Materials and Design 41 (2012) 131141

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Materials and Design

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Study on mechanical and tribo-performance of rice-husk lled glassepoxy

hybrid composites
Arun Kumar Rout a,, Alok Satapathy b
a
School of Mechanical Engineering, KIIT University, Bhubaneswar 751 024, India
b
Department of Mechanical Engineering, National Institute of Technology, Rourkela 769 008, India

a r t i c l e i n f o a b s t r a c t

Article history: This paper describes the development of multiphase hybrid composites consisting of epoxy reinforced
Received 15 March 2012 with glass-ber and lled with rice husk particulates. It further investigates the mechanical properties
Accepted 1 May 2012 and erosion wear response of these composites and presents a comparison between the unlled and lled
Available online 11 May 2012
samples. The erosion wear experiments are conducted as per design of experiment approach using Tagu-
chis orthogonal arrays. The Taguchi approach enables us to determine optimal parameter settings that
Keywords: lead to minimization of the erosion rate. The results indicate that impact velocity, ller content, impinge-
Polymer matrix composite
ment angle and erodent size inuence the wear rate signicantly. The experimental results are in good
Mechanical properties
Erosion wear
agreement with values from the mathematical and articial neural network (ANN) model. The objective
Design of experiment of the present work is to fabricate a new class of epoxy based low cost hybrid composites reinforced with
Articial neural network glass ber and lled with rice husk powder in different weight proportions and to study the mechanical
and erosion wear performance of these composites. This study reveals that hardness, tensile modulus,
impact energy and erosion resistance of these new class hybrid composites are improving with ller
addition while a steady decline in tensile and exural properties are observed.
2012 Elsevier Ltd. All rights reserved.

1. Introduction
In recent years, polymers and their composites are slowly
replacing the conventional materials in many engineering applica-
tions. They have been used in various engineering elds starting
from space craft applications to industrial usages due to high spe-
cic strength, high modulus, low density and better wear resis-
tance [1]. Being light weight they are the most suitable materials
for weight sensitive applications, but their high cost sometimes re-
stricts for general applications. Use of low cost, easily available ll-
ers is therefore useful to improve the properties and to lower the
overall cost of components [2,3]. Hard particulate llers consisting
of ceramic or metal particles with glass ber are being used these
days to improve wear resistance of the polymer even up to three
orders of magnitude [4]. The inclusion of such particulate llers
into polymers for commercial applications is primarily focused at
the cost reduction and stiffness improvement [5]. Various
researchers [69] have reported that the wear resistance of poly-
mers is improved by the addition of llers. Some of the llers
which are effective in reducing friction and wear are MoS2, CuO,
CuS, Al2O3, graphite, etc. Mutlu et al. [10] have investigated the
friction and wear performance of phenolic composites lled with
Corresponding author. Tel.: +91 674 2375858.
E-mail addresses: aroutfme@kiit.ac.in (A.K. Rout), satapathy.alok@gmail.com (A.
Satapathy).
various llers like Cu powder, barite, Al2O3, cashew dust and
graphite for low cost automotive brakes. In another study, Mutlu
et al. [11,12] have investigated the tribological properties of phe-
nolic composite brake lining lled with various llers along with
boric acid. They found improved wear resistance in boric acid
added samples. Mohan et al. [7] have incorporated tungsten car-
bide and tantalum niobium carbide hard powders as llers in
glassepoxy to study the abrasive wear behavior. Most of the
above studies are carried out on the dry sliding and abrasive wear
performance of different polymer matrix composites lled with
various types llers.
A review of literature shows that llers like red mud [13], alu-
mina [14], SiC [15], y ash [16] have been incorporated into the
polymer matrix to study the erosion wear performance. It has been
observed that the rate of material loss due to erosion reduce signif-
icantly with the addition of such hard particulate llers.
Solid particle erosion wear, a typical wear mode, is the loss of
material that results from repeated impact of small solid particles.
Examples of such applications are helicopter rotor blades, pump
impeller blades, aircraft engine blades, pipelines carrying sand slur-
ries and structural components operating in desert environments
[17]. It causes surface degradation, surface roughening, scooping
appearance and reduction in functional life of the component.
Hence, it is essential to study the erosion resistance of materials like
polymer composites before any specic application. The research
efforts in this eld are mainly focused on studying the inuence of

0261-3069/$ - see front matter 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.matdes.2012.05.002
132 A.K. Rout, A. Satapathy / Materials and Design 41 (2012) 131141

experimental conditions like erodent velocity, impingement angle, neural network (ANN) has been proposed for better analysis and
erodent characteristics and target related parameters like ber prediction of wear performance of these composites.
orientation and ber content [18]. The effect of ber content, ber
orientation, ller content and experimental conditions like impinge-
ment angle, erodent velocity, erodent size, erodent temperature, 2. Experimental details
standoff distance and erosion efciency, etc. on erosion wear perfor-
mance of polymer composites have been reviewed earlier by Barko- 2.1. Materials
ula and Karger-Kocsis [19] and Patnaik et al. [20]. Tewari et al. [17]
have studied the solid particle erosion characteristics of polyaryle- In the present work, epoxy resin (LY 556) is used as the matrix
therketone composites reinforced with unidirectional carbon ber. material and its common name is bisphenol-A-diglycidyl-ether
The effect of y ash content, impingement angle and erodent veloc- and it chemically belongs to epoxide family. The epoxy resin
ity on solid particle erosion of glassepoxy composites have been and the corresponding hardener (HY 951) are supplied by Ciba Gei-
studied by Srivastava and Pawar [16]. Biswas and Satapathy [21] gy India Ltd. Epoxy is chosen primarily because of its excellent
have incorporated red mud as ller in glassepoxy and bamboo- dimensional, thermal stability and good corrosion resistance [6].
epoxy composites. They found that for similar test conditions bam- Rice husk is used as the ller material because it is a bio-waste
boo based composites exhibits much better erosion resistance than and has low density of 0.12 gm/cc [27]. The husk is collected from
glassepoxy composites. Bagci and Imrek [22] have investigated the Shiva Shakti Rice Mill, Dhenkanal, Odisha, India. The collected husk
solid particle erosion of glassepoxy composites lled with boric is dried in a woven with a temperature of 105 C for removal of
acid. They found minimum erosion wear in the unlled samples moisture and then sieved to an average particle size in the range
and the rate of erosion increases linearly with the impact velocity. of 8090 lm.
Bio based llers like pine wood dust (PWD) [2] and sh scale [23]
have been used as ller in epoxy matrix to study the sliding and ero-
2.2. Details of laminate fabrication
sion wear performance. It is found that pine wood dust (PWD) pos-
sess good ller characteristics as it improves the wear resistance of
Bi-directional E-glass ber mats are reinforced in epoxy resin
the polymer resin.
and four different weight proportions of rice husk (0 wt.%, 5 wt.%,
Though a good amount of work is reported on erosion wear
10 wt.% and 15 wt.%) are added as the ller material to prepare
study of polymer composites, however, there is no such report
the composites C1, C2, C3, and C4 respectively. Glass bers and
available in the literature on solid particle erosion wear study of
epoxy resin have modulus of about 72.5 GPa and 3.42 GPa respec-
composites containing bio llers like rice husk. Rice husk is an
tively and possess density of 2590 kg/m3 and 1100 kg/m3 respec-
inexpensive byproduct of human food processing and is considered
tively. The room temperature curing epoxy resin is mixed with
as an agricultural waste, largely available from rice milling indus-
the corresponding hardener (HY 951) in a weight ratio of 10:1 as
tries. Because of large production of rice, approximately 600 mil-
per the recommendation. The mixture of resin, hardener and rice
lion tons/year, there is a large amount of rice husk waste which
husk is stirred manually to disperse the particulate llers in the
is about 20 wt.% of the total rice production [24]. The major com-
matrix. The mixing is done thoroughly before fabrication of the
ponents of rice husk are 32% cellulose, 21% hemicelluloses, 22% lig-
composite samples. The weight percentage of glass ber in all
nin and 15% mineral ash. The mineral ash is composed of 96.34%
the composites is kept xed at 40 wt.%. The dimension each glass
SiO2, 2.11% K2O, 0.45% MgO, 0.2% Fe2O3, 0.41% CaO and 0.08%
ber mat is kept 200 mm  200 mm. The composite laminates
MnO2 [25]. It has been utilized in many useful applications such
are made by conventional hand-lay-up technique followed by light
as light weight concrete [26], an insulating material, llers in plas-
compression molding technique. A stainless steel mold having
tics, building materials, panel boards and activated carbon [27],
dimension of 210  210  40 mm3 is used for the fabrication pur-
electricity generation [28], husk-fueled steam engines [29] etc.
pose. A mold releasing agent (silicon spray) is used for easy re-
Rice husk has been used as a reinforcing material for recovery of
moval of the composite laminate from the mold after curing.
used rubber tire in powder form using sintering method [30]. Cre-
Proper care has been taken to ensure a uniform distribution of rice
spo et al. [31] have studied the mechanical properties of plasticized
husk particulates within the sample as these particles have a ten-
PVC composites by incorporating rice husk as llers. Yang et al.
dency to clump and tangle together when mixed. The casting of
[32] prepared a composite sample with polypropylene as the ma-
each composite laminate is cured under a load of about 35 kg for
trix and rice husk our as the reinforcing ller and studied the
24 h. Then the composite casting has been removed from the mold
physical, mechanical and morphological properties. Premalal
and again it is post-cured in air for another 24 h. Ten layers of fab-
et al. [33] also used rice husk as organic ller in polypropylene
rics are used to obtain about 4.5 mm thick laminates. Specimens of
and observed that these composites exhibit relatively lower yield
suitable dimensions are prepared from the laminate using a dia-
strength, Youngs modulus, exural modulus and higher elongation
mond tipped cutter for mechanical characterization and erosion
at break as compared to those of talc lled composites. Though
wear testing. The prepared samples for tensile test and wear test
many low-end as well as high end application areas such as elec-
are shown in Figs. 1 and 2 respectively. The designation and de-
tricity generation, particle boards, light weight concrete, building
tailed composition of the composites samples under investigation
materials, rice husk fueled steam engines, as ller material in var-
are listed in Table 1.
ious polymers, etc. are cited in the literature for rice husk based
products, but there is hardly any mention of its potential use in tri-
bological situations where synthetic bers/llers are widely used 2.3. Mechanical test details
in spite of its low cost, low density, low thermal conductivity, bio
degradability and several other advantages. 2.3.1. Density
Therefore, the objective of the present work is to fabricate a The theoretical density of a composite material can be obtained
new class of epoxy based low cost hybrid composites reinforced by using the following equation given by [34].
with glass ber and lled with rice husk powder in different Each composite sample under this investigation consists of
weight proportions and to study the mechanical and erosion wear three components namely ber, matrix and particulate ller and
performance of these composites. Erosion wear experiments have six numbers of specimens with same composition are used to get
been conducted as per Taguchi design of experiment and articial the mean value of density. The theoretical density of the composite
 A.K. Rout, A. Satapathy / Materials and Design 41 (2012) 131141 133

2.3.2. Micro-hardness
Leitz micro-hardness tester is used for measurement of micro-
hardness. A diamond indenter, in the form of a right pyramid with
a square base and an angle 136 between opposite faces, is forced
into the composite specimen under a load F = 24.54 N for a loading
time of 20 s. Minimum six numbers of indentations has been made
on each sample to obtain an average value of hardness. Vickers
hardness number is calculated by using the following equation.
F
HV 0:1889 3
L2

XY
And L 4
2
where L is the diagonal of the square impression in mm, X is the
horizontal length in mm and Y is the vertical length in mm.

2.3.3. Tensile strength

Fig. 1. Specimens prepared for mechanical characterization.
The tensile strength is generally performed on the at speci-
mens. The dog-bone type specimen with end tabs is commonly
used for tensile test. ASTM-D3039-76 [35] standard test method
is employed for tensile test of composite specimens. The dimen-
sion of the samples for the test is 150 mm  10 mm  4.5 mm.
The test is performed in the universal testing machine Instron
1195 at across head speed of 10 mm per minute. Six numbers of
specimens with same composition are used to get the mean value
of the tensile strength.

2.3.4. Flexural and inter laminar shear strength

The short beam shear (SBS) test is performed on the composite
samples for calculating inter-laminar shear strength (ILSS). The test
is conducted as per the ASTM-D2344-84 [36] standard for the pre-
pared samples. The dimension of the samples for the test is
60 mm  10 mm  4.5 mm. Universal testing machine Instron
1195 is used for the test. The cross head speed for the test is main-
tained at 10 mm/min and the test is repeated six times for each
sample to obtain the mean value of inter laminar shear strength.
The ILSS is calculated as per following equation:
Fig. 2. Specimens prepared for erosion test. 3P
ILSS 5
4bt
Here, P is the maximum load applied, b is the width of specimen
Table 1
Designation and detailed composition of the composites. and t is the thickness of the specimen. The same maximum value of
load P is used to calculate the exural strength (FS) also. A span of
Designation Composition
40 mm is used for obtaining both ILSS and FS. By using the follow-
C1 Epoxy + 40 wt.% glass ber ing equation FS is calculated.
C2 Epoxy + 40 wt.% glass ber + 5 wt.% rice husk
C3 Epoxy + 40 wt.% glass ber + 10 wt.% rice husk 3PL
C4 Epoxy + 40 wt.% glass ber + 15 wt.% rice husk FS 2
6
2bt
Eqs. (5) and (6) are generally used to obtain the ILSS and FS respec-
tively for composite materials.
specimen in terms of weight fraction can be obtained as per the
following equation 2.3.5. Impact strength
Low velocity instrumented impact tests are done as per ASTM
1 D256 [37] using an impact tester. The pendulum impact testing
qct 1
W f =qf W m =qm W p =qp machine measures the notch impact strength of the material by
shattering the V-notched specimen with a pendulum hammer.
where q and W represent the density and weight fraction
The standard specimen for ASTM D256 is 64  12.7  4.5 mm3
respectively. The sufx m, f and ct stand for the matrix, ber and
and the depth under notch is 10.2 mm. The machine is adjusted
the composite specimen respectively. The sufx p indicates the
such that the blade on the free hanging pendulum just barely con-
particulate ller material. However, the actual density qce of
tacts the specimen (zero position). Since there are practically no
the composite specimen can be determined experimentally by
losses due to bearing friction, etc. (<0.3%), the testing conditions
Archimedes principle. The volume fraction of voids (Vv) in the com-
may be regarded as ideal. The specimens are clamped in a square
posite samples is calculated by using the following equation:
support and are struck at their central point by a hemispherical
qct  qce bolt with diameter of 5 mm. The respective values of impact
Vv 2
qct energy of different specimens are recorded directly from the dial
134 A.K. Rout, A. Satapathy / Materials and Design 41 (2012) 131141
indicator. The test is repeated six times for each specimen to obtain
the mean value of impact strength.
2.4. Solid particle erosion test
To evaluate the performance of composites under erosive
conditions, experiments are conducted as per ASTM G76 [38] on
the test rig (TR-470) supplied by DUCOM Ltd. The test rig consists
of an air compressor, an air drying unit, a conveyor belt type par-
ticle feeder, an air particle mixing and accelerating chamber. The
dried and compressed air is then mixed with the silica sand having
40100 lm size, which is fed constantly by a conveyor belt feeder
into the mixing chamber and then accelerated by passing the mix-
ture through a convergent brass nozzle of 3 mm internal diameter.
The setup is capable of creating erosive situations for assessing
erosion wear resistance of the composite samples. The erodent
particles impact the specimen which can be held at different angles
with respect to the direction of erodent. In the present study, dry
silica sand of four different mean particle sizes (40 lm, 60 lm,
80 lm and 100 lm) are used as erodent. The samples are cleaned
with acetone, dried and weighed to an accuracy of 0.1 mg before
and after the erosion trials using a precision electronic balance. The
weight loss is recorded for subsequent calculation of erosion rate.
The process is repeated at least three times till the erosion rate at-
tains a constant value called steady state erosion rate.
2.4.1. Scanning electron microscopy (SEM)
The surface morphology of the specimens is examined by the
SEM JEOL JSM-6480LV. The worn out surfaces are mounted on
stubs with silver paste. A thin lm of platinum is vacuum evapo-
rated onto the samples for better conductivity before the
examination.
2.5. Experimental design
Taguchi design of experiment is a simple, efcient and system-
atic approach to optimize performance, quality and cost [39]. This
experimental procedure have been used earlier for parametric ap-
praisal of erosion behavior of glass ber reinforced polyester hy-
brid composites by Mahapatra et al. [40] and Patnaik et al. [15].
The selection of control factors is the most important part in the
design of experiment. Therefore, a large number of factors are ini-
tially included so that the non signicant variables can be identi-
ed easily. Factors like impact velocity, ller content,
impingement angle and erodent size, etc. largely inuence the ero-
sion rate of polymer composites [20]. The impact of these four fac-
tors on erosion of polymer composites is therefore studied in this
work using an L16 orthogonal array design. The xed and variable
parameters chosen for the test are given in Table 2 and the selected
levels of the four control factors are listed in Table 3.
In a conventional full factorial design, 44 = 256 number of
experiments are required to study four parameters each at four
levels, where as in Taguchi design of experiment only 16 number
of experiments are required, thus offering a greater advantage with
respect to cost and time of experiment. The experimental observa-
tions are further transformed into signal-to-noise (S/N) ratios. The
Table 2
Setting of parameters.
Control factors Symbols Fixed parameters
Velocity of impact Factor A Erodent Silica sand
Rice husk content Factor B Erodent feed rate (g/min) 10.0 1.0
Impingement angle Factor C Nozzle diameter (mm) 3 cycles, learning rate, error tolerance, momentum parameter, noise
Erodent size Factor D Length of nozzle (mm) 80
Standoff distance 100 mm
Table 3
Control factors and their selected levels.
Control factor Level
I II III IV Units
A: Velocity of impact 30 40 50 60 m/s
B: Rice husk content 0 5 10 15 wt.%
C: Impingement angle 45 60 75 90
D: Erodent size 40 60 80 100 lm
S/N ratio for minimum erosion rate is coming under Lower is bet-
ter (LB) characteristics and the logarithmic transformation of loss
function is shown below as:
 
S 1
10log10 Ry2 7
N n
where n is the number of observations and y is the observed data.
In Table 4, each of the columns, from second to fth, represents
a test parameter and a row stands for a test condition, which is
nothing but a combination of the parameter levels. The plan of
experiment is: the second column is assigned to impact velocity
(A), the third column to rice husk content (B), the fourth column
to impingement angle (C) and the fth column to erodent size
(D) to estimate the erosion rate (Er).
2.6. Neural network analysis
An articial neural network (ANN) is a computational system
that simulates the micro-structure (neurons) of biological nervous
system and has been used to solve a wide variety of complex, non-
linear problems in various elds. For prediction of wear in poly-
mers, this technique has been used by Velten et al. [41] and
Zhang et al. [42]. The wear behavior of polymeric materials is con-
sidered as a complex and non-linear problem with respect to its
parameters and operating conditions. In order to obtain minimum
erosion rate, appropriate combination of operating parameters
have to be planned properly. Therefore techniques like articial
neural network (ANN) are needed to study the interrelated effect
of parameters on the wear process. It is a technique that involves
database training to predict inputoutput correlation and com-
posed of many cross-linked simple processing units called neurons.
The network can learn directly from examples without any prior
formulae about the nature of the problem. A neural network gen-
erally consists of three parts connected in series as input layer, hid-
den layer and output layer. The information is accepted by input
layer, processed in hidden layer and nally the results exported
in the output layer. The details of this methodology are described
by Rajasekaran and Vijayalakshmi Pai [43].
In the present study, rice husk content, impact velocity,
impingement angle and erodent size are taken as the four input
parameters and erosion rate as output parameter. Experimental re-
sult sets are used to train the neural network. The database of the
network is divided into three categories i.e. (i) a validation cate-
gory which is required to dene the neural network and adjust
the number of neurons for each layer, (ii) a training category,
which is used for adjustment of network weights and (iii) a test
category, which is used to the set that validates the results of the
training protocol. The input variables are normalized so as to lie
same range group of 0 to1. The output layer has one neuron to rep-
resent erosion rate. About 80% of the experimental result data are
used to train the network and different ANN structures with vary-
ing number of neurons in the hidden layer are tested at constant
factor and slope parameter. Based on the least error criterion, one
structure is selected for training of inputoutput data which is
 A.K. Rout, A. Satapathy / Materials and Design 41 (2012) 131141 135

Table 4 Table 6
Experimental design using L16 orthogonal array. Measured and theoretical densities of the composites.

Test Velocity of Rice husk Impingement Erodent size Composites Measured density Theoretical density Volume fraction
run impact A (m/sec) content B ( wt.%) angle C () D (lm) (gm/cc) (gm/cc) of voids (%)
1 30 0 45 40 C1 1.412 1.430 1.25
2 30 5 60 60 C2 0.898 0.934 3.85
3 30 10 75 80 C3 0.647 0.693 6.63
4 30 15 90 100 C4 0.502 0.551 8.89
5 40 0 60 80
6 40 5 45 100
7 40 10 90 40
8 40 15 75 60 behavior. The modied values of the properties of the composites
9 50 0 75 100 under this investigation are presented and compared against the
10 50 5 90 80 unlled glassepoxy composites in Tables 6 and 7.
11 50 10 45 60
12 50 15 60 40
13 60 0 90 60 3.1. Mechanical properties
14 60 5 75 40
15 60 10 60 100 3.1.1. Density
16 60 15 45 80
The theoretical and measured densities, along with the corre-
sponding volume fraction of voids, are presented in Table 6. It
may be noted that the composite density values calculated theo-
Table 5 retically using Eq. (1) are not in agreement with the experimental
Input parameters selected for training. values. The difference is a measure of voids and pores present in
Input parameters for training Values the composite. It is clear from Table 6 that in C1 the volume frac-
tion of voids is negligible, and this is due to the absence of partic-
Error tolerance 0.01
Learning rate (b) 0.01
ulate llers. With the addition of ller materials, more voids are
Momentum parameter(a) 0.002 found in the composites. As the ller content increases from
Noise factor (NF) 0.001 5 wt.% to 15 wt.%, the volume fraction of voids is also found to in-
Number of epochs 10,00,000 crease proportionately. Similar observations have been found ear-
Slope parameter () 0.5
lier by previous researchers [1316]. The density of a composite
Number of hidden layer neuron (H) 10
Number of input layer neuron (I) 4 depends on the relative proportion of matrix and reinforcing mate-
Number of output layer neuron (O) 1 rials, and is one of the important factors determining the proper-
ties of the composite. The void content is the difference between
the values of the measured and theoretical density of the compos-
ite. The voids signicantly affect some of the mechanical properties
and even the performance of the composite. Higher void contents
usually mean lower fatigue resistance and greater tendency to
water penetration and weathering [34]. The knowledge of void
content is desirable for an estimation of the quality of the compos-
ites. It is understandable that a good composite should have fewer
voids. However, the presence of voids is unavoidable in composite
making, particularly in hand-lay-up technique.

Fig. 3. The three layer neural network.
presented in Table 5. The multi-layered neural network is the most
widely applied neural network, which has been utilized in most of
the research works for material science reviewed by Zhang and
Friedrich [44]. The three layer neural network used in this work
is shown in Fig. 3. The learning rate is varied in the range of
0.0010.1 during training of inputoutput data. In the present
work, the number of neurons in the hidden layer is varied and opti-
mized to 10. Software NEURALNET have been used for neural com-
putation with back propagation algorithm and the erosion rate is
predicted within and beyond the experimental domain.
3. Results and discussion
The characterization of the composites reveals that inclusion of
rice husk particulate ller has strong inuence not only on the
mechanical properties of the composites but also on their erosion
3.1.2. Micro-hardness
The measured hardness values of all the four composites are
presented in Table 7. It can be seen that the hardness is affected
signicantly with addition of rice husk particles.
It is observed that the micro-hardness, which is considered to
be one of the important factors in composites for determination
of wear rate, increases with increase in ller content. With the in-
crease in rice husk content from 0 wt.% to 15 wt.% the hardness is
found to increase from 34 Hv to 43 Hv. This implies an increment
of 26% in hardness of the rice husk lled composites. This improve-
ment in hardness with the incorporation of ller can be explained
as follows: during hardness test, a compressive load is in action. So
the solid ller phase and matrix phase would be pressed together
and touch each other more tightly. Thus the interface can transfer
pressure more effectively although the interfacial bond strength
may be poor. This results in enhancement of hardness. Similar
property modication has been reported for y ash, alumina and
SiC particles lled in polymer composites by previous woks
[45,14,15].
3.1.3. Tensile properties
The tensile strengths and moduli of glassepoxy composites
lled with rice husk are shown in Table 7. It is found that, there
is a gradual drop in tensile strength with increase in ller content.
136 A.K. Rout, A. Satapathy / Materials and Design 41 (2012) 131141
Table 7
Mechanical and physical properties of the composites.
Composites Mean hardness Tensile strength
(Hv) (MPa)
C1 34 362.5
C2 37 278.26
C3 39 228.88
C4 43 144.35
The unlled glassepoxy composite has strength of 362.5 MPa in
tension, and this value drops to 278.26 MPa, 228.88 MPa and
144.35 MPa with rice husk addition of 5 wt.%, 10 wt.% and
15 wt.% respectively. Similar observations have been found by Cre-
spo et al. [31] for plasticized PVC composites and Yang et al. [32]for
polypropylene matrix composites containing rice husk llers. The
present results are also consistent with previous woks for red
mud, alumina, y ash and copper slag lled glassepoxy/polyester
composites [1316,46]. Mahapatra et al. [40] and Findik et al.
[47]found an increasing trend in tensile strength of glasspolyester
composites (without ller) with increasing ber loading. This
improvement can be attributed to more ber reinforcement
(wt.%) as the bers are the load carrying members in a polymer
matrix. Similarly, Unal et al. [3] have found that the tensile
strength of nylon composite increases with the increase in ller
addition. However, the inuence of ller addition has been signif-
icant up to 10 wt.%. This type of behavior of the polymer compos-
ites reinforced with/without ber and lled with/without micro-
sized llers may be explained as follows: The ller particles,
depending upon their type, shape and size, possess better ller
characteristics (interfacial adhesion) with the polymer matrix up
to certain wt.% so that an improvement in strength is observed.
The reduction in tensile strength with ller addition may be due
to the chemical bond strength between ller particles and the ma-
trix body is too weak to transfer the tensile load or the sharp cor-
ners of irregular shaped ller particles result in stress
concentration zones in the matrix body during tensile loading or
due to the increase in void percentage in the composites with in-
crease in ller content.
A review of earlier research [47,48] suggests that normally glass
ber in the composite restrain the deformation of resin matrix and
which reduces the tensile strain. So, even if the tensile strength re-
duces, modulus of the composite is expected to increase. In the
present study, the tensile modulus of the glassepoxy composites
(as shown in Table 7) has increased from 5.5 GPa to 6.03 GPa with
ller addition up to 15 wt.%. This improvement is attributed to the
relatively lower strain rates of the composites C2, C3 and C4 as com-
pare to C1. Similar observations have been found by Unal et al. [3]
for nylon 6 composites containing talc and kaolin llers. They have
explained the percolation theory which states that a matrix zone
around each particle is affected by a stress concentration. There-
fore, if the ller addition increases then the distance between each
stress concentration zone will be small enough to form a percola-
tion network and due to which the modulus of the composite
increases.
3.1.4. Flexural and inter-laminar shear strength
Table 7 shows the exural strengths of the composites obtained
experimentally from bend tests. It is observed that the exural
strength of the composite is reducing with increase in ller con-
tent. Similar observations have been found earlier by previous
researchers for red mud and alumina lled glassepoxy composites
[13,14]. This might be due to the poor dispersion of micro sized
rice husk particles in the epoxy matrix and a greater possibility
of the existence of voids in the composites.
Tensile modulus Flexural strength ILSS Impact energy
(GPa) (MPa) (MPa) (J)
5.5 388.8 26.8 0.77
5.7 358.8 22.57 0.79
5.8 322.17 19.26 0.82
6.03 269.52 18.54 0.84
Composite materials used in structures are prone to fail in
bending and therefore the development of new composites with
improved exural properties is essential. The stress between the
consecutive lamina of a layered composite is called inter laminar
shear stress. The results on the inter-laminar shear strength of
the glassepoxy composites are presented in Table 7. The ILSS of
glassepoxy composite without ller is measured as 26.8 MPa.
With the addition of rice husk, ILSS of laminates decreases to
18.54 MPa for composites containing 15 wt.% rice husk ller. The
reduction may be related with the formation of voids in the epoxy
matrix, which are generally located at the inter-laminar region of
composites.
3.1.5. Impact strength
The recorded impact energy values of different composites dur-
ing the impact test are presented in Table 7. It shows that the resis-
tance to impact loading of glassepoxy composites improves with
addition of ller. However, this improvement is not very signi-
cant. It is seen that the resistance to impact loading of glassepoxy
(C1) composite increases by about 9% with addition of ller
(15 wt.%) into it. Similar observations have been found by Patnaik
et al. [45] for glasspolyester composites lled with alumina and
by Biswas and Satapathy [46] for glassepoxy composites lled
with copper slag. A review of literature states that the mobility
of polymer chain is constrained by the ller content, which reduces
their ability to deform freely and makes the material less ductile
[49]. Therefore, the energy absorbing capability of the composite
reduces with ller addition. Unal et al. [3] have found a reduction
in impact properties of nylon composites lled with talc and kaolin
as single additions. However, in case of mixed-compound (10 wt.%
kaolin + 20 wt.% talc) addition, they noticed an improvement of
7.6% in impact strength. Therefore, the content of ller and ber
is to be decided judiciously before any specic application keeping
the strength in mind.
3.2. Morphology of worn samples
Erosion wear behavior can be grouped as ductile and brittle cat-
egories. Thermoplastic matrix composites usually show ductile
erosion whereas thermosetting polymer matrices erode in a brittle
manner. However, there is a dispute about this failure classication
as the erosive wear behavior depends strongly on the experimental
conditions and composition of the target material [18]. To charac-
terize the morphology of eroded surfaces and to identify the mode
of material removal, the samples are observed under a scanning
electron microscope. Figs. 4a4e represent the surface microstruc-
tures of rice husk lled epoxy composites. The SEM observation of
the eroded surfaces appears that the composites under consider-
ation exhibit several forms of erosion and material removal pro-
cess. Fig. 4a shows micrograph of the eroded C4 surface at an
impingement angle of 90, impact velocity of 30 m/s and erodent
size of 100 lm. Here, a relatively small fraction of the material is
seen to be removed from the surface although formation of a large
amount of grooves is visible. However, crack formation and prop-
agation are not seen. This may be due to either large erodent size,
 A.K. Rout, A. Satapathy / Materials and Design 41 (2012) 131141 137

Crater formation

Multiple grooves in the matrix body

Fig. 4c. Scanning electron micrograph of the eroded surface showing the formation
Fig. 4a. Scanning electron micrograph of multiple grooves of the composite at of crater.
impingement angle of 90, impact velocity of 30 m/s and erodent size of 100 lm.

Transeverse fiber cracks

Array of exposed fibers

Fig. 4d. Scanning electron micrograph of the composite showing transverse cracks
Fig. 4b. Scanning electron micrograph of the eroded surface of the composite and ber fragmentation at impingement angle of 75 and impact velocity of 60 m/s.
showing array of exposed ber at impingement angle of 60 and impact velocity of
50 m/s.

Fiber fragmentation Filler fragmentation

which helps in crack formation, or lower impact velocity that has
not favored the crack propagation. Fig. 4b shows the micrograph
of the eroded C4 surface at an impingement angle of 60 and an
impact velocity of 50 m/s. The exposed bers are clearly visible
during repeated impact of sand particles. The matrix covering the
ber seems to be chipped off and erosion along the bers with
clean removal of matrix body at the interface is observed. Fig. 4c
shows the crater formation due to penetration of hard silica sand
particles onto the surface which causes material removal mostly
from the matrix region.
Fig. 4d shows a portion of the composite surface eroded at an
angle of 75 and impact velocity of 60 m/s. When the erodent
strikes the composite at an angle, the parallel component of veloc-
ity with respect to ber orientation causes local removal of resin
material from the impact surface and the transverse component
of velocity induces bending stress in the exposed bers, which Fig. 4e. Scanning electron micrograph of the eroded surface showing ber and ller
fragmentation and longitudinal cracks at impingement angle of 90 and impact
are not supported by the resin matrix (as seen in Fig. 4d). The in-
velocity of 60 m/s.
duced bending stress in the ber causes intensive debonding and
breakage. As the impact angle of the particle shifts towards larger
values, the effect of normal force becomes dominant. Fig. 4e illus- This is a case of the erodent particles striking aggressively on the
trates the wear morphology of the material after normal erosion at composite surface at high impingement angle with high impact
90 and at high impact velocity of 60 m/s. At this impingement an- velocity. During repeated impact of the erodent, carrying higher
gle there is no parallel component of particle speed and force. energy, the bers beneath the matrix layer break and undergo frag-
Hence, many bers are cracked into small fragments and they mentation resulting loose debris. Similar observations have been
are removed from their places partly with the surrounding matrix. found by Biswas and Satapathy [21] for red mud lled glassepoxy
138 A.K. Rout, A. Satapathy / Materials and Design 41 (2012) 131141

composites. The exposed bers are broken into fragments and thus
can be easily removed from the worn surfaces. The presence of rice
husk particles in the matrix helps in absorbing a good fraction of
the erodent kinetic energy and therefore, energy available for plas-
tic deformation of epoxy becomes less. This also delays the initia-
tion of ber exposure as compared with the composite without
ller.
3.3. Erosion test results and Taguchi analysis
The erosion wear rates of glassepoxyrice husk composites as a
function of impingement angle are shown in Fig. 5. Steady state ero-
sion wear rates have reached during the erosion periods for each
impingement angle. It is observed that the rate of mass loss of the
eroded samples vary with the erosion time at each impingement an-
gle (15, 30, 45, 60, 75 and 90). It is well known that impinge-
ment angle has a great inuence on erosion processes and for
ductile materials the peak erosion normally occurs between 15
and 20 angles, whereas for brittle materials the maximum erosion
takes place at normal impact [20]. In the present study, the variation
of erosion wear rate of the glassepoxyrice husk composites with
impingement angle has been studied by conducting experiments
under specied operating conditions. It is found that peak erosion
occurs at an impingement angle of 60 for the unlled as well as
the rice husk lled glassepoxy composites as shown in Fig. 5. This
indicates that these composites are neither ductile nor brittle.
Epoxy matrix is a ductile material whereas both glass ber and rice
husk particles are brittle materials. Therefore, the fabricated
composite becomes semi-ductile in nature. Similar observations
have been found by previous researchers for other ller materials
in glassepoxy/polyester matrices [1316,21,23]. Biswas and Sata-
pathy [46] have found maximum erosion at 45 impingement angle
for the copper slag lled epoxy composites whereas erosion rate is
maximum at 60 impingement angle for the unlled samples. Sim-
ilarly, Bagci and Imrek [22] have found maximum erosion at 30
impingement angle for the boric acid lled epoxy composites. This
behavior of the hybrid composites may be attributed to the inu-
ence of different experimental parameters (erodent size, erodent
temperature, type of erodent, standoff distance, erodent velocity,
etc.) during the test [20] or interfacial adhesion of ber/ller with
the matrix body or it may be due to the orientation of ber and dis-
persion of ller in the matrix.
In Table 8, the erosion rates of different composites for all 16 test
runs and their corresponding S/N ratios are given. Each value is in
fact the average of two replications. The overall mean for the S/N ra-
tio of the erosion rate is found to be 45.803 dB. The analysis was
made using the software specially used for design of experiment
applications known as MINITAB 14. Before any attempt is made
to use this simple model as a predictor for the measure of perfor-
mance, the possible interactions between the control factors must
be considered. Thus, factorial design incorporates a simple means
of testing for the presence of interaction effects. Analysis of the re-
sults leads to a conclusion that a factor combination of A3, B4, C1, and
D1 gives minimum erosion wear rate as shown in Fig. 6. Further,
Table 9 indicates the order of the control factors as impingement
angle (C), rice husk content (B), impact velocity (A) and erodent size

600

500
Erosion rate (mg/kg)

400

300

200
0 wt% 5 wt%
100
10 wt% 15 wt%

0
15 30 45 60 75 90
Impingement angle (degree)

Fig. 5. Effect of impingement angle on the erosion rate of the composite.

Table 8
Experimental design using L16 orthogonal array.

Test runs A velocity of impact (m/s) B rice husk content (wt.%) C impingement angle () D erodent size (lm) Er erosion rate (mg/kg) S/N ratio (dB)
1 30 0 45 40 189.78 45.5650
2 30 5 60 60 180.89 45.1483
3 30 10 75 80 206.65 46.3047
4 30 15 90 100 186.65 45.4206
5 40 0 60 80 207.28 46.3311
6 40 5 45 100 186.54 45.4154
7 40 10 90 40 183.43 45.2694
8 40 15 75 60 215.76 46.6794
9 50 0 75 100 204.28 46.2045
10 50 5 90 80 211.58 46.5095
11 50 10 45 60 176.43 44.9314
12 50 15 60 40 164.12 44.3032
13 60 0 90 60 231.25 47.2816
14 60 5 75 40 212.51 46.5476
15 60 10 60 100 203.48 46.1704
16 60 15 45 80 173.25 44.7735
 A.K. Rout, A. Satapathy / Materials and Design 41 (2012) 131141 139

Fig. 6. Effect of control factors on erosion rate.

Table 9
S/N ratio response table for erosion rate.

Level A (velocity of impact) B (rice husk content) C (impingement angle) D (erodent size)
1 45.61 46.35 45.17 45.42
2 45.92 45.91 45.49 46.01
3 45.49 45.67 46.43 45.98
4 46.19 45.29 46.12 45.80
Delta 0.71 1.05 1.26 0.59
Rank 3 2 1 4

(D) in decreasing order according to their signicance on the
erosion rate. It thus can be concluded that erodent size has least ef-
fect as compared with other factors on the wear rate.
3.4. Development of mathematical model for minimum erosion rate
For the present investigation, an attempt has been made to nd
out optimal setting of control factors for minimum erosion wear
rate. The single objective optimization requires quantitative deter-
mination of the relationship between erosion wear rate and control
factors. In order to derive the wear rate in terms of a mathematical
model, the following equation is suggested:
Er K 0 K 1  A K 2  B K 3  C K 4  D
Er is the erosion rate in mg/kg and Ki (i = 04) are the model con-
stants. A is the impact velocity (m/s), B is the rice husk content
(wt.%), C is the impingement angle () and D is the erodent size
(lm). The constants are calculated using non-linear regression
analysis with the help of SYSTAT 14 software and the following
relation is obtained:
Er 145:761 0:332  A  1:5  B 0:574  C 0:110  D
The correctness of the calculated constants is conrmed as high
correlation coefcient (R2) to the tune of 0.997 is obtained for ero-
sion wear rate and therefore the model is quite suitable to use for
further analysis. A comparison of erosion rate of the composites
with the experimental values is presented in Table 10 and the per-
centage error varies between 0% and 13%, which lies within the
acceptable limit.
Another predictive model based on ANN is employed, and the
experimental results are compared with it. The neural network is
constructed using the experimental database. About 80% of data
are used for training, whereas 20% of data are used for testing of
the model. The selected and optimized parameters for training of
the ANN model have been presented in Table 5. A comparison of
erosion rate between the ANN model and the experimental values
is presented in Table 11. It is observed that the maximum error be-
tween ANN model and experimental wear rate is 010%. However,
this error can be further reduced if the number of test patterns will
be increased. The present study demonstrates the application of
ANN for prediction of wear rate in a complex process such as solid
particle erosion of polymer composites.
3.5. Conrmation experiment
The conrmation experiment is the nal test in the design of
8 experiment process. The objective of the conrmation experiment
is to validate the conclusions drawn during the analysis phase. The
conrmation experiment is performed by conducting a new set of
factor settings A3B2C3D3 to predict the erosion wear rate. A predic-
tion equation can be formulated using Taguchis approach to esti-
mate S/N ratio for erosion rate as [50].
g1 T A3  T  C3  T
 B2  T  D3  T
 10
9 where g1 is predicted average; T is overall experimental aver-
age; and A3 ; B2 ; C3 and D3 are the mean responses for factors at
designated levels. By combining like terms, the equation reduces
to:
g1 A3 B2 C3 D3  3T 11
The new arbitrary combination of factor levels A3, B2, C3 and D3
is used to predict the wear rate through prediction equation (Eq.
(11)) and the S/N ratio is found to be 46.401 dB. An experiment
was conducted under factor combination of A3, B2, C3 and D3 and
the result was compared with the value obtained from predictive
equation as shown in Table 12. The resulting model seems to be
140 A.K. Rout, A. Satapathy / Materials and Design 41 (2012) 131141

Table 10 (2) The hardness, tensile modulus and impact energy of these
Comparison of experimental and predictive equation results. new class hybrid composites are improving with ller addi-
Test Erosion rate (mg/kg) Error tion while a steady decline of tensile and exural properties
run
Result obtained from Result obtained from
(%) are observed.
experimentation predictive equation (3) Such hybrid composites possess fairly good potential for
1 189.78 185.951 2.017
application in erosive situations like engineering structures
2 180.89 189.26 4.62 in dusty environment and low cost building materials in
3 206.65 192.571 6.81 deserts. The content of rice husk is to be decided judiciously
4 186.65 195.881 4.94 keeping the strength and wear attack in mind. These com-
5 207.28 202.281 2.41
posites, in general may also be recommended for applica-
6 186.54 188.371 0.98
7 183.43 190.141 3.65 tions like partition boards, false ceilings, pipe lines carrying
8 215.76 186.191 13.7 coal dust, light weight vehicles, etc.
9 204.28 216.411 5.93 (4) The erosion wear performance of glass epoxy composites
10 211.58 215.321 1.76
improves with the incorporation of particulate llers.
11 176.43 166.511 5.62
12 164.12 178.701 8.82
Among the three weight percentages of rice husk in the
13 231.25 223.941 3.16 composite, 15 wt.% rice husk composites has shown maxi-
14 212.51 205.631 3.23 mum erosion resistance.
15 203.48 196.121 3.61 (5) A study on the dependence of erosion wear on impingement
16 173.25 177.811 2.63
angle reveals semi-ductile nature of the composite and the
peak erosion rate is found to be occurring at 60 impinge-
ment angle for all the composites.
Table 11 (6) Two predictive models; one based on ANN approach and the
Comparison of experimental and ANN results. other on Taguchi approach are proposed. It is demonstrated
that these models well reect the effects of various factors
Test Erosion wear rate (mg/kg) Error
Run (%)
on the erosion loss and their predictive results are consistent
Result obtained from Result obtained from ANN with experimental observations. The predicted and experi-
experimentation prediction
mental values of erosion wear rate shows good agreement
1 189.78 187.741 1.07 and validate the remarkable capability of a well trained neu-
2 180.89 185.379 2.48
3 206.65 201.953 2.27
ral network for this kind of processes.
4 186.65 188.116 0.78 (7) Factors like impingement angle, ller content, impact veloc-
5 207.28 206.031 0.60 ity and erodent size are found to be the signicant control
6 186.54 186.400 0.07 factors in decreasing order affecting erosion rate.
7 183.43 183.167 0.14
(8) In future, this study can be extended to new hybrid compos-
8 215.76 215.830 0.03
9 204.28 204.662 0.18 ites using different llerber combinations, and the result-
10 211.58 212.014 0.20 ing ndings can be similarly analyzed.
11 176.43 176.993 0.31
12 164.12 163.538 0.35
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