Optimization of dry sliding wear behaviour of zirconium filled bismaleimide nanocomposites

1. Proceedings of the 2nd International Conference on Current Trends in Engineering and Management ICCTEM -2014
INTERNATIONAL JOURNAL OF MECHANICAL ENGINEERING
17 – 19, July 2014, Mysore, Karnataka, India
AND TECHNOLOGY (IJMET)
ISSN 0976 – 6340 (Print)
ISSN 0976 – 6359 (Online)
Volume 5, Issue 9, September (2014), pp. 62-70
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IJMET
© I A E M E
OPTIMIZATION OF DRY SLIDING WEAR BEHAVIOUR OF ZIRCONIUM
FILLED BISMALEIMIDE NANOCOMPOSITES
S.M. Darshan1, B. Suresha2, B.N. Ravi Kumar3
1, 3Department of Mechanical Engineering, Bangalore Institute of Technology, Bangalore, Karnataka, 560004, India
2Department of Mechanical Engineering, The National Institute of Engineering, Mysore, Karnataka, 570008, India
ABSTRACT
The mechanical properties and dry sliding wear behavior of bismaleimide BMI) nanocomposites with varying
weight percentage of zirconium dioxide (ZrO2) filler have been studied in the present work. The influence of independent
parameters such as sliding velocity (A), normal load (B), filler content (C), and sliding distance (D) on dry sliding wear
behaviour has been considered using Taguchi's L27 orthogonal array. The results showed that the coefficient of friction of
ZrO2 filled BMI nanocomposites decreased with the ZrO2 content increased. The specific wear rate of the BMI and ZrO2
filled BMI nanocomposites decreased as the sliding distance increased and a clear transition in friction and wear behavior
was observed in neat BMI and their nanocomposites. The high wear resistance of the nanocomposites is discussed in
terms of impact and dynamic mechanical strengths. Improvements in mechanical and tribological properties of these
nanocomposites make them promising candidates for bearing applications. It was found that the silane modification of
the ZrO2 particles improved the wear resistance, impact strength, and hardness BMI nanocomposites as well. Taguchi's
results indicate that the normal load played a significant factor affecting the wear rate followed by sliding velocity,
sliding distance and ZrO2 loading.
Keywords: ZrO2 Filled BMI Nanocomposites, Wear, Specific Wear Rate, Wear Mechanisms.
1. INTRODUCTION
Present day industries are experiencing an escalating trend in the applications of particulate and fiber reinforced
polymer matrix composites. Polymers and their composites are extensively used in tribological application because of
light weight, excellent strength to weight ratios, resistance to corrosion, non-toxicity, easy of fabrication, design
flexibility, self-lubricity, better coefficient of friction, and wear resistance. Some of these applications related to
mechanical engineering experience surface interactions with the surroundings as well as with the pairing element. Such
applications call for better understanding of the tribological behavior of the material under study. A few examples of
components used in tribological applications are gears, cams, wheels, brakes, bearing liners, rollers, seals, clutches,
bushings, transmission belts, pump handling industrial fluids and pipes carrying contaminated water [1].
An improvement in the tribological behavior of polymers is usually expected as a result of introducing fillers
into the matrix. Studies of introducing additional phases, e.g., inorganic fillers, have been successfully developed and
thus extended its applications in the past decades [2, 3]. Effects of fillers on the mechanical performances of composites
strongly depend on their properties, shape, size and aggregate degree, surface characteristics and loading. Studies have
shown that mechanical properties of polymer composites filled with smaller particles (fine particles) are superior to those
with larger ones at micron level. In recent years, great efforts devoted to the development of nanoparticle-filled polymer
composites have made it possible to investigate the effect on the mechanical properties [4].

2. Proceedings of the 2nd International Conference on Current Trends in Engineering and Management ICCTEM -2014
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In recent years, nanoparticles have been used as fillers in polymeric composites for improving the tribological
performance of the materials (nano-Al2O3/polyphenylene sulfide (PPS), nano-TiO2/epoxy, nano-SiO2/polyarylate, nano-
ZrO2/polyetheretherketone (PEEK), nano-Si3N4/ bismaleimide). When nanoparticles are incorporated into the matrix,
both microstructure and properties of the composites can be improved. Zhang et al. [5, 6] systematically studied the wear
resistance of epoxy filled with short carbon fiber, graphite, polytetrafuroethylene (PTFE) and nano-TiO2 under different
sliding conditions. The spherical nano-TiO2 was able to apparently reduce the friction coefficient during sliding and
consequently reduce the shear stress, contact temperature and wear rate of fiber reinforced epoxy composites [6]. In order
to improve the friction and wear behavior of polymeric materials, one typical concept is to reduce their adhesion to the
counterpart material and to enhance their mechanical properties. This can be achieved quite successfully by using
inorganic fillers. Ng et al. [7] verified that nanoparticles can remarkably reduce the wear rate, while micron sized
particles cannot. Rong et al. [8] conformed that the dispersion state of the nanoparticles and micro-structural
homogeneity of the fillers improved the wear resistance significantly. The way of nanoparticle incorporation must be
considered as a very important key point to receive the desired material properties. The addition of different fillers
favorably stiffens the material and may also increase the strength under certain load conditions.
Bismaleimide (BMI) Resins are relatively young class of thermosetting polymers that are gaining acceptance by
industry because they combine a number of unique features including excellent physical property retention at elevated
temperatures and in wet environments, almost constant electrical properties over a wide range of temperatures, and
nonflammability properties. Their excellent processibility and balance of thermal, mechanical, and electrical properties
have made them popular in advanced composites. The application of BMI composite materials is being expanded,
especially for military aircraft structures. BMI was synthesized from 4, 4’- bismaleimidodiphenylmethane and maleic
acid anhydride, with the synthesis being followed by cyclodehydration. BMI was synthesized according to the method
for synthesis of allyl ether novlak described in [9]. Many modified BMI resin systems have been developed. Among
them a two-component high performance resin system based on BDM and O,O’-diallyl bisphenol A (DBA), coded as
BDM/DBA has been proved to have outstanding toughness, good humidity resistance, excellent thermal and mechanical
properties [10]. Hence, the BDM/DBA resin was chosen as the base resin in the present work.
Zirconium dioxide, which is also referred to as zirconium oxide or zirconia, is an inorganic metal oxide that is
mainly used in ceramic materials. Zirconium dioxide succeeds zirconium as a compound of the element zirconium that
most frequently occurs in nature [11]. Its great hardness, low reactivity, and high melting point have made it the oldest
mineral that can be found on the earth.
Majority of research studied detailed experimental work with effect of one factor by keeping all other factors
fixed, this approach is not advisable because in actual environment there will be combined effects of interacting factors
influencing the abrasive wear. Hence in this study an attempt is being made to study the interacting effects of factors
along with the main effect. To achieve this, design of experiments based on Taguchi method is adopted. This method is
advocated by Taguchi and Konishi [12]. Taguchi’s technique uses special design of orthogonal arrays to study the entire
parameter space with only a small number of experiments. Taguchi’s technique also helps in optimizing the critical
parameters [13].
In this study, we have developed a new type of ZrO2 nanoparticles filled BMI composites. A high shear mixing
procedure was used to uniformly disperse the ZrO2 nanoparticles into the BMI resin system. Effect of incorporation of
ZrO2 nanoparticles on impact strength, dynamic mechanical strength and dry sliding wear behaviour have been
investigated. The influence of independent parameters such as sliding velocity (A), normal load (B), filler content (C),
and sliding distance (D) on dry sliding wear behaviour has been considered using Taguchi's L27 orthogonal array.
2. EXPERIMENTAL PROCEDURE
2.1 Materials
4, 4’ –Bismaleimidodiphenylmethane (BDM) and O,O’ –diallylbisphenol A(BA) were supplied by ABR
Organics Limited, Hyderabad (India), Zirconia(ZrO2) nanoparticles were purchased from sigma Aldrich,
Bangalore(India).
The zirconia represents the ceramic nanocrystalline phase with size range of 60-100 nm (Fig 1). Along with a
spherical shape, their large number is characterized by a very high specific surface area of 100m2/g. This powder
contains particle agglomerates with sizes in the micrometer range (Fig 1), which consists of ZrO2 primary nanoparticles
sticking strongly together. Primary nanoparticles attract each other due to adhesive inter particle ‘van der Waals’ forces,
which originate from the materials surface energy.

3. Proceedings of the 2nd International Conference on Current Trends in Engineering and Management ICCTEM -2014
17 – 19, July 2014, Mysore, Karnataka, India
64
Fig. 1: Microstructure of zirconium nanoparticles
2.2 Preparation of ZrO2 filled BMI nanocomposites
Appropriate content of zirconia nanoparticles were added into BA at room temperature (25C) with vigorous
mechanical agitating. The mixture was agitated for 2 h followed by ultrasonic stirring for another 2 h to obtain a
homogeneous suspension. The detailed procedure of fabrication of zirconia filled BMI nanocomposites were given in
Elsewhere [3].
2.3 Dynamic Mechanical Analysis
DMA is a technique, which is used to study the stress, temperature and frequency of the material when it is
subjected to a small deformation by sinusoidal load. DMA is used to measure the stiffness and damping in terms of
storagemodulus, loss modulus and tan . The approach is often used to determine glass transition temperature, as well.
The dimensions of the specimens were 3.2mm×12.5mm×63.5mm. The tests were conducted at a heating rate
5.0°C/minute from 0oC to 280oC at a frequency of 1.0Hz for the neat BMI and nano ZrO2 filled BMI.
2.4 Dry sliding wear measurements
Unlubricated pin-on-disc sliding wear tests were carried out in order to determine the tribological properties of
the nanocomposites. The disc material is made up of En-32 steel (diameter 160mm and 8 mm thickness) having hardness
value of HRc 65. The surface roughness of the disc varies from 0.02 to 0.06 μm. A constant 114 mm track diameter was
used throughout the experimental work. Sliding was performed in air with the ambient temperature of around 25C, over
different sliding distance at a sliding velocity of 0.5 m/s and a normal load of 40 N. Prior to wear testing, all specimens
were cleaned, that is, the sample was abraded with water-abrasive paper (600 grit) and a super-fine water-abrasive paper
successively. Then both the steel ring and the specimen were cleaned with acetone and distilled water. The wear process
takes some material away from the sample. This mass loss can accurately be measured by determining the weight of the
specimen before and after the experiment. A characteristic value, which describes the wear performance under the chosen
conditions for a tribo-system is the specific wear rate (Ks):
D
m
× ×
=
mm
N m
F L
K
N
s
3
r
(1)
Where m is the mass loss, is the measured density of the composite, FN is the normal load applied and L is the sliding
distance. In order to take repeatability into account, results from the friction and wear tests were obtained from three
readings and the average value was adapted in our results.
2.5 Experimental design
Design of experiments is the powerful analysis tool and analyzing the influence of the control factors on the
performance output. The most important stage is the design of experiments lies in the selection of the control factors.
Four parameters, namely, sliding velocity(A), normal load(B), filler content(C), and sliding distance(D) each at three
levels, are considered in this study in accordance with L27(313) orthogonal array design. Control parameters and their
levels are indicated in table. Four parameters each at three levels would require 34= 81runs in a full-factorial experiment,

4. Proceedings of the 2nd International Conference on Current Trends in Engineering and Management ICCTEM -2014
17 – 19, July 2014, Mysore, Karnataka, India
whereas Taguchi’s factorial experiment approach reduces it to only 27 runs offering a great advantage. The plan of the
experiment is as follows: the first column of the Taguchi orthogonal array is assigned to the sliding velocity (A), the
second column to the normal load (B), the fifth column to the fiber content (C), the ninth column to sliding distance (D),
and remaining columns are assigned to their interactions and experimental errors.
65
Table 1: control factors and levels used in the experiment
LEVELS
Control factor I II III Units
A: Sliding velocity 0.5 1 1.5 m/s
B: Normal load 20 40 60 N
C: Filler content 0 5 10 %
D: Sliding distance 1000 2000 3000 M
The experimental observations are transformed into signal-to-noise (S/N) ratio. There are several S/N ratios
available depending on the type of characteristic, which can be calculated as logarithmic transformation of the loss
function. For lower is the better performance characteristic S/N ratio is calculated as per
: S/N = -10 log [1/n (y2)] (2)
Where “n” is the number of observations and “y” is the observed data. “Lower is the better” (LB) characteristic,
with the above S/N ratio transformation, is suitable for minimization of wear rate. A statistical analysis of variance
(ANOVA) is performed to identify the control parameters that are statistically significant. With the S/N ratio and
ANOVA analyses, the optimal combination of wear parameters is predicted to acceptable level of accuracy. Finally
conformation of experiments is conducted to verify the optimal process parameters obtained from the parameters design.
3. RESULTS AND DISCUSSION
3.1 Effects of concentrations of ZrO2 on the impact strength
The impact tests were performed using a Charpy impact tester according to the ASTM-D256. The impact
strength of the neat BMI is 1.4 kJ/m2 and the impact strength of nanocomposites increases to 2.2kJ/m2 for 5 wt% ZrO2
filled BMI composite. It is obvious that all the nanocomposites have improved impact strength.
All ZrO2 filled BMI nanocomposites show better performance, because they have more contact area with BMI
resin at the same particle loading and also because more interaction forces can occur, such as hydrogen bonding and Van
der Waals interaction. According to the craze mechanism, the addition of nanoparticles can lead to formation of more
crazes, and more impact energy can be absorbed compared with micron particles [14].
Of all the ZrO2 filled BMI composites, the 10 wt% ZrO2 filled BMI composite showed the highest impact
strength (2.8 kJ/m2). This is about two times that of neat BMI. This can be explained by the fact that ZrO2 nanopartilces
have the special two-dimensional nanostructure and fewer agglomerates compared with other nanostructures. It is well
known that nanopartilces have a high surface area, which results in excellent interfacial combinations of BMI resin with
silanated ZrO2 nanoparticles. In addition, the ZrO2 nanoparticles embedded in the BMI matrix work like load bearing
material in reinforced polymer, forming crack pinning and immobilizing the polymer, thus leading impact energy to be
conceded quickly.
3.2 Effects of concentrations of ZrO2 on the dynamic mechanical strength
The storage modulus versus temperature curve provides valuable information about the stiffness of a material as
a function of temperature, and it is sensitive to structural changes. DMA results for the nanocomposite systems show a
consistent trend of decreased storage modulus over the pure BMI (Fig.2). It seems reasonable to assume that a better
impregnation of the 5% wt ZrO2 nano-filler in to BMI will amplify the effect of stress transfer under loaded condition
due to increased filler-matrix bonding and degree of crosslinking action. On the other hand, large microsized clusters
formed during the mechanical agitation leads to marginal changes in storage and loss moduli from 5% to 10% of filler
loading.
Loss modulus is the capacity of a material to dissipate energy when placed when stressed. The addition of ZrO2
to the BMI matrix should increase the loss modulus. This is due to the fact that polymer segments bond to the surface, the
loops and chains that extend toward the bulk matrix are expected to support a mechanical interlocking with the bulk
chains.
Glass transition temperature reported here is the temperature corresponding to the peak of tan curves.
Referring to Fig 2, increase the glass transition temperatures from 860C to 1020C was observed with increase in filler
content from 5% to 10% of filler loading. This increase in, Tg, is probably due to the molecular weight effect, more

5. Proceedings of the 2nd International Conference on Current Trends in Engineering and Management ICCTEM -2014
17 – 19, July 2014, Mysore, Karnataka, India
contact area of nano ZrO2 with BMI resin at the same particle loading and also because more interaction forces can
occur, such as hydrogen bonding and Van der Waals interaction.
66
Fig. 2(a): DMA test result for neat BMI
Fig. 2(b): DMA test result for 5% ZrO2 filled BMI
Fig. 2(c): DMA test result for 10% ZrO2 filled BMI

6. Proceedings of the 2nd International Conference on Current Trends in Engineering and Management ICCTEM -2014
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3.3 Effects of concentrations of ZrO2 on the specific wear rate
67
Plots of specific wear rate (ks) as a function of sliding distance for neat BMI and ZrO2 filled BMI
nanocomposites are shown in Fig. 3. The sliding between neat BMI and a flat steel countersurface, under a load of 40 N
and at 1 m/s, resulted in a specific wear rate of 3.815×10-5 mm3/Nm for 1000 m sliding distance. The order of wear
resistance behavior of BMI nanocomposites is as follows; 5 10 0% by weight of ZrO2 filler loading. BMI containing
5 wt% of ZrO2 had the smallest ks, while ks of neat BMI increased to some extent at an excessive content of ZrO2
particles (5 wt%), possibly owing to the poor adhesion of the nanoparticles by the BMI matrix and the conglomeration
of the nanoparticles at a too high filler content. With the addition of 5 wt% ZrO2 in BMI, the ks decreased. This behaviour
is in agreement with that of hardness results.
It is already known that majority microfillers are more effective in reducing the wear of different polymers. In
the case of neat BMI, wear debris consists of shear deformed polymer matrix containing broken pulverized matrix
particles and wear powder of the metallic countersurface. The particles can either be lost from the contact zone or
remains there for a fixed time as a transfer layer. In such cases, their polymer component can cushion the countersurface
asperities and reduce the effective toughness, but the pulverized matrix particles and wear powder of the metallic
countersurface can act as a third body abrasive leading to enhanced roughening of the countersurface. During wear
process, no transfer film was formed on the countersurface leading to higher ks for neat BMI. The wear loss is low for
ZrO2 filled BMI nanocomposites compared to neat BMI. At the start of sliding, the two surfaces of all the asperities were
in contact with each other. As shear forces were applied, the asperities deformed, and the ZrO2 particles protrude out
from the surface of the sample. Initially, BMI matrix wears out and only ZrO2 nanoparticles remain in contact with the
countersurface. As sliding distance increases the wear rate decreases, the ZrO2 nanoparticles wear out the steel
countersurface. Due to extreme hardness of the countersurface, ZrO2 nanoparticles adhere to the matrix and excess filler
concentration was noticed on the composite surface after prolonged sliding. During sliding, a rolling effect of
nanoparticles could reduce the shear stress and the contact temperature.
Fig. 3: Effect of sliding distance on specific wear rate
Hence, it was proposed that during the sliding process many of the hard particles were embedded in the soft
polymeric transfer films on the countersurface and grooved the sample surface. In this way, the distance between the
countersurface and the sample was also enhanced i.e., the particle acted as spacers. This in turn, can cause a reduction in
the adhesion between the contacting surfaces. Moreover, as the nanoparticles were free to move, they tend to be
dispersed uniformly over the transfer films during the wear process, which would result in a more uniform contact stress
between the contact surfaces and in turn minimizes the stress concentration. This ensured that the specific wear rate of
ZrO2 filled BMI was lower under higher sliding distance.
3.4 Statistical Analysis of wear rate by the Taguchi Technique
The analysis was made using the software MINITAB 17 specifically used for the design of experiment
applications. The parametric influence on dry sliding wear behaviour of the composite test specimen has been determined
by adopting the Taguchi technique. Experiments have been conducted as per standard L27 orthogonal array, using 3 levels
for each of 4 operational parameters, that is sliding velocity, normal load, filler content and sliding distance. The details
of orthogonal array along with the output parameter, that is, wear rate, is as shown in Table 2.

7. Proceedings of the 2nd International Conference on Current Trends in Engineering and Management ICCTEM -2014
17 – 19, July 2014, Mysore, Karnataka, India
68
Fig. 4 shows graphically the effect of the control factors on specific wear rate. Process parameter settings with
the highest S/N ratio always give in the optimum quality with minimum variance. The graphs show the change of the S/N
ratio when the setting of the control factor was changed from one level to the other. The best wear rate was at the higher
S/N values in the response graphs. From the plots it is clear that factor combination of A3, B2, C2, D3 and gives minimum
specific wear rate. Thus minimum specific wear rate for the developed composites is obtained when filler content and
normal load are at medium level, and the sliding velocity and sliding distance are at the highest level.
Analysis of the results leads to the conclusion that as far as minimization of wear rate is concerned, factors
sliding velocity, normal load, filler content and sliding distance have significant effect. From the interaction effects of
control parameters it is well known that interactions do not occur when the lines on the interaction plots are parallel and
strong interactions occur between parameters when the lines cross. Examination of interaction results yields a small
interaction between control parameters. In order to justify the insignificant factor and insignificant interaction a further
statistical analysis (ANOVA) was carried out.
3.5 ANOVA and the Effects of Factors
ANOVA is a statistical design method used to break up the individual effects from all control factors. The
percentage contribution of each control factor is employed to measure the corresponding effect on the quality
characteristic. The significance of operational parameters, that is, sliding velocity, normal load, filler content and sliding
distance, analysis of variance (ANOVA) is performed on experimental data. The ANOVA allows analyzing the influence
of each variable on the total variance of the results. Table 4, shows the results of ANOVA for the wear of the test
samples. From Table 3 it is evident that normal load plays a significant role followed by, sliding velocity, sliding distance
and filler content.
Table 2: Standard orthogonal L27 array with output results
Sl no Sliding
Velocity
(m/s)
Load
(N)
Filler
content
(%)
Sliding
Distance
(m)
Specific
wear rate
(mm3/Nm)
1 0.5 20 0 1000 3.21259
2 0.5 20 5 2000 4.30731
3 0.5 20 10 3000 3.50298
4 0.5 40 0 2000 3.11220
5 0.5 40 5 3000 2.28418
6 0.5 40 10 1000 3.19021
7 0.5 60 0 3000 3.74803
8 0.5 60 5 1000 6.65675
9 0.5 60 10 2000 4.69149
10 1.0 20 0 2000 2.81102
11 1.0 20 5 3000 2.21892
12 1.0 20 10 1000 4.12851
13 1.0 40 0 3000 2.34252
14 1.0 40 5 1000 1.95787
15 1.0 40 10 2000 2.43957
16 1.0 60 0 1000 4.81889
17 1.0 60 5 2000 3.13259
18 1.0 60 10 3000 3.87830
19 1.5 20 0 3000 3.74803
20 1.5 20 5 1000 3.52416
21 1.5 20 10 2000 2.81489
22 1.5 40 0 1000 1.80708
23 1.5 40 5 2000 1.66419
24 1.5 40 10 3000 1.81404
25 1.5 60 0 2000 3.88188
26 1.5 60 5 3000 3.91513
27 1.5 60 10 1000 3.87830

8. Proceedings of the 2nd International Conference on Current Trends in Engineering and Management ICCTEM -2014
17 – 19, July 2014, Mysore, Karnataka, India
M a in Ef fe ct s Plo t fo r SN ra t io s
D at a M ean s
Source DF Adj SS Contribution
SLIDING VELOCITY 2 3.9924 12.31
NORMAL LOAD 2 18.0114 55.56
FILLER CONTENT 2 0.0453 0.14
SLIDIND DISTANCE 2 1.9766 6.10
Error 18 8.3890 25.89
Total 26 32.4147
69
0 .5 1.0 1.5
- 7
- 8
- 9
- 10
- 11
- 12
- 13
2 0 4 0 6 0 0 5 10 10 0 0 2 0 0 0 3 0 0 0
SLID IN G V ELO CITY
Mean of SN ratios
N O RM AL LO AD FILLER CO N TEN T SLID IN D D ISTAN CE
Sig n a l-t o -n o ise: Sm a l ler is b et t er
Fig. 4: Effect of control factors on wear rate(S/N ratio).
Table 3: Analysis of variance for wear rate
4. CONCLUSIONS
%
This experimental investigation into the mechanical and tribological behavior of nano ZrO2 filled BMI
nanocomposites leads to the following conclusions.
The addition of the ZrO2 filler material has resulted in increased impact strength of the nanocomposite structure.
From the DMA results, storage moduli and loss moduli of BMI increased with the incorporation of nano ZrO2.
The dry sliding wear performance of neat BMI and ZrO2 filled BMI nanocomposites are in the following order:
BMI 1OZrO2-BMI 5ZrO2-BMI. This can be explained from an examination of the variation of specific wear
rate.
At higher sliding distance, the abrasive wear mechanisms could govern the interaction between the surfaces in
contact. In this condition the wear resistance of neat BMI could be increased by filling the matrix with ZrO2
nanoparticles. In particular, from the tests conducted, the dry sliding wear behaviour of 5 wt.% ZrO2 filled BMI
nanocomposites are better compared to neat BMI and with higher ZrO2 filler filled BMI nanocomposites.
Design of experiment approach by Taguchi method enable us to analyze successfully the wear behavior of the
composite with the sliding velocity, normal load, filler content, and sliding distance as test variables. From the S/N
ratio analysis, the optimal combination of wear parameters is obtained as A3B2C2D3 to minimize wear rate.
ANOVA results indicated indicate that normal load plays a significant role followed by, sliding velocity, sliding
distance, and filler content.
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