviour. An insufficient adhesion leads
rapidly to a delamination of the NCD-coating and
to a substrate revelation. The inclined impact
test is an efficient test method facilitating the
assessment of the NCD film substrate interface
at ambient and elevated temperatures [48-51].
Z. Doni et al. studied the evolution of the
functional integrity state in a comparative way
for two contact pairs (Ti6Al4V/Al2O3 and
Ti6Al4V/steel ball) in dry and corrosive
environment [52]. The investigation showed the
behavior of TI6Al4V alloy under reciprocating
wear sliding conditions in a comparative way for
two different counter materials, bearing steel
and ceramic balls (Al2O3 99.6 %) in dry and
corrosive environment (an aqueous solution of
3.5 % NaCl). It aimed to highlight the tribological
characteristics that showed invariability during
the test and provided a high level of functional
integrity of the surface. The conclusions drawn
from this work were as follows; (a) in dry
condition the Ti6Al4V/Al2O3 contact pair
showed a high functional integrity degree of the
surfaces in terms of surface quality,
characterized by roughness parameters Sa, Sq
and Sy, while for the Ti6Al4V/steel ball based on
the roughness parameter Sv; (b) in the case of
Ti6Al4V/steel ball contact pair a better
functional integrity (evaluated based on the
weight loss) occurred for higher applied loads
than in the case of lower loads; (c) from the
point of view of the electrochemical behavior a
higher functional integrity occurred in the case
of Ti6Al4V/Al2O3 contact pair at lower applied
loads (assessed through parameters Ecorr and
Icorr); (d) the electrochemical parameters for
Ti6Al4V/Al2O3 contact pair are at a lower level
than those of the Ti6Al4V/steel ball contact pair;
(e) the evolution of the roughness parameters
and the structural affinity between TI6Al4V alloy
and the bearing ball conduced to a higher
functional integrity level from the point of view
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 S.H. Din et al., Tribology in Industry Vol. 38, No. 4 (2016) 530-542

of the evolution of COF by comparison to
Ti6Al4V/Al2O3 contact pair [53-56].
A comparison has been documented between
nanocrystalline diamond (NCD) and
microcrystalline diamond (MCD) coatings on
titanium alloy (Ti6Al4V) substrates with
architectures of Ti6Al4V/NCD and
Ti6Al4V/MCD, using hot filament chemical
vapor deposition (HFCVD) technique. A detailed
analysis of friction and wear behavior in
ambient air for the two separate coatings has
been studied. Their tribological behavior is
studied as a function of the diamond coatings
characteristics. The effect of diamond quality on
the tribological behavior of the two types of
coatings has been investigated. The friction
characteristics of the diamond coated Ti6Al4V
substrates has been compared with uncoated
one, using ball on disc type linear reciprocating
micro-tribometer, sliding against smooth alumina
(Al2O3) ceramic ball under dry sliding conditions.
Al2O3 is a promising ceramic material used at high
temperature because of its excellent chemical
stability, good mechanical and electrical
properties, and wear and corrosion resistance.
2. EXPERIMENTAL DETAILS
17 mm, was placed above the samples. A rotary
pump was used to continuously pump the hot
filament chemical vapor deposition (HFCVD)
chamber, while methane (45 sccm) diluted in
excess of hydrogen (2250 sccm), were
quantified in at carefully controlled rates. The
assembly of gas distribution allowed the control
of the gas flow patterns in and around both the
filament assembly and the sample to ensure
uniformness in the coatings. A two color
pyrometer monitored the temperature of
tungsten filament. It was found to be 2200 C. A
k-type thermocouple was used to measure the
temperature of titanium alloy samples. The
thermocouple was located beneath the titanium
alloy samples. It was found to be 800 C. The
whole growth process was performed for 3
hours and the thickness of the film was
estimated to be 3 m. The detailed growth
parameters for depositing MCD and NCD films
are listed in Table 1.
Table 1. Growth parameters for the deposition of
MCD and NCD coatings.
Coating Substrate Substrate Filament Methane Duration
type Pressure Temp. (C) Temp. Conc. (hrs)
(Torr) (C) (CH4/H2)
%
MCD 36 800850 2200 2 3
NCD 12 800850 2200 4 3

Titanium alloy (Ti6Al4V) samples of 25 mm X 25 Raman spectra of the deposited films were
mm in dimensions were polished using silicon recorded using a confocal microscope (Alpha
carbide (SiC) and cleaned with deionized water. 300, Witec) with an excitation radiation of 532
The samples were etched in the solution of HF: nm of a Nd:YAG laser operated at less than 20
H2O2: DI water. The samples were rinsed in mW. The surface roughness and microstructure
deionized water three times for three minutes were observed using a field emission SEM
each. The samples were removed and blown dry (Quanta 3D, FEI). The detailed experimental
with air gun. The mirror finish was obtained by conditions are given in Table 2.
polishing the samples by diamond paste (1m).
An ultrasonicator was used to clean the samples Table 2. Experimental conditions.
with acetone for 30 minutes and then dried S. No. Parameters Operating Conditions
thoroughly by a hot drier. Dimethyl sulphoxide 1 Normal Load 1, 5, 10 N
(DMSO) solution containing diamond seedings of 2 Sliding Velocity 8 cm/s
size 4 m were used. Before deposition of nano- 3 Relative Humidity 70 ( 5)%
diamond films, the titanium alloy samples were 4 Duration of Rubbing 15 minutes
5 Surface Condition Dry
dispersed in it. This is done by using a low power
6 Materials Tested Ti6Al4V, MCD and NCD
ultrasonicator for 15 minutes. The samples were 7 Ball Material Alumina (Al2O3)
again cleaned with ethanol in an ultra-sonicator 8 Diameter of ball 6 mm
for 1 minute and placed inside the cold walled 9 Stroke length 5 mm
aluminum chamber of hot filament chemical 10 Frequency 2 Hz
vapor deposition (HFCVD) system (sp3 Diamond 11 Temperature 301 C
Roughness Factor (Ra)
Technologies Inc. USA). An array of 31 parallel Ti6Al4V 0.38 m
wires of (0.12 mm) diameter filaments, with 12 12
NCD 0.18 m
mm wire to wire spacing and standoff distance of MCD 0.26 m

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2.1 Method of deposition when sliding against smooth Al2O3 ceramic ball,
under the application of 1-10 N loads.
Hot filament chemical vapor deposition system
(HFCVD, Model 650 series, sp3, Diamond 3.1 Scanning Electron Microscopy
Technologies) with excellent process control
unit system was used for the deposition of The scanning electron microscopy was used to
diamond films, using the growth rate of 1 m/hr. study the morphology and grain size of diamond
Deposition parameters such as chamber films. With the increase in methane
pressure and methane concentration were concentration, secondary nucleation takes place
controlled easily during the experiment by using which changes the nature of existing grains from
throttle valve and mass flow controllers microcrystalline to nanocrystalline. Therefore, a
respectively. Hydrogen (H2) and methane (CH4) cauliflower type of morphology is generally
were used as the precursor gases and their flow shown by the top-layer (NCD) of multilayer CVD
rates were completely controlled using mass diamond coatings [57]. The MCD coating
flow controllers. An arrangement of tungsten exhibits clear multi-facet diamond crystals. Fig. 1
wires (diameter 0.12 mm) in systematic order (a) shows the general surface morphology of the
were used as hot filaments for the activation of NCD coating, whereas Fig. 1 (b) shows the
these precursor gases and the distance between surface morphology of the MCD coating.
filament and substrate was kept 17 mm. The
grain size of the diamond films were
automatically controlled by maintaining both
methane concentration and chamber pressure.
The toxic by product gases or exhaust gases
produced after the deposition process from the
HFCVD chamber were diluted using nitrogen
(N2) gas. However, N2 gases were used before
and after the diamond growth process of flush
the chamber. CVD chamber was made of
aluminum with cooling channels and the
temperature of the chamber was maintained at
~55 C using a circulating water chiller.

3. RESULTS AND DISCUSSIONS

The friction measurement was carried out for

the total sliding time of 20 minutes using ball on
disc type linear reciprocating micro-tribometer,
sliding against smooth alumina (Al2O3) ceramic
ball, under the application of increased normal
load. After friction measurement the wear tracks
formed on the surfaces of NCD, MCD and
Ti6Al4V were characterized using Raman
Spectroscopy and scanning electron microscopy
(SEM) techniques. However, the compositional
analysis for the formation of tribo-layer
observed on the wear tracks of NCD and MCD
coatings were confirmed using energy
dispersive spectroscopy (EDS) technique after
friction measurement. Also nanoindentation
tests were carried out using Berkovich
nanoindentation data. In this research, it is
aimed to find the variations in frictional Fig. 1. CVD-diamond coatings, (a) Surface morphology of
characteristics with the duration of rubbing NCD coatings, (b) Surface morphology of MCD coatings.

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3.2 Raman Spectroscopy
Raman spectroscopy was used to identify the
chemical structure and crystalline quality of the
diamond coatings. In this respect, stress free
crystalline diamond coating exhibits Raman
peak at 1332 cm1 corresponding to the first-
order phonon mode of T2g symmetry [42].
Raman spectrum of MCD coating confirms the
microcrystallinity. First order Raman peak shift
towards higher side centered at 1333 cm1 is
indicative of the presence of residual
compressive stress in both the coatings (Fig. 2).
Mainly, this compressive residual stress is due to
the difference in thermal expansion coefficients
of the substrate and coating [30-31].
Residual stresses can be calculated from = -
0.348 (vm v0) GPa for fundamental Raman peak
at vm, where v0 =1332 cm-1 and vm = 1333 cm-1.
Thus both MCD and NCD diamond coatings
contain a compressive stress of - 0.348 GPa,
where negative sign indicates compressive
stress. MCD exhibits columnar structure of
grains and faceted form of surface morphology.
In case of NCD coatings, two other peaks 1 and
3 are characteristics of in-plane (C-H) and
Fig. 2. Raman spectra of CVD-diamond coatings, (a) NCD and (b) MCD.
Fig. 3. (a) Loaddisplacement curve for NCD coating, (b) Loaddisplacement curve for MCD coating.
534
stretching (C-C) vibrational modes, respectively.
The presence of these modes was ascribed to the
formation of transpolyacetylene (TPA) chain in
the grain boundaries which is a well-known
characteristic of NCD coatings. A cauliflower
type of growth is generally seen with the NCD
coatings [36-46].
3.3 Mechanical and Tribological Properties
Figures 3 (a) and (b) show the load
displacement curves for the polished NCD and
MCD coatings. Indentation tests were performed
on each coating using nanoindentation
technique. It was evident from the load
displacement curves that the NCD coating was
less resistant to deformation in comparison to
the MCD coating. The indentation depth for MCD
coating was 65 nm, whereas for NCD coating, it
was 72 nm. The hardness of NCD and MCD
coatings were found to be ~38 GPa and ~55
GPa, respectively and these values are in
agreement with the earlier reports on diamond
films [58-60]. Hardness of NCD coatings was
found to be inferior to that of MCD coatings
because of the presence of non-diamond phases
at the grain boundaries.
 S.H. Din et al., Tribology in Industry Vol. 38, No. 4 (2016) 530-542

Fig. 4. Tribological characteristics of Ti6Al4V substrates sliding against alumina ball. (a) Coefficient of friction vs
duration of rubbing at 1 N, 5 N and 10 N, (b) Average coefficient of friction vs. normal load.

Fig. 5. Tribological characteristics of MCD coatings sliding against alumina ball. (a) Coefficient of friction vs
duration of rubbing at 1 N, 5 N and 10 N, (b) Average coefficient of friction vs. normal load.

Fig. 6. Tribological characteristics of NCD coatings sliding against alumina ball, (a) Coefficient of friction vs
duration of rubbing at 1 N, 5 N and 10 N, (b) Average coefficient of friction vs. normal load.

3.4 Friction Characteristics of the NCD and
MCD Coatings against Alumina Balls
Frictional characteristics of uncoated Ti6Al4V,
MCD and NCD were studied, sliding against
smooth Al2O3 ceramic ball using ball on disc type
linear reciprocating micro-tribometer, for a
sliding speed of 8 m/s and a load of 1 N, 5 N and
10 N. The average values of coefficient of friction
corresponding to virgin substrate, MCD and NCD
coatings were calculated as ~0.625-0.38,
~0.305-0.27 and 0.068-0.053, respectively by
increasing the normal load from 1-10 N, for the
total duration of 20 minutes. Tribological
characteristics of Ti6Al4V substrate sliding
against alumina ball is shown in figure 4. The
coefficient of friction decreases with increase in
load, shown in Fig. 4 (a) and the average
coefficient of friction, shown in Fig. 4 (b)
decreases from 0.625 to 0.38. Similarly, the
values of coefficient of friction corresponding to
MCD coating decrease under the same input

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operating conditions, as shown in Fig. 5 (a). The

average coefficient of friction in MCD coatings
decrease from 0.305 to 0.27, as shown in Fig. 5
(b). Tribological characteristics of NCD coatings
against alumina ball are shown in Fig. 6. The
NCD coatings show least coefficient of friction
among all the tested materials. The values of
coefficient of friction corresponding to NCD
coatings decrease under the same conditions. As
the load increases the coefficient of friction
decreases. The average coefficient of friction
decreases from 0.068 to 0.053. This observed low
friction coefficient of NCD coating in comparison
to that of MCD coating was observed due to the
presence of graphitic carbon phases at the grain
boundaries and also due to small grain size.
However, in case of MCD coating, the observed
initial higher value of friction coefficient is mainly
due to high surface roughness which becomes
smoother with sliding time.

The noisy fluctuations of the friction coefficient

have been observed at 1 N. These fluctuations
are due to surface roughness. At the beginning of
the applied load we can observe a peak which
corresponds to the adaptation of the contact of
both counter-faces. After the tests carried out in
these conditions, the diamond coating on the
disc is found to be intact as shown by the optical
microscope in Fig. 7 and indicated by the surface
roughness values which remain constant. Figure
7 (a), (b) and (c) show the surface morphology
of the wear tracks corresponding to virgin
Ti6Al4V substrate, MCD and NCD coatings at 10
N load, respectively. It has been clearly observed
from all the wear tracks that with the increase in
load the track width increases, and therefore
corresponding coefficient of friction decreases
for both the types of coatings. At the end of the
test carried out at 10 N, a wear track of 966 m,
673 m and 426 m in width was formed on the
Ti6Al4V substrate, MCD and NCD diamond Fig. 7. Images of wear track of CVD-diamond
coated discs, respectively. The detailed coatings, (a) surface morphology of virgin substrate,
mechanical and tribological experimental results (b) Surface morphology of NCD coatings, (c) Surface
morphology of MCD coatings.
are listed in Table 3.

Table 3. Mechanical and tribological results.

No variation of the total volume wear rate as a
function of sliding distance was evidenced
Variation in during the test because the vertical
Elastic
Material Hardness (H) Coefficient of
Modulus
Friction displacement was weak, a few micrometers at
the end of the test. At this point, the final wear
Ti6Al4V ~10 GPa ~510 ~0.625-0.38
rate of the ball is indeed about 3x10-17 m3 (N/m).
MCD ~55 G Pa ~1150 ~0.305-0.27 The wear of the diamond coated disc is too low
NCD ~ 38 G Pa ~1050 ~0.068-0.053 to be measured and the wear track is just

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 S.H. Din et al., Tribology in Industry Vol. 38, No. 4 (2016) 530-542
polished, as observed by SEM. This lack of
coating wear of the disc results from the short
test duration due to the ball wearing more
quickly. Alumina is a chemically inert ceramic
compound and sliding interaction of diamond
coatings against alumina material is purely
mechanical. The stable and low friction
coefficient of the NCD coating was attributed to
the chemical inertness of the mating materials
and also due to the continuous availability of the
lubricious non-diamond graphitic phases at the
grain boundaries of NCD coating. On the other
hand, slightly high and unstable friction
behavior was observed during the sliding of
MCD coating against alumina ball. The high run-
in friction behavior of the MCD coating was
attributed to its sharp and rough surface
asperities.
The tribological characteristics of CVD diamond
coatings depend on their grain size, grain
boundary strength and the presence of non-
diamond phases [61]. Also, the wear and friction
behavior of the tribo-contact pairs during dry
sliding depends on the extrinsic conditions such
as normal load, sliding velocity and mainly on
the type of interaction, whether mechanical or
chemical [62]. The contact between two sliding
surfaces occurs at asperities and these asperities
act as stress concentrators. CVD diamond
coatings are highly wear resistant and
chemically inert while sliding against most of the
ceramics and undergo only mechanical wear by
means of asperity fracture and abrasive damage
[63]. Grooves may form on the wear surfaces in
sliding contact due to the abrasive micro-wear
mechanisms [64]. Purely mechanical wear
produces rough contact surfaces and generally
shows stable friction behavior. Whereas, the
tribo-chemical interactions or tribo-oxidation of
the mating parts produces tribo-debris or tribo-
layer at the contact interface and modify the
contact stresses [65]. These tribolayers of the
reaction products are generally softer than the
substrate and affect the wear and friction
properties, especially under un-lubricated
conditions [66]. The friction characteristics of
diamond coating mainly depend on the counter
face material. In the case of non-diamond sliders,
the friction is influenced by the formation of a
transfer layer during run-in period. Bull et al.
found that the initial friction between CVD
diamond coating and sapphire was ~ 0.2, but
raised rapidly to ~ 0.6, which was attributed to
the formation of thick transfer layer [67].
Diamond is considered as self-lubricating
material and the low friction coefficient values
attained by many researchers is mainly due to
its extreme chemical inertness (no chemical
interaction/bonding) and sliding induced
graphitization or re-hybridization of carbon. The
chemistry of the sliding environment such as
relative humidity and use of vacuum, inert gases
or any other gases may affect the friction and
wear characteristics of the diamond films [68-
69]. The wear and friction of diamond coatings
are found to be normally low only in air and
relatively dry inert gas environment, whereas, in
vacuum and at high temperatures, the friction
and wear are much higher [70-71]. Gaseous
adsorbates such as hydrogen or oxygen can
effectively passivate the free -bonds on the
surface of diamond. When these -bonds
become highly passive, then the adhesion
component of the friction significantly reduces
and such diamond surface exhibits low friction
coefficient [72]. Roy et al. investigated the
friction response of the H-terminated and O-
terminated NCD films and found that the H-
terminated diamond films show low friction
coefficient in comparison to that of O-terminated
NCD films, which was attributed to the
hydrophobic nature of the former one [73].
High surface roughness of the faceted MCD
coatings has a detrimental effect on the friction
and wears characteristics [74]. However, these
coatings hardly show any wear but severely
abrade counter face materials due to the hard
and sharp asperities [75]. Generally MCD
coatings exhibit high run-in friction behavior
and stabilize to the lower value after a long
sliding distance. In the case of NCD coatings, the
friction coefficient falls to a much lower steady
state value soon after a short run-in period. The
low friction coefficient of the NCD coating is due
to the presence of non-diamond carbon phases
that are present at the grain boundaries. The
roughness of the NCD coatings will have less
detrimental effect on friction and wear
characteristics in comparison to MCD coatings
[76].
3.5 Wear track Analysis by Raman
Spectroscopy and EDS
Figures 8(a) and 8(b) show the Raman spectra of
wear tracks corresponding to NCD and MCD
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coatings at 10 N loads. The presence of residual
stresses in NCD and MCD wear tracks are
calculated from = -0.348 (vm v0) GPa for the
fundamental Raman peak at Vm = 1334 cm-1 [77].
Hence, wear track of both diamond coatings
contain residual compressive stresses of -0.348
GPa, under the application of normal load.
Fig. 8. Raman spectra of wear track of CVD-diamond
coatings, (a) NCD and (b) MCD.
Fig. 9. Energy dispersive X-ray analysis (EDXA) of
MCD Coatings.
538
Fig. 10. Energy dispersive X-ray analysis (EDXA) of
NCD Coatings.
Figures 9 and 10 show the compositional
analysis of the tribo-layer formed on the MCD
and NCD coatings, respectively. Tribo-chemical
wear and tribo-oxidation of Al2O3 under un-
lubricated conditions is a well-known
phenomenon and formation of tribo-debris or
tribo-layer is anticipated. Tribo-layer formation
was obvious from images of the wear tracks.
Tribo-layer formation was not continuous and it
was localized according to the contact asperities
and observed as smooth and shiny flakes [78].
No tribo-layer formation was observed on the
Al2O3 ball and the wear was mainly due to the
mechanical fragmentation and tribo-oxidation.
These small fragments and the tribo-products of
the Al2O3 ball are transferred to the wear track
on the NCD and MCD coatings [79]. Further, the
small fragments are mechanically smeared and
thermally treated during multi-cycle sliding
process to form glassy amorphous tribo-layer
[80]. Wear of the NCD and MCD coatings was
negligible during the sliding test, except the
blunting/crushing of sharp asperities/peaks of
the NCD and MCD coatings during the run-in time.
Further, the surface of the NCD and MCD coatings
was completely protected by the tribo-layer
formed with the aid of oxide tribo-products from
the Al2O3 ball. The wear of the Al2O3 ball was
mainly tribo-oxidation wear and the possible
mechanical (abrasive) wear only during run-in
time due to the interaction with the sharp
asperities of the NCD and MCD coatings.
4. CONCLUSION
MCD and NCD coatings have yielded the super-
hardness of ~55 GPa and ~38 GPa, respectively.
The observed low hardness of the NCD coating
in comparison to that of MCD coating was
attributed to the presence of non-diamond
 S.H. Din et al., Tribology in Industry Vol. 38, No. 4 (2016) 530-542
graphitic phases at the grain boundaries. NCD
coatings show low average friction coefficient of
~0.068-0.053 at different loads, when sliding
against Al2O3 ball, whereas MCD show average
friction coefficient of ~0.305-0.27, when sliding
against Al2O3 ball. The present analysis reveals
that the coefficient of friction of CVD-diamond
coatings decreases with the increase of load, and
becomes steady after certain duration of sliding.
The observed low coefficient of friction of NCD
coating is due to the presence of graphitic carbon
phases at the grain boundaries, and also because
of its small grain size. However, MCD coating has
shown the higher value of coefficient of friction
but higher hardness. It can be concluded that NCD
coatings increase the tribological properties
while as the MCD coatings enhance the
mechanical properties. Therefore, maintaining an
appropriate level of normal load and using
appropriate type of diamond coating, friction may
be kept to some lower value to improve
mechanical processes. These coatings are of great
interest for further analysis because of their
combination of hardness, low friction coefficient
and elastic modulus.
Acknowledgment
The Authors would like to thank Prof. M. S.
Ramachandra Rao, R. K. Dumpala, MSRC lab, IIT
Madras, for the deposition of coatings and Dr. C.
Anandan (Surface Engineering Division, NAL,
Bangalore, India) for carrying out tribological
tests, Prof. Kamal K. Kar, IIT Kanpur and G. N.
Lolpuri, A. H. Sofi, NIT Srinagar.
REFERENCES
[1] D. Rats, L. Vandenbulcke, R. Herbin, R. Benoit, R.
Erre, V. Serin and J. Sevely, Characterization of
diamond films deposited on titanium and its alloys,
Thin Solid Films, vol. 270, pp. 177-183, 1995.
[2] M.I. De Barros, L. Vandenbulcke and J.J. Blche,
Influence of diamond characteristics on the
tribological behaviour of metals against
diamond-coated Ti6Al4V alloy, Wear, vol. 249
no. 1-2, pp. 6777, 2001.
[3] M. Geetha, A.K. Singh, R. Asokamani and A.K.
Gogia, Ti based biomaterials, the ultimate choice
for orthopaedic implants - a review, Progress in
Materials Science, vol. 54, pp. 397425, 2009
[4] C.B. Collins, F. Davanloo, T.J. Lee, D.R. Jander, J.H.
You, H. Park and J.C. Pivin, The bonding of
protective films of amorphic diamond to
titanium, Journal of Applied Physics, vol. 71, pp.
3260, 1992.
[5] T.P. Ong and R.P. Chang, Properties of diamond
composite films grown on iron surfaces, Applied
Physics Letters, vol. 58, pp. 358, 1991.
[6] P.S. Weiser, S. Prawer and A. Hoffman, Carbon
diffusion in uncoated and titanium nitride
coated iron substrates during microwave
plasma assisted chemical vapor deposition of
diamond, Jounal of Applied Physics, vol. 72, pp.
4643, 1992.
[7] J. Spinnewyn, M. Nesladek and C. Asinari,
Diamond nucleation on steel substrates,
Diamond and Related Materials, vol. 2, no. 2-4,
pp. 361-364, 1993.
[8] X. Lei, B. Shen, S. Chen, L. Wang and F. Sun,
Tribological behavior between micro-and nano-
crystalline diamond films under dry sliding and
water lubrication, Tribology International, vol.
69, pp. 118127, 2014.
[9] F. Zivic, M. Babic, S. Mitrovic and P. Todorovic,
Interpretation of the Friction Coefficient During
Reciprocating Sliding of Ti6Al4V Alloy Against
Al2O3, Tribology in Industry, vol. 33, no. 1, pp.
36-42, 2011.
[10] J. Chraponski and W. Szkliniarz, Quantitative
metallography of two-phase titanium alloys,
Materials characterization, vol. 46, pp. 149 154,
2001.
[11] Y.S. Li, C.Z. Zhang, H.T. Ma, L.Z. Yang, L.L. Zhang,
Y. Tang, X.J. Li, L.L. He, R. Feng, Q. Yang and A.
Hirose, CVD nanocrystalline diamond coatings
on Ti alloy: A synchrotron-assisted interfacial
investigation, Materials Chemistry and Physics,
vol. 134, no. 1, pp. 145 152, 2012.
[12] M.I. De Barros, L. Vandenbulcke, J. Fontaine, G.
Farges, M. Vayer and R. Erre, Tribological
performance of diamond coated Ti6Al4V alloy
with respect to diamond characteristics, Surface
Coating Technology, vol. 127, no. 2-3, pp. 193
202, 2000.
[13] S.J. Askari, Tribological characteristics of
nanocrystalline diamond films grown on
titanium, Surface Engineering, vol. 25, pp. 482
486, 2009.
[14] L. Chandra, M. Chhowalla, G.A.J. Amaratunga and
T.W. Clyne, Residual stresses and debonding
of diamond films on titanium alloy substrates,
Diamond and Related Materials, vol. 5, no. 6-8,
pp. 674681, 1996.
539
 S.H. Din et al., Tribology in Industry Vol. 38, No. 4 (2016) 530-542
[15] T. Grogler, E. Zeiler, M. Dannenfeldt and S.M.
Rosiwal, R.F. Singer, Growth stages of chemical
vapor deposited diamond on titanium alloy
Ti6Al4V, Diamond and Related Materials, vol. 6,
no. 11, pp. 16581667, 1997.
[16] X.L. Peng and T.W. Clyne, Formation and
adhesion of hot filament CVD diamond films on
titanium substrates, Thin Solid Films vol. 293,
no. 1-2, pp. 261269, 1997.
[17] S.S. Perry, J.W. Ager II., G.A. Somorjai, R.J. McClell,
M.D. Drory, Interface characterization of
chemically vapor deposited diamond on
titanium and Ti6Al4V, Journal of Applied
Physics, vol. 74, no. 12, pp. 75427550, 1993 .
[18] S.J. Askari, F. Akhtar, G.C. Chen, Q. He, F.Y. Wang,
X.M. Meng and F.X. Lu, Synthesis and
characterization of nano-crystalline CVD
diamond film on pure titanium using Ar/CH4/H2
gas mixture, Materials Letters, vol. 61, no. 11-
12, pp. 21392142, 2007.
[19] M.A. Lowe, A.E. Fischer and G.M. Swain
Formation of a crack-free and debonding-
resistant boron-doped diamond thin film on
titanium using a dual-coating strategy, Jounal of
Electrochemical Society, vol. 153, no. 11, pp.
506511, 2006.
[20] E. Tal-Gutelmacher and D. Eliezer, Hydrogen
cracking in titanium-based alloys, Journal of
Alloys and Compounds, vol. 404406, pp. 621
625, 2005.
[21] D.S. Shin, I.M. Robertson and H.K. Birnbaum,
Hydrogen embrittlement of titanium: in situ
TEM studies, Acta Metallurgica, vol. 36, pp. 111
124, 1988.
[22] E. Buccioni, E. Braca, J.M. Kenny and M.L.
Terranova, Processingstructureadhesion
relationship in CVD diamond films on titanium
substrates, Diamond and Related Materials, vol.
8, no. 1, pp. 1724, 1999.
[23] Y.S. Li, Y. Tang, Q. Yang, C. Xiao and A. Hirose,
Growth and adhesion failure of diamond thin
films deposited on stainless steel with ultra-thin
dual metal interlayers, Applied Surface Science,
vol. 256, no. 24, pp. 76537657, 2010.
[24] A.C. Ferrari and J. Robertson, Raman
spectroscopy of amorphous, nanostructured,
diamondlike carbon, and nanodiamond, Philos.
Trans. Royal Society of London A, vol. 362, pp.
24772512, 2004.
[25] W. Kulisch, C. Popov, S. Boycheva, L. Buforn, G.
Favaro and N. Conte, Mechanical properties of
nanocrystalline diamond/amorphous carbon
composite films prepared by microwave plasma
chemical vapor deposition, Diamond and
540
Related Materials, vol. 13, no. 11-12, pp. 1997-
2002, 2004.
[26] S.J. Askari, G.C. Chen, F. Akhtar and F.X. Lu,
Adherent and low friction nano-crystalline
diamond film grown on titanium using
microwave CVD plasma, Diamond and Related
Materials, vol. 17, no. 3, pp. 294-299, 2008.
[27] Q.P. Wei, Z.M. Yu, L. Ma, D.F. Yin and J. Ye, The
effects of temperature on nanocrystalline diamond
films deposited on WC13wt.% Co substrate with
WC gradient layer, Applied Surface Science, vol.
256, no. 5, pp. 1322-1328, 2009.
[28] C. Y. Wang, F.L. Zhang, T. C. Kuang and C. L. Chen,
Chemical/mechanical polishing of
diamond films assisted by molten mixture of
LiNO3 and KNO3, Thin Solid Films, vol. 496, no. 2,
pp. 698-702, 2006.
[29] Q.F. Su, J.M. Liu, L.J. Wang, W.M. Shi and Y.B. Xia,
Effects of activated hydrogen etching on surface
roughness and optical properties of diamond
films, Scripta Materialia, vol. 54, no. 11, pp.
1871, 2006.
[30] S.K. Sarangi, A. Chattopadhyay and A.K.
Chattopadhyay, Effect of pretreatment methods
and chamber pressure on morphology, quality
and adhesion of HFCVD diamond coating on
cemented carbide inserts, Applied Surface
Science, vol. 254, no. 13, pp. 3721-3733, 2008.
[31] F.J.G. Silva, A.J.S. Fernandes, F.M. Costa, A.P.M.
Baptista and E. Pereira, A new interlayer
approach for CVD diamond coating of steel
substrates, Diamond and Related Material, vol.
13, no. 4-8, pp. 828-833, 2004.
[32] S.H. Seo, T.H. Lee and J.S. Park, Roughness
control of polycrystalline diamond films grown
by bias-enhanced microwave plasma-assisted
CVD, Diamond and Related Materials, vol. 12, no.
10-11, pp. 1670-1674, 2003.
[33] S.A. Catledge, P. Baker, J.T. Tarvin and Y.K.
Vohra, Multilayer nanocrystalline/
microcrystalline diamond films studied by laser
reflectance interferometry, Diamond and
Related Materials, vol. 9, no. 8, pp. 1512-1517,
2000.
[34] M. Vojs, M. Vesely, R. Redhammer, J. Janik, M.
Kadlecikova, T. Danis, M. Marton, M. Michalka
and P. Sutta, Double bias HF CVD
multilayer diamond films on WCCo cutting
tools, Diamond and Related Materials, vol. 14,
no. 3-7, pp. 613-616, 2005.
[35] S. Takeuchi, S. Oda and M. Murakawa, Synthesis
of multilayer diamond film and evaluation of its
mechanical properties, Thin Solid Films, vol.
398399, pp. 238-243, 2001.
 S.H. Din et al., Tribology in Industry Vol. 38, No. 4 (2016) 530-542
[36] Y.Q. Hou, D.M. Zhuang, G. Zhang, M.S. Wu and J.J.
Liu, Tribological performances of diamond film
and graphite/diamond composite film, Wear,
vol. 253, no. 7-8, pp. 711-719, 2002.
[37] K. Uppireddi, B.R. Weiner and G. Morell,
Synthesis of nanocrystalline diamond films by
DC plasma-assisted argon-rich hot filament
chemical vapor deposition, Diamond and
Related Materials, vol. 17, no. 1, pp. 55-59, 2008.
[38] P. Bruno, F. Benedic, A. Tallaire, F. Silva, F.J.
Oliveira, M. Amaral, A.S. Fernandes, G. Cicala and
R.F. Silva, Deposition of
nanocrystalline diamond films on silicon nitride
ceramic substrates using pulsed microwave
discharges in Ar/H2/CH4 gas mixture, Diamond
and Related Materials, vol. 14, no. 3-7, pp. 432-
436, 2005.
[39] P.W. May, J.A. Smith and Y.A. Mankelevich,
Deposition of NCD films using hot filament CVD and
Ar/CH4/H2 gas mixtures, Diamond and Related
Materials, vol. 15, no. 2-3, pp. 345-352, 2006.
[40] Y.P. Ma, F.H. Sun, H.G. Xue, Z.M. Zhang and M.
Chen, Deposition and characterization of
nanocrystalline diamond films on Co- cemented
tungsten carbide inserts, Diamond Related
Materials, vol. 16, no. 3, pp. 481-485, 2007.
[41] T. Sharda, T. Soga, T. Jimbo and M. Umeno,
Growth of nanocrystalline diamond films by
biased enhanced microwave plasma chemical
vapor deposition, Diamond and Related
Materials, vol. 10, no. 9-10, pp. 1592-1596, 2001.
[42] F. Sun, Y. Ma, B. Shen, Z. Zhang and M. Chen,
Fabrication and application of nano
microcrystalline composite diamond films on the
interior hole surfaces of Co cemented tungsten
carbide substrates, Diamond and Related
Materials, vol. 18, no. 2-3, pp. 276282, 2009.
[43] S. Prawer and R.J. Nemanich, Raman
spectroscopy of diamond and doped diamond,
Philos Trans R Soc Lond A, vol. 362, pp. 2537
2565, 2004.
[44] J. Gunnars and A. Alahelisten, Thermal stresses
in diamond coatings and their influence on
coating wear and failure, Surf Coat Technol, vol.
80, pp. 303312, 1996.
[45] R. Polini, E. Traversa, A. Marucci, G. Mattei and
G. Marcheselli, A Raman Study of Diamond
Film Growth on CoCemented Tungsten
Carbide, J Electrochem Soc, vol. 144, no. 4, pp.
13711375, 1997.
[46] H. Kuzmany, R. Pfeiffer, N. Salk and B. Gnther,
The mystery of the 1140 cm 1 Raman line in
nanocrystalline diamond films, Carbon, vol. 42,
no. 5-6, 911917, 2004.
[47] K.D. Bouzakis, G. Skordaris, E. Bouzakis, D.
Tasoulas, P. Charalampous, T. Kotsanis, S.
Kombogiannis and O. Lemmer, Explanation of
the Wear Behaviour of NCD Coated Carbide
Tools Facilitated by Appropriate Methods for
Assessing the Coating Adhesion Deterioration at
Elevated Temperatures, Tribology in Industry,
vol. 37, no. 3, pp. 309-319, 2015.
[48] M.A. Chowdhury, D.M. Nuruzzaman, A.H. Mia
and M.L. Rahaman, Friction Coefficient of
Different Material Pairs Under Different Normal
Loads and Sliding Velocities, Tribology in
Industry, vol. 34, no. 1, pp. 18-23, 2012.
[49] V. Bria, D. Dima, G. Andrei, I.G. Birsan and A.
Circiumaru, Tribological and Wear Properties of
Multi-Layered Materials, Tribology in Industry,
vol. 33, no. 3, pp. 104-109, 2011.
[50] S. Mitrovic, M. Babic, D. Adamovic, F. Zivic, D.
Dzunic and M. Pantic, Wear Behaviour of Hard
Cr Coatings for Cold Forming Tools Under Dry
Sliding Conditions, Tribology in Industry, vol. 34,
no. 1, pp. 44-48, 2012.
[51] M. Merklein, T. Schrader and U. Engel, Wear
Behavior of PVD-Coatings, Tribology in Industry,
vol. 34, no. 2, pp. 51-56, 2012.
[52] Z. Doni, M. Buciumeanu and L. Palaghian,
Topographic and Electrochemical Ti6Al4V Alloy
Surface Characterization in Dry and Wet
Reciprocating Sliding, Tribology in Industry, vol.
35, no. 3, pp. 217224, 2013.
[53] K. Bobzin, N. Bagcivan, M. Ewering and R.H.
Brugnara, Vanadium Alloyed PVD CrAlN
Coatings for Friction Reduction in Metal
Forming Applications, Tribology in Industry, vol.
34, no. 2, pp. 101-107, 2012.
[54] A. Sagalovych, V. Sagalovych, A. Kononyhin, V.
Popov, A. Lubchenko and A. Olejnik, The
Tribological Investigations of Multicomponent
Multilayered Ion-Plasma Coatings Avinit,
Tribology in Industry, vol. 33, no. 2, pp. 79-86,
2011.
[55] A.A. Minewitsch, Some Developments in
Triboanalysis of Coated Machine Components,
Tribology in Industry, vol. 33, no. 4, pp. 153-
158, 2011.
[56] F. ivi, N. Grujovi, S. Mitrovi, D. Adamovi, V.
Petrovi, A. Radovanovi, S. uri and N. Pali,
Friction and Adhesion in Porous Biomaterial
Structure, Tribology in Industry, vol. 38, no. 3,
61-37, 2016.
[57] W. Kulisch and C. Popov, On the growth
mechanisms of nanocrystalline diamond films,
Phys Status Solidi A, vol. 203, no. 2, pp. 203219,
2006.
541
 S.H. Din et al., Tribology in Industry Vol. 38, No. 4 (2016) 530-542
[58] R. Dumpala, N. Kumar, C.R. Kumaran, S. Dash, B.
Ramamoorthy and M.S. Ramachandra Rao,
Adhesion characteristics of nano-and micro-
crystalline diamond coatings: Raman stress
mapping of the scratch tracks, Diamond and
Related Materials, vol. 44, pp. 7177, 2014.
[59] R. Ramesham, T. Roppel and R.W. Johnson,
Characterization of polycrystalline diamond
thin films grown on various substrates, Thin
Solid Films, vol. 212, no. 1-2, pp. 96-103, 1992.
[60] W.C. Oliver, G.M. Pharr, An improved technique
for determining hardness and elastic modulus
using load and displacement sensing indentation
experiments, Journal of Materials Research, vol.
7, pp. 1564-1583, 1992.
[61] S.J. Bull and A. Matthews, Diamond for wear and
corrosion applications, Diamond and Related
Materials, vol. 1, no. 1011, pp. 10491064, 1992.
[62] V.A. Muratov, T. Luangvaranunt and T.E. Fischer,
The tribochemistry of silicon nitride: effects of
friction, temperature and sliding velocity,
Tribology International, vol. 31, no. 10, pp. 601
611, 1998.
[63] S.J. Bull, Tribology of carbon coatings: DLC,
diamond and beyond, Diamond and Related
Materials, vol. 4, no. 56, pp. 827836, 1995.
[64] K. Kato, Micro-mechanisms of wear wear
modes, Wear, vol. 153, no. 1, pp 277-295, 1992.
[65] A.S. Blomberg, S. Hogmark and J. Lu, An electron
microscopy study of worn ceramic surfaces,
Tribology International, vol. 26, pp. 369-381, 1993.
[66] T.E. Fischer and H. Tomizawa, Interaction of
tribochemistry and microfracture in the friction and
wear of silicon nitride, Wear, 105, 29-45, 1985.
[67] S.J. Bull, P.R. Chalker, C. Johnston and V. Moore,
The effect of roughness on the friction and wear
of diamond thin films, Surface and Coatings
Technology, vol. 6869, pp. 603-610, 1994.
[68] A. Erdemir, M. Halter, G.R. Fenske, C. Zuiker, R.
Csencsits, A.R. Krauss and D.M. Gruen, Friction
and Wear Mechanisms of Smooth Diamond Films
During Sliding in Air and Dry Nitrogen, Tribology
Transactions, vol. 40, pp. 667-675, 1997.
[69] N. Kumar, R. Radhika, A.T. Kozakov, K.J.
Sankaran, S. Dash, A.K. Tyagi, N.H. Tai and I.N.
Lin, Humidity-dependent friction mechanism in
an ultrananocrystalline diamond film, Journal of
Physics D: Applied Physics, vol. 46, no. 27, pp.
275501, 2013.
542
[70] S. Chandrasekar and B. Bhushan, The role of
environment in the friction of diamond for
magnetic recording head applications, Wear,
vol. 153, pp. 79-89, 1992.
[71] K. Miyoshi, R.L.C. Wu, A. Garscadden, P.N. Barnes
and H.E. Jackson, Friction and wear of plasma-
deposited diamond films, Journal of Applied
Physics, vol. 74, pp. 4446-4454, 1993.
[72] A. Erdemir, Friction and wear of diamond and
diamond-like carbon films, Proceedings of the
Institution of Mechanical Engineers, Part J:
Journal of Engineering Tribology, vol. 216, pp.
387-400, 2002.
[73] M. Roy, S. Ghodbane, T. Koch, A. Pauschitz, D.
SteinmllerNethl, A. Tomala, C. Tomastik and F.
Franek, Tribological investigation of
nanocrystalline diamond films at low load under
different tribosystems, Diamond and Related
Materials, vol. 20, pp. 573-583, 2011.
[74] H. Miki, A. Tsutsui, T. Takeno and T. Takagi
Friction properties of partially polished CVD
diamond films at different sliding speeds,
Diamond and Related Materials, vol. 24, pp. 167-
170, 2012.
[75] I.P. Hayward, I.L. Singer and L.E. Seitzman, Effect
of roughness on the friction of diamond on cvd
diamond coatings, Wear, vol. 157, pp. 215-227,
1992.
[76] I.S. Forbes and J.I.B. Wilson, Diamond and hard
carbon films for microelectromechanical
systems (MEMS)a nanotribological study,
Thin Solid Films, vol. 420421, pp. 508-514,
2002.
[77] R. Polini, E. Traversa, A. Marucci, G. Mattei and
G. Marcheselli, A Raman Study of Diamond Film
Growth on Co-Cemented Tungsten Carbide,
Journal of the Electrochemical Society, vol. 144,
pp. 1371-1375, 1997.
[78] K. Holmberg, A. Matthews and H. Ronkainen,
Coatings tribologycontact mechanisms and
surface design, Tribology International, vol. 31,
pp. 107-120, 1998.
[79] M. Godet, The third-body approach: A
mechanical view of wear, Wear, vol. 100, pp.
437-452, 1984.
[80] A. Blomberg, S. Hogmark and J. Lu, An electron
microscopy study of worn ceramic surfaces,
Tribology International, vol. 26, pp. 369-381,
1993.
 Vol. 38, No. 4 (2016) 543-551

Tribology in Industry

RESEARCH
www.tribology.fink.rs

The Wear behavior of UHMWPE against Surface

Modified CP-Titanium by Thermal Oxidation

B.T. Prayoga a, S. Suyitno a, R. Dharmastiti a

a Departement of Mechanical Engineering, Universitas Gadjah Mada, Bulaksumur 55281 Yogyakarta, Indonesia.

Keywords:
Sliding wear
UHMWPE
CP-titanium
Thermal oxidation duration
Corresponding author:
Benidiktus Tulung Prayoga
Departement of Mechanical
Engineering,
Universitas Gadjah Mada,
Bulaksumur 55281, Yogyakarta
Indonesia.
E-mail: beni@ugm.ac.id
ABSTRACT
The effects of thermal oxidation duration on hardness, roughness, and
wettability of the CP-titanium surfaces were investigated in this paper.
The thermal oxidation treatment was done at 700 oC for 12-36 hours in an
air atmosphere. The wear behavior of the UHMWPE sliding against
treated thermal oxidation of the CP-titanium was tested by a pin-on-plate
tribometer under lubrication of the solution of 75 % distilled water and 25
% bovine serum. The results showed that the layer of the oxide titanium
was formed on the surface after being treated by the thermal oxidation for
12-36 hours. The oxide titanium layer was dominated by rutile form of
TiO2, that offers an improvement of hardness and wettability of the CP-
titanium surfaces. The average wear factor of the UHMWPE reduced
significantly when the sliding against of the CP-titanium was modified by
the thermal oxidation, and the lowest average wear factor was reached
when the sliding against the 12 hour oxidized CP-titanium counterfaces.
2016 Published by Faculty of Engineering

1. INTRODUCTION low friction, and biocompatible. The bearing that

In general, artificial human joints are composed
of at least two components that are arranged,
such a manner so that it can function like natural
joints. Metallics and polyethylene biomaterial
are the most common materials used as a joint
implant component. They are combined
particularly in the joint implant, that is, one of
the components is made of metal, and others of
the polyethylene [1]. The most popular type of
polymer in the joint implant is called ultra-high
molecular weight polyethylene (UHMWPE). It
has been widely used as a bearing material in
total joint replacement, especially in hip and
knee implant, due to its high wear resistance,
made of UHMWPE have excellent performed in
vivo. The only major issue is wear and the wear
particles on the in vivo durability of the
prosthesis [2].
The metallic biomaterials, titanium, stainless
steel, and Co Cr are used in the overwhelming
majority of the joint implants [3,4]. Recently,
titanium and titanium alloys are intensively
studied for use in medicine, particularly in
dental and orthopedic [5]. It is because the
titanium and titanium alloys have higher
mechanical properties, lightweight, corrosion-
resistant, non-toxic, low modulus, non-magnetic
and higher biocompatibility than stainless steel

543
 B.T. Prayoga et al., Tribology in Industry Vol. 38, No. 4 (2016) 543-551
or cobalt alloy [5,6]. Additionally, they are very
reactive metals and will quickly react to form
oxide layer when exposed to the atmosphere.
The compact oxide layer will form easily at the
surface, so that they have excellent corrosion
resistance [79]. The oxide layer is compact and
stable, but the layer which is automatically
formed is thin, and it is not enough to improve
the wear resistance. All joint prostheses are
articulated with a boundary or mixed lubrication
that allows the bearing surface in the contact
and results in the generation of wear debris [11].
In the total joint replacement, the UHMWPE
wear debris is the main issue due to the wear
debris is recognized as a leading cause of failure
of the total joint replacement [12]. The debris of
the wear will cause damage to body tissue
surrounding the implant [3,12]. The weakness of
the titanium and titanium alloy are poor
tribology properties when rubbing against itself
or other materials [14]. Therefore, it has limited
their extensive use in biomedical implant
[13,14].
The one of the methods to improve the
tribological properties of titanium is the surface
modification. Several studies have been
conducted to investigate surface modification of
the titanium and titanium alloy material through
anodic oxidation, DLC coating, SMAT, and
thermal oxidation to improve the wear behavior
[1316]. Thermal oxidation (TO) is very
straightforward and inexpensive method.
Therefore, this treatment is very promising for
improvement of the wear behavior of the
titanium which would be used as the load-
bearing implant [19,20].
The hard and thick TiO2 layers can be obtained on
the surface of the CP-titanium by the thermal
oxidation method. This method exploits the low
resistance of the titanium to oxidation and
oxygen diffusion at high temperature. According
to previous studies [8,19,21], the two primary
parameters to obtain optimum TiO2 layer are
temperature and duration of the thermal
oxidation treatment. Satendra Kumar et al. [23]
investigated the formation of rutile TiO2 during
thermal oxidation of CP-Ti was minimal at 650 oC.
At the low temperature (below 500 oC) the kinetic
reaction was slow, but at a high temperature
(above 800 oC) would affect on the spallation of
the oxide layer, so the oxidation temperature was
chosen as an optimum temperature between 600
544
and 700 0C [24]. The long duration (more than 72
hours) gave the effect of the spallation of the
oxide layer, but if the duration was very low (less
than 5 hours) the oxide layer formed was thin
[25]. In the previous investigation, the thermal
oxidation at 700 oC for several duration could
reduce the wear of the UHMWPE-CP-
titanium/Ti64 counterparts. Wang et al. [26]
investigated the wear of Ti64 that was treated by
the TO and UHMWPE; they found that the wear
volumes decreased 68 % for treated samples
compared to the untreated specimen. Xiong et al.
[27] investigated the wear properties of the
UHMWPE sliding against modified titanium
alloys. The friction coefficients of the UHMWPE
sliding against thermal oxidation treated
specimens under bovine serum that were
decreased by 63 %. All studies used the pin on
disk tribometer.
A linear reciprocating movement generated on
the uni-directional pin on plate tribometer is a
more realistic motion for investigating wear
mechanism of the joint implant material. The
intermittent motion at the end of stroke can
represent the natural joint movement [27,28].
The aim of this study was to investigate whether
the effect of the duration of the thermal
oxidation on the surface treatment of the CP
titanium at 700oC was able to reduce the wear of
the UHMWPE tested using a reciprocating pin-
on-plate tribometer.
2. MATERIAL AND METHODS
2.1 Materials preparation
The CP-titanium cast was used in this study. The
specimens as-received from the investment
casting cut by milling machine to the dimension
of 55 mm x 18 mm x 3 mm. After that, the
specimens were annealed at 900oC for 2 hours in
an argon environment and then cooled in the
furnace to obtain a uniform initial
microstructure condition. The specimens were
ground with abrasive paper #600, 1200, 5000,
and finished with diamond paste to obtain
average surface roughness (Ra 0.1 m). All of
the specimens were ultrasonically cleaned in
distilled water for 15 minutes and degreased
with alcohol before treatment. In this study, all
of the thermal oxidation processes were
performed at 700 oC.
 B.T. Prayoga et al., Tribology in Industry Vol. 38, No. 4 (2016) 543-551
The oxidation process was performed in a
chamber furnace (Thermo Scientific, USA) in an
air atmosphere. The specimens were heated in
room temperature at 700 oC with the ramp rate
was the default of the furnace setting. The holding
time was set 12 and 36 hours (not including the
ramp). After the holding time had been reached,
the specimens were cooled naturally in the
furnace. The specimens were weighed prior and
after oxidation with microbalance with an
accuracy 0.00001 g (Ohaus).
2.2 Surface characterizations
The specimen surface roughness was measured
using a contact stylus profilometer (Surfcorder,
Kosaka, Japan). The measurement was
conducted at 19 different locations to obtain the
medium arithmetic value (Ra) of the samples.
All samples were cleaned up using alcohol,
rinsed in distilled water, and dried prior to the
observation and measurement.
The surface morphology of the oxide layer
formed in surface CP-titanium was examined
using a scanning electron microscope (JSM-
6510LA, JEOL, Ltd., Japan). The examinations
were conducted on the untreated, 12, and 36
hours treated sample. X-ray diffraction (XRD)
was undertaken using Monochromatic X-ray
radiation from a copper tube with a wavelength
of K1 = 1.5406 to identify phases presence in
the thermally oxidized samples. The X-ray tube
was supplied by an electric current at a voltage
of = 40 kV and intensity of I = 30 mA. The
scanning was done in an angular range from 10o
to 90o.
The surface hardness examinations were
determined using a Vickers microhardness
tester (Buehler, USA). The tests were conducted
with indentation load 0.49 N for 15 s. The
measurement of the average hardness was done
for seven different locations at the surface.
The surface wettability was taken from the
measurements of the drop static contact angle
between the bovine serum solution (75 %
distilled water and 25 % bovine) and sample
surface at room temperature. A bovine solution
droplet was deposited five times at three
different locations on the surface of each sample.
The droplet of the bovine solution image was
obtained using a USB digital microscope
attached in water drop equipment (Gaosuo,
China) and then the droplet contact angles were
analyzed.
2.3 Unidirectional reciprocating wear test
The wear test was performed for untreated and
the oxidized CP-titanium specimen with the
UHMWPE in the 6 station unidirectional
reciprocating pin-on-plate tribometer. The device
was built in our laboratory. The flat-ended
UHMWPE pins having the dimension of the 9
mm, and 15 mm length were prepared as
counterpart specimen. Prior to wear testing, all the
UHMWPE pin specimens were allowed to soak in
distilled water for 2 weeks to prevent the moisture
uptake during the wear test. The density of the
UHMWPE was assumed 0.9737 gr/cm3.
The UHMWPE pins were installed at the upper
of the plate sample moving unidirectional
reciprocating. The normal load on the pin was
180 N which was provided with the lever
mechanism, so that it corresponded to 2.8 MPa
of nominal contact stress. The frequency for
reciprocating motion was set 1 Hz and the
sliding distance was set to 25 mm giving a
sliding velocity of 50 mm/s. The wear tests were
done at a room temperature. The lubricant used
in this study was a solution of 25 % bovine
serum and 75 % of distilled water. To prevent
the lubricant from the bacterial growth the
sodium azide were added (0.1 % v/v).
The wear tests were run with a total sliding
distance of about 75 kms. The tests were
interrupted at regular intervals 12.5 kms and the
wear was measured by the weight loss. The wear
device was shut off then the pins and plates were
removed for weighing every regular interruption.
Prior to weighing, the pins and plates were
cleaned with an ultrasonic cleaner in distilled
water for 15 minutes and lapped with tissue.
The samples were weighed using a microbalance
with an accuracy 0.00001 g (Ohaus). The
average wear factor was calculated as
accumulated volume loss (mm3), divided by the
unit of force (N) times total sliding distance (m).
The average wear factor (WF) was determined
from Eq (1):
Wear Volume (mm3 )
WF (1)
Load ( N ) x sliding dist (m)
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3. RESULT AND DISCUSSION layer which covered the entire of the sample
surface.
3.1 Microstructure initial state

Microscopic metallographic examinations

showed that the CP-titanium cast after being
annealed at 900 oC for 2 hours was characterized
by a grain structure with the equiaxial grains
shape (Fig. 1).

Fig. 2. XRD patterns of untreated and thermal

oxidation of CP-titanium at 700 oC for 12 and 36 hours.

Fig. 1. The microstructure CP-titanium cast after

annealed at 900 oC for 2 hours.

3.2 Surface morphology

Figure 2 shows the diffractogram obtained for

CP-titanium samples untreated and TO-treated
at 700 C for 36, 12 hours. According to JCPDS
card (No. 88-1175), the peaks at diffraction
angle 2 = 27o, 36o , and 55o indicating TiO2 in
rutile phase [30]. Thermal oxidation treatment
samples showed peaks as the rutile phase were
dominant. This condition means that the
oxidized surface is mainly composed by the
rutile form of TiO2. Increasing the duration of
the treatment, the composition of the oxide layer
would be dominated by rutile TiO2. It has been
reported that the thermal oxidation of pure
titanium at high temperature (650-700 oC) and
for short times to obtain to the formation of
rutile TiO2 [8,23,28]. The oxidation temperature
and duration of treatment employed in this
study were sufficient for the formation of the
rutile oxide. As known, rutile phase is a stable
structure of TiO2 with high hardness so the
thermal oxidation treatment of the CP-titanium
would improve the wear behavior [10]. The SEM
images of the surface sample for untreated and
treated at 700 C for 12 and 36 hours are shown
in Fig. 3. The surface of the sample of the CP- Fig. 3. The SEM image of the surface sample, (a)
titanium that was treated at the temperature untreated, (b) treated at 700 oC for 12 and (c) treated
700 C revealed the existence of a uniform oxide at 700 oC for 36 hours.

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After 12 hours of the oxidation, the oxide layer

covers throughout the surface (Fig. 3b). The
grains of the oxides formed were noticeably
larger after being treated at 700 C for 36 hours
than 12 hours. The oxide layer was relatively
smooth for a sample oxidized for 12 hours but it
would be relatively coarse when oxidation time
was increased to 36 h. According to the literature
[32], the formation of an oxide layer on the
surface of pure metal were done in four steps,
first, oxygen adsorption at the surface, second,
the formation of oxide nucleation, third, lateral
growth of the nuclei and the last, formation of a
compact oxide layer. When the lateral growth of
the nuclei is terminated, the metal surface is
completely covered by the oxide layer. Fig. 4 The surface microhardness of untreated and
treated CP-titanium.
From the Fig. 3, It can be seen that the oxide
layer grows through the formation and
agglomeration that become very fine grains of
oxide particles (Fig. 3b). Along with increasing
time of the treatment (36 hours), the oxide
particles would grow to be larger (Fig. 3c). This
is similar to the study of the growth of the oxide
layer was found in a paper [33].

Figure 4 shows the surface microhardness of

untreated and thermal oxidation treated samples
measured on the surface of the oxide layer. The
surface hardness of the treated CP-titanium at 700
OC for 36 hours (Hv = 8.3 GPa) was approximately

three times higher than the surface hardness of the

untreated CP-titanium (Hv = 2.78 GPa). It can be
seen that the hardness enhances by the increased
Fig. 5 The surface roughness of untreated and treated
duration of the treatment. The thermal oxidation CP-titanium.
conducted for only 12 h at a temperature of 700
C made it possible to obtain an oxide layer
almost thrice harder than the untreated
material. But in the longer duration of treatment
no increase of hardness that did not significantly
increased. This is similar to the studies that
reveal the increase of the duration of the
treatment would increase the microhardness
[33]. In addition, the surface roughness also
increased by the increase of the duration of the
thermal oxidation treatment (Fig. 5). Compared
with the untreated sample, the surface
roughness of the treated sample increased
significantly about two times. The increase of the
surface roughness was consistent with the
papers [20,23,33]. Surface roughness before the
thermal oxidation (Ra = 0.1 m) increased to
0.26 m and 0.30 m in the thermal oxidation at Fig. 6 The static contact angle of untreated and
700 oC for 12 and 36 hours, respectively. treated CP-titanium.

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The increase of the surface roughness was
caused by the growth of the oxide layer on the
surface. This can be described by the formation
of large agglomerations oxide grains on the
surface. Grains of the oxide began to cover the
surface and grow larger in size when the
duration increased (Fig. 3).
however, the oxide layer formed on the surface
of the samples were able to reduce the wear of
the UHMWPE. Specifically for couples the
UHMWPE and CP-titanium-treated, showed that
the surface roughness also affected the wear
though it was not significant.

The effect of the thermal oxidation duration in

the contact angle is shown in Fig. 6. The static
contact angle of the untreated sample was about
67o. However, the contact angle of treated
sample for 12 and 36 hours were lower than
that of the untreated sample. The decrease was
about 12-20o. The lower static contact angle
means the wettability of the surface improves.
This is in good agreement with the studies that
reveal the increase surface roughness would
reduce static contact angle [35]. The good
wettability or low contact angle means the
lubricant covered the sample surface easily and
it potentially reduced the friction and wear. The
film of lubricant that covers the surface will Fig. 7 Effects of thermal oxidation duration of CP-
prevent the surface from rubbing each other. titanium counterfaces on the wear of UHMWPE.

3.3 Tribological test

The graphic of the volume loss compared sliding

distance, for the UHMWPE sample against
untreated and treated thermal oxidation of the
CP-titanium plate as shown in Fig. 7. It is obvious
by comparing untreated and treated sample that
the wear of the UHMWPE sample was
significantly reduced by treated thermal
oxidation of the CP-titanium counterface
irrespectively with the duration of the treatment.

The average wear factor for the UHMWPE pins

against untreated and thermal oxidation CP-
titanium are shown in Fig. 8. It was noticed that
the wear factor decreased significantly from
1.25 x 10-7 mm3/N m to 3.54 x 10-8 mm3/N m
and 5.87 x 10-8 mm3/N m after the thermal
oxidation for 12 and 36 hours, respectively. The
CP-titanium sample treated for 12 hours showed
the fewest wear of the UHMWPE compared with
the 36 hours treated and untreated. The average
wear factor of the UHMWPE pins against 12
hours and 36 hours thermal oxidation treated
samples were reduced 3.5 and 2 times that of
the UHMWPE pins against untreated CP-
titanium respectively. Although the samples
subjected to thermal oxidation had a higher
surface roughness than the untreated samples,
Fig. 8 Average wear factor of UHMWPE sliding
against untreated and treated CP-titanium.
The figures of the worn surfaces of the CP-
titanium plate and pin tested under bovine serum
as lubricant are shown in Fig. 9. The wear track of
the untreated CP-titanium plate (Fig. 9a) was
marked by relatively deep and wide grooves.
Thus is an indication of severe abrasive wear.
This matched with the UHMWPE counterface also
experiences severe damage marked by several
grooves (Fig. 9b). The different wear track can be
seen in Figs. 9c-9f, which found only a few
scratches on the surface of the treated CP-
titanium and UHMWPE surface. This indicates

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that the thermal oxidation treatment can improve
wettability and reduce wear.
The surface of the CP-titanium was covered by
the oxide layer composed of TiO2 oxide which
improved hardness and wears resistance. The
formation of TiO2 can be held responsible for an
increase the surface roughness and enhance in
the wettability. The coarse grain oxide will offer
greater surface contact and provide micro
spaces between grains (Fig. 3) that play as
lubricants pocket to increase hydrodynamic
lubrication which results in a decrease of wear
rate. The thermal oxidation treatment can be
suitable to reduce the wear of corresponding
UHMWPE and hinder the generation of abrasive
particles. In the case of the untreated CP-
titanium counterfaces, although with smooth
surfaces, the average wear factor is higher than
the treated sample, because the auto oxide layer
is thin so that it can not inhibit the wear sliding.
The thin oxide layer will peel off as wear debris
or will penetrate in the UHMWPE and lead to
scratching of the CP-titanium surface which, in
turn, leads to severe abrasive wear to both
articulate surfaces. The wear mechanism of the
UHMWPE/untreated CP-titanium couple may be
attributed to the mechanisms of third body
wear. This study has shown that the wear of the
UHMWPE was greater against CP-titanium plate
treated for 36 hours than against 12 hours
treated plates, due to the roughening by thermal
oxidation duration. In the case of the rough CP-
titanium thermal oxidation treated surface, the
coarse of oxide grains accelerated the wear
because of the high point or asperities on the
surface to produce wear by an abrasive wear
mechanism.

Fig. 9. Worn surfaces of plate and pins (a) untreated CP-titanium; (b) UHMWPE sliding against untreated CP-
titanium; (c) 12 hours thermal oxidation CP-titanium; (d) UHMWPE sliding against 12 hours thermal oxidation
CP-titanium; (e) 36 hours thermal oxidation CP-titanium; (f) ) UHMWPE sliding against 36 hours thermal
oxidation CP-titanium. The arrows indicate as sliding direction.

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4. CONCLUSION
The rutile TiO2 layer was formed on the surface
of the CP-titanium after the thermal oxidation
treatment at 700 oC in an air atmosphere. The
surface microhardness of the treated CP-
titanium for 36 hours was 8.3 GPa that was three
times higher than that of the untreated CP-
titanium. The thermal oxidation treatment of the
CP-titanium could reduce the UHMWPE average
wear factor with the reduction of 71.6 % and
52.9 % for 12 and 36 hours, respectively. The
biotribological test revealed that the thermal
oxidized CP-titanium decreased the wear of the
UHMWPE, which indicated that the thermal
oxidation treatment of the CP-titanium could be
a potential candidate of the surface treatment
for artificial joints.
Acknowledgement
This work was financially funded by the Ministry
of Research, Technology and Higher Education
of the Republic of Indonesia through Doctoral
Program Scholarship. The authors are grateful to
Mr. Arfan Abdillah for his contribution to some
parts of this experiment.
REFERENCES
[1] S.M. Kurtz, UHMWPE Biomaterials Handbook, 2
nd. Burlington, MA, USA: Academic Press, 2009.
[2] F. ivi, M. Babi, S. Mitrovi, D. Adamovi and S.
Pelemis, Friction Coefficient of UHMWPE
During Dry Reciprocating Sliding, Tribology in
Industry, vol. 36, no. 3, pp. 281286, 2014.
[3] M. Niinomi, Recent research and development
in titanium alloys for biomedical applications
and healthcare goods, Sci. Technol. Adv. Mater.,
vol. 4, no. 5, pp. 445454, 2003.
[4] R. Geetha, M., Singh, A.K., Asokamani and A.K.
Gogia, Ti based biomaterials, the ultimate choice
for orthopaedic implants - A review, Prog. Mater.
Sci., vol. 54, no. 3, pp. 397425, 2009.
[5] F.A. Shah, M. Trobos, P. Thomsen and A.
Palmquist, Commercially pure titanium (cp-Ti)
versus titanium alloy (Ti6Al4V) materials as
bone anchored implants - Is one truly better
than the other?, Mater. Sci. Eng. C, vol. 62, pp.
960966, 2016.
[6] M. Niinomi, Mechanical biocompatibilities of
titanium alloys for biomedical applications, J.
550
Mech. Behav. Biomed. Mater. I, pp. 3042, 2008.
[7] M. Kulkarni, A. Mazare, E. Gongadze, .
Perutkova, V. Kralj-Igli, I. Miloev, P. Schmuki, A
Igli and M. Mozeti, Titanium nanostructures
for biomedical applications, Nanotechnology,
vol. 26, pp. 118, 2015.
[8] B. Li, J. Li, C. Liang, H. Li, L. Guo, S. Liu and H.
Wang, Surface roughness and hydrophilicity of
titanium after anodic oxidation, Xiyou Jinshu
Cailiao Yu Gongcheng/Rare Met. Mater. Eng., vol.
45, no. 4, pp. 858862, 2016.
[9] K. Anioek, M. Kupka, A. Barylski and G. Dercz,
Mechanical and tribological properties of oxide
layers obtained on titanium in the thermal
oxidation process, Appl. Surf. Sci., vol. 357, pp.
14191426, 2015.
[10] D. Siva Rama Krishna, Y. L. Brama and Y. Sun,
Thick rutile layer on titanium for tribological
applications, Tribol. Int., vol. 40, pp. 329334,
2007.
[11] R. Dharmastiti, D.C. Barton, J. Fisher, A. Edidin
and S. Kurtz, The wear of oriented UHMWPE
under isotropically rough and scratched
counterface test conditions, Biomed. Mater.
Eng., vol. 11, pp. 241256, 2001.
[12] M.A. Hussein, A.S. Mohammed, N. Al-aqeeli and
S. Arabia, Wear Characteristics of Metallic
Biomaterials: A Review, Materials (Basel)., vol.
8, pp. 27492768, 2015.
[13] M.A. Gepreel and M. Niinomi, Biocompatibility of
Ti-alloys for long-term implantation, J. Mech.
Behav. Biomed. Mater., vol. 20, pp. 407415, 2013.
[14] D. Tigani, M. Fosco, R. Ben Ayad and R. Fantasia,
Orthopaedic implant materials and design, in
Wear of orthopaedic implants and artificial joints,
S. Affatato, Ed. Cambridge, UK: Woodhead
Publishing Limited, 2012, p. 137.
[15] P.A. Dearnley, K.L. Dahm and H. imenoglu, The
corrosion wear behaviour of thermally oxidised
CP-Ti and Ti 6Al 4V, Wear, vol. 256, pp. 469
479, 2004.
[16] H.J. Long and M. Rack, Titanium alloys in total
joint replacement--a materials science
perspective, Biomaterials, vol. 19, no. 18, pp.
16211639, 1998.
[17] A.F. Yetim, Investigation of wear behavior of
titanium oxide films, produced by anodic
oxidation, on commercially pure titanium in
vacuum conditions, Surf. Coatings Technol., vol.
205, no. 6, pp. 17571763, 2010.
[18] A. Escudeiro, M.A. Wimmer, T. Polcar and A.
Cavaleiro, Tribological behavior of uncoated and
DLC-coated CoCr and Ti-alloys in contact with
 B.T. Prayoga et al., Tribology in Industry Vol. 38, No. 4 (2016) 543-551

UHMWPE and PEEK counterbodies, Tribol. Int., [28] S. Liza, A.S.M.A. Haseeb, H.H. Masjuki and A.A.
vol. 89, pp. 97104, 2015. Abbas, The Wear Behaviour of Crosslinked
UHMWPE under Dry and Bovine Calf Serum
[19] M. Wen, C. Wen, P.D. Hodgson and Y.C. Li,
Lubricated Conditions, Tribol. Trans., vol. 56, pp.
Tribological Behaviour of Pure Ti with a
130140, 2013.
Nanocrystalline Surface Layer Under Different
Loads, Tribol. Lett., vol. 45, no. 1, pp. 5966, 2012. [29] F.J. Gonzlez-mora, V.A. Hoffmann, M. Stroosnijder,
R. Espinar, E. Llamas, J.M. Mariano and F. Gil,
[20] S. Wang, Z. Liao, Y. Liu and W. Liu, Influence of
Influence of different CoCrMo counterfaces on
thermal oxidation duration on the microstructure
wear in UHMWPE for artificial joints, J. Biomed.
and fretting wear behavior of Ti6Al4V alloy, Surf.
Sci. Eng., vol. 4, pp. 375382, 2011.
Coatings Technol., vol. 159, pp. 139151, 2015.
[30] K. Thamaphat, P. Limsuwan and B.
[21] H. Dong, W. Shi and T. Bell, Potential of
Ngotawornchai, Phase Characterization of TiO2
improving tribological performance of UHMWPE
Powder by XRD and TEM, Nat. Sci., vol. 42, pp.
by engineering the Ti6Al4V counterfaces, Wear,
357361, 2008.
vol. 225229, pp. 146153, 1999.
[31] M.C. Garca-Alonso, L. Saldaa, G. Valls, J.L.
[22] S. Wang, Z. Liao, Y. Liu and W. Liu, Influence of
Gonzlez-Carrasco, J. Gonzlez-Cabrero, M.E.
thermal oxidation temperature on the
Martnez, E. Gil-Garay and L. Munuera, In vitro
microstructural and tribological behavior of
corrosion behaviour and osteoblast response of
Ti6Al4V alloy, Surf. Coatings Technol., vol. 240,
thermally oxidised Ti6Al4V alloy, Biomaterials,
pp. 470477, Feb. 2014.
vol. 24, no. 1, pp. 1926, 2003.
[23] S. Kumar, T.S.N.S. Narayanan, S.G.S. Raman and S.
[32] J. Dai, J. Zhu, C. Chen and F. Weng, High
K. Seshadri, Thermal oxidation of CP Ti-An
temperature oxidation behavior and research
electrochemical and structural characterization,
status of modifications on improving high
Mater. Charact., vol. 61, pp. 589597, 2010.
temperature oxidation resistance of titanium
[24] N. Somsanith, T.S.N.S. Narayanan, Y.K. Kim, I.S. alloys and titanium aluminides: A review, J.
Park, T.S. Bae and M.H. Lee, Surface medication Alloys Compd., vol. 685, pp. 784798, 2016.
of Ti-15Mo alloy by thermal oxidation: Evaluation
[33] S. Kumar, T.S.N.S. Narayanan, S.G.S. Raman and
of surface characteristics and corrosion
S.K. Seshadri, Thermal oxidation of CP-Ti:
resistance in Ringers solution, Appl. Surf. Sci.,
Evaluation of characteristics and corrosion
vol. 356, pp. 11171126, 2015.
resistance as a function of treatment time, Mater.
[25] Y. Bailey, R. Sun, R. Bailey and Y. Sun, Sci. Eng. C, vol. 29, no. 6, pp. 19421949, 2009.
Unlubricated sliding friction and wear
[34] E. Arslan, Y. Totik, E. Demirci and A. Alsaran,
characteristics of thermally oxidized
Influence of surface roughness on corrosion and
commercially pure titanium, Wear, vol. 308, no.
tribological behavior of CP-Ti after thermal
12, pp. 6170, 2013.
oxidation treatment, J. Mater. Eng. Perform., vol.
[26] S. Wang, Y. Liu, C. Zhang, Z. Liao and W. Liu, The 19, no. 3, pp. 428433, 2010.
improvement of wettability, biotribological
[35] B. Arifvianto, Suyitno, M. Mahardika, P. Dewo, P.T.
behavior and corrosion resistance of titanium
Iswanto and U.A. Salim, Effect of surface
alloy pretreated by thermal oxidation, Tribol.
mechanical attrition treatment (SMAT) on
Int., vol. 79, pp. 174182, 2014.
microhardness, surface roughness and
[27] D. Xiong, Y. Yang and Y. Deng, Bio-tribological wettability of AISI 316L, Mater. Chem. Phys., vol.
properties of UHMWPE against surface modified 125, no. 3, pp. 418426, 2011.
titanium alloy, Surf. Coatings Technol., vol. 228,
pp. S442S445, 2013.

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Tribology in Industry

RESEARCH
www.tribology.fink.rs

Effect of Composition on Mechanical Properties of

Mullite-WC Nano Composites Prepared by Spark
Plasma Sintering

H. Rajaei a, I. Mobasherpour a, M. Farvizi a, M. Zakeri a

a Ceramics Department, Materials and Energy Research Center, Karaj, Iran.

Keywords: ABSTRACT
Mullite
Mullite-WC composites were prepared from Mullite and WC powders by
WC spark plasma sintering at 1400 C for a holding time of 180 s under 30
Nano composite MPa. Microstructure, strength, and hardness of the mullite-WC
Spark plasma sintering composites were studied. The mullite-WC composite containing 5-20
wt% WC reached over 94 % theoretical density. The strength and
Corresponding author: Vickers hardness of mullite-(10 wt%) WC sintered composite reached
maximum values of 298 MPa, and 1589 HV, respectively demonstrating
Iman Mobasherpour that the introduction of WC significantly enhances the mechanical
Ceramics Department, Materials and properties of the mullite matrix.
Energy Research Center, Karaj, Iran.
E-mail:Iman.Mobasherpour@gmail.com 2016 Published by Faculty of Engineering

1. INTRODUCTION can markedly deteriorate the densification and

During the recent decades, researchers
conducted extensive studies on ceramics based
composites and nano composites [111]. Results
established that for reinforced ceramics, the
creep rate is lower by two up to three orders of
magnitude, and the strength is higher by two up
to three times compared to the ceramics
without reinforcements [2,3,5,8].
Nevertheless, fabrication of dense composites is
a challenge because the reinforcing phases are
often carbides, nitrides or borides, which are
very difficult to densify. On top of that, there
have been a lot of difficulties in achieving a
uniform dispersion of reinforcing phases in the
matrix. Agglomeration of reinforcing particles
degrade the properties of the produced
composites. The processing difficulties are
aggravated when reinforcing phases are sub
micrometer or nanometer sized powders
because finer particles tend to form stronger
agglomerates [12].
Mullite (3Al2O3.2SiO2) has been considered a
good candidate for high temperature application
[13] because of its marvelous properties, such as
good chemical and thermal stability, low thermal
expansion and conductivity coefficient, low
dielectric constant and high creep resistance
[14]. However, application of mullite is largely
limited because of its rather low strength and
fracture toughness [14]. Continuous reinforced
mullite matrix composites have been extensively

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investigated recently in order to improve the m, and the number percentage of the particles
inherent brittleness of monolithic mullite below 9 m was 90 %.
ceramic [15-19]. Continuous silicon carbide
fiber- or aluminosilicate reinforced mullite
matrix composites have been used in advanced
applications, such as aero engines, stationary gas
turbines and heat exchangers [20]. Nevertheless,
these mullite composites are not much reliable
at temperatures higher than 1500 C because of
the severe degradation of silicon carbide or
aluminosilicate phases [21].

Tungsten carbide (WC) is a superior candidate

as second phase material and it is extensively
used in cutting tools and protective coatings
because of its unique combination of properties
viz. high melting temperature, extremely hard,
chemical stability, excellent abrasive and
Fig. 1. Scanning electron micrographs of primarily
corrosion resistance [22].
WC powder.

Spark plasma sintering (SPS) or plasma pressure

compaction is a technique for densifying any
class of materials, especially those that are
difficult to be sintered by the conventional
techniques [23]. Presence of plasma in spark
plasma sintering systems is still unproven.
Specific advantages of SPS over the conventional
sintering techniques are: (1) a faster heating
rate, which avoids mass transport mechanisms
that do not contribute to the densification (2) a
shorter dwell time, which retains finer
microstructures, and (3) DC pulse voltage, which
contributes to an enhanced mass transport
through electro-migration [24].
In this study, SPS technique was used to prepare
mullite-WC composites, and influence of
composition on microstructures and mechanical
properties of composites was investigated.
2. EXPERIMENTAL PROCEDURE
2.1 Materials
WC powder was provided by Alfa Aesar Co. (Art
No.12070). Figure 1 shows a SEM image of the
pure WC powder. As can be seen, it consist WC
particles exhibiting severe initial agglomeration.
Particle size distribution analysis was performed
for the WC powder by the dynamic laser
scattering technique using Fritsch particle sizer
analysts. It can be found from Fig. 2 that the
mean particle size (D50) of the powder was 3.20
Fig. 2. Particle size analyses of WC powder.
A fine mullite (3Al2O3.2SiO2) powder was
synthesized by sol-gel process using aluminum
nitrate (Art No. 101086, Merck Co.) and tetra
ethyl ortho silicate (TEOS) (Art No. 800658,
Merck Co.) as starting materials. The detailed
synthesis procedure is reported in literature [25].
Phase identification of the synthesized mullite
powders were performed by X-ray diffraction
(XRD) method using a CuK, Siemens
diffractometer. Particle size of the synthesized
mullite powder was obtained by field emission
scanning electron microscopy (FE-SEM Mira 3-
XMU).
2.2 SPS operation
WC and mullite powders were mixed by a ball
mill to produce mullite-WC (0-20 wt%)
mixtures. The wet milling was performed in a
plastic vial for 12 h at a speed of 200 rpm in
presence of 50 ml ethanol. The mixed powders

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were dried and then passed through a sieve with crosshead speed of 0.5 mm/min. For each set of
a pore-opening size of 100 m. Using a graphite compositions, at least five specimens were
die with an inner diameter of 50 mm, Powders tested for both strength and hardness
were sintered by an SPS machine (SPS-20T-10, measurements.
Easy fashion metal products trade Co.). Standard
DC pulse ONOFF sequence with current 2.6 kA
was chosen for all the experiments. The heating 3. RESULTS AND DISCUSSION
rate was 1 C/s and sintering was performed
under vacuum at a temperature of 1400 C for a 3.1 Characterization of mullite
holding time of 180 sec with pressure 30 MPa.
The temperature of die was measured by an Morphology of synthesized mullite single
optical pyrometer. particles is shown in Fig. 3. The particles have a
spindle-like morphology with an average
2.3 Characterization particle size in the range of 80200 nm. Figure 4
shows XRD pattern of synthesized mullite
Siemens diffract meter with Cu K radiation ( = powder compacted at elevated temperature.
0.1541 nm) was used to study the phase Mullite is main phase in the specimen sintered at
evolution of sintered samples. Diffraction 1400 C and diffraction peaks of -Al2O3, Al or Si-
measurements were performed at 30 kV /20mA spinel not be observed in pattern.
with scanning speed of 1 /min for scanning
range of 2080 with intervals of 0.02.
Morphology of synthesized mullite and
microstructure evolution of sintered samples
were investigated by a field emission scanning
electron microscopy (FE-SEM) Mira 3-XMU
operating at 30 kV and scanning electron
microscopy (SEM) ZEISS operating at 15 kV,
respectively.

Using distilled water, ASTM C373-88 standard

via Archimedes method was applied in order to
study changes in the density of samples. The
mean density values were obtained by averaging
values of densities of three specimens for each
composition. Theoretical densities of mullite
(3.05 g/cm3), and WC (15.63 g/cm3) were used
Fig. 3. Scanning electron micrographs of synthesized
to calculate relative densities. mullite powder.

Following ASTM-C1327-08 standard, the Vickers

hardness was measured using a micro hardness
tester (MVK-H21, Akashi Co.) with a load of 1 kg
for a holding time of 15 sec. Surface of samples
was prepared for the hardness tests through
polishing with 1m diamond slurry. 5
measurements for each sample were averaged
to evaluate Vickers hardness. Specimens with
dimensions of 20mm4mm2mm were cut and
machined for bending strength tests according Fig. 4. XRD of synthesized mullite powder compact at
to ASTM C1161-13. The entire specimen surface elevated temperature.
was ground by an 800-grit diamond wheel and
surface facing to the tensile machine was 3.2 Effect of composition
polished by diamond slurries. Bending strength
of samples was measured at room temperature Figure 5 shows XRD patterns of the mullite-WC
by a three-point bending test operating with a (5, 10, 15, and 20 wt.%) composites sintered at

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1400 C for a sintering time of 180 sec. Patterns
reveal the presence of only mullite and WC
phases, which indicates that there was no
reaction between mullite and WC during milling
or sintering process. This finding is similar to the
results reported in literature for Al2O3-WC [26],
and mullite-TiC [19] composites.
Figure 6 shows the effect of content WC on
relative density of sintered composites.
Considering Fig. 6 and table 1, one can realize
the sintering behavior of the mullite-WC
composites with different compositions. Despite
the detrimental effect of the presence of WC
phase on sintering, all of samples have reached
over 94 % of their theoretical density (TD).
Mullite-10 wt% WC sample reached the highest
relative density compared to other
compositions.

Contact points between particles are highly

resistant to current flow and contribute to an
increased heating. The temperature at those
localized heating zones exceeds melting
Fig. 5. XRD pattern of Mullite-(5 %wt) WC, Mullite- temperature of material. The cumulative effect
(10 %wt) WC, Mullite-(15 %wt) WC and Mullite-(20 from all such zones results in an improved
%wt) WC sintered at 1400C for 180s. densification at rather lower sintering
temperatures compared to conventional
Table 1. Relative densities and mechanical sintering techniques [18]. The effectiveness of
properties of various Mullite-WC composite samples
low temperature sintering in SPS can be
that were analyzed after sintered at 1400 C for 180 s
by SPS.
explained as follows: Firstly during spark
plasma sintering, high heating rate enables
Relative Bending Hardness
Composition
density (%) strength (MPa) (HV)
sample to skip over the low-temperature regime
Mullite 94.1 220 1269 where the nondensifying mechanism (surface
Mullite-(5 wt%) diffusion) is active and sample proceeds directly
94.6 235 1528
WC into the elevated temperature regime where
Mullite-(10 wt%) densifying mechanisms predominate. Thus, SPS
96 298 1589
WC
suppresses the grain pre coarsening before
Mullite-(15 wt%)
95.5 273 1568 actual sintering starts [30]. Secondly, electric
WC
Mullite-(20 wt%) discharge, electric shock pressure and
95.1 245 1536
WC mechanical pressure during SPS also improve
mass transport between ceramic particles and
It is well known that mullite has very poor sinter thus sintering progress is significantly better in
ability and could be sintered to full density only SPS compared to the pressure less sintering and
at temperature higher than 1700 C [2729]. even hot pressing methods [31, 32].
Table 1 shows relative densities and mechanical
properties of sintered mullite-WC samples. Figure 7 shows, SEM micrographs of polished
cross section of mullite-WC composites
containing 5, 10, 15 and 20 wt% sintered at
1400 C for 180 sec. Due to rather low sintering
temperature, short sintering time and pining
effect of the WC particles on grain growth of
mullite matrix, a fine matrix grained
microstructure is observed for composites with
different amount of WC. The microstructure is
homogeneous and WC particles are present
inside at the grain boundaries. As Fig. 7c shows,
WC is well uniformly distributed in mullite
matrix. Figure 7b shows that microstructure of
mullite-(10 wt%) WC sintered composites is
better densified and contains less pores in
Fig.6. Sintering curves of Mullite-WC composite powder. comparison with the other composites.

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Fig. 7. SEM micrographs of Mullite-WC composites:
(a) Mullite-(5 %wt) WC; (b) Mullite-(10 %wt) WC; (c)
Mullite-(15 %wt) WC; (d) Mullite-(20 %wt) WC
sintered at 1400 C for 180s by SPS.
Fig. 8. Plots of effect composition on the strength of
Mullite-WC composite.
Figure 8 shows, effect composition on strength of
mullite-WC composites. The strength increases
steadily by increasing WC content up to 10 wt%.
The strength of mullite-WC (5, 10, 15 and 20 wt%)
composites reach 235 MPa, 298 MPa, 273MPa
and 245 MPa, respectively. In comparison with
rather poor strength of the monolithic mullite
sintered by conventional sintering method (200
MPa) [33], and the monolithic mullite sintered by
SPS (220 MPa), the strength of present mullite-
WC composites is significantly improved. The
increase in Youngs modulus [33], refinement of
556
microstructure and residual stress strengthening
effects resulted by the presence of WC particles in
the matrix are the important factors that improve
strength. Besides, formation of dislocation
networks in the matrix and the strengthening by
grain boundaries also contribute to increase in
strength [2,3]. According to Fig. 7, by increase of
WC content more than 10 wt% up to 20 wt% the
agglomeration of WC particle occurred. Duos to
rather high sintering temperature of WC, the
agglomeration of WC phases and increase of
porosity have detrimental effect on sintering
behavior and mechanical properties.
Fig. 9. Effect of WC content on the Vickers hardness
of Mullite-WC composite sintered at 1400 C for 180 s
by SPS.
Figure 9 shows Vickers hardness of sintered
mullite-WC composites. Mullite-10 wt. % WC
composite achieved the highest hardness value of
1589 HV. The high hardness of WC particles
dispersed in mullite matrix caused an increase in
hardness. Hardness values for composite materials
ranged between 15.3 and 15.9 GPa, which are
significantly improved compared to that of pure
mullite (12.7 GPa). The hardness values of mullite-
WC composites in the present study are
comparable with values reported in literature for
alumina-WC [6], and mullite-TiC [19] composites.
The hardness of sintered mullite-WC composites
decreases with an increase in WC content over 10
wt%. This decrease in hardness is explained by the
lowering relative density of mullite-WC (15 or 20
wt%) composites (Fig. 6).
4. CONCLUSION
Spark plasma sintering of mullite-WC composite
powders was investigated. The sinterability of
 H. Rajaei et al., Tribology in Industry Vol. 38, No. 4 (2016) 552-558
composites increased steadily by increasing WC
content up to 10 wt%. Because of suppressed
grain coarsening and enhanced mass transport by
electric discharge, highly densified mullite-WC
composites were produced at 1400 C by SPS.
Composite with WC content of 5-20 wt% have
reached over 94 % of their theoretical density.
The strength and Vickers hardness of mullite-WC
(10 wt%) composite sintered at 1400 C had a
maximum value of 298 MPa and 1589 HV,
respectively. The strength and hardness of
sintered mullite-WC composites decrease by an
increase in WC content over 10 wt%.
REFERENCES
[1] A. Mukhopadhyay and B. Basu, Consolidation
microstructureproperty relationships in bulk
nanoceramics and ceramic nanocomposites: a
review, Int. Mater. Rev., vol. 52, no. 5, pp. 257-
288, 2007.
[2] K. Niihara, A. Nakahira and T. Sekino, New
Nanocomposite Structural Ceramics, Materials
Research Society Symposium Proceedings, vol.
286, pp. 406413, 1993.
[3] K. Niihara, New Design Concept of Structural
Ceramics (Ceramic Nanocomposites), J. Ceram.
Soc. Jpn., vol. 99, no. 1154, pp. 974982, 1991.
[4] J.H. Zhao, C.S. Laura, P.H. Martin, M.C. Helen and
A.M. Gary, Mechanical Behavior of Alumina
Silicon Carbide (Ceramic Nanocomposites), J. Am.
Ceram. Soc., vol. 76, no. 2, pp. 503510, 1993.
[5] U. Hisao, T. Hidekazu, T. Takeyoshi, N. Atsushi
and N. Koichi, Pressureless Sintering of
Al2O3/TiC Nanocomposites, Powder Metall., vol.
41, no. 10, pp. 12261231, 1994.
[6] A. Nakahira, K. Niihara, Sintering Behaviours
and Consolidation Process for Al2O3/SiC
Nanocomposites, J. Ceram. Soc. Jpn., vol. 100, no.
4, pp. 448-453, 1992.
[7] L. Gao, H.Z. Wang, J.S. Hong, H. Miyamoto, K.
Miyamoto, Y.Nishikawa and D. De la Torre, SiC-
ZrO2(3Y)-Al2O3 nanocomposites superfast
densified by spark plasma sintering, Nanostruct.
Mater., vol. 11, no. 1, pp. 4349, 1999.
[8] Y. Eiichi, Q.L. Bao and K. Niihara, The Effects of
Fine SiC Particles on the Creep of MgO at High
Temperatures, J. Ceram. Soc. Jpn., vol. 100, no.
1160, pp. 514519, 1992.
[9] W.Q. Li and L. Gao, Processing, microstructure
and mechanical properties of 25 vol% YAG-
Al2O3 nanocomposites, Nanostruct. Mater., vol.
11, no. 8, pp. 10731080, 1997.
[10] L. Gao, H.Z. Wang, J.S. Hong, H. Miyamoto, K.
Miyamoto, Y. Nishikawa and S. Torre,
Mechanical Properties and Microstructure of
Nano-SiC-Al2O3 Composites Densified by Spark
Plasma Sintering, J. Eur. Ceram. Soc., vol. 19, no.
5, pp. 609613, 1999.
[11] H.Z. Wang, L. Gao and J.K. Guo, Fabrication and
Microstructure of Al2O3-ZrO2(3Y)-SiC
Nanocomposites, J. Eur. Ceram. Soc., vol. 19, no.
12, pp. 21252131, 1999.
[12] Y.J. Lin and C.P. Tsang, Fabrication of mullite/SiC
and mullite/zirconia/SiC composites by dual in-
situ reaction syntheses, Mater. Sci. Eng., A, vol.
344, no. 1-2, pp. 168-174, 2003.
[13] T.R. Prabhu, Airworthiness Certification of Fe-
Si3N4-graphite Brake Composites for Military
Aircraft, Tribology in Industry, vol. 37, no. 4
pp.491-499, 2015.
[14] Y. Wang, H. Cheng and J. Wang, Effects of the
single layer CVD SiC inter phases on mechanical
properties of mullite fiber-reinforced mullite
matrix composites fabricated via a sol gel
process, Ceram. Int., vol. 40, no. 3, pp. 4707
4715, 2014.
[15] Z.I. Zaki, Nasser Y.Mostafa and Y.M.Z. Ahmed,
Synthesis of dense mullite/MoSi2 composite for
high temperature applications, Int. J. Refract.
Met. Hard Mater, vol. 45, pp. 23-30, 2014.
[16] K.K. Chawla, Interface engineering in mullite
fiber/mullite matrix composites, J. Eur. Ceram.
Soc., vol. 28, no. 2, pp. 447453, 2008.
[17] F.W. Zok, Developments in oxide fiber
composites, J. Am. Ceram. Soc., vol. 89, no. 11,
pp. 33093324, 2006.
[18] D. Ghahremani, T. Ebadzadeh and A.
Maghsodipour, Spark plasma sintering of
mullite: Relation between microstructure,
properties and spark plasma sintering (SPS)
parameters, Ceram. Int., vol. 41, no. 5, pp. 6409-
6416, 2015.
[19] D. Ghahremani, T. Ebadzadeh and A.
Maghsodipour, Densification, microstructure
and mechanical properties of MulliteTiC
composites prepared by spark plasma
sintering, Ceram. Int., vol. 41, no. 2, pp. 1957-
1962, 2015.
[20] M.A. Mattoni, J.Y. Yang, C.G. Levi and F.W. Zok,
Effects of combustor rig exposure on a porous-
matrix oxide composite, Int. J. Appl. Ceram.
Technol., vol. 2, no. 2, pp. 133140, 2005.
557
 H. Rajaei et al., Tribology in Industry Vol. 38, No. 4 (2016) 552-558

[21] H. Schneider, J. Schreuer and B. Hildman,
Structure and properties of mullite a review, J.
Eur. Ceram. Soc., vol. 28, no. 2, pp. 329344, 2008.
[22] K.N. Pramoda, L. Hao-Tung, C. Man-Ping, C. Wei-
Hsio and H. Jow-Lay, Microstructure analysis
and mechanical properties of a new class of
Al2O3WC nanocomposites fabricated by spark
plasma sintering, J. Eur. Ceram. Soc., vol. 33, no.
15-16, pp. 3095-3100, 2013.
[23] A. Lanzutti, M. Lekka, E. Marin and L. Fedrizzi,
Tribological Behavior of Thermal Spray Coatings,
Deposited by HVOF and APS Techniques, and
Composite Electrodeposits Ni/SiC at Both Room
Temperature and 300 C, Tribology in Industry,
vol. 35, no. 2, pp. 113122, 2013.
[24] K. Sairama, J.K. Sonber, T.S.R.Ch. Murthy, C.
Subramanian, R.K. Fotedar, P. Nanekar and R.C.
Hubli, Influence of spark plasma sintering
parameters on densification and mechanical
properties of boron carbide, Int. J. Refract. Met.
Hard Mater., vol. 42, pp. 185192, 2014.
[25] Z. Guimin, W. Yucheng, F. Zhengyi, W. Hao, W.
Weiming, Z. Jinyong and Z. Qingjie, Synthesis of
Mullite at low temperature and its chemical
composition, J. Chin. Ceram., vol. 36, pp. 1542-
1547, 2008.
[26] D. Jianxin, D. Zeliang, Z. Jun, L. Jianfeng and
C.Tongkun, Unlubricated friction and wear
behaviors of various alumina-based ceramic
composites against cemented carbide, Ceram.
Int., vol. 32, no. 5, pp. 499-507, 2006.
[27] O. Hiroshi, K. Toshi, N. Atsushi and K. Niihara,
Microstructure and Mechanical Properties of
Mullite Ceramics, J. Ceram. Soc. Jpn., vol. 98, no.
1138, pp. 541547, 1990.
[28] M. Ismail, N. Zenjiro and S. Shigeyuki,
Microstructure and Mechanical Properties of
Mullite Prepared by the Sol-Gel Method, J. Am.
Ceram. Soc., vol. 70, no. 1, pp. C7C8, 1987.
[29] K. Hidehiro, S. Hisao and I. Takahiro,
Densification of Sol-Gel-Derived Mullite
Ceramics after Cold Isostatic Pressing up to 1
GPa, J. Am. Ceram. Soc., vol. 81, no. 1, pp. 173
179, 1998.
[30] S.W. Wang, L.D. Chen and T. Hirai, Densification
of Al2O3 Powder Using Spark Plasma Sintering,
J. Mater. Res., vol. 15, no. 4, pp. 982987, 2000.
[31] K. Hiroshi, Science and New Applications of
Electric Discharge Consolidation, J Jpn Soc
Powder Powder Metall, vol. 45, no. 11, pp.1050
1054, 1998.
[32] T. Masao, Trends in Advanced SPS Spark Plasma
Sintering Systems and Technology. Functionally
Gradient Materials and Unique Synthetic
Processing Methods from Next Generation of
Powder Technology, J. Soc. Powder Technol., vol.
30, no. 11, pp. 790804, 1993.
[33] M. I. Osendi and C. Baudin, Mechanical
Properties of Mullite Materials, J. Eur. Ceram.
Soc., vol. 16, no. 2, pp. 211-224, 1996.

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Tribology in Industry

RESEARCH
www.tribology.fink.rs

Modelling and Simulation of a Manipulator with

Stable Viscoelastic Grasping Incorporating Friction

A. Khurshid a, Z. Khan b, V. Chacko b, A. Ghafoor c, M.A. Malik d, Y. Ayaz c

a Department of Mechatronics Engineering, Air University, Sector E-9, Islamabad 44000, Pakistan,
b NanoCorr, Energy and Modelling (NCEM), Faculty of Science & Technology, Bournemouth University, Dorset BH12
5BB United Kingdom,
c School of Mechanical and Manufacturing Engineering, National University of Sciences and Technology Sector H-12,

Islamabad 44000, Pakistan,

d Department of Mechanical Engineering, Air University, Sector E-9, Islamabad 44000, Pakistan.

Keywords: ABSTRACT
Anthropomorphic arm
Design, dynamics and control of a humanoid robotic hand based on
Computer aided design anthropological dimensions, with joint friction, is modelled, simulated and
Multi-body mechanics simulation analysed in this paper by using computer aided design and multibody
Dynamics dynamic simulation. Combined joint friction model is incorporated in the
Joint friction joints. Experimental values of coefficient of friction of grease lubricated
Bond graph model sliding contacts representative of manipulator joints are presented.
Viscoelasticity Human fingers deform to the shape of the grasped object (enveloping
grasp) at the area of interaction. A mass-spring-damper model of the
grasp is developed. The interaction of the viscoelastic gripper of the arm
Corresponding author:
with objects is analysed by using Bond Graph modelling method.
Zulfiqar Khan Simulations were conducted for several material parameters. These
NanoCorr, Energy and Modelling, results of the simulation are then used to develop a prototype of the
(NCEM), proposed gripper. Bond graph model is experimentally validated by using
Faculty of Science & Technology, the prototype. The gripper is used to successfully transport soft and
Bournemouth University, fragile objects. This paper provides information on optimisation of
Dorset BH12 5BB, friction and its inclusion in both dynamic modelling and simulation to
United Kingdom. enhance mechanical efficiency.
E-mail: zkhan@bournemouth.ac.uk
2016 Published by Faculty of Engineering

1. INTRODUCTION manipulators in hazardous environments

Robotic manipulators are usually used for tasks
which have been historically performed by
human beings by using their hands e.g. in a
factory production line. The use of robotic arms
is beneficial in several ways as it helps to
accomplish repetitive tasks which can cause
fatigue in human beings, use of robotic
reduces risk to human beings (in a paint shop on
a factory floor) and exposure to airborne
hazardous particles can be avoided. The aim of
this research is to develop a humanoid hand
with joint friction model and viscoelastic end
effectors to provide solutions for performing
automated mechanical tasks at maximum
performance.

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 A. Khurshid et al., Tribology in Industry Vol. 38, No. 4 (2016) 559-574
Mechanics of robotic manipulators have been
investigated over the past half a century.
Mechanics analyses of manipulators have
progressed from kinematic to a more complex
dynamic analysis over the past two decades.
Modelling of complex manipulator linkage
mechanisms is now increasingly possible and is
being captured more accurately. However, two
areas of manipulator mechanisms require
further analysis. The first is the dynamic
simulation of mechanical manipulators and the
effect of joint friction on the dynamics, and the
second is, the analysis of interfacial mechanisms
between the gripper (manipulator end effector)
and corresponding object.
Dynamic simulations have become increasingly
popular with increasing computational power
and the availability of a wide range of software
tools [1]. Several software tools have diverse
capabilities in terms of applications. This
improves the quality of simulation and reduces
the design cycle time. In mechanical systems,
the use of a virtual prototype leads to reduction
in the overall design cost [2] and virtual
prototyping accurately simulates the
performance of a system. Visualisation of
mathematical models as prototypes in a virtual
space provides a better understanding of
system performance.
Human fingertips provide soft contact grasping
and take on the shape of the object at the
interface. Finger deformation at the contact
plateaus between 0.2 and 0.9N according to [3]
and deformation limit is reached at 1 N.
Modified Hertzian contact theory for finger
deformation and a power law model has been
derived for the deformation of the finger by [4].
Therefore, deformable fingers are superior in
comparison to hard grippers and moreover,
hard grippers can damage the object. The
property of softness also helps in maintaining an
increased area of contact during grasping and
manipulation which confines the object from
moving thus providing a stable grasp [59].
Friction at such contact occurs mainly through
adhesion [3]. The importance of contact surface
engineering has been highlighted in [10] with the
introduction of a velvet surface on the gripper.
Novel granular material gripper has been
presented in [11] which provides an alternative
to fingered grasping end effector. Vision based
grasping has been presented in [12].
560
So far several significant contributions have
been made in the design of various grippers for
grasping and in-grasp fine manipulation
[10,11,1315]. Detailed classification may be
found in [16]. Kinematics and dynamics of
general robotic manipulators has been
presented in [17,18]. A history of robotic arms
is given by Monkman [19]. Some of the notable
anthropomorphic manipulators are the
Salisbury hand (Stanford hand), the Barret hand
and the Karlsruhe hand.
The need for task specific robot grippers was
addressed through grippers designed to the
shape of the workpiece [20]. The same concept
has been presented in [13,21]. For use in special
environments, the requirement and design of an
adaptive finger has been highlighted in [13].
Modification of PUMA robot arm by fitting a
humanoid hand with 16 degrees of freedom
fingers have been presented in [22].
Postural synergies to control the end effector
was presented in [23]. Slip sensing of grasped
objects using skin acceleration sensors bonded
to silicone skin has been presented by [24]. The
application of screw theory for modelling a
heavy manipulator has been presented in [25].
Dexterity is the capability of the manipulator to
perform certain complex tasks autonomously.
Dexterity can be divided into grasping and
internal manipulation [16]. However, the
dexterity or firmness of grasping is often
sacrificed while performing in-grasp fine-
manipulation where a pinching grasp is
necessary [26]. When holding an object in
between fingertips, in-grasp manipulation
becomes easy but the chances of slippage and
unstable grasp increase at the same time [27].
Therefore, an enveloping grasp is required
which is quite dexterous. In-grasp fine
manipulation then becomes difficult to achieve.
Therefore, the development of such a gripper
that makes it possible to provide dexterous
grasping and in-grasp fine manipulation
simultaneously is a daunting task. Human hand
has been analysed from this perspective and the
novel Huminitive Gripper is introduced.
The structure of the finger is a key aspect of any
anthropomorphic gripper. The finger is made up
of flesh with blood vessels inside, and a covering
of skin[28]. The fleshy part of the finger imparts
 A. Khurshid et al., Tribology in Industry Vol. 38, No. 4 (2016) 559-574

stiffness while the blood inside provides viscous material properties and deterioration has been
damping. Combination of the two leads to performed by researchers [3436]. There are
viscoelastic property of fingers. These soft two approaches to achieve fine manipulation of
fingers deform at contact to take on the shape the grasped object (i) by manipulating fingers as
of the object which ultimately delivers a grasp in a human hand [3739] or (ii) using the finger
that is both dexterous and firm. The fingers are tips for fine manipulation of the grasped object
visco-elastic and return to their initial shape [10,26,40,41]. The use of soft fingertips in
after the object is released from the grasp. To grasping objects leads to stable grasping [24,
study the role of stiffness and damping in soft 42]. Yet a category for research on a human
grasping, Bond graph model of soft fingers using hand like gripper having soft contact capability
a spring-damper combination is developed. and rotating fingers seems to be absent. This has
Interfacial friction between soft fingertips and been categorised as Huminitive Gripper by [9],
the object is incorporated into the contact. This and comprises all grippers which resemble and
is followed by an analysis of the gripper to perform soft grasping and fine manipulation like
evaluate the effects of materials properties on a human hand. The classification of grippers has
grasping mechanism within a soft contact. been explained in [19] (also see Table 1 and
Table 2). Prehension is the hands ability to grasp
Table 1. Gripper Classification According to Physical and hold objects of different size and shape,
Principle of Operation [19]. compared to apprehension, which is the hands
Prehension
Gripper Type Typical Examples
ability to understand through active touch [16].
Method
Clamps (external The choice of manipulator actuators determines
fingers, internal fingers,
the performance of the manipulators i.e. their
Impactive chucks, spring clamps),
tongs (parallel, shear, dynamics and control. Some of the latest and
angle, radial) futuristic actuators have been evaluated. Shape
Pins, needles and Memory alloys (SMA) deliver large strokes at fast
Intrusive
Ingressive hackles contraction rates and have long life. The analysis
Non- intrusive Hook and Loop of an SMA based miniature manipulator with
Vacuum Vacuum suction
Suction cup/bellows
parallel mechanism has been presented in [43].
Magento Permanent SMAs are currently be expensive, prone to
Astrictive hysteresis, require strengthening and have a low
adhesion Magnet/Electromagnet
Electro
Electrostatic field
energy capacity [44]. Carbon Nano-tubes and
adhesion polymer fibres have a high work capacity, but
Thermal Freezing, melting
need to be redrawn between cycles and were
Chemical Permatrack adhesives
Contigutive
Capillary action, surface found to be expensive [45]. Work on electro-
Fluid dynamically driven organic fibres which could
tension
render large strokes has been presented in [46].
Table 2. Other Grasping Methods not normally However, they require special electrolytic
categorized [19]. envelope, counter electrode, containment
Material systems which make them both heavy and
Gripper Example application
Type expensive. Pneumatic Air Muscles have been
Rigid
Loose materials such as nuts presented in [47,48]. These now have novel
Spoon and bolts pumping mechanism, significant low pressure
Flexible Powders and viscous fluids
actuation but can only be actuated linearly with
Determinate topology for
Hook
Rigid
example castings radial expansion. Muscles for controlling the
Flexible Waste material sorting finger are long interwoven and form complex
dynamic structures. With several competing
End effector is the point of interaction with technologies showing advancements that address
objects in the task environment. Several the drawbacks, high performance human muscle
investigations have been focussed on object substitutes that can be used to activate
manipulation and a fine motion in the past mechanisms is still closer to reality [46, 49].
decade [12,2932]. Tactile [33], visual and Improvements of the hysteresis characteristics of
grasping controls of multi-fingered robotic SMAs, the life of CNT wires and decreasing the
hands [23] has been investigated. Research on size of the electrolytic envelope in electrodynamic

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fibres will lead to the development of high
performance actuators for robotic manipulators
in the future. SMA and CNT based actuation
seems to be promising for actuators of the future.
This paper has been organised into modelling,
simulation and experimentation parts.
Mechanical modelling of the manipulator and the
gripper are presented in the following section.
2. MODELLING
The kinematics of the manipulator in the
Cartesian coordinate system, the dynamics of
the arm developed by using the Newton Euler
method of formulation, combined joint friction
model comprising Coulomb, Viscous and
Stribeck friction have been described along with
the control of the arm and the development of
grasping model using Bond Graph method is
presented in the section.
1.1. Kinematics
Kinematics pertains to the motion of bodies in a
robotic mechanism with no regard to the forces or
torques that cause the motion [17]. Kinematic
model of the arm is made of the geometric
relations between links in space and their time
derivatives which are; velocity and acceleration.
The term Forward Kinematics (FK) usually
referring to calculations of end effector position
for a given input parameters. Inverse kinematics
(IK) on the other hand is referring to joint state
parameters calculations from the end effector
position. The process of computing IK is complex
for higher number of links. Further description
of general kinematics may be found in [17].
Here, Denavit-Hartenberg coordinate
assignment convention is used [50], [51]. The
general kinematic transformation for expressing
a point on link i in the coordinate system of the
i 1 link can be expressed as [50]:
pi 1 Aii1 pi
cos i cos i sin i sin i sin i a i cos i
sin
cos i cos i sin i sin i a i sin i
Aii1 i
0 sin i cos i di
0 0 0 1
562
where i = 1,2,3,4, Aii1 is the planar kinematic
transformation matrix including rotations and
translations. pi pix piy
piz 1 ,
T
is the
coordinates of the transformation. For this work
forward kinematics has been calculated by
simulation program and the end effector positions
corresponding to input joint angles have been
obtained. Dynamic model of the manipulator
mechanism is presented in the next section.
1.2. Dynamics
Dynamic model defines the relationship
between force and/or torque parameters during
the operation of a linkage and/or mechanism.
According to Featherstone and Orin, The
dynamic equations of motion provide the
relationships between actuation and contact
forces acting on robot mechanisms, and the
acceleration and motion trajectories that result
[18]. Forward dynamics refers to the calculation
of the joint trajectories given the actuation
forces or torques. Inverse dynamics refers to the
calculation of forces and/or torques at joints
given the joint positions and its derivatives [18].
Various methods of dynamic modelling have
been described in literature: 1) Newton Euler
method [52], 2) Euler Lagrange Method [53] and
3) Kanes equation method [54]. The arm may be
considered as a constrained multi-link
pendulum. Rigid body dynamics equation may
be expressed as [52]:
D( ) H ( ,) G( ) B() (3)
where represents joint angles, D() represents
inertia, H(, ) represents Coriolis and
centripetal forces, G() represents gravity
forces, B( ) represents frictional forces,
represents the joint torques.
Friction is an important phenomenon that
affects manipulator motion. It is non-linear and
can affect control and positioning of the arm.
Therefore, dynamic model of manipulators need
(1) to incorporate friction. The practical obstacle is
the variation of friction behaviour with the type
of joint e.g. anti-friction ball bearings exhibit
different behaviour from pin and bush joints.
The type of surface finish, lubricant, lubrication
condition and the influence of agents determine
the friction behaviour of joints [55]. In this work,
(2) a friction model composed of Coulomb, viscous
 A. Khurshid et al., Tribology in Industry Vol. 38, No. 4 (2016) 559-574
and Stribeck friction is used. Friction values can
change due to the influence of environment, as
well as wear and tear. brk represents the
breakaway friction torque which occurs at the
start of motion. br.thr represents the threshold
breakaway friction torque i.e. the value of torque
immediately before the beginning of motion, C
represents the Coulomb friction torque, vthr
represents the threshold velocity for motion and
cvisc , ctrans represent the coefficients of viscosity
and translation respectively. The numerical
coefficients have been assumed and have been
listed in. The revolute friction model used in the
dynamic simulation is represented by the
following equations [56]:
f = ( C + ( brk - C ).exp(-cv ))sign( ) + f (4)
( C + ( brk - C ).exp(-c v th r ))sign(-c vth ) fthr )
f =
thr
where equation 5 applies in the region of friction
transition i.e. thr . The value of the
parameters is given below in Table 3.
Table 3. Parameters for friction modelling.
Variable Name Value
brk 25 N m
C 20 N m
cv 0.001 N m s/rad
C trans 10 s/rad
thr 1e-4 rad/s
br.thr 24.995 N m
The friction model for finger contact is given by [3]:
F N m
Where F is the friction force, is the coefficient
of friction, N is the normal force and m is an
arbitrary constant ( 0.3). In this work, friction
term in the bond graph model is termed as Rf.
1.3. Control
The developed dynamic model is used for
simulation by using a PID controller as shown in
Fig. 1. The advantage of using a PID controller is
the simplicity of design and the ability of the
controller to accommodate the temporal
variations. The term P accounts for the present
error values, term I includes historical error
values and the D value accounts for the future
values of error based on the trend. The equation
for the PID controller is given by:
t
d e(t )
u (t ) K p e(t ) K i e(t ) d t K d (7)
0
dt
where Kp is the proportional gain, Ki is the
integral gain, and Kd is the derivative gain, e(t) is
the error in signal between set point value and
process variable, t is the time and u(t) is the
control signal. The tuned parameters for the
controller are given as P (=144.7), I (=2.4), D
(=0.01) and N (=2963.35). Results have been
presented in Section 4.1.
(5)
Fig. 1. Schematic of PID Controller.
1.4. Soft contact grasping model
The robotic gripper grasping a cylindrical object
has been developed, which has been used to arrive
at the required softness to maintain a stable grasp.
Fig. 2 shows various cylindrical objects being
grasped by using fingers alone. The deformation of
the fingers is clearly visible in Fig. 2b.
(6)
Fig. 2 a. Soft Fingers Grasping a Knob for Fine
Manipulation [9], b. Three finger grasp of a cylindrical
object.
Three fingers were modelled as soft bodies by
using linear mass, spring and damper effects
(Fig. 3). Terms Sf1, Sf2 and Sf3 are the forces
induced by three fingers for grasping the object.
Interfacial friction opposes gravity, preventing
the object from slipping through the grasp. The
frictional forces are denoted by Rf1, Rf2 and Rf3
at the interface of the gripper and object, the
damping coefficients given by Rd1, Rd2 and Rd3.
Ks1, Ks2 and Ks3 denotes spring stiffness.
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applications [57,58]. Material for the links was

then selected to be aluminium alloy material
(Al6061). The links were then assembled. The
relative link motion is constrained by a one
degree of freedom revolute joint between the
links (Fig. 4). The simulation of arm dynamics
has been explained in the next section.

Fig. 3 Schematic diagram of three fingers gripping a

cylindrical object with the actual finger deformation
(inset).

Fingers masses are given as Mf1, Mf2 and Mf3.

Mo is used to denoted the object mass and Se its
weight. Here linear viscoelasticity of soft
material has been assumed. Rf, Ks, and Rd were Fig. 4 CAD Design for the humanoid robotic
positive time-invariant [41]. manipulator with single degree of freedom joints.

1.5. Development of the Virtual Prototype

2. Simulation
Computer aided design environment is used to
develop a prototype of the arm by using the 2.1. Dynamics of the arm
bottom up approach. Dimensions suitably close
to the human arm were assumed for this design The novel modelling method considers the
and their approximated values have been listed concept of frame based physical modelling. The
in Table 4. dynamics of the arm have been simulated. The
simulations were performed on a workstation
Table 4. Dimensions suitably approximated values powered by a multi-core processor running at
(these can be modified in the future based on 3.20 GHz, with 32 GB RAM running Windows 7
anthropometrics). Professional operating system, equipped with
Part Name Mass (kg) Length (mm) a dedicated Graphics Processing Unit (GPU). The
Upper Arm 0.14 118 model was developed in the CAD environment
Lower Arm 0.947 249
and was exported to the multibody dynamics
platform.
Forearm 0.257 423
Hand 0.395 170 Fig. 5 shows a graphical layout of the block
diagram. The advantage of the method is that
Forearm was given a complex form (using loft) links may be iteratively redesigned without
to highlight the versatility of the CAD design having to redesign the whole mechanism. The
process. The calculation of link properties such system also uses physical signals, which can be
as mass, centre of gravity and moments of interfaced with Simulink for control design. In
inertia are automated in this process. This this case, a PID controller has been used to
helps to overcome the tedious calculations for control the plant based on input values. The
each link for complex designs. Al6061 alloy is model is simulated and the controller is tuned to
used widely in manufacturing robot follow the input signal. The results are presented
manipulators for its high its strength to weight in following sections.
ratio and superior machineability and wider

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Fig. 5. Block diagram layout of SimMechanics 2nd generation diagram.

Fig. 6. The contact model of three fingers represented by a Bond graph.

2.2. Bond Graph Model of the hand 3. EXPERIMENTATION

The bond graph model for the three-finger
gripping contact has been presented in Fig. 6.
Application of Bond graph method for various
dynamic systems has been discussed in detail by
Khurshid et al. [5961]. Further details of Bond
graph construction may be found in [41].
Simulation was performed by using 20Sim.
Results from the multi-body dynamics
environment and Bond graph simulation have
been presented in Section 5.3.
Two sets of experiments have been presented in
this section. The first set measures the friction
coefficient through the tribo-testing of steel alloy
pair lubricated by grease. The alloy combination
is found in pin and bush sliding joints bearings
used in manipulator arms. Similar experiments
have been reported in [6264]. The
reciprocating mechanism is driven by a scotch
yoke mechanism. The displacement is 5 mm and
the loading is provided by a cantilevered loading
mechanism. The results will provide insight into
the performance of grease lubricated contacts

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with frequent start stops and conformal contact
mechanism. The coefficient of friction was
measured for contacts lubricated by commercial
off the shelf molybdenum grease. Three load
conditions were used for the tests ranging from
25 N to 45 N. The experimental setup for micro-
friction tribo-testing is shown in Fig. 7.
The developed gripper design has been
designed for light objects with soft contact with
viscoelastic material at tips. Like human
fingers, the soft fingertips change their shape to
the object being grasped. Planetary gears
mechanisms in two of the fingers enable them
to provide in-grasp manipulation. This gives the
gripper the ability to grasp objects having
complex shapes. When the egg was gripped,
picked and placed from one place to the other,
there was no slippage found practically because
of the friction between the egg and soft finger
tips was greater than that with the tomato due
to the rough surface of the egg. Similarly, no
slippage was observed when the tomato is
gripped as well. This is because the object is
soft and the surface area between the soft
finger tips and the tomato surface increases.
The results have shown successful gripping
without slippage.

Fig. 7. Experimental setup for micro-friction tribo-testing.

Fig. 8 Process followed by the robotic manipulator in

handling the objects.

The second set of results involves the

experimental evaluation of the effectiveness of
the soft fingertips used to move a soft object and
a fragile object between two locations. The
process cycle is outlined in
Fig. 8. The results from the simulations are used
to develop an end effector with a viscoelastic
interface. The gripper was used to fulfil two
tasks successfully. The first task was to pick and
place an object which had a smooth exterior and
soft composition, i.e. a fruit (tomato) was chosen
for its smooth exterior surface and soft body.
Fig. 10 shows the grasping, picking and placing
of the egg. The second task was performed with
a fragile object namely an uncooked egg. The
object was picked and placed safely without
cracking. The friction parameters for soft finger
surfaces have been calculated from the
simulations. Both objects remained intact during
the experiments because of the soft material
(having viscoelastic property) beneath the
surface of the fingers [41].

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Fig. 9. Gripper having three soft fingers. Grasping, picking, based on the equations (4-7) and presented.
and placing of the tomato have been demonstrated. Comparison of the end effector motions for
different solvers has been presented in

Fig. 14. Simulations of complex systems require

verification and this has been achieved through
the comparison of the results.

Fig. 11. Manipulator space in 3 dimensions.

Fig. 10. Experiments with the developed gripper

having three soft fingers. Grasping, picking and
placing of the raw egg are demonstrated.

4. RESULTS AND DISCUSSION

4.1. Dynamic Simulation

The results of the dynamic simulation of the

arm have been presented below. The reach of
the manipulator or the extent it traverses the
workspace has been illustrated in Fig. 11.
Execution times for the different solvers vary.
ODE15s solver takes most execution time
followed by ODE23s, ODE23tb and ODE23t.
ODE15s is suitable for solving stiff differential
equations and differential algebraic equations
(DAE). Friction torque generated at the joints is
presented in Fig. 12. A PID controller has been
used to generate control torque which is shown
in Fig. 13. Friction torques have been generated

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Fig. 12. Comparison of friction torque generated at

the three joints for different simulations.

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Fig. 14. Comparison of end effector motion in task

manipulator task space for different simulations.

Fig. 13. Control torques from the controller for the

three planar joints of the manipulator.

Fig. 15. Coefficient of friction measured by using

micro-friction tribometer.
Comparison of the friction torques generated in
joints gives an insight on the effect of the
numerical solver on the solution. Stiff solvers
have been selected where smaller step sizes are
required. The difference in output parameters
may be attributed to the solver step size.
Simulations 1, 3 and 4 appear to agree.
Simulation 3 takes minimum execution time.
Therefore, solvers used in simulations 1, 3 and 4
may be suitable for simulation involving friction.

4.2. Coefficient of friction from micro-friction

test

The coefficient of friction is measured by using

reciprocating micro friction tribometer. It is
observed that the value of friction was stabilised
in 200-300 s into the test which was conducted
for 10 minutes. The values of the coefficient of
friction were observed to lie between 0.08 and
0.11 for the fully lubricated contact conditions.
Therefore, low frictional torqueses are likely to
be generated in newer machinery with close fit
at the joints. However, with continued usage of
mechanism, there is likely to be wear in the joint
which will alter friction and affect the joint
dynamics. The results from Bond graph
simulation are presented in Fig. 15.

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4.3. Bond graph Simulation
The objective of this research is to pick and place
the fragile and soft objects without slippage by
using a soft fingered gripper. 20Sim [65] was
used for simulation of Bond graph model. In
simulation, it was found that after gripping the
object, the displacement due to its weight is
considerably small, i.e., only in micrometres.
Experimental results show that there is no
slippage after gripping the object.
a)
b)
c)
Table 5. Simulation results from 20Sim [41].
570
Fig. 16. a. Velocity of object during grasping at
stiffness = 10 N/m, damping = 5ns/m and friction = 5
N.s/m, b. Velocity of object during grasping at
stiffness = 10 N/m, damping = 10 N.s/m and friction
= 10 N.s/m, c. Velocity of object during grasping at
stiffness = 20 N/m, damping = 20 N.s/m and friction
= 20 N.s/m.
Simulations have been repeated for a range of
stiffness and damping values to study the effect of
these parameters on the friction and the system
stability. The values of Rd and Rf in each soft finger
were varied from 5 N.s/m to 20 N.s/m and that of
Ks was varied from 10 to 20 N/m. The mass of the
object was fixed at 100g for all simulations.
Consolidated table containing all the simulated
results are given in [41] (Error! Reference
source not found.). The velocity of the object and
its displacement for 1N force was observed. The
velocity of the object after gripping has been
shown in Fig. 16. The object slips initially during
the grasping. Steady state value of zero
displacement was achieved after 200
milliseconds.
5. CONCLUSIONS
This paper addresses two challenges. The first
challenge is the rapid development of
manipulator mechanics using high end virtual
prototypes which is extended to include the
effects of joint friction parameters. With the
increase in computational resources, virtual
prototyping has been increasingly used to model
the mechanics of new designs, leading to both
time and cost savings. In this work, it is
demonstrated this by using computer aided
drawing and multibody dynamics to develop the
prototype of a humanoid manipulator.
Additionally, the friction model has been
incorporated into the joints of the robotic arm.
The value of the coefficient of friction from tribo-
tests has been used to run several simulations of
the manipulator mechanics.
The second problem analysed in this paper deals
with the issue of effective grasping of soft and
fragile objects. Bond Graph method is used to
model the end interactions of the viscoelastic
grip on fragile objects. Simulation of the model
demonstrates the stabilising effect of linear
viscoelastic fingertips grasping fragile objects.
 A. Khurshid et al., Tribology in Industry Vol. 38, No. 4 (2016) 559-574

Ks1 = Rd1 = Rf1 = Settling Time

Ks2 = Rd2 = Rf2 = Peak velocity Peak Displacement Steady State Value of
for Steady State
# Ks3 Rd3 Rf3 [m/s] [mm] Displacement [mm]
Velocity [s]
[N/m [N.s/ [N.s
] m] /m] vx vy vz vx vy vz x y z x y z
1 10 5 5 -1.2 -1.7 -1.4 0.4 0.5 0.4 -0.036 -0.12 -0.05 -0.025 -0.043 -0.032
2 10 10 10 -2.6 -2.8 -2.7 0.5 0.8 0.5 -0.6 -0.14 -0.08 -0.025 -0.043 -0.032
3 10 15 15 -4.0 -4.2 -4.1 0.3 1.0 0.6 -0.072 -0.14 -0.089 -0.028 -0.037 -0.032
4 10 20 10 -5.5 -5.5 -5.5 0.4 0.8 0.7 -0.08 -0.137 -0.09 -0.030 -0.037 -0.032
5 20 5 5 -1.3 -1.7 -1.4 0.6 0.8 0.6 -0.037 -0.126 -0.091 -0.032 -0.036 -0.033
6 20 10 10 -2.7 -2.9 -2.8 0.6 0.9 0.6 -0.06 -0.14 -0.08 -0.032 -0.036 -0.033
7 20 20 10 -5.5 -5.5 -5.5 0.4 0.8 0.6 -0.08 -0.137 -0.09 -0.032 -0.036 -0.033

Optimised values of damping and stiffness for
stable grasp are determined from the
experimentations. Soft fingertips and rotation
mechanism have been designed. The property of
viscoelasticity of material is used in fine tuning
the grip at the fingertips. It has been concluded
based on the results of simulation that by
varying the values of parameters as stiffness,
damping and friction at the contact interface,
velocity of grasped object and displacement
during grasping can be controlled. These
parameters also influence the peak value of
velocity and stability of the grasp and their
variation can be used for performing in-grasp
fine manipulation of the object. Successful
experiments were performed by gripping,
picking and placing two objects, a fragile egg and
a soft tomato.
Acknowledgement
The authors acknowledge the support of Air
University and National University of Sciences
and Technology, Islamabad, Pakistan.
REFERENCES
[4] N. Xydas and I. Kao, Modeling of Contact
Mechanics and Friction Limit Surfaces for Soft
Fingers in Robotics, with Experimental Results,
Int. J. Rob. Res., vol. 18, no. 9, pp. 941950, 1999.
[5] K.B. Shimoga and A.A. Goldenberg, Soft
materials for robotic fingers, Robot. Autom.
1992. Proceedings., IEEE Int. Conf., vol. 2, pp.
13001305, 1992.
[6] A. Ghafoor, J.S. Dai and J. Duffy, Fine motion
control based on constraint criteria under pre-
loading configurations, J. Robot. Syst., vol. 17,
no. 4, pp. 171185, 2000.
[7] A. Ghafoor, J.S. Dai and J. Duffy, Stiffness Modeling
of the Soft-Finger Contact in Robotic Grasping, J.
Mech. Des., vol. 126, no. 4, pp. 646656, 2004.
[8] J.S. Dai, D.R. Kerr and R. Group, A six-
component contact force measurement device
based on the Stewart platform, Proc. Inst. Mech.
Eng. Part C J. Mech. Eng. Sci., vol. 214, no. 5, pp.
687697, 2000.
[9] A. Khurshid, A. Ghafoor, M. A. Malik and M.
Afzaal, Robotic Grasping and Fine Manipulation
Using Soft Fingertip, Adv. Mechatronics, pp.
155174, 2011.
[10] V. Tincani et al., Implementation and control of
the Velvet Fingers: A dexterous gripper with
active surfaces, in: 2013 IEEE Int. Conf. Robot.
Autom., pp. 27442750, May 2013.

[1] S. Ivaldi, V. Padois and F. Nori, Tools for
dynamics simulation of robots: a survey based
on user feedback, CoRR, pp. 1-15, 2014.
[2] M. Dooner, J. Wang and A. Mouzakitis, Dynamic
modelling and experimental validation of an
automotive windshield wiper system for
hardware in the loop simulation, Syst. Sci.
Control Eng., vol. 3, no. 1, pp. 230239, 2015.
[11] E. Brown et al., From the Cover: Universal
robotic gripper based on the jamming of
granular material, Proc. Natl. Acad. Sci., vol. 107,
no. 44, pp. 1880918814, 2010.
[12] M. Popovi et al., A strategy for grasping
unknown objects based on co-planarity and
colour information, Rob. Auton. Syst., vol. 58, no.
5, pp. 551565, 2010.

[3] S.E. Tomlinson, R. Lewis and M.J. Carr, The
effect of normal force and roughness on friction
in human finger contact, Wear, vol. 267, no. 58,
pp. 13111318, 2009.
[13] V.N. Dubey and R.M. Crowder, Grasping and
control issues in adaptive end effectors, Proc.
DETC04 ASME 2004 Des. Eng. Tech. Conf.
Comput. Inf. Eng. Conf., pp. 19, 2004.
[14] L.U. Odhner et al., A compliant, underactuated

571
 A. Khurshid et al., Tribology in Industry Vol. 38, No. 4 (2016) 559-574
hand for robust manipulation, Int. J. Rob. Res.,
vol. 33, no. 5, pp. 736752, 2014.
[15] H.-J. Cha, K.C. Koh and B.-J. Yi, Stiffness
modeling of a soft finger, Int. J. Control. Autom.
Syst., vol. 12, no. 1, pp. 111117, 2014.
[16] L. Biagiotti, F. Lotti, C. Melchiorri and G. Vassura,
How Far Is the Human Hand? A Review on
Anthropomorphic Robotic End-effectors Basic
concepts, Hand, p. 1-21, 2004.
[17] K. Waldron, K. Waldron, J. Schmiedeler and J.
Schmiedeler, Kinematics, Springer Handb.
Robot., pp. 933, 2008.
[18] R. Featherstone and D.E. Orin, Dynamics,
Robotics, pp. 3565, 2008.
[19] G.J. Monkman, S. Heute, R. Steinmann and H.
Schunk, Introduction to Prehension
Technology, Robot grippers, pp. 118, 2007.
[20] P. Schneider and W. Servis, Robot grippers in
systems projects, Ind. Robot An Int. J., vol. 15,
no. 4, pp. 211215, 1988.
[21] R. Alqasemi, S. Mahler and R. Dubey, A Double
Claw Robotic End-Effector Design, Recent
Advances in Robotics, pp. 16, 2007.
[22] B.M. Jau, Dexterous Telemanipulation with Four
Fingered Hand System, Robot. Autom. 1995.
Proceedings., 1995 IEEE Int. Conf., vol. 1, pp. 338
343, 1995.
[23] D. Prattichizzo, M. Malvezzi and A. Bicchi, On
motion and force controllability of grasping
hands with postural synergies, IEEE Trans.
Robot., vol. 2, no. 6, pp. 116, 2010.
[24] M.R. Tremblay and M.R. Cutkosky, Estimating
friction using incipient slip sensing during a
manipulation task, in: Proceedings IEEE
International Conference on Robotics and
Automation, 1993, pp. 429434.
[25] W.H. Ding, H. Deng, Q.M. Li and Y.M. Xia,
Control-orientated dynamic modeling of
forging manipulators with multi-closed
kinematic chains, Robot. Comput. Integr. Manuf.,
vol. 30, no. 5, pp. 421431, 2014.
[26] L.U. Odhner, R.R. Ma and A.M. Dollar, Precision
grasping and manipulation of small objects from
flat surfaces using underactuated fingers,
Proceedings - IEEE International Conference on
Robotics and Automation, pp. 28302835, 2012.
[27] M.R. Cutkosky and P.K. Wright, Friction,
Stability and the Design of Robotic Fingers, Int.
J. Rob. Res., vol. 5, no. 4, pp. 2037, 1986.
[28] S.E. Tomlinson, R. Lewis and M.J. Carr, Review of
the frictional properties of fingerobject contact
when gripping Proc. Inst. Mech. Eng. Part J J. Eng.
572
Tribol., vol. 221, no. 8, pp. 841850, 2007.
[29] M. Gabiccini, A. Bicchi, D. Prattichizzo and M.
Malvezzi, On the role of hand synergies in the
optimal choice of grasping forces, Auton.
Robots, vol. 31, no. 23, pp. 235252, 2011.
[30] J. Aleotti and S. Caselli, Part-based robot grasp
planning from human demonstration, Proc. - IEEE
Int. Conf. Robot. Autom., pp. 45544560, 2011.
[31] D. Song, K. Huebner, V. Kyrki and D. Kragic,
Learning Task Constraints for Robot Grasping
using Graphical Model Bayesian Network, pp.
15791585, 2010.
[32] D. Berenson and S.S.S. Srinivasa, Grasp synthesis
in cluttered environments for dexterous hands,
2008 8th IEEE-RAS Int. Conf. Humanoid Robot.
Humanoids 2008, pp. 189196, Dec. 2008.
[33] J.S. Son, E.A. Monteverde and R.D. Howe, A
tactile sensor for localizing transient events in
manipulation, in: Proceedings of the 1994 IEEE
International Conference on Robotics and
Automation, 1994, pp. 471476.
[34] M. H. Nazir, Z. Khan and K.R. Stokes, Modelling
of metal-coating delamination incorporating
variable environmental parameters, J. Adhes. Sci.
Technol., vol. 29, no. 5, pp. 392423, 2015.
[35] M.H. Nazir, Z.A. Khan and K.R. Stokes, A holistic
mathematical modelling and simulation for
cathodic delamination mechanism a novel and
an efficient approach, J. Adhes. Sci. Technol., vol.
29, no. 22, pp. 24752513, 2015.
[36] M.H. Nazir, Z.A. Khan and K.R. Stokes,
Optimisation of interface roughness and
coating thickness to maximise coatingsubstrate
adhesion a failure prediction and reliability
assessment modelling, J. Adhes. Sci. Technol.,
vol. 29, no. 14, pp. 14151445, 2015.
[37] D. Keymeulen and C. Assad, Investigation of the
Harada Robot Hand For Space, Jet Propuls. Lab., 2001.
[38] J.A. Bagnell et al., An integrated system for
autonomous robotics manipulation, 2012
IEEE/RSJ Int. Conf. Intell. Robot. Syst., pp. 2955
2962, 2012.
[39] M.T. Mason, A. Rodriguez, S.S. Srinivasa and A.S.
Vazquez, Autonomous manipulation with a
general-purpose simple hand, Int. J. Rob. Res.,
vol. 31, no. 5, pp. 688703, 2012.
[40] A. Khurshid, A. Ghafoor and M.A. Malik, Modeling
and Analysis of Soft Contact in Robotic Grasping
Using Bond Graph Methods, Adv. Mater. Res., vol.
189193, pp. 17861792, 2011.
[41] A. Khurshid, A. Ghafoor, M.A. Malik and Y. Ayaz,
Modeling and analysis of robotic grasping using
soft fingertips, in: Proceedings CLAWAR2013,
 A. Khurshid et al., Tribology in Industry Vol. 38, No. 4 (2016) 559-574
2013, pp. 642650.
[42] J.C. Trinkle, On the Stability and Instantaneous
Velocity of Grasped Frictionless Objects, IEEE Trans.
Robot. Autom., vol. 8, no. 5, pp. 560572, 1992.
[43] M. Salerno, K. Zhang, A. Menciassi and J. S. Dai, A
novel 4-DOFs origami enabled, SMA actuated,
robotic end-effector for minimally invasive
surgery, in: 2014 IEEE International Conference
on Robotics and Automation (ICRA), 2014, pp.
28442849.
[44] S. Degeratu, P. Rotaru, S. Rizescu and N.G. Bzdoac,
Thermal study of a shape memory alloy (SMA)
spring actuator designed to insure the motion of a
barrier structure, J. Therm. Anal. Calorim., vol. 111,
no. 2, pp. 12551262, 2013.
[45] X. Zhang et al., Strong Carbon-Nanotube Fibers
Spun from Long Carbon-Nanotube Arrays,
Small, vol. 3, no. 2, pp. 244248, 2007.
[46] C.S. Haines et al., Artificial muscles from fishing
line and sewing thread, Science, vol. 343, no.
6173, pp. 868872, 2014.
[47] J.M. Hollerbach, I.W. Hunter and J. Ballantyne, A
comparative analysis of actuator technologies
for robotics, Robot. Rev. 2, 1991.
[48] E.T. Roche et al., A bioinspired soft actuated
material, Adv. Mater., vol. 26, no. 8, pp. 1200
1206, 2014.
[49] J.A. Lee, R.H. Baughman and S.J. Kim, High
performance electrochemical and
electrothermal artificial muscles from twist-
spun carbon nanotube yarn, Nano Converg., vol.
2, no. 1, p. 8, 2015.
[50] A.J. Koivo, Kinematics of Excavators (Backhoes)
for Transferring Surface Material, J. Aerosp.
Eng., vol. 7, no. 1, pp. 1732, 1994.
[51] B. Donald, Forward Kinematics: The Denavit-
Hartenberg convention.
[52] A.J. Koivo, M. Thoma, E. Kocaoglan and J.
Andrade-Cetto, Modeling and Control of
Excavator Dynamics during Digging Operation,
Journal of Aerospace Engineering, vol. 9, no. 1.
pp. 1018, 1996.
[53] B.P. Patel and J.M. Prajapati, Dynamics of Mini
Hydraulic Backhoe Excavator: A Lagrange-Euler
(LE) Approach, Int. J. Mech. Aerospace, Ind.
Mechatron. Manuf. Eng., vol. 8, no. 1, pp. 202
211, 2014.
[54] S. alini, G. Bokovi and M. Nikoli, Dynamic
modelling of hydraulic excavator motion using
Kanes equations, Autom. Constr., vol. 44, pp.
5662, Aug. 2014.
[55] N.K. Myshkin and A.Y. Grigoriev, Roughness and
texture concepts in tribology, Tribology in
Industry, vol. 35, no. 2, pp. 97103, 2013.
[56] The Mathworks Inc. UK, Rotational Friction,
Mathworks Documentation, 2015.
[57] C.S. Ramesh, S. Khan, K. Zulfiqar and K.S. Sridhar,
Slurry Erosive Wear Behavior of Hot Extruded
Al6061-Si3N4 Composite, Mater. Sci. Forum, vol.
773774, pp. 454460, 2013.
[58] C.S. Ramesh, M.L. Shreeshail, G. Harsha and K.
Zulfiqar, Air Jet Erosion Wear Behavior of Al6061-
SiC-Carbon Fibre Hybrid Composite, Mater. Sci.
Forum, vol. 773774, pp. 547554, 2013.
[59] A. Khurshid and M.A. Malik, Modeling and
Simulation of an automotive system by using
Bond Graphs, in: 10th International Symposium
on Advanced Materials ISAM, 2007.
[60] A. Khurshid and M.A. Malik, Bond Graph
Modeling and Simulation of Impact Dynamics of
a Car Crash, in: 5th International Bhurban
Conference On Applied Sciences And Technology
IBCAST, 2007.
[61] M.A. Malik and A. Khurshid, Bond graph modeling
and simulation of mechatronic systems, in: 7th
International Multi Topic Conference, 2003. INMIC
2003., 2003, pp. 309314.
[62] M.A. Chowdhury, D.M. Nuruzzaman, A.H. Mia,
and M.L. Rahaman, Friction coefficient of
different material pairs under different normal
loads and sliding velocities, Tribology in
Industry, vol. 34, no. 1, pp. 1823, 2012.
[63] M.A. Chowdhury, D.M. Nuruzzaman, B.K. Roy, S.
Samad, R. Sarker and A.H.M. Rezwan,
Experimental Investigation of Friction
Coefficient and Wear Rate of Composite
Materials Sliding against smooth and rough mild
steel counterfaces, Tribology in Industy, vol. 35,
no. 4, pp. 286296, 2013.
[64] J. Lakshmipathy and B. Kulendran,
Reciprocating wear behaviour of 7075Al/SiC
and 6061Al/Al2O3 composites: A study of effect
of reinforcement, stroke and load, Tribology in
Industry, vol. 36, no. 2, pp. 117126, 2014.
[65] University of Twente, 20sim, 2015.
Nomenclature
Angle between z axes of coordinate systems of
i
two consecutive links
actual Output angular parameters from the model
desired Desired input angle for simulation
i Joint rotation angles between links
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i Angular velocity position

FK Forward Kinematics
i Angular acceleration IK Inverse Kinematics
G Gravity Forces Matrix
brk Breakaway torque
H Centripetal forces matrix
br.thr Threshold breakaway torque
Ks Springs stiffness in each soft finger (N/m)
C Coulomb friction torque
Arbitrary constant in the friction contact
Control torque m
model
Coefficient of Friction
Mf Mass of each finger (kg)
Angular velocity
Mo Mass of the object being grasped (kg)
thr Threshold angular velocity
Filter coefficient (PID controller), Normal force
Aii1 Kinematic transformation matrix N
at contact
B Friction Forces matrix ODE Ordinary differential equation
cv Coefficient of viscous friction pi Coordinates of ith frame
ctrans Coefficient of transition PID Proportional Integral Derivative Controller
CAD Computer Aided Design Rf Friction at each soft finger contact (Ns/m)
D Inertia Matrix Rd Damping in each soft finger (Ns/m)
DAE Differential Algebraic Equations Sfi Force applied on ith soft finger (N)
DOF Degrees(s) of Freedom Se Weight of the object (N)
e Error signal between control and actual

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 Vol. 38, No. 4 (2016) 575-584

Tribology in Industry

RESEARCH
www.tribology.fink.rs

Numerical Analyses of the Non-Newtonian Flow

Performance and Thermal Effect on a Bearing
Coated with a High Tin Content

K. Mehala a, N. Bendaoud a, A. Youcefi a

aUniversity of the Sciences and Technology of Oran Mohammed Boudiaf, 1505 El Menaour Bir El Djir Oran Algeria
Faculty of mechanical engineering, Engineering department, Algeria.

Keywords:
Thermal effect
Non-Newtonian flow
Plain cylindrical journal bearing
Coated
Corresponding author:
Kadda Mehala
University of the Sciences and
Technology of Oran Mohammed
Boudiaf, 1505 El Menaour Bir El Djir
Oran Algeria
Faculty of mechanical engineering,
Engineering department
E-mail: postegraduation@yahoo.com
ABSTRACT
The hydrodynamic bearings are stressed by severe workings conditions,
such as speed, load, and the oil will be increasingly solicit by pressure and
shear. The Newtonian behavior is far from being awarded in this case, the
most loaded bearings operating at very high speeds; the shear rate of the
oil is of higher order.
A numerical analysis of the behavior of non-Newtonian fluid for plain
cylindrical journal bearing finite dimension coated with antifriction
material with a high tin content, for to facilitate the accommodation of
the surfaces and save the silk of the shaft in the case of a contact. this
analyses is implemented using the code-ANSYS CFX, by solving the energy
equation with the finite difference method, considering that laminar
regime and the fluid is non Newtonian by using the power law Ostwald
model, the coefficient n is equal to 1.25 and for different model such as
Bingham, cross and Hereshek-Bulkley model.
This study aims to better predict the non-Newtonian behavior of the oil
film in bearings operating under more severe conditions. The purpose
conducted during this study is to predict the effect of non-Newtonian
behavior of the film; the journal bearing operating under severe
conditions, the speed of rotation varies from 1000 to 9000 rpm and the
bearing working under radial load 2 to 10 kN. Temperature and the
pressure within the fluid film assumed non-Newtonian are high, with a
coefficient n greater than 1 that is to say for viscoelastic fluids.
2016 Published by Faculty of Engineering

1. INTRODUCTION viscosity versus shear rate. The viscoelastic effects

The non-Newtonian effects can be of two kinds:
the shear-thinning effects and viscoelastic effects.
The shear-thinning effects, often simply called
non-Newtonian effects, result in a variation of the
are more complex, but in simple terms, we can say
that the viscoelastic fluids have a memory of their
deformities. There are several models that can
represent the viscoelastic behavior. Among them,
the simplest and most used is the Maxwell model,

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 K. Mehala et al., Tribology in Industry Vol. 38, No. 4 (2016) 575-584
which takes into account two parameters:
viscosity and relaxation time.
The plain journal bearing have been largely used
in industrial applications for more than a
century. However, the thermal behaviour in the
journal bearing became only recently the object
for the researchers, while considering the fluid
has a non-Newtonian behaviour.
Hirst and Moore [1] present a study in 1974 on
non-Newtonian behavior in the
elastohydrodynamic lubrication, they stated in
their study that low values, the shear rate is
directly proportional to the shearing force, but
higher values, the shear rate increases faster than
the shear stress, this phenomenon depends on
the pressure and molecular size of the fluid film.
In 1985, Hutton [2] performs an experimental
study on the effect of lubricant on the u
performance sliding bearing, the experimental
results performed on a bearing in order to verify
the theory that the capacity of the load is
generated by the elasticity viscoelastic lubricants.
Gecim [3] published in 1990 a review of the
literature on shear-thinning effects. He shows
some examples and technical solutions for the
treatment of non-Newtonian effects in plain
bearings. He introduced a new incorporating act,
based on the Cross of law. The advantage of this
law is that it has a single parameter to adjust
(the stability coefficient), compared to the Cross
equation which uses three parameters.
During the same period, Rastogi and Gupta [4,5]
analyze the importance of viscoelastic effects in
bearings subjected to dynamic loads that they
use the Maxwell model. They showed a decrease
Load carrying capacity in the presence of a
viscoelastic behavior.
Lemaitre and Berker [6] realized two years later
a study on the modeling of non-Newtonian
effects in plain bearings. They propose an
extension of the cavitation Elrod algorithm for a
non-Newtonian behavior of the fluid, using the
finite volume method.
In 2000, Zhang and Cheng [7] propose a non-
Newtonian thermohydrodynamic analysis in
conditions of mixed lubrication. Both non-
Newtonian effects (shear thinning and
576
viscoelastic) are included. They show that there
is significant influence of the shear thinning
effect on the minimum thickness on the power
loss and leakage flow dynamic bearings.
However, the viscoelastic effect has no
significant influence on these parameters and
can more or months influence the load capacity
bearings, compared to operating conditions.
In 2001 and 2002 Wang et al. [8,9] have also
addressed the influence of shear thinning effects
in dynamic bearings, while taking into account
the non-Newtonian behavior and the effect of
the geometry of the elliptical -form palier- ave
rough surfaces. They show that it has a
significant reduction in the minimum film
thickness and power dissipation.
In the same year, Zhang [10] continues the study
with an analysis TEHD dynamic bearings. It
happens almost the same conclusions as in the
THD study. Moreover, he argues that the
viscoelastic effect tends to reduce the variation
of pressure over time and thus reduce the
pressure peaks and the elastic deformation.
In 2003 Kane [11] show the effect of the
roughness and non-Newtonian effects in severe
contact lubricated such as bearings. He
presented a new modified Reynolds equation
called non-Newtonian, using the rheological
laws and the basics of continuum mechanics
applied to thin film. Solving this equation gives
the influential parameters on geometry and
rheology, these results were validated with the
non-Newtonian theory.
Fatu [12] in 2005 present a numerical and
experimental modeling of the lubrication of motor
bearings subjected to severe operating conditions
with the laws of variation of the suitable viscosity,
it stinks meter highlight the respective influence of
non-effects Newtonian and piezovisqueux in the
complex case of big end bearings. Fatu showed
that piezovisqueux effect turns out to be most
significant effect on the behavior of the bearing,
the non-Newtonian effect.
In 2012, Singh and al [13], present a study on the
performance of pivoted curved slider bearings
by suggest that the fluid is non Newtonian, by
using the Rabinowitsch Fluid Model. The results
show that steady state film pressure, load
carrying capacity and centre of pressure,
 K. Mehala et al., Tribology in Industry Vol. 38, No. 4 (2016) 575-584

calculated numerically for various values of 2.1 Basic Equations

viscosity index, have been significant with the
non-Newtonian behavior of the fluid. The equation describing the flow in the gap is the
generalized Reynolds equation (Dowson, [16]).
Javorova and his colaborators, have been
presented in 2016 [14], a study on 3 p Ra 2 3 p I 2 h
Gh Gh h1 (1)
hydrodynamics Journal Bearings Considering L2 z J 2 t
Elastic Deformation and Non-Newtonian fluid,
by using the Rabinowitsch fluid model. They where:
have showed that higher values of film pressure
and load carrying capacity have been obtained h h/C, y y/h, / 0 , t t,
for dilatant lubricants, while for pseudoplastic
lubricants; pressure in oil film is less significant. C2
p p , z z/L
0Rs2
The present study investigates the effect of
y I2
1
temperature in laminar regime by resolution of the
G y d y ,
energy equation with the finite difference method. J 2
This analysis studied the impact the behavior non- 0

Newtonian fluid for journal bearing working under 1

y
sever operating condition. The non-Newtonian I2 dy, (2)
behavior of lubricants (oils containing polymers 0
PM3) was analyzed numerically. Moreover, the 1
1
fact that the oils containing polymers should have J2 dy
a decrease in viscosity and normal stress at a high 0
shear rate, so having a non-Newtonian behavior, In order to get pressure field, Reynolds type
rheological properties were examined according to boundary conditions are considered. The
the levels of operating conditions by Moritsugu boundary conditions for pressure are
KASAI in 2010 [15]. summarized by the following equations:
- at the bearing sides:
2. THEORETICAL ANALYSES

p , L / 2 0 (3)
In order to theoretically predict the temperature - At the limit of the rupture zone traditional
field throughout a plain bearing, one ought to Reynolds boundary conditions are
create a 3D thermohydrodynamic theoretical applied:
model. The schematic representation of the
p
journal bearing is presented in Fig. 1. p r 0 (4)
Y
r

The temperature in the bush is given by the

bidimensional energy equation in polar
RB coordinates:
W
T 1 T 1 2T
B cB kB r 2 2 (5)
X
t r r r r
e
The temperature in the shaft is supposed to be
OB
uniform in the circumferential direction, due to
OS
RS its rotation; the energy equation reduces to a
unidimensional form:
T 1 T
s cs ks r (6)
t r r r
Fig. 1. Schematisation of plain
Fig.1 Schematisation of plainjournal bearing.
journal bearing

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 K. Mehala et al., Tribology in Industry Vol. 38, No. 4 (2016) 575-584

Heat flux continuity condition was imposed at where 0 is the zero shear viscosity,
the interface between the oil film and the shaft:
viscosity at infinite shear, time constant, is an
T
o
T exponent of power law and is a parameter that
2k s kF d (7) describes the transition from the low shear and
r r Rs
I y y 0
power law behavior region.
While at the interface between the oil film and
the bush the heat flux continuity condition is: 2.2.2 Viscoplastic oils

T T The nonlinear viscoplastic oil are characterized

kB kB (8)
y y h
r r RB
by a shear threshold it has two phases: liquid
and solid as example fats. In this section we
The initial temperature condition for the present the fluids and Bingham Hereshek-
transient problem is: Bulkley.
T t 0
T0
a) Bingham model
2.2 Empirical relationships for viscosity
The Bingham fluid viscoplastic are characterized
by a single elastic 0, over which the said fluids
When the viscosity is not independent of shear rate,
it is necessary to use several parameters to describe behave as Newtonian fluids. The viscosity is is
the mechanical behavior of the fluid. A number of expressed by:
empirical models provide this description. 0

0 (4)

2.2.1 Pseudo plastic Fluids

Fluid conducting a pseudo-plastic viscosity
decreases when the shear stress increases, their
rheological behavior are not linear these are
monophasic oils such as heavy oils.
a) Model of power law Ostwald: In a certain
range of shear rates, the viscosity can be
represented as a power law,
molten polymers:
n 1
0 (1)
Newtonian fluid corresponds to n = 1 and a
shear-thinning fluid is represented by n <1.
where 0 reference viscisity.
b) Hereshek-Bulkley model
The model Hereshek-Bulkley presents the
nonlinear case from that of Bingham, this model
is a combination of yield strength and plastic
nickname behavior of the power law, this law is
particularly for presented in the following form:
n 1 0
K
(5)
2.2.3 Expression of the pressure field with
non-Newtonian behavior oil film

The model of the power law can be used for Eg the power model Ostwald, the relationship of
fluids such as rubber, adhesive, polymers or the pressure field is given in the following form:
certain body fluids for isothermal flow. In the

case where the temperature varies in the field, it
6C 0 n 1 L
is possible to introduce the temperature T: p( , z ) sin Z (6)
(h r ) 3
4
n 1
0 e eT (2)
2.3 Thermal Deformations
b) Carreau model: The tile model is an
extension of the power law model that involves The thermal deformations of the bush and shaft
five parameters: may have important influence on the bearing
behaviour, the thermal displacement relative to

the shaft radius the initial temperature, T0, is
[1 ( ) a ]n 1 / a (3)
0 Timoshenko and Goodier in 1974 [17]:

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 K. Mehala et al., Tribology in Industry Vol. 38, No. 4 (2016) 575-584

2 s Rs
u s (t )
Rs T (r, t ) T rdr
0
0 (9)

The thermal displacement of the bush u B ( ) is

computed using the Finite element method.

2.4 Film thickness

Due to the thermal deformations of both the

shaft and the bush, the film thickness is given by
the following expression:
h C1 cos( ) ( ) (10)

with: Fig. 2. Finite element mesh of the bearing.

( ) u B ( ) u s (11)
3.1 Results and Discussed

The main features of the bush are presented in

3. NUMERICAL RESOLUTION ON THE Table 1.
THERMOOHYDRODYNAMIC EFFECT OF
THE BEARING ON TRANSIENT REGIME Table 1. Operating conditions and geometric
characteristics of the journal bearing.
In this part, we present the transient analysis on Bearing diameter D (mm) 100
speed effect for plain journal bearing and for Bearing lemgth L (mm) 80
thermohydrodynamic behaviour in lubricated Radial clearance C (mm) 0.09
Length of supply groove Lg (mm) 70
mechanism.
Food opening diameter do (mm) 14
Lubricant type
This study is carried out by the ANSYS CFX code Density of oil PM3
for obtain the pressure field distribution with Specific heat of lubricant (kg/m3) 800
energise equation resolution, by using the Finite Oil viscosity at 40C Cp (j/kgK) 2000
Oil viscosity at 80C
Differential Method. The both shaft and bush Rotational speed 1 (mm/s) 17,49
deformation is obtained with displacement Radial load 2 (mm/s) 8,003
equation resolution by Finite Elements Method. Ambient temperature N (r/min) 1000-9000
The discretization of the geometry in a number Supply pressure W (kN) 2-10
of elements finished well is presented in Fig. 2. Ta (C) 60
Pa (MPa) 0.04
In this meshing, nodes number is 31200 and
element number is 244201.
Pressure/Temperature

1) Velocity variation for load 2000 N and n=1.25

Pressure

1000 rpm 3000 rpm 5000 rpm

7000 rpm 9000rpm

Fig. 3. 3D view for pressure distribution.

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 K. Mehala et al., Tribology in Industry Vol. 38, No. 4 (2016) 575-584

Maximum pressure according rotational velocity There is the creation of the rupture zone of
for radial load 2000 N and for power law highly significant oil film, for Angular coordinate
Ostwald model, the coefficiet n is equal to 1.25, 200 to 250 for a bearing operating under
Is preseted in Fig. 4a. Import values for pressure velocity of 9000 rpm and for radial load 2000 N.
is noted for higly velocity (9000 rpm). Increses The pressure drop reaches 0.08 MPa.
is estimated of 90 per cent for velocity ranging of
1000 to 9000 rpm. Figure 5 show the pressure distribution of the
median plain cylindrical journal bearing for
radial load 2000N and n = 1,25
radial load 2000, 6000 and 10000 N and for
200000 rotational velocity 9000 rpm, for power law
Ostwald model with n = 1.25.
180000
maximum pressure (Pa)

650000
600000
160000 550000
500000 n = 1,25 N = 9000rpm
450000
2000 N
140000 400000
350000
6000N
300000 10 000N

Pressure (Pa)
120000 250000
200000
150000
100000
100000 50000
0
-50000
80000 -100000
0 2000 4000 6000 8000 10000 -150000
-200000
Rotational velocity (rpm) -250000
-300000
Fig. 4a. Maximum pressure according rotational 0 50 100 150 200 250 300 350
velocity for radial load 2000 N and n=1.25 Model of Angular coordinate ()
power law Ostwald. Fig. 5. Circumferentiel pressure for different radial
load for velociy 9000 rpm and n=1.25 (Model of
n = 1,25 W= 2000N
power law Ostwald).
200000

180000
1000 rpm
The significate pressure values is noted for
160000
3000 pm radial load of 10000 N, and the rupture zone is
5000 rpm
140000
7000 rpm highly significant for radial load 10000 N.
120000 9000 rpm
pressure (Pa)

100000
Temperature
80000

60000
Temperature evolution in medi n plain journal
40000
bearing for velocity ranging of 1000 to 9000 rpm
20000
is presented in Fig. 6. This figure shows clearly
0
that sigignificat temperature is obtain for velocity
150 200 250 300 350
7000 and 9000 rpm, for bearing subjected to
Angular coordinate ()
radial load 2000 N and lubricat by non newtonein
Fig. 4b. Circumferentiel pressure for different fluid with coefficient n equal to 1.25.
rotational velocity and for radial load 2000 N and
n=1.25 (Model of power law Ostwald).
1000 rpm 3000 rpm 5000 rpm
Pressure distribution of the median plain
cylindrical journal bearing for rotational velocity
1000 to 9000 rpm and for radial load 2000 N, is
illustrates in Fig. 4b, for power law Ostwald
model with n = 1.25. 7000 rpm 9000 rpm

The maximum pressure increases up to 180000

Pa for rotational speed ranging from 1000-9000
rpm, the increase is estimated by 76 per cent. It
is situated at angular coordinate 170 and 190. Fig. 6. 3D view for temperature distribution.

580
 K. Mehala et al., Tribology in Industry Vol. 38, No. 4 (2016) 575-584

The Average temperature according rotational Figure 8 presents the circumferentiel distribution
velocity for radial load 2000 N and n=1.25 of temperature for different radial load (2000,
(Model of power law Ostwald), is shown in Fig. 6000 and 10 000N) and for rotational velocity
7a, obtained from the numerical analysis in 9000 rpm, n=1.25 (power law Ostwald model).
6000, 9000, 11 000, 13 000 and 15 000 rpm and The maximum values for temperature is noted for
a radial load of 2000 N. The feeding condition is low radial load (2000 N).
presented in the Table 1. An increase of
335
temperature is estimated of 4 per cent with
increases the velocity from 1000 to 9000 rpm. n = 1,25 N = 9000 rpm
330
Radial load 2000 n and n= 1,25 2000 N
328 6000 N
10 000N

Temperature (K)
326 325

324
Average temperature

320
322

320

315
318

316
310
314 0 50 100 150 200 250 300 350
Angular coordinate ()
312
0 2000 4000 6000 8000 10000
Fig. 8. Circumferentiel temperature for different
Roational velocity (rpm)
radial load and for rotational velocity 9000 rpm
Fig. 7a. Average temperature according rotational n=1.25 (Model of power law Ostwald).
velocity for radial load 2000 N and n=1.25 (Model of
power law Ostwald). These digital temperature results were validated
335 with experimental results; that were presented
by the Bendaoud and al in 2012 [17] while
n = 1,25 W = 2000N
330
considering the fluid is Newtonian, Fig. 9.
1000 rpm
3000 pm
5000 rpm Figure 9 present circemfereciel temperature
Temperature (K)

7000 rpm
325
9000 rpm ditribution for radial load 2000 N and rotational
velocity 5000 rpm for experiment data and
320 Numerical resul for fluid newtonian. The Search
result is a reasonable agreement, the gap is
315 estimated 6 per cent.

47
310
0 50 100 150 200 250 300 350 46
Angular coordinate ()
Temperature (C)

45
Fig. 7b. Average temperature for different rotational 44
velocity for radial load 2000 N and n=1.25 (Model of
43
power law Ostwald).
42
experimental temperature
However, the Fig. 7b illustrates the distribution 41 numerical temperature
of the average temperature in median plan for 40
journal bearing. Rotational velocity is ranging of 0 100 200 300 400
1000 to 9000 rpm. The bearing is subjected to angular coordinate ()
radial load of 2000 N and fluid low is considered
non-Newtonian fluid. This figure shows clearly Fig. 9. circemfereciel temperature ditribution for
that the significant temperature is located for radial load 2000 N and rotational velocity 5000 rpm.
angular coordinate 50 to 120. The import
values are noted for velocity of 9000 rpm.

581
 K. Mehala et al., Tribology in Industry Vol. 38, No. 4 (2016) 575-584

2) Pressure and temperature for different (n) Maximum value obtains for velocity of 9000 rpm
for load 2000N and velocity 1000 rpm is 0.064; this value is between 0.05 and 0.2 (limit
lubrication).
Maximum pressure for different n for power law
Ostwald model is presented in figure 10, for 2000N

radial load of 2000N and rotational speed 1000 0,07

rpm. The maximum value for pressure is obtain
for n equal to 1.5 and is estimates by 250000 Pa. 0,06

Pressure increase with increases of the 0,05

Friction coefficient
coefficient n, this increases is estimated by 65
per cent. 0,04

Radial load 2000 N

0,03
280000 veleocity 1000 rpm

260000 0,02
240000
0,01
220000
maximum pressure (Pa)

200000 0,00
0 2000 4000 6000 8000 10000
180000
rotational velocity (rpm)
160000

140000 Fig. 12. Friction coefficient according rotational

120000 velocity for n=1.25 (Model of power law Ostwald).
100000

80000 Figure 13 presents the variation of the

0,2 0,4 0,6 0,8 1,0 1,2 1,4 1,6 maximum pressure with velocity variation of
Rotational velocity (rpm) 1000 to 9000 rpm, for tree different radial load
Fig. 10. Maximum pressure for different n (Model of (2000, 6000 and 10000 N), the fluid is
power law Ostwald). considered non-Newtonian with n=1.25.
Important values are obtained for radial loads
For the variation of the average temperature 10000 kN.
(Fig. 11), Temperature is significate for
coefficient n equal to 1.5. 2000N
6000N
10 000N
750000
radial load 2000 n
314,1
velocity 1000 rpm 700000

650000
314,0
Maximum pressure (Pa)

600000

550000
313,9
500000
Average temperature (K)

313,8
450000

313,7 400000

350000
313,6
300000

313,5 250000

200000
313,4 0 2000 4000 6000 8000 10000
rotational velocity (rpm)
313,3

313,2
0,2 0,4 0,6
Fig. 11. Average temperature for different n (Model
of power law Ostwald).
Figure 12 presents the variation of the friction
coefficient according rotational speed 1000 to
9000 rpm and for radial loads of 2000 N, this
variation is carried out by power law Ostwald
with n = 1.25. Friction coefficient has an increase
(0.005-0.064), is estimated of 80 per cent.
Fig. 13. Maximum pressure variation according
0,8 1,0 1,2 1,4 1,6 rotational velocity for different radial load (Model of
n power law Ostwald).
Average temperature according velocity for tree
different radial load (2000, 6000 and 10000N)
for power law Ostwald model with n = 1.25, is
presented in Fig. 14. The significate values for
temperature are noted for bearing operating
under radial load 2000 N. The maximum value is
328 K.

582
 K. Mehala et al., Tribology in Industry Vol. 38, No. 4 (2016) 575-584

2000N
330 6000N
The power law Ostwald model gives a realistic
10 000N temperature variation unlike the other model.
328
Knowing that the temperature increases with
326 increasing the rotation speed of the bearing.
Average temperature (K)

324

322
4. CONCLUSION
320

318 Most oils are considered to have a linear

316 variation in the shear stress versus shear rate,
314
for some highly additive oils and which operate
under severe stress; the behavior is no longer
312
0 2000 4000 6000 8000 10000 Newtonian. One speaks in this case, a non-
rotational velocity (rpm) Newtonian behavior.
Fig. 14. Average temperature according velocity for
different radial load (Model of power law Ostwald). To represent these behaviors, we expose a
numerical study on the behavior of non-
Figures 15 and 16 illustrates respectively the Newtonian fluid with several rheological models
maximum pressure and average temperature such as the simplest model of Oswald (also
variation according rotational velocity for known as the power law), Bingham, cross and
different non-Newtonian model and for radial Hereshek-Bulkley model. The thermal effect
load of 2000 N. has been included on the behavior of the bearing
to obtain the temperature map. The bearing
Power law Ostwald model
Bingham model alloy coated with an anti-friction high tin
14000000
Hereshek-Bulkley model
Cross model
content (Babbitt 88 % Tin).
12000000
Temperature is high and reaches a maximum
Maximum pressure (Pa)

10000000
value of 328 K, a bearing for operating at a speed
8000000 of 9000 rpm and which is subjected to a radial
6000000
load of 2000 N. The temperature increases 15 K.
4000000
However, the maximum pressure reached a
2000000 value of 0.18MPa and it is noted in the angular
0
position of the bearing of from 170 to 190 by
0 2000 4000 6000 8000 10000 varying the rotation speed of bearing of 1000
Rotational velocity (rpm)
rpm to 9000.
Fig. 15. Maximum pressure variation according
rotational velocity for different model and load 2000 N. Temperature and the pressure within the fluid
Power law Ostwald model film assumed non-Newtonian are high, with a
Bingham model
Hereshek-Bulkley model
coefficient n greater than 1 that is to say for
334
cross model viscoelastic fluids.
332

330

328 REFERENCES
Average temperature (K)

326

324 [1] W. Hirst and A.J. Moore; Non-Newtonian

322 Behaviour in Elastohydrodynamic Lubrication,
320 Proceedings of the Royal Society of London. Series
318 A, Mathematical and Physical Sciences, vol. 37,
316
pp. 101-121, 1974.
314

312
[2] J.F. Hutton, K.P. Jackson and B.P. Williamson,
0 2000 4000 6000 8000 10000 The effects of lubricant rheology on the
rotational velocity (rpm)
performance of journal bearings, ASLE
Fig. 16. Average temperature according velocity for transactions, vol. 29, pp. 52-60, 1985.
different model and for load 2000 N.

583
 K. Mehala et al., Tribology in Industry Vol. 38, No. 4 (2016) 575-584
[3] B.A. Gecim, "Non-Newtonian Effects of
Multigrade Oils on Journal Bearing
Performance", STLE Tribology Transaction, vol.
33, pp. 384-394, 1990.
[4] A. Rastogi and R.K. Gupta, "Lubricant Elasticity
and the Performance of Dynamically Loaded
Short Journal Bearings", Journal of Rheology, vol.
34, no. 8, pp. 1337-1356, 1990.
[5] A. Rastogi and R.K. Gupta, "Accounting for
Lubricant Shear Thinning in the Design of Short
Journal Bearings", Journal of Rheology, vol. 35,
no. 4, pp.589-603, 1991.
[6] F. Lematre and A. Berker, "Non-Newtonian
Cavitation Analysis in Journal Bearings", Elsevier
Journal of Non-Newtonian Fluid Mechanics, vol.
59, pp. 31-48, 1995.
[7] C. Zhang, "Thermoelastohydrodynamic of non-
newtonian dynamically loaded journal bearing
in mixed lubrication direct problem", ASME
Jounal of Tribology, vol. 124, pp. 178-185, 2002.
[8] P. Wang, T.G. Keith and K. Vaidyanathan, "Non-
Newtonian Effects on the Performance of
Dynamically Loaded Elliptical Journal Bearings
Using a Mass-Conserving Finite Element
Cavitation Algorithm", STLE Tribology
Transaction, vol. 44, no. 4, pp. 533-542, 2001.
[9] P. Wang, T.G. Keith and K. Vaidyanathan,
"Combined Surface Roughness Pattern and Non-
Newtonian Effects on the Performance of
Dynamically Loaded Journal Bearings", STLE
Tribology Transaction, vol. 45, no. 1, pp. 1-10, 2002.
[10] C. Zhang, Y. Wang, Q. Wang and, C. Lin, "A mixed
tehd analysis and experimantal of journal bearing
under severe operating conditions", Tribology
International, vol. 35, pp. 395-407, 2002.
[11] M. kane , "leffet de la rugosit et des effets non-
newtoniens dans les contacts svres lubrifis",
Thse de Doctorat, Institut national des sciences
appliques de Lyon, 2003.
[12] A. Fatu, "Numerical and experimental modeling
of the lubrication of motor bearings subjected to
drying conditions", Doctoral thesis, doctoral
school of sciences for the engineer of the
University of Poitiers, 2005.
[13] U.P. Singh, R.S. Gupta and V.K. Kapur, On the
Performance of Pivoted Curved Slider Bearings:
Rabinowitsch Fluid Model, Tribology in
Industry, vol. 34, no. 3, pp. 128-137, 2012.
584
[14] J. Javorova, A. Mazdrakova, I. Andonov and A.
Radulescu, Analysis of HD Journal Bearings
Considering Elastic Deformation and Non-
Newtonian Rabinowitsch Fluid Model, Triboloby
in Industry, vol. 38, no. 2, pp. 186-196, 2016.
[15] M. Kasai, "Reducing friction and improving the
reliability of the bearing lubrication with
automotive engine oils". Thesis, University of
Poitiers, specialty Mechanical Engineering,
Industrial Engineering, Transportation, 2010.
[16] A. Dowson, A Generalised Reynolds Equation
for Fluid Film Lubrication Int. Jour. Mech. Sc.,
vol. 4 pp. 159-170, 1962.
[17] N. Bendaoud, K. Mehala, A. Youcefi and M. Fillon,
An experimental and numerical investigation in
elastohydrodynamic behaviour of a plain
cylindrical journal bearing heavily loaded
Tribology- Proceedings of the Institution of
Mechanical Engineers, Part J: Journal of
Engineering Tribology, vol. 226, no. 10, pp. 809-
818, 2012.
[18] K. Mehala, N. Bendaoud and A. Youcefi,
Evolution of the lubrication regime of a
cylindrical journal bearing in the starting phase,
Industrial Lubrication and Tribology, vol. 66, no.
3, pp. 379386, 2014.
NOMENCLATURE
cs: specific heat [J/kg.k]
e: eccentricity [m]
h: film thickness [m]
k: thermal conductivity[w/m.K]
p: pressure [MPa]
t: time [s]
us:thermal deformation of the shaft [m]
uB:thermal deformation of the bush [m]
x, y: Cartesian coordinate, x = Rs
C: bearing clearance [m]
L: bearing length [m]
OB: bush center
Os: shaft center
Rs: shaft radius [m]
RB: bush radius [m]
T: temperature [C]
T0: initial temperature [C]
W: load [N]
 Vol. 38, No. 4 (2016) 585-589

Tribology in Industry

RESEARCH
www.tribology.fink.rs

Influence of the Previous Preheating Temperature

on the Static Coefficient of Friction with Lubrication

M. ivkovi a, M. Mateji b, D. Miljani c, Lj. Brzakovi a, V. Koovi b

a Higher Technical School of Mechanical Engineering, Radoja Krstia 19, 37240 Trstenik, Serbia,
b Faculty of Engineering, University of Kragujevac, Sestre Janji 6, 34000 Kragujevac, Serbia,
c TAMIA LTD, Trebjeka 6/28, 81400, Niki, Montenegro.

Keywords:
Static coefficient of friction
High temperatures
Temperature heat treatment
Lubrication
Oxidation layer
Corresponding author:
Marija Matejic
Faculty of Engineering,
University of Kragujevac,
Sestre Janji 6,
34000 Kragujevac, Serbia
E-mail: marija.jeremic@kg.ac.rs
ABSTRACT
Experimental investigations static coefficient of friction in lubricated
conditions and pre-heating of the sample pin at high temperatures is
discussed in this paper. The static coefficient of friction was measured in
the sliding steel copper pins per cylinder of polyvinylchloride. Pins are
previously heated in a special chamber from room temperature to a
temperature of 800 oC with a step of 50 C. Tribological changes in the
surface layer of the pins caused by pre-heating the pins at high
temperatures and cooling systems have very significantly influenced the
increase in the coefficient of static friction. The results indicate the
possibility of improving the friction characteristics of metal materials
based on their thermal treatment at elevated temperatures.
2016 Published by Faculty of Engineering

1. INTRODUCTION motionless body [3,4]. The coefficient of static

Surface roughness and condition of the contact
surface is of great interest and importance in
many applications including fluid flow. Numerous
theories are based on hypotheses and different
observations, which occur from experimental
data and explain the influence of different contact
surfaces on the value of the coefficient of friction.
In researches [1,2] the authors show that
increasing the temperature of the body in contact
has a significant impact on increasing the
coefficient static of friction. Static friction is
realized at the moment of macro tangential
displacement of a moving body in relation to a
friction depends on a number of parameters,
primarily the contact surface, normal load,
atmosphere and temperature, surface absorption,
surface finish and material of contact surfaces [5-
9]. Experimental tests [10-15] are based on the
observation of changes in the coefficient of static
friction due to changes in temperature of the
contact surfaces. In these studies, it is found that
the influence of increased temperature leads to
tribochemical changes on the surfaces of contact
pairs. The changes are shown in the form of the
appearance of oxides, borides, carbides and
nitrides, which causes the change in the
coefficient of static friction. It is observed that

585
 M. ivkovi et al., Tribology in Industry Vol. 38, No. 4 (2016) 585-589
keeping the contact pairs at higher temperatures
increases the oxide layer, which results in the
increasing of the coefficient of static friction.
When the surface contact between the contact
pairs becomes completely based on the contact of
iron oxide, it leads to stabilization of the
coefficient of static friction due to appropriate
chemical and thermal reactions [10]. According to
[16] it is experimentally confirmed that the
coefficient of static friction of tool steel has a
lower value at temperatures around 800 C.
Experimental results indicate that the coefficient
of static friction between the contact pair of
nitrided tool steel and boroned steel is lower at
higher temperatures compared to tool steel
without surface nitriding. Reducing the
coefficient of friction with increasing temperature
can possibly be connected to the formation of a
concentrated oxide layer, which is caused by
oxidation at higher temperatures [16]. Vanadium
(V) significantly reduces the coefficient of friction
at higher temperatures due to the ability of
forming lubricating oxides, V2O5 [16,17].
Experimental tests [18] show that the TiN coating
has a higher coefficient of friction during the
entire temperature range from 25 C to 700 C,
compared to the VN coating. Researches show
that the reason for the decreasing coefficient of
static friction of VN coatings is the previously
formed oxide layer which consists mainly of
V2O5 oxide. The mentioned oxide has a low shear
strength and very low melting point, which leads
to lower coefficients of static friction at higher
temperatures because of its crystallographic
structure [19].
Experimental research of static coefficient of
friction with the previous preheating contact
element from ambient temperatures up to
800OC, in steps of 50OC were carried out in this
paper. The contact element is cooled after pre-
heating to room temperature. We considered the
contact pair that makes steel copper pin with the
characteristics defined in DIN 8559 and pipe of
polyvinylchloride (EN1452-2). Whereby the pair
of contact during the measurement process in
fluid flow - oil. The measurement procedure is
identical to the measurements explained in the
framework by reference [20].
586
2. EXPERIMENTAL INVESTIGATIONS
Experimental investigations were carried out
with the previous thermal preparation the pin as
one of the contact pairs. Pins are previously
heated by the temperature from room
temperature to 800 C with a step of 50 C.
During the measurement process - sliding the
pin per cylinder (pipe) is conducted in a fluid
flow. Namely, tube is filled with fluid and sealed
in order to create identical conditions of
lubrication. The studies were conducted on
tribometer for measuring the static coefficient of
friction, which is described in details in [20]. The
sample (pin) is heated to a certain temperature
in a special chamber (Fig. 1), then cooled to
room temperature. After cooling to room
temperature, the sample is placed in cylinder
filled with fluid (Fig. 2). Considered the contact
pair that makes steel copper pin whose
characteristics are defined in DIN 8559 and tube
from polyvinyl chloride whose characteristics
are defined in standard (EN1452-2). Figure 2
shows the levelled position of the contact pair in
the middle of the fluid (oil) in which the tube is
rigidly attached to the platform measuring
device (tribometer).
Fig. 1. The sample is heated in the chamber
Rotating the platform at a specific angle of the ,
sliding occurs the pin per cylinder in the middle
of the fluid (Fig. 3). The angle at which the
sample begins with a sliding scale is read with a
tribometer. From the paper [20] it is known that
the tg is equal the static coefficient of friction.
 M. ivkovi et al., Tribology in Industry Vol. 38, No. 4 (2016) 585-589

3. ANALYSIS OF RESULTS

The experimental results are shown in the

diagram in Fig. 4. From the diagram, it can
clearly be seen growing trend static coefficient
of friction with increasing temperature of the
previous heat treatment pins. Oscillations trend
shows increase in the coefficient of friction as a
result of different levels of influence of certain
temperature range.

Fig. 2. The sample in levelled position.

Fig. 4. Dependence of the static coefficient of friction

s from the previous preheating temperature T.
Fig. 3. Rotating the platform and begin sliding the pin.
From the given diagram, it can be concluded that
of the previous temperature heat treatment pins
Was performed a total of 17 experimental tests.
have a very significant impact on the value of the
Each of the experimental test was repeated 30
coefficient of static friction. The consequence of
times, in order to reliably determine the mean
the increase in the coefficient of static friction is
value of the coefficient of friction. Obtained the
essentially related to structural changes in the
mean value of the coefficient of static friction for
surface layer and the oxide layer was formed as
certain values of the previous temperature heat
a result of the previous heat treatment.
treatment pins are given in Table 1.

Table 1. Calculated mean value of the coefficient of In the first measurement at room temperature
static friction s depending on test temperatures. coefficient of static friction is s=0.24. After the
second and third measurements, heating the
Pretreatment temperature of
specimen [oC]
s [-] sample to 50 C and 100 C and cooling, the
23 0.24
static coefficient of friction rises to s= 0.44. The
50 0.33
increase in the static coefficient of friction can be
100 0.44 largely attributed to the formation of an
150 0.39 oxidation layer on the surface of the sample.
200 0.31 With further heating the sample to 150 C and
250 0.60 200 C occurs decline in the static coefficient of
300 0.46 friction to values s=0.39 and s=0.31. For
350 0.39 further heating the samples to 800 C
400 0.52 temperature occur certain decline in and
450 0.45 increase the static coefficient of friction which
500 0.45 can be seen from the diagram in Fig. 4. Static
550 0.53 coefficient of friction is an intricate process
600 0.55 governed by a combination of factors, such as
650 0.54 the real area of contact, the contact geometry,
700 0.55 the surface roughness of the members in
750 0.61 contact, the load, and the temperature. When a
800 0.66 specimen over a cylindrical groove, a component

587
 M. ivkovi et al., Tribology in Industry Vol. 38, No. 4 (2016) 585-589
of the force of friction related to slip arises and,
therefore, surface films can manifest their
influence. The temperature elevation affects all
of the above listed factors, since it favours a
decrease in the hardness of the metals in
contact, changes in the con tact geometry due to
thermal expansion, as well as removing water
and contamination films. All of these effects can
increase the static coefficient of rolling friction;
therefore, they require serial tests with variable
parameters to be carried out. The tribometer
with the inclined plane can be efficient in these
tests because of the simplicity and clarity of
measurements.
4. CONCLUSION
The obtained results indicate a very significant
impact of the previous heat treatment pins on
the measured value of the coefficient of static
friction. Previous thermal preparation of the pin
as a contact element (pre-heating and cooling
pins) causes structural changes and the creation
of the oxide layer, which is characterized by
higher coefficients of friction. According to the
research results for a given temperature range,
there was a nearly threefold increase in the
value of the coefficient of static friction. This fact
points to the possibility increase friction
characteristics of metal materials based on heat
treatment, which opens a wide space for
research and optimization of friction gears in
terms of improving their characteristics in real
industrial systems.
Acknowledgement
This work has been performed as a part of
activities within the projects TR 35021 and OI
172005. These projects are supported by the
Republic of Serbia, Ministry of Education,
Science and Technological Development, whose
financial help is gratefully acknowledged.
REFERENCES
[1] B. Jeremic, D. Vukelic, P. Todorovic, I. Macizic, M.
Pantic, D. Dzunic and B. Tadic, Static Friction at
High Contact Temperatures and Low Contact
Pressure, Journal of Friction and Wear, vol. 34,
no. 2, pp. 114119, 2013.
588
[2] P. Todorovic, M. Blagojevic, Dj. Vukelic, I.
Macuzic, M. Jeremic, A. Simic and B. Jeremic,
Static rolling friction coefficient at high
temperature, Journal of Friction and Wear, vol.
34, no. 6, 2013.
[3] Elena Loredana Deladi, Static Friction in
Rubber-Metal Contacts with Application to
Rubber Pad Forming Processes, PhD thesis,
University of Twente, Twente, 2006.
[4] N.K. Myshkin, C.K. Kim and M.I. Petrokovets,
Introduction to tribology, CMG Publishers, Seoul,
1997.
[5] K.-H. Zum Gahr and K. Voelker, Friction and
wear of SiC fiberreinforced borosilicate glass
mated to steel, Wear, vol. 225, no. 2, pp. 885
895, 1999.
[6] P. Blau, The significance and use of the friction
coefficient, Tribol. Int., vol. 34, no. 9, pp. 585
591, 2001.
[7] B. Ivkovic, M. Djurdjanovic and D. Stamenkovic,
The Influence of the Contact Surface Roughness
on the Static Friction Coefficient, Tribology in
Industry, vol. 22, no. 3&4, pp. 4144, 2000.
[8] U. Muller and R. Hauert, Investigations of the
coefficient of static friction diamond-like carbon
films, Surface and Coatings Technology, Vol.
174175, pp. 421426, 2003.
[9] B. Polyakov, S. Vlassov, L.M. Dorogin, P. Kulis, I.
Kink and R. Lohmus, The effect of substrate
roughness on the static friction of CuO
nanowires, Surface Science, vol. 606, pp. 1393
1399, 2012.
[10] C. Vergne, C. Boher, R. Gras and C. Levaillant,
Influence of oxides on friction in hot rolling:
Experimental investigations and tribological
modeling, Wear, vol. 260, pp.957975, 2006.
[11] R. Rodriguez-Baracaldo, J.A. Benito, E.S. Puchi-
Cabrera and M.H. Staia, High temperature wear
resistance of (TiAl)N PVD coating on untreated
and gas nitrided AISI H13 steel with different
heat treatments, Wear, vol. 262, pp. 3809, 2007.
[12] J.L. Mo, M.H. Zhu, B. Lei, Y.X. Leng and N. Huang,
Comparison of tribological behaviours of AlCrN
and TiAlN coatings deposited by physical vapour
deposition, Wear, vol. 263, pp. 14239, 2007.
[13] Z.P. Huang, Y. Sun and T. Bell, Friction
behaviour of TiN, CrN and (TiAl)N coatings,
Wear, vol. 173, pp. 1320, 1994.
[14] M.H. Staia, M.D. Alessandria, D.T. Quinto, F.
Roudet and M. Marsal Astort, High temperature
tribological characterisation of commercial
TiAlN coatings, J Phys: Condens Matter, vol. 18,
pp. 172736, 2006.
 M. ivkovi et al., Tribology in Industry Vol. 38, No. 4 (2016) 585-589
[15] P.Eh Hovsepian, D.B. Lewis, Q. Luo, W-D. Mnz,
P.H. Mayrhofer and C. Mitterer, TiAlN based
nanoscale multilayer coatings designed to adapt
their tribological properties at elevated
temperatures, Thins Solid Films, vol. 485, pp.
160168, 2005.
[16] J. Hardell, E. Kassfeldt and B. Prakash, Friction
and wear behaviour of high strength boron steel
at elevated temperatures of up to 800 C, Wear,
vol. 264, pp.788799, 2008.
[17] K. Kutschej, P.H. Mayrhofer, M. Kathrein, P.
Polcik and C. Mitterer, Influence of oxide phase
formation on the tribological behaviour of Ti
AlVN coatings, Surf Coat Technol, vol. 200, pp.
17317, 2005.
[18] N. Fateh, G.A. Fontalvo, G. Gassner and C. Mitterer,
Influence of high-temperature oxide formation on
the tribological behaviour of TiN and VN coatings,
Wear, vol. 262, pp.11521158, 2007.
[19] E. Lugscheider, O. Knotek, K. Bobzin and S.
Barwulf, On the structure and oxidation
mechanisms in nanoscale hard coatings, Surf.
Coat. Technol., no. 133134, pp. 362368, 2000.
[20] P. Todorovi, M. Blagojevi, M. Jeremi, A.
Stankovi, A. Markovi, B. Trifunovi and M.
Miljkovi, The Impact of One Heat Treated
Contact Element on the Coefficient of Static
Friction, Tribology in Industry, vol. 35, no. 4
pp.345-350,2013.
589
 Vol. 38, N 4 (2016)

Tribology in Industry
Journal of the Serbian Tribology Society

www.tribology.fink.rs

AIMS, SCOPE AND AREAS: The aim of Tribology in Industry journal is to publish quality experimental and
theoretical research papers in fields of the science of friction, wear and lubrication and
any closely related fields.

The scope includes all aspects of materials science, surface science, applied physics and
mechanical engineering which relate directly to the subjects of wear and friction.

Topical areas include, but are not limited to: Friction, Wear, Lubricants, Surface
characterization, Surface engineering, Nanotribology, Contact mechanics, Coatings,
Alloys, Composites, Bearings, Tribological design, Biotribology, Green Tribology.

GUIDE FOR AUTHORS INFO: Manuscripts should describe the original work of the authors that has not been
previously published in a refereed journal and is not currently under consideration for
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public responsibilities of the legality and originality of the work.

The manuscript should be prepared according to the Guide for Authors, no longer than
15 pages.
a
For more information go to: http://www.tribology.fink.rs/guide.html
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SUBMISSION OF MANUSCRIPT: Manuscripts should be submitted by using the Journal's online submission system on
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Go to: http://www.tribology.fink.rs/openconf/openconf.php

SUBSCRIPTION: Single issue (Europe) - 40 ; Single issue (Other) - 50

Annual subscription - four issues (Europe) - 120 ; four issues (Other) - 150
Rapid publication - 100

INDEXING: SCOPUS
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KoBSON
COBISS
CIP -
,

621.7

TRIBOLOGY in Industry: journal of the Serbian Tribology Society /

editor-in-chief S. [Slobodan] Mitrovi. - 1979, br. 1 - . - Kragujevac:
Faculty of Engineering, University of Kragujevac, 1979-
(Kragujevac: Mainac). - 30 cm

Tromeseno. - Drugo izdanje na drugom medijumu:

Tribology in Industry (Online izd.) = ISSN 2217-7965
ISSN 0354-8996 = Tribology in Industry
COBISS.SR-ID 47528450