Physico-Mechanical and Tribological Properties of

Nanoclay Filled Friction Composite Materials Using

Taguchi Design of Experiment Approach

Tej Singh,1 Amar Patnaik,2 Ranchan Chauhan,3 Pankit Chauhan,4 Naresh Kumar1
1
Department of Mechanical Engineering, Manav Bharti University, Solan 173229, India

2
Department of Mechanical Engineering, M.N.I.T, Jaipur 302017, India

3
Department of Mechanical Engineering, Shoolini University, Solan 173229, India

4
Department of Mechanical Engineering, J.N.G.E.C. Sundernagar 175018, India

In this article, nanoclay filled organic–inorganic fiber INTRODUCTION

reinforced brake friction composites are designed, fab-
ricated by compression molding and then investigated
their physical, chemical, mechanical, and tribological
properties. It is observed that density of the composites
increased due to incorporation of inorganic contents
(nanoclay/lapinus), which are quite heavier than organic
contents (Kevlar/graphite) in the composites. Similarly,
as far as mechanical properties are concerned the
hardness, tensile strength, and flexural strength of the
composites increased with the decrease in the nano-
clay/lapinus fiber content but at the same time the
organic contents i.e., both Kevlar fiber and graphite
content are in the increased order of proportionality.
Finally, Taguchi design of experiment technique (L16
orthogonal array design) is implemented to evaluate the
optimal factor settings simultaneously wear loss of the
brake friction composites. In this experimental analysis,
four input control factors have been taken such as
composition, load, Speed, and distance at four levels
each to obtain the wear rate and coefficient of friction
of the fiber reinforced brake friction composites. The
overall mean for the signal-to-noise (S/N) ratio of the
coefficient of friction and wear rate of the brake friction
composites is found to be 29.20 db and 96.72 db,
respectively. At the end, a confirmation experiment is
conducted between the experimental result and
predicted theoretical result in order to validate the
experimental result. POLYM. COMPOS., 00:000–000, 2016.
C 2016 Society of Plastics Engineers
V
Correspondence to: T. Singh; e-mail: tejschauhan@gmail.com
DOI 10.1002/pc.24101
Published online in Wiley Online Library (wileyonlinelibrary.com).
C 2016 Society of Plastics Engineers
V materials. Liu et al. [15] concluded that nano rubber
Polymer based composite friction materials in automo-
tive braking application is one of the most complicated
composite material as it contains a polymer matrix as a
binder inside which a number of reinforcing fibers, fillers,
and property modifiers are distributed to achieve the
desired stringent level of braking objectives like stable
and high friction coefficient, low wear, and noise under
varying operating speeds and loads [1, 2]. A vast amount
of literature has been published on improving the tribio-
logical performance of friction materials by mean of
exploring fibers, fillers, binders and property modifiers
[3–7]. Generally, asbestos fibers, due to its economical
factor and containing desirable properties of brake friction
material have been used as a fibrous reinforcement. How-
ever, due to health concerns, most of the developed coun-
tries had banned the use of asbestos due to its
carcinogenic nature and had forced the friction industry
to seek alternative of asbestos [8]. Different kinds of
fibers, like natural, organic, inorganic, ceramic, metallic,
and their various combinations have been reported as a
replacement for asbestos in friction materials [9–13].
In the last two decades, noticeable developments in non-
asbestos fiber are used for manufacturing of based brake
friction materials. Therefore, the suitableness of fiber or
mixtures of fibers has been incorporated to match the per-
formance of hazardous asbestos fiber based friction materi-
als. In this regard, Murr and Soto [14] established a
comparison between carbon/clay based nanotubes and car-
cinogenic chrysotile asbestos nanotubes which revealed
that incorporation of carbon/clay nanotubes become an
obvious curiosity regarding their potential in brake friction

POLYMER COMPOSITES—2016

FIG. 1. Scanning electron micrograph of nanoclay (magnification
20,0003).
inclusion in friction formulation improves the friction level
and stability with temperature and wear resistance. Hwang
et al. [16] while studying the role of carbon nanotube on the
friction and wear performance of friction materials had con-
cluded that the incorporation of carbon nanotube exhibits
high and stable friction coefficient, high thermal strength,
and wear resistance. Similarly, Singh et al. [17–23] reported
inclusion of multi-walled carbon nanotubes and nanoclay
into friction material formulations and observed that
the friction materials efficiency improved in-terms of
better thermo-mechanical properties, wear resistance, and
improved coefficient of friction respectively [24–26]. In the
present study, the friction materials based on quaternary
combination of nanoclay, lapinus, Kevlar, and graphite are
prepared and studied the wear/frictional analysis on pin-
on-disc test rig. As the other types of test rigs like chase
[27], Krauss [28], pad-on-disc [6], dynamometer [29], etc.
are used by most of the researchers for tribological assess-
ment. However, these tests are lengthy and complicated
whereas, pin-on-disc test allow a reliable and quick deter-
mination of tribological properties [30].
EXPERIMENTAL DETAIL
Materials and Fabrication
The friction composite material used in the present study
consists of straight phenol-formaldehyde (PF) resin of
Novolac type (JA 10), Kevlar fiber (IF 258; Twaron, Teijin,
Germany), lapinus fiber (RB 220, Lapinus Intelligent fibers,
Holland), nanoclay (Cloisite 30B, Southern Clay) (Scan-
ning electron microscope image as shown in Fig. 1), barites,
and graphite amounting to 100% by weight are fabricated.
The details of the composite composition and the designa-
tion are shown in Table 1. The friction materials are devel-
oped as per the standard method reported in our previous
report [21]. The ingredients are mixed with a plough shear
2 POLYMER COMPOSITES—2016
TABLE 1. Detail of the composite designation and composition.
Composition (wt%)
Composite
designation PF resin BaSO4 Kevlar Lapinus Graphite Nanoclay
NC-1 15 50 2.5 27.5 2.25 2.75
NC-2 15 50 5.0 25.0 2.50 2.50
NC-3 15 50 7.5 22.5 2.75 2.25
NC-4 15 50 10.0 20.0 3.00 2.00
type mixer for 30 min to ensure mechanical isotropy of the
composites. Formulation is carried out at room temperature
and hot molding is performed at 1558C under 15 MPa pres-
sure. Post curing of the fabricated composites is carried out
at 1508C for 5 h in an oven. The specimen of size 25 mm 3
10 mm 3 10 mm are cut by diamond cutter from the fabri-
cated friction composites for this research work as shown in
Fig. 2.
Physical, Chemical, and Mechanical Characterization
The density of the fabricated friction composites are
determined using a standard water displacement method
and void contents are calculated by normalization of the
theoretical density with respect to the experimental density.
Acetone extraction (for the estimate of uncured resin pres-
ent in the friction composite) of the cured powdered mix
has been carried out on a Soxhlet apparatus. Water absorp-
tion is carried out according to ASTM D570-98 standard,
whereas, heat swelling is measured according to SAE J160
JNU 80 standard. The ash content is then determined by
roasting the powdered sample at higher temperature i.e.,
800 6 108C in a muffle furnace following as per industrial
norms. The mechanical properties such as hardness as a
measure of resistance to indentation under loads, tensile
strength, and tensile modulus defining response to axial
stress, flexural strength, and modulus defining response to
bending stress, compressive strength defining response to
compressive stress, shear/cross breaking strength for the
characterization of composite integrity throughout the bulk
and across the bulk-adhesive interface and compressibility
FIG. 2. (a) Fabricated brake friction material and (b) specimen’s
dimensions. [Color figure can be viewed in the online issue, which is
available at wileyonlinelibrary.com.]
DOI 10.1002/pc

FIG. 3. The schematic diagram of pin on disc set-up. [Color figure can be
viewed in the online issue, which is available at wileyonlinelibrary.com.]
characteristics were determined following standards con-
forming to industrial practice.
Tribo-Performance Evaluation
A pin-on-disc type test rig (supplied by DUCOM, India)
as per ASTM G 99 (Fig. 3) used for the tribological assess-
ment of friction materials under dry sliding condition at
room temperature [31]. The counter body is a disc made of
hardened ground steel (EN-32, hardness 72 HRC and surface
roughness 0.6 lRa). The specimen is held stationary within
the specimen holder which is normal to the disc surface.
Generally, the pressure varies between 0.3–2 MPa and the
sliding Speed varies between 1–10 m/sec in real brake sys-
tems [32]. Hence, tests are conducted with four different slid-
ing Speeds i.e., 1.67, 3.34, 5.01, and 6.68 m/sec under four
different normal loads i.e., 80 N, 120 N, 160 N, and 200 N,
respectively. The material loss from the friction composite
surface is measured using a precision electronic balance. The
specific wear rate (mm3/Nm) is calculated as [33]:
experiment design, it is required 44 5 256 runs to study these
four parameters each at four levels, whereas, Taguchi’s
approach reduces it to only 16 runs offering a great advantage
in terms of experimental time and cost. Further, the signal-to-
noise (S/N) ratio which is used to measure the performance
output and as S/N ratio is chosen based on three categories of
quality characteristics; lower-the-better, nominal-the-better,
and higher-the-better, respectively. The process parameter
with the highest S/N ratio yields the most favorable quality
with lowest variance. This work is mainly focused on brake
friction material low wear and high coefficient of friction for
automobile allocation. Therefore, higher-the-better character-
istic is chosen for coefficient of friction and lower-the-better
characteristic is selected for wear rate. The S/N ratio can be
calculated from the following equations [34, 35]:
Higher2the2better characteristic :
 
S 1 X1 (2)
52103log
N m a2
Lower2the2better characteristic :
S 1 X 2  (3)
52103log b
N m
where a represents the coefficient of friction response, b
represents the wear response, and m denotes the number
of experiments.
The contribution of each process parameter on the coefficient
of friction and wear performance of fabricated friction composite
materials is calculated by using following steps [36]:
I. First step: determination of S/N ratio.
II. Second step: calculation of overall mean ratio. In this step,
 
the overall mean NS ratio is calculated as [37]:
16  
S 1 X S
5 : (4)
N 16 i51 N i

Dm III. First step: calculation of sum of squares. In this step, the

Specific wear rate5 (1) sum of squares (U) due to variation about the overall mean
qtVS FN
is calculated as [38]:
where Dm is the mass loss (g), q is the density of the 16  
X 2
S S
composite (g/mm3), t is the test duration (sec), VS is the U5 2 : (5)
N i N
sliding Speed (m/sec), and FN is the normal load (N). i51
For the ith process parameter, the sum of squares due to
variation about the mean (Ui ) is:
Experimental Design
TABLE 2. Levels for various control factors used in the experiment.
In this study, Taguchi design of experimental technique is
used to determine the optimal process parameters for tribologi- Level
cal properties analysis. The tribological tests on the fabricated
friction composites are carried out under different operating Control factor I II III IV
conditions by considering four parameters varying at-a-time in
each experimental run, viz., composition, normal load, sliding A: Composition (wt%) NC-1 NC-2 NC-3 NC-4
B: Load (N) 80 120 160 200
speed, and sliding distance each at four levels as listed in
C: Speed (m/s) 1.67 3.34 5.01 6.68
Table 2. The impact of these four parameters are studied using D: Distance (m) 1,000 2,000 3,000 4,000
L16 (44) orthogonal array design. In conventional full factorial

DOI 10.1002/pc POLYMER COMPOSITES—2016 3

TABLE 3. Physical, chemical, and mechanical properties of the fric- RESULTS AND DISCUSSION
tion composites.

Properties NC-1 NC-2 NC-3 NC-4 Physical, Chemical, and Mechanical Properties
Density (g/cm3) 2.14 2.12 2.11 2.09 The details of physical, chemical, and mechanical proper-
Void content (%) 0.186 0.175 0.160 0.147 ties of the friction composites are shown in Table 3. It is
Acetone extraction (%) 0.73 0.76 0.74 0.71 observed that with the increase in the nanoclay/lapinus con-
Ash content (%) 72.52 69.09 68.25 67.84
Water absorption (%) 1.32 1.09 1.15 0.94
tent the density and void content of the composites increases.
ASTM D 570-98 The enhancement in density may attribute to addition of inor-
Heat swelling (%) 0.57 0.53 0.78 0.61 ganic (nanoclay/lapinus) content, which is heavier than
SAE J 160 JNU80 organic (Kevlar/graphite) content. The lower content of nano-
Shear strength (kgf) 1,150 1,380 1,430 1,380
clay/lapinus disperse readily in the matrix and hence fill the
Hardness (HRL) 94 91 97 99
ASTM D785 voids, whereas, with the increase in content of nanoclay/lapi-
Tensile strength (MPa) 8.80 11.52 12.71 15.36 nus, the chances of agglomeration increases which leads to
ASTM D3039-76 development of void as found in experimentally [21]. The
Tensile modulus (GPa) 1.12 1.15 1.21 1.35 acetone extraction may not show any regular trend with the
ASTM D3039-76
Failure strain (%) 0.78 1.01 1.05 1.14
composition. The friction composites shows almost similar
ASTM D 3039-76 values of acetone extraction lies in between 0.71–0.76%
Flexural strength (MPa) 29.47 33.92 37.50 46.54 which is in the range of prescribed industrial norms. The ash
ASTM D2344-84 contents of the composites are increased with increase in
Flexural modulus (GPa) 2.20 2.52 2.69 3.46
nanoclay and lapinus fiber contents having higher thermal sta-
ASTM D2344-84
Failure strain (%) 0.64 0.76 0.89 0.93 bility as compared to decrease in Kevlar fiber and graphite
ASTM D 2344-84 contents. Water absorption, heat swelling, and shear strength
Compressive strength (MPa) 40.49 43.14 50.40 56.38 does not show any regular trend with the composition. How-
Compressibility (%) 1.61 1.12 1.04 0.95 ever, the variations of mechanical properties, i.e., hardness,
tensile, and flexural strength are increased with the decrease
  !2 in the nanoclay and lapinus fiber content and with corre-
X4
S S sponding increase in Kevlar fiber and graphite content,
Ui 5 2 : (6)
j51
N ij N respectively. However, at higher nanoclay contents the frac-
tion of hard lapinus fibers is much higher, hence chances of
IV. Fourth step: contribution percentage. Finally, the percent agglomeration make the composite more prone to the genera-
contribution of individual process parameter can be calcu- tion of inherent structural discontinuities. Such aspects related
lated as [38]: to the poor structural integrity of the composites contribute to
a reduced hardness, tensile, and flexural strength. Further-
Ui
Contribution; %i 5 3100: (7) more the higher content of nanoclay and lapinus fiber lead to
U
improper distribution in the matrix and that increase void con-
tent of the composites. Increase in the void content of the

TABLE 4. Experimental designs with coefficient of friction, specific wear rate, and S/N ratio.

A: Composition B: Load C: Speed D: Distance Coefficient S/N ratio WS

Experiment run (wt%) (N) (m/s) (m) of friction (db) (mm3/Nm) S/N ratio (db)

1 NC-1 80 1.67 1,000 0.44 27.131 8.004 3 1026 101.933

2 NC-1 120 3.34 2,000 0.42 27.535 1.774 3 1025 95.020
3 NC-1 160 5.01 3,000 0.39 28.179 3.483 3 1025 89.161
4 NC-1 200 6.68 4,000 0.36 28.874 4.172 3 1025 87.593
5 NC-2 80 3.34 3,000 0.45 26.936 1.214 3 1025 98.314
6 NC-2 120 1.67 4,000 0.40 27.959 1.325 3 1025 97.557
7 NC-2 160 6.68 1,000 0.37 28.636 1.260 3 1025 97.990
8 NC-2 200 5.01 2,000 0.33 29.630 2.147 3 1025 93.365
9 NC-3 80 5.01 4,000 0.36 28.874 1.399 3 1025 97.083
10 NC-3 120 6.68 3,000 0.37 28.636 2.004 3 1025 93.963
11 NC-3 160 1.67 2,000 0.30 210.458 1.160 3 1025 98.708
12 NC-3 200 3.34 1,000 0.28 211.057 1.541 3 1025 96.246
13 NC-4 80 6.68 2,000 0.30 210.458 6.814 3 1026 103.332
14 NC-4 120 5.01 1,000 0.37 28.636 8.058 3 1026 101.875
15 NC-4 160 3.34 4,000 0.28 211.057 1.494 3 1025 96.512
16 NC-4 200 1.67 3,000 0.22 213.152 1.136 3 1025 98.891

4 POLYMER COMPOSITES—2016 DOI 10.1002/pc

 TABLE 5. Response table for signal to noise ratios of coefficient of
friction.

Level A: Composition B: Load C: Speed D: Distance

1 27.930 28.350 29.675 28.865

2 28.290 28.191 29.146 29.520
3 29.756 29.582 28.830 29.225
4 210.825 210.678 29.151 29.191
Delta 2.896 2.487 0.845 0.655
Rank 1 2 3 4

and 5, which are made using MINITAB [15]. From Table 4,

FIG. 4. Effect of control factors on coefficient of friction. [Color figure can
be viewed in the online issue, which is available at wileyonlinelibrary.com.]
composites increases the compressibility but decreases the
compressive strength.
Taguchi Analysis for Tribo-Performance
In general, the friction and wear performance of friction
composites considerably improves with nanoclay and lapi-
nus fiber loading [21]. In this regard, the intention of this
study is to seek out the vital factors and combination of fac-
tors influencing the process to attain higher coefficient of
friction and minimum wear rate. Taguchi design of experi-
ment methodology and the important factors affecting tribo-
logical properties of friction composite are identified.
The analysis is presented in Table 4 and depicted in Figs. 4
the overall mean for the S/N ratio for coefficient of friction
and wear rate are found to be 29.20 db and 96.72 db,
respectively. The S/N ratio response of coefficient of fric-
tion and wear rate are given in Tables 5 and 6, from which
composition is the most significant factor closely followed
by normal load, while sliding speed and sliding distance
have almost identical influence on the coefficient of friction
and wear rate of the friction composites. Analysis of these
results are concluded that the combination of factors A1,
B2, C3, and D1 yield higher coefficient of friction whereas,
combination of A4, B1, C1, and D1 gives minimum wear
rate as shown in Figs. 4 and 5. Friction performance
increases with the increase in nanoclay/lapinus content
whereas wear performance increases with the increase in
Kevlar and graphite content in the composites. The increase
in friction performance with respect to composition may be
attributed due to the enhancement of inorganic/abrasive
natured component (i.e., nanoclay and lapinus), whereas,
the increased wear performance may be due to the enhance-
ment of organic natured component (i.e., Kevlar and graph-
ite). With the increase in inorganic/abrasive components,
the generation of third bodies between the tribo-couple (i.e.,
brake pad and disc) increases resulting in enhanced friction
performance by third body abrasion mechanism. Further,
importance of each process parameters considered namely:
composition, normal load, sliding speed, and distance are
determined by using Eqs. 3–7 and given in Tables 7 and 8.
From Tables 7 and 8, it revealed that composition has
greatest influence on the coefficient of friction and wear
rate of friction composites with 53.68%, and 33.35%,
respectively, and closely followed by the load with 40.52%
and 30.24%.

TABLE 6. Response table for signal to noise ratios of specific wear

rate.

Level A: Composition B: Load C: Speed D: Distance

1 93.43 100.17 99.27 99.51

2 96.81 97.10 96.52 97.61
3 96.50 95.59 95.37 95.08
4 100.15 94.02 95.72 94.69
FIG. 5. Effect of control factors on specific wear rate. [Color figure can Delta 6.73 6.14 3.90 4.83
be viewed in the online issue, which is available at wileyonlinelibrary. Rank 1 2 4 3
com.]

DOI 10.1002/pc POLYMER COMPOSITES—2016 5

TABLE 7. Contribution of process parameters on coefficient of TABLE 9. Results of the confirmation experiments.
friction.
Optimum control parameters
Sum of squares
Overall due to variation Prediction Experimental Error
Process mean (NS ) about the Sum of
parameter ratio mean (Ui ) squares (U) %-contribution Coefficient of friction
Level A1B2C3D1 A1B2C3D1 %
Composition 29.2003 5.3932 10.0476 53.68 S/N ratio (db) 29.2151 29.1104 1.14
Load 4.0711 40.52 Wear rate
Speed 0.3679 03.66 Level A4B1C1D1 A4B1C1D1 %
Distance 0.2154 02.14 S/N ratio (db) 108.94 105.286 3.35

Confirmation Experiments CONCLUSIONS

In design of experiment, the confirmation experiment Nanoclay filled Kevlar-lapinus fibers reinforced brake
is the final step conducted to validate the interference friction composite materials have been fabricated and eval-
drawn during the analysis phase. It is performed by con- uated their physical, chemical, mechanical, and tribological
sidering the new set of factor A1B2C3D1 to predict coeffi- properties. The physical and mechanical properties of these
cient of friction and A4B1C1D1 to predict the wear rate. friction composites have been found to be highly dependent
The results of confirmation tests conducted with the opti- on the formulation. Higher nanoclay/lapinus content has led
mum design parameters are presented in Table 9. The to increase in density, void content, ash content, and com-
estimated S/N ratio for coefficient of friction and wear pressibility whereas higher graphite/Kevlar content led to
rate can be calculated with the help following predictive increase in hardness, flexural strength, tensile strength, and
equations:
compressive strength, respectively. The optimum parameter
for the formulation with highest coefficient of friction and
gf 5T 1ðA1 2T Þ1ðB2 2T Þ1ðC3 2T Þ1ðD1 2TÞ (8)
lowest wear rate is obtained by using Taguchi method. The
gw 5T 1ðA4 2T Þ1ðB1 2T Þ1ðC1 2T Þ1ðD1 2T Þ (9) combination of control factors A1B2C3D1 offers highest
coefficient of friction and A4B1C1D1 offer minimum wear
where gf is the predicted average for coefficient of fric- rate of the brake friction material. Finally, the degrees of
tion, gw is the predicted average for wear rate, T is the influence of the selected parameters on the friction and
overall experimental average, and A1B2C3D1 and wear performance of friction composites are determined.
A4B1C1D1 are the mean response for factors at designated
The results revealed that composition has major influence
levels for coefficient of friction and wear rate,
on coefficient of friction and wear rate of friction compo-
respectively.
sites followed by normal load.
The S/N ratio of coefficient of friction by the predic-
tive equation is found to be 29.2151 db and from the
experimental results the S/N ratio is found to be 29.1104
ACKNOWLEDGMENTS
db. The S/N ratio value of wear rate by the predictive
equation is found to be 108.94 db and from the experi- Authors gratefully acknowledge the support of Allied-
mental results value of S/N ratio is found to be 105.286 Nippon Industries Limited, Sahibabad, India, for extending
db, respectively. The resulting model seems to be capable their facilities to carry out a part of this research work.
of predicting coefficient of friction and wear rate to a rea-
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