Materials and Design: Amar Patnaik, MD Abdulla, Alok Satapathy, Sandhyarani Biswas, Bhabani K. Satapathy
Materials and Design: Amar Patnaik, MD Abdulla, Alok Satapathy, Sandhyarani Biswas, Bhabani K. Satapathy
Materials and Design: Amar Patnaik, MD Abdulla, Alok Satapathy, Sandhyarani Biswas, Bhabani K. Satapathy
a r t i c l e i n f o a b s t r a c t
Article history: In this study, thermal conductivity of particulate filled polymer composites is investigated experimen-
Received 9 June 2009 tally by guarded heat flow meter method in accordance with ASTM E 1530. The objective of this research
Accepted 28 July 2009 is to attain a better understanding of global and local thermal behavior of a composite system through
Available online 6 August 2009
basics of thermal properties. The results obtained from this study are compared with an existing theoret-
ical model for validation purposes of pine bark reinforced epoxy based resin composites with and with
Keywords: out particulate filler content. To this end, a correlation has been made between the thermal conductivity
Polymer composite
and specific wear resistance of the tested samples, highlighting the importance of the insulating material.
Thermal conductivity
Particulates
The relationship between control factors and performance outputs are established by means of non-lin-
Specific wear rate ear regression analysis resulting in a valid mathematical model. Finally, a popular evolutionary approach
known as genetic algorithm (GA) is used to generalize the method of finding out optimal factor settings
for minimization of thermal conductivity and specific wear rate.
Ó 2009 Elsevier Ltd. All rights reserved.
1. Introduction given by Progelhof [3]. Procter and Solc [4] used Nielsen model
as a prediction to investigate the thermal conductivity of several
Commonly used polymer materials such as polyethylene (PE), types of polymer composites filled with different fillers, and con-
polypropylene (PP), polyvinyl chloride (PVC) or polyamide are firmed its applicability. Nagai [5] found Bruggeman model for
good electrical and thermal insulators. Recent applications of poly- Al2O3/epoxy system and a modified form of Bruggeman model
mers as heat sinks in electronic packaging require new composites for AlN/epoxy system are both good prediction theories for thermal
with relatively high thermal conductivity. Improved thermal con- conductivity. Bollampally and Wong [6] found that Agari model
ductivity in polymers may be achieved either by molecular orien- predicts better than Maxwell model for thermal conductivity of
tation or by the addition of conductive fillers. During the last few SiO2/epoxy composite at high percentage of filler.
decades, however, in the microelectronic systems, great effect However, it is not always possible to manufacture polymer ob-
has been contributed to improving higher integration density, fas- jects of a desired shape with a prescribed orientation value and in
ter performance, miniaturization of electronic devices and lower the desired direction. Hence a more practical method to increase
cost [1,2]. Therefore, the power density in the electronic devices the thermal conductivity of a polymer is needed. The addition of
is becoming larger and larger. That turns the researchers’ focus thermally conductive particles or short fibers to the polymers dur-
to be placed on the thermal conductivity in order to get heat-dis- ing the injection molding process seems to be a good method to
sipating composites. The prediction of thermal conductivity of obtain conductive polymers. Such filled polymers with higher
composites comprises a significant portion of the heat transfer lit- thermal conductivities than unfilled ones are becoming a more
erature. Many reports concerning about the thermal conductivity important area of study because of the wide range of applications,
of polymer composites, associated with various thermal conduc- e.g., in electronic packaging in applications with decreasing geo-
tive models or equations for predicting the thermal conductivity, metric dimensions and increasing output of power, like in com-
have been published. They are either theoretically based or are puter chips or in electronic packaging [7,8].
empirical which means to include one or more experimentally In this study, thermal conductivity of particulates filled fiber
determined (or empirical) parameters. A good overview has been reinforced polymer composites is investigated by two different
manufacturing methods. The results clearly show that the in-
* Corresponding author. Tel.: +91 9437188085. creased filler concentration leads to higher thermal conductivity
E-mail address: [email protected] (A. Patnaik). that can be correlated to the reduced dry sliding wear rate of the
0261-3069/$ - see front matter Ó 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.matdes.2009.07.046
838 A. Patnaik et al. / Materials and Design 31 (2010) 837–849
latter affects strongly the thermal conductivity of the composite, Effect of different materials and manufacturing methods
hence the resistance to wear. At the end, an optimization technique Compression molding/hand lay-up techniques
is applied to addresses the relationship between thermal conduc- Glass fiber/carbon fiber reinforced Pine bark reinforced
tivity and the specific wear resistance of the worn composites un- composites composites
der different operating conditions. L T Th L T Th
2.1. Matrix material bark is reinforced in three different resins to prepare the composite
with and without filler content by two different manufacturing
Unsaturated isophthalic polyester resin (Elastic modulus techniques such as conventional hand-lay-up technique and com-
3.25 GPa, density 1.35 g/cc) is the matrix material. Two percent pression molding process, respectively. Herein, the thermal con-
of cobalt nephthalate (as accelerator) is mixed thoroughly in iso- ductivity measurement in the transverse direction means that a
phthalic polyester resin and then 2% methyl-ethyl-ketone-perox- sample is prepared in such a way that heat flow direction is trans-
ide (MEKP) as hardener is mixed in the resin prior to verse to primary fiber orientation of the sample; similarly, the
reinforcement. Epoxy LY 556 resin, chemically belonging to the thermal conductivity measurement in the longitudinal direction
‘epoxide’ family is used as the matrix material. Its common name means heat flowing along the fiber direction; and the thermal con-
is Bisphenol A Diglycidyl Ether. Vinyl ester resins (EPN-1138) are ductivity measurement in the thickness direction means heat flow-
addition products of various epoxide resins and unsaturated ing through-the-thickness direction. The thermal conductivity of
monocarboxylic acids, most commonly methacrylic acid. The low an anisotropic composite material depends on the resin nature, fi-
temperature curing epoxy resin (Araldite LY 556) and correspond- ber type and architecture, fiber weight fraction, manufacturing
ing hardener (HY951) are mixed in a ratio of 10:1 by weight as rec- technique, direction of heat flow and operating temperature, lead-
ommended. The polyester, epoxy and Vinyl ester resins and the ing to a high degree of complexity.
respective hardeners are supplied by Ciba Geigy India Ltd.
2.5. Thermal conductivity test matrix
2.2. Fiber materials
The research proceeded as outlined in Table 1. The test matrix
In this work, three different types of fibers are taken for exper- has included various material parameters and process parameters,
imental purposes. Out of which two conventional fibers (woven leading to a spectrum of composite samples for their thermal con-
roving E-glass fibers and carbon fiber) and one natural fiber (pine ductivities along 0° and 90° fiber orientations and through-the-
bark) have been used as the reinforcing material in all the compos- thickness direction. It should be noted that sample preparation is
ites. Natural fibers are becoming potential alternatives for glass fi- the most challenging part of the entire process. Many tools are
ber reinforced composites in many applications [9]. used specially for sample preparation in addition, attention to
environmental and health safety issues are also needed. The test
2.3. Filler materials samples are prepared in the form of 10 cm rectangular plate using
compression molding and hand lay-up methods. Ideally all sam-
Two conventional fillers: aluminium and copper powder and ples for three-dimensional measurements should be cut from same
one industrial waste: cement by-pass dust (CBPD) are chosen to block by diamond cutter. Technically this poses a great difficulty in
be used as particulate fillers in pre-determined proportions in var- manufacturing such a block in terms of proper alignment of fabric
ious composites prepared for this investigation. While, aluminium and wet out.
and copper have conventionally been used in many composite Typically, FRP laminate has a thickness of 3–8 mm. A 10 cm
applications, the industrial waste cement by-pass dust (CBPD) rectangular plate is cut from this type of laminate to measure its
can be considered as non-conventional materials for use as fillers thermal conductivity with heat flowing through-the-thickness
in polymer composites. It is a fine powdery material similar in direction. Both the above discussed approaches are used to prepare
appearance to Portland cement. It is generated during the calcining samples in the present study. As a result, we have successfully pre-
process in the kiln. As the raw materials are heated in the kiln, dust pared a couple of samples that allow for thermal conductivity mea-
particles are produced and then carried out with the exhaust gases surements in transverse, longitudinal, and through-the-thickness
at the upper end of the kiln. These gases are cooled and the accom- directions.
panying dust particles are captured by efficient dust collection sys-
tems. Lime (CaO) constitutes about 40% of CBPD composition. 3. Experimental approach for thermal conductivity
Other compounds include SiO2, Al2O3, Fe2O3, K2O, Na2O and Cl. measurements
2.4. Composite preparation There are various test methods available for thermal
conductivity measurement and each method depends mainly on
E-glass fiber/carbon fiber are reinforced with respective resin configuration of a material and job requirement. One principal
also added particulate filler materials to prepare samples with dif- experimental method for determinations of thermal conductivity
ferent wt%. All these filler materials are thoroughly dispersed in the is discussed below:
resin by mechanical stirring. The resins used for this study were vi-
nyl ester, polyester and epoxy. Test specimens are prepared using 3.1. Guarded heat flow meter
0%, 4%, and 8% of filler by weight percentages are taken in this work
to determine conductivity properties in three different directions This method is based on two dimensional steady state tech-
(i.e. longitudinal, transverse and through-the-thickness) and spe- niques and is used to measure and compare thermal properties
cific wear rate of the composites. E-glass fiber/carbon fiber/pine of materials under controlled conditions and their ability to
A. Patnaik et al. / Materials and Design 31 (2010) 837–849 839
maintain required thermal conductance levels [9]. The specimen tween the polished surfaces, each controlled at different tempera-
and a heat flux transducer (HFT) are sandwiched between two flat tures, using pneumatic load. The pressure is maintained at 10 psi
plates controlled at different temperatures, to produce a heat flow using pressurized air supply. As an option, coolant water is circu-
through the stack. A cylindrical guard surrounds the test stack and lated through heat sink. A circular low temperature heat insulation
is maintained at a uniform mean temperature of the two plates, in ring is wrapped around the lower stack of the assembly to restrain
order to minimize the lateral leak of heat. At steady state, the dif- heat flow to outside atmosphere. The entire system is maintained
ference in temperature between the surfaces contacting the speci- in a thermally insulated glass chamber. Unitherm is completely
men is measured with temperature sensors embedded in the automatic while testing as the apparatus is completely controlled
surfaces, together with the electrical output of the HFT. The output by a computer. The test system is hooked to the computer by
voltage is proportional to the heat flow through the specimen, HFT means of an USB cable.
and the interfaces between the specimen and the apparatus. The Considering the operation of the system, the sample to be tested
coefficient of thermal conductivity can be obtained by prior cali- is prepared into a flat surface on both sides and thermal compound
bration of system with the specimens of know thermal is applied on the sample to reduce thermal resistance caused due
conductivity. to surface roughness. Then the prepared sample is placed in be-
tween two polished surfaces and a pneumatic pressure of 10 psi
is applied on the top portion of the stack. The sample can be tested
3.2. Experimental set-up in the temperature range from 50 °C to 300 °C. For steady state
heat transfer, the user can divide the testing into different zones,
A guarded heat flow meter method has been developed for ther- called as set point temperatures. In this thesis the testing was di-
mal conductivity measurements. This is achieved by using a ther- vided into three temperature zones i.e. 60, 80, and 100 °C. For high-
mal conductivity testing system Unitherm model 2022 from er thermal conductivity materials, a difference of 50° is
ANTER Corp., Pittsburgh, PA. This unit is supplied with a mid range recommended for the machine. At every set point temperature,
flux module covering a thermal resistance range from 0.01 to the system checks for steady state heat flow through the sample
0.05 m2 K/W and is able to measure the thermal conductivity of and thermal conductivity is measured.
materials in the range of 0.1–40 W/m K in terms of test standard
ASTM E 1530. The materials that can be tested include metals, 3.3. Operation principle of Unitherm 2022
ceramics, polymers, composites and glass. The test samples need
to be prepared in a form of 2-in. diameter circular discs with their By definition thermal conductivity means ‘‘The material prop-
thickness depending on the materials’ thermal conductivity. The erty that describes the rate at which heat flows with in a body
thermal conductivity machine is supplied with three different sets for a given temperature change.” For one-dimensional heat con-
of calibration samples span the operating range (R) from 0.0005 to duction the formula can be given as
0.01, 0.002 to 0.02 and 0.01 to 0.05 m2 K/W. These samples are
tested for conductivity values and compared with the given values T1 T2
Q ¼ KA ð1Þ
by the manufacturer for calibration purpose. x
A schematic picture shown in Fig. 1 represents the system func- where Q is the heat flux (W), K is the thermal conductivity (W/m K),
tioning in detail. The assembly is a stack of parts with different A is the cross-sectional area (m2), T1T2 is the difference in temper-
functionalities. The heater on top and bottom helps to maintain ature (K), x is the thickness of the sample (m). The thermal resis-
steady state heat transfer through the sample, two polished sur- tance of a sample can be given as
faces on top and bottom the sample transfer heat from top and bot-
tom of heaters with reduced thermal resistance through surface. A T1 T2
R¼ ð2Þ
reference calorimeter is placed under the lower plate, which acts as Q =A
a heat flux transducer. The heat sink at the bottom avoids excessive
where R is the resistance of the sample between hot and cold sur-
temperature from the system. The sample is compressed in be-
faces (m2 K/W). From Eqs. (1) and (2) we can derive that
x
K¼ ð3Þ
Pneumatic load R
In Unitherm 2022 the heat flux transducer measures the Q value
and the temperature difference can be obtained between the upper
Top heater
plate and lower plate. Thus the thermal resistance can be calcu-
Upper plate (TU ) Guard heater
lated between the upper and lower surfaces. Giving the input value
of thickness and taking the known cross-sectional area, the ther-
Test sample mal conductivity of the samples can be calculated using Eq. (3).
Lower plate (Tm )
Heat flux transducer 3.4. Dry sliding wear test apparatus
Reference
Calorimeter To evaluate the performance of these composites under dry
(TL) sliding condition, wear tests are carried out in a pin-on-disc type
friction and wear monitoring test rig (supplied by DUCOM) as
Bottom heater per ASTM G 99. The schematic diagram of pin-on-disc set-up is
shown in Fig. 2. The counter body is a disc made of hardened
ground steel (EN-32, hardness 72 HRC, surface roughness
Heat sink
0.6 lRa). The specimen is held stationary and the disc is rotated
while a normal force is applied through a lever mechanism. A ser-
ies of test are conducted with three sliding velocities of 210, 261
and 314 cm/s under three different normal loading of 10 N, 20 N
Fig. 1. Schematic model showing the system arrangement in Unitherm 2022. and 30 N. The material loss from the composite surface is
840 A. Patnaik et al. / Materials and Design 31 (2010) 837–849
Taguchi design of experiment is a powerful analysis tool for where ‘n’ the number of observations, and y the observed data.
modeling and analyzing the influence of control factors on perfor- ‘‘Lower is better” (LB) characteristic, with the above S/N ratio trans-
mance output. The most important stage in the design of experi- formation, is suitable for minimizations of erosion rate. The stan-
ment lies in the selection of the control factors. Therefore, dard linear graph by Glen [10] as shown in Fig. 3, is used to
initially a large number of factors are included so that non-signif- assign the factors and interactions to various columns of the orthog-
icant variables can be identified at earliest opportunity. In the pres- onal array.
ent work, the impact of five such parameters are studied using L27 The plan of the experiments is as follows: the first column was
(313) orthogonal design. The operating conditions under which ero- assigned to sliding velocity (A), the second column to normal load
sion tests are carried out are given in Table 2. (B), the fifth column to filler content (C) and the ninth column to
Four parameters viz., sliding velocity, normal load, filler content sliding distance (D), the third and fourth column are assigned to
and sliding distance, each at three levels, are considered in this (A B)1 and (A B)2, respectively to estimate interaction between
study. Four parameters each at three levels would require 34 = 81 sliding velocity (A) and normal load (B), the sixth and seventh col-
runs in a full factorial experiment. Whereas, Taguchi’s factorial umn are assigned to (B C)1 and (B C)2, respectively, to estimate
experiment approach reduces it to 27 runs only offering a great interaction between the normal load (B) and filler content (C), the
advantage. eighth and eleventh column are assigned to (A C)1 and (A C)2,
The experimental observations are transformed into a signal-to- respectively, to estimate interaction between the sliding velocity
noise (S/N) ratio. There are several S/N ratios available depending (A) and filler content (C). The remaining columns are assigned to
on the type of characteristics. The S/N ratio for minimum erosion error columns, respectively.
rate coming under smaller is better characteristic, which can be
calculated as logarithmic transformation of the loss function as
shown below. 4. Experimental results and discussion
Table 3 0.45
Thermal conductivity values of different resins.
0.40
0.5 E-glass fiber (50 wt%) reinforced with epoxy resin composite is
manufactured in two different methodologies i.e. by hand-lay-up
0.4 technique and compression molding method. The thermal conduc-
tivity values are obtained by testing in through-the-thickness
0.3 direction as shown in Table 5. For glass/epoxy composites, manu-
facturing method has little effect on thermal conductivity. Experi-
0.2 mental results show that compression molding method samples
Neat Epoxy resin
have higher thermal conductivity than the hand-lay-up technique.
0.1 4wt% Aluminium filled composite
The potential cause for this variation in thermal conductivity might
8wt% Aluminium filled composite
0
be due to air voids. Two potential reasons are suggested for forma-
60 70 80 90 100 tion of air voids: (1) stitching closely packs the fabric layers, leav-
ing small air pockets between the layers, and applied resin might
Temperature (Degree-C)
not seep through the air gaps fully, these air pockets hinder full
Fig. 4a. Thermal conductivity variations with temperature of aluminium filled conductivity; and (2) during composite fabrication by hand-lay-
epoxy. up technique the formation of holes can not be neglected and
842 A. Patnaik et al. / Materials and Design 31 (2010) 837–849
Table 5
Thermal conductivity of E-glass fiber/epoxy resin composites.
Table 6 Table 7
Thermal conductivity of E-glass fiber/epoxy resin composites. Thermal conductivity of carbon fiber/epoxy resin composites.
Heat flow Thickness Thermal conductivity (W/m K) Heat flow Thickness Thermal conductivity (W/m K)
direction (mm) direction (mm)
Test-1 Test-2 Test-3 Test-1 Test-2 Test-3
(60 °C) (80 °C) (100 °C) (60 °C) (80 °C) (100 °C)
Transverse 3.228 0.279 0.297 0.334 Carbon fiber reinforced epoxy resin composite for 40% fiber loading
direction Through-the-thickness 3.772 0.245 0.262 0.283
Longitudinal 4.300 0.246 0.271 0.301 Transverse direction 4.325 0.457 0.500 0.541
direction Longitudinal direction 5.176 0.787 0.965 1.231
Through-the- 5.663 0.320 0.340 0.357
Carbon fiber reinforced epoxy resin composite for 60% fiber loading
thickness
Through-the-thickness 4.165 0.312 0.320 0.337
Transverse direction 5.179 0.429 0.447 0.463
Longitudinal direction 5.664 1.367 1.941 2.227
may even formation of a thin interfacial gap between the fiber and
resin due to inadequate interfacial compatibility acting like air void
and in turn reducing the thermal conductivity. These factors poten- isotropic; (3) thermal conductivity of carbon composites through-
tially change thermal conductivity by around ±0.05 W/m K. For all the-thickness direction is close to that of neat resin, indicating that
samples thermal conductivity increases slightly with increased in thermal property of the resin plays a major role in this direction;
test temperature. (4) carbon composites result in lower thermal conductivity values
in through-the-thickness direction than glass fiber composite. This
4.3. E-glass reinforced epoxy resin composite in all the three directions observation is in accordance with the results published in the liter-
ature [12] and (5) as shown in Table 7, through-the-thickness ther-
The thermal conductivity values of E-glass/epoxy resin compos- mal conductivity of carbon/epoxy resin composite for 40 wt% is
ite blocks in longitudinal, transverse and through-the-thickness consistent with that of carbon/epoxy resin composite for 60 wt%.
directions are listed in Table 6. It is observed that the thermal con- Carbon fiber is orthotropic in nature and the conductivity of the
ductivity in through-the-thickness direction is higher than that in carbon fiber along the axis would be higher than in other directions
the transverse direction, which in turn is higher than the conduc- because of the basal plane formation along the axis. These basal
tivity in longitudinal direction. The conductivity value is supposed planes are closely packed in the order of angstrom units, which
to be higher in longitudinal direction. However, in this case, bi-ax- helps in transferring heat quickly and by virtue of its property car-
ial fabric might have led to this anomaly. Further more, the sample bon fibers contracts upon heat due to negative expansion coeffi-
preparation also influences the results. After cutting the sample in cient further reducing the distance between the basal planes.
0 and 90 directions the fiber would be in the direction of heat flow Thus thermal conductivity increased linearly in longitudinal direc-
and these fibers form a corrugated shape on the top and bottom tion in the measured temperature range of 60–100 °C. In trans-
surfaces. According to the sample requirements of the test facility, verse direction, conductivity would be much lower than that of
these surfaces are supposed to be smooth with a tolerance of in longitudinal direction due to lack of basal planes. Moreover, car-
±0.005 inch, which is difficult to achieve with the available re- bon sheets would be sized to have good compatibility with the re-
sources. However, the thermal conductivity value of the E-glass/ sin, and this sizing causes an insulating layer and thus hinders heat
epoxy resin block showed no significant change with respect to flow in case of through-the-thickness direction. This glossy sizing
the direction of fiber. The fiber weight fraction for this block is over the carbon tow might be the reason for lower conductivity
determined as 49.8%. The low thermal conductivity of balanced of carbon composite in through-the-thickness direction than that
bi-axial E-glass fabric in 0 and 90 directions (i.e. in horizontal of a glass fiber composite. To test the effect of fiber weight fraction
plane) resulted in heat conduction to be nearly uniform in both of a composite on thermal conductivity, another carbon/epoxy re-
longitudinal and transverse directions. sin block was made with higher fiber compactness and tested. The
results are also included in Table 7. The results are compared
graphically in Fig. 5.
4.4. Carbon fiber reinforced epoxy resin composites
The thermal conductivity values of carbon fiber/epoxy resin 4.5. Natural fiber reinforced epoxy resin composites
composite materials in longitudinal, transverse and through-the-
thickness directions are listed in Table 7. The following observa- The thermal conductivity of natural fiber reinforced epoxy com-
tions are made from the test results of carbon fiber/epoxy resin posites have an extremely low thermal conductivity as shown in
composite material: (1) the thermal conductivities of carbon com- Table 8 and also shown in Fig. 6, much lower than neat epoxy,
posites are the highest along the fiber direction, medium in the demonstrating excellent thermal insulation characteristics. Thus
transverse direction and lowest in through-the- thickness direc- after studying all the three combinations i.e. glass fiber/epoxy re-
tion; (2) carbon composites have significantly different thermal sin, carbon fiber/epoxy and pine bark/epoxy resin composite, pine
conductivity values in three directions – strongly anisotropic. This bark reinforced epoxy resin composite shows excellent thermal
is distinctively different from E-glass composite materials for insulation characteristics as compared to other two combination
which thermal conductivities in three directions are close – almost of composites. Therefore, in this study pine bark and epoxy resin
A. Patnaik et al. / Materials and Design 31 (2010) 837–849 843
2.5
0.5
0
60 70 80 90 100
Temperature (Degree-C)
Fig. 5. Thermal conductivity variations for carbon fiber/epoxy resin composites.
0.3
Thermal conductivity (W /m-K )
0
60 70 80 90 100
Temperature (Degree-C)
Fig. 6. Thermal conductivity variations for natural fiber/epoxy resin composites.
844 A. Patnaik et al. / Materials and Design 31 (2010) 837–849
Table 9
Theoretical models for transverse/longitudinal effective thermal conductivity.
Table 10 Before any attempt is made to use this simple model as a predictor
Thermal conductivity of the samples using theoretical model. for the measures of performance, the possible interactions be-
tween the control factors must be considered. Thus factorial design
Composites Kf (along the Kf (along Km Vf (%) Vm (%)
axis of fiber) transverse incorporates a simple means of testing for the presence of the
direction) interaction effects.
E-glass fiber/epoxy resin 0.7 0.6 0.263 50 50 Analysis of the result leads to the conclusion that factor combi-
Carbon fiber/epoxy resin 8 0.54 0.263 50 50 nation of A3, B2, C1 and D3 gives minimum specific wear rate as
Pine bark/epoxy resin 0.3 0.36 0.263 50 50 shown in Fig. 7a and for minimum thermal conductivity the levels
CBPD/epoxy resin 0.74 0.63 0.263 7 93 of factor settings are shown in Fig. 7b such as A3, B3, C3 and D1. The
Pinebark/CBPD/epoxy resin 0.5 0.5 0.263 36.4 63.4
interaction graphs are shown in Fig. 8a and b for specific wear rate
Pinebark/CBPD/epoxy resin 0.5 0.5 0.263 26.1 73.9
and thermal conductivity, respectively.
control factors on specific wear rate and thermal conductivity of 4.8. Surface morphology
the particulate filled pine bark reinforced epoxy resin composites.
The analysis is made using the popular software specifically used The surfaces of the specimens are examined directly by scan-
for design of experiment applications known as MINITAB 15. ning electron microscope JEOL JSM-6480LV. Fig. 9 presents the
Table 11
Comparison between experimental values and theoretical values.
Method/model Manufacturing techniques Pine bark/epoxy resin composite Epoxy resin/CBPD composite Pine bark/CBPD/epoxy resin composite
Experimental Hand lay-up techniques 0.272 0.268 0.196
Inverse rule of mixture Hand lay-up techniques 0.281 0.293 –
Hamilton–Crosser formula Hand lay-up techniques – – 0.206
Error (%) 3.20% 10.23% 4.85%
Table 12
Experimental design using L27 orthogonal array.
Sl No. Sliding velocity, Normal load, Filler content, Sliding distance, Wear rate, S/N ratio (dB) Thermal conductivity, S/N ratio (dB)
A (cm/s) B (N) C (%) D (m) Ws (mm3/N m) K (W/m K)
1 210 10 0 3000 0.0006736 63.432 0.128 17.8558
2 210 10 4 4000 0.0005250 65.597 0.158 16.0269
3 210 10 8 5000 0.0000946 80.482 0.176 15.0897
4 210 20 0 4000 0.0000282 90.995 0.139 17.1397
5 210 20 4 5000 0.0001414 76.991 0.125 18.0618
6 210 20 8 3000 0.0002300 72.765 0.109 19.2515
7 210 30 0 5000 0.0002403 72.385 0.127 17.9239
8 210 30 4 3000 0.0000953 80.418 0.114 18.8619
9 210 30 8 4000 0.0001906 74.398 0.120 18.4164
10 261 10 0 4000 0.0000600 84.437 0.128 17.8558
11 261 10 4 5000 0.0000082 101.72 0.131 17.6546
12 261 10 8 3000 0.0002183 73.219 0.130 17.7211
13 261 20 0 5000 0.0000034 109.37 0.132 17.5885
14 261 20 4 3000 0.0000618 84.180 0.138 17.2024
15 261 20 8 4000 0.0002167 73.283 0.154 16.2496
16 261 30 0 3000 0.0000331 89.603 0.138 17.2024
17 261 30 4 4000 0.0000479 86.393 0.153 16.3062
18 261 30 8 5000 0.0002501 72.038 0.133 17.5230
19 314 10 0 5000 0.0000017 115.39 0.146 16.7129
20 314 10 4 3000 0.0001476 76.618 0.127 17.9239
21 314 10 8 4000 0.0002893 70.773 0.157 16.0820
22 314 20 0 3000 0.0000098 100.17 0.140 17.0774
23 314 20 4 4000 0.0000021 113.55 0.135 17.3933
24 314 20 8 5000 0.0004016 67.924 0.118 18.5624
25 314 30 0 4000 0.0000128 97.856 0.116 18.7108
26 314 30 4 5000 0.0000116 98.711 0.122 18.2728
27 314 30 8 3000 0.0002576 71.781 0.111 17.8558
A. Patnaik et al. / Materials and Design 31 (2010) 837–849 845
85
80
Mean of SN ratios
75
85
80
75
A B
18.00
17.75
17.50
17.25
Mean of SN ratios
17.00
210 261 314 10 20 30
C D
18.00
17.75
17.50
17.25
17.00
0 4 8 3000 4000 5000
scanning electron microscope of with and without particulate tomicrograph shown in Fig. 9c and d depict severe damage to the
filled pine bark–epoxy composite worn surfaces under various test matrix, more pine bark breakage and some of the pine bark are
conditions. To correlate the wear data better, SEM graphs pre- pulled-out from the matrix surface (Table 4, experiment no. 6).
sented in Fig. 9a and b to pertaining to a load of 10 N and at differ- The worn surface is deformed and the pine bark had been torn
ent sliding distances for Pine bark reinforced epoxy composites are from epoxy matrix when the load is 20 N in Fig. 9d.
considered. Fig. 9a shows the wear surfaces of unfilled composite From Fig. 9e shows the material is removed from the sample
at a load of 10 N, 3000 m sliding distance and Fig. 9b shows the mostly by the adhesion mode. It can be seen that there is a plastic
wear surface of unfilled composite of load 20 N, 4000 m sliding dis- flow of the matrix material in the sliding direction. It is under-
tance, respectively. The large patches formed on the worn surface standable that as the sliding proceeds, the resin soften due to fric-
of composite are consisted of fine worn particles of polymer matrix tional heat generation. As a result, the cement by-pass dust
and damage fibers accumulated together by the thermo-mechani- particles and the pine bark easily tear the matrix and gradually
cal processes at a load of 20 N. Meanwhile, the patches appeared get aligned along the sliding direction. These particles by virtue
on the rubbing surface are likely to shield the block from damage of their size, shape, brittleness and high hardness influence and
by the hard asperities on the counter face surface and are thus modify the wear behavior of the composites. Further, crack forma-
helpful in reducing wear. At higher sliding distance (3000 m), pho- tion and propagation can be seen Fig. 9f at the matrix fiber inter-
846 A. Patnaik et al. / Materials and Design 31 (2010) 837–849
90
85
80
75
70
18.0
SN ratios
17.5
17.0
16.5
16.0
210 261 314
A
Fig. 8b. Interaction graph between A B for thermal conductivity.
face, which also contribute to material loss over the test duration. From Table 13a, one can observe that the filler content
Extensive pine bark fragmentation indicated that the adhesive (p = 0.049), sliding velocity (p = 0.107) and sliding distance
strength between fiber, matrix and filler material became weak (p = 0.370) have great influence on specific wear rate. The interac-
while the high frictional heat accumulated in the contacting tion between sliding velocity filler content (p = 0.288) shows sig-
surface. nificance of contribution on the wear rate and the factor normal
load (p = 0.564) and sliding velocity normal load (p = 0.969)
4.9. ANOVA and the effects of factors and normal load filler content (p = 0.743) present less signifi-
cance of contribution on specific wear rate.
In order to understand a concrete visualization of impact of var- Similarly, From Table 13b, one can observe that the filler con-
ious factors and their interactions, it is desirable to develop analy- tent (p = 0.082), sliding distance (p = 0.135) and sliding distance
sis of variance (ANOVA) table to find out the order of significant (p = 0.433) have great influence on thermal conductivity. The inter-
factors as well as interactions. Tables 13a and 13b show the results action between sliding velocity filler content (p = 0.288) shows
of the ANOVA with the specific wear rate. This analysis was under- significance of contribution on the thermal conductivity and the
taken for a level of confidence of significance of 5%. The last column factor normal load (p = 0.564), sliding velocity normal load
of the table indicates that the main effects are highly significant (p = 0.969) and normal load filler content (p = 0.743) present less
(all have very small p-values) [14]. significance of contribution on thermal conductivity.
A. Patnaik et al. / Materials and Design 31 (2010) 837–849 847
Fig. 9. SEM micrographs of the worm pine bark-epoxy composites filled with cement by-pass dust.
Source DF Seq SS Adj SS Adj MS F P The confirmation experiment is the final test in the design of
experiment process. The purpose of the confirmation experiment
A 2 1084.3 1084.3 542.2 3.33 0.107
B 2 205.8 205.8 102.9 0.63 0.564 is to validate the conclusions drawn during the analysis phase.
C 2 1698.1 1698.1 849.1 5.21 0.049 The confirmation experiment is performed by conducting a new
D 2 384.7 384.7 192.4 1.18 0.370 set of factor settings A2C1D3 to predict the specific wear rate. The
AB 4 80.5 80.5 20.1 0.12 0.969 estimated S/N ratio for specific wear rate can be calculated with
AC 4 1044.6 1044.6 261.2 1.60 0.288
the help of following prediction equation:
BC 4 320.8 320.8 80.2 0.49 0.743
Error 6 977.9 977.9 163.0
Total 26 5796.8 g 1 ¼ T þ A2 T þ C 1 T
h i
þ A2 C 1 T A2 T C 1 T þ D3 T ð6Þ
g 2 ¼ A1 C 3 þ D3 T ð9Þ where f1 is the normalized function for specific wear rate, f2 is nor-
A new experimental set-up with factor levels at A1C3 and D3 is malized function for thermal conductivity, C is violation coefficient,
considered to predict the S/N ratio for thermal conductivity and K is a penalty parameter, usually the value is 10 and Z is the perfor-
is found to be g 2 ¼ 18:3418 dB. For each performance measure, mance output.
an experiment was conducted for a different factor combination Subjected to constraints:
and compared with the result obtained from the predictive equa- Amin 6 A 6 Amax ð15Þ
tion as shown in Tables 14a and 14b. The resulting model seems
C min 6 C 6 C max ð16Þ
to be capable of predicting specific wear rate and thermal conduc-
tivity to a reasonable accuracy. An error of 3.14% for the S/N ratio of Dmin 6 D 6 Dmax ð17Þ
specific wear rate and 3.72% for the S/N ratio thermal conductivity
where w1 and w2 are the weighting factors for normalized specific
is observed. However, the errors can be further reduced if the num-
wear rate and thermal conductivity functions used in the objective
ber of measurements is increased. This validates the development
function of optimization process. The weighting factors are selected
of the mathematical model for predicting the measures of perfor-
in such a manner that their sum is equal to one. A higher weighting
mance based on knowledge of the input parameters.
factor for an objective indicates more emphasis on it. The min and
max in Eqs. (15)–(17) represent lowest and highest control factor
6. Multi-objective optimization of control parameters settings, respectively (Table 2).
Genetic algorithm (GA) was used to obtain the optimum
Machining settings that satisfy multiple objectives of minimiza- machining parameters for multi-objective outputs by using the
tion of wear rate and minimization of thermal conductivity need to several combinations of the weight. The larger the weighting fac-
be determined. The mathematical model suggested here is in the tor, the greater the improvement in the machining performance
following form. outputs. The computational algorithm was implemented in C++
Table 15
Optimum operating conditions for multi-performance with different weighting factors.
code. Genetic algorithms (GAs) are mathematical optimization about 92% (for 4 wt% addition) and by about 97% (for 8 wt%
techniques that simulate a natural evolution process. They are addition).
based on the Darwinian theory, in which the fittest species sur- 2. The thermal conductivity along longitudinal direction in case of
vives and propagate while the less successful tend to disappear. carbon/epoxy resin composite is almost twice the conductivity
The concept of genetic algorithm is based on the evolution process in transverse and three times greater than through-the-thick-
and was introduced by Holland [15]. Genetic algorithm mainly de- ness direction. But in case of natural fiber reinforced epoxy
pends on the following types of operators: reproduction, crossover, composite there is no significant change in thermal conductiv-
and mutation. Reproduction is accomplished by copying the best ity values as compared to those in case of glass fiber/carbon
individuals from one generation to the next, in what is often called fiber reinforced epoxy composites.
an earliest strategy. The best solution is monotonically improving 3. Experimental results obtained from pine bark/Epoxy resin sam-
from one generation to the next. The selected parents are submit- ple in longitudinal and through-the-thickness direction are in
ted to the crossover operator to produce one or two children. The good agreement with the values obtained from theoretical
crossover is carried out with an assigned probability, which is gen- models. In longitudinal direction, rules of mixture showed an
erally rather high. If a number randomly sampled is inferior to the upper bound value and in through-the-thickness direction
probability, the crossover is performed. The genetic mutation inverse rule of mixture showed a lower bound experimental
introduces diversity in the population by an occasional random data.
replacement of the individuals. The mutation is performed based 4. SEM micrographs for pine bark reinforced epoxy composite
on an assigned probability. A random number is used to determine show fairly good bonding with the matrix. The addition of
if a new individual will be produced to substitute the one gener- cement by-pass dust in the pine bark-epoxy composite further
ated by crossover. The mutation procedure consists of replacing enhances the capability of material and improves the structural
one of the decision variable values of an individual, while keeping integrity of material under sliding wear condition.
the remaining variables unchanged. The replaced variable is ran-
domly chosen, and its new value is calculated by randomly sam-
pling within its specific range. A weighting factor is used to References
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