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CHAPTER 3

MATERIALS, PROCESSING AND EXPERIMENTATION

3.1 INTRODUCTION

This chapter deals with materials, testing equipments and

experimental methods implemented in the current study. The type of matrix,
reinforcement material and the fillers used for fabricating hybrid composites
has been discussed. The experiment details for (i) mechanical tests such as
hardness test, tensile test, flexural test and also dynamic mechanical analysis
test (ii) dry sliding wear tests and (iii) two-body and three-body abrasive
wear tests of unfilled and silane-treated SiC filled C-E hybrid composites are
discussed in the following sections.

3.2 MATERIALS

Composites are made of reinforcing fibers or fillers and matrix

materials. Matrix surrounds the fibers, acting as load transferring medium and
thus protecting those fibers against chemical and environmental attack. For
the present study, following materials have been considered for preparing
composites.1) Matrix material: Epoxy resin 2) Reinforcement material: Bi-
directional carbon fabric and 3) Filler material: Silane-treated SiC particulates.

3.2.1 Matrix Materials

Epoxy is the matrix materials used and it consists of medium

viscosity epoxy resin (LY 556) and HY 951 room temperature curing
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hardener along with diluent DY 02. All these materials are supplied by
Hindustan Ciba Giegy Ltd, Mumbai, India. The properties of the materials are
listed in Table 3.1. In general, the thermoset polymeric epoxy resin consists of
superior properties such as good mechanical properties, enhanced chemical
and corrosion resistance and ease of processing. Due to its wide applications,
epoxy resin was selected as the matrix material for the current study.

Table 3.1 The ingredients of matrix system

Trade Density
Ingredients Chemical name Supplier
name (g/cm3)
Epoxy LY 556 Diglycidal Ether of 1.16
Resin bisphenol A (DGEBA) Hindustan
Ciba Giegy
Hardener HY 951 Triethylenetetramine 0.95 Ltd
(TETA)

3.2.2 Fiber Materials

The bi-directional carbon fabric is considered as reinforcement

material in this study. The main properties of the carbon fibers are highlighted
in Table 3.2.

Table 3.2 Properties of carbon fibers

Properties Carbon (T300)

3
Specific gravity (g/cm ) 1.78-2.15
2
Fabric weight (g/m ) 300
Fiber diameter (µm) 8-10
Tensile strength (MPa) 3515-6380
Tensile modulus (GPa) 240-410
Strain to failure (%) 2.9
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3.2.3 Filler Materials

In the present study, silane-treated silicon carbide particulates have

been selected as a filler and second reinforcement material. The addition of
hard silane-treated SiC particles provides the improved strength, stiffness,
wear resistance, fatigue resistance, thermal conductivity and reduced thermal
expansion properties to composites. The physical and mechanical properties
of Silicon Carbide (SiC) are shown in Table 3.3.

Table 3.3 Physical and mechanical properties of used silicon carbide

(SiC) particles

Properties Value
Density 3.2 g/cm3
Particle size 5–10 µm
Shape Tetrahedral
Moh’s hardness 9.5
Filling mass 1250–1400 kg/m3
Thermal dissociation point 2300°C
Crystallographic lattice hexagonal Į and ȕ phase

3.3 PREPARATION OF THE COMPOSITES

3.3.1 Preparation of Composite Test Samples

A mould of size 550 mm×550 mm× 6 mm was prepared using mild

steel plates. Interior surfaces of the moulds were finely polished and chrome
plated. All the surfaces of the moulds were layered with Teflon sheet. The
part coming in contact with surface of the composite to be cast, were smeared
with a uniform layer of silicone releasing agent in order to facilitate the
release of the composite slab. The bi-directional carbon fabric (diameter 6–8 µm)
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reinforced with the LY556 Epoxy resin matrix materials, added with HY951
room temperature curing hardener and diluent DY021 (all supplied by
Hindustan Ciba Giegy) have been considered for panel fabrication. Ten layers
of fabric were used to obtain about 3 mm thick laminates. Particulate-filled
carbon fabric-reinforced epoxy composite was prepared by hand lay-up
procedure, followed by compression moulding. The filler material used is SiC
powder of size 5–10 µm. The SiC filler was treated with 2% organo-reactive
silane coupling agent.

3.3.2 Carbon Fabric and Particulate Reinforced Epoxy Composites

Carbon fabric (T-300), which is compatible with epoxy resin, has

been used as the reinforcement. The epoxy resin was mixed with the hardener
in the ratio 100:12 by weight. The dry hand lay-up technique as shown in
Figure 3.1 was used to fabricate the composite.

Figure 3.1 Hand lay-up technique setup

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The stacking procedure involved placing the fabric one above other
with the resin mix well spread between the fabrics. A porous Teflon film was
placed on the completed stack. To ensure uniform thickness of the sample, a
spacer of size 3 mm was used. The mould plates were coated with a release
agent in order to avoid damage to the solidified panel upon separation.

Figure 3.2 Compression moulding

The panel was prepared by hand lay-up technique and followed by

compression moulding as shown in Figure 3.2. The total assembly was kept in
a hydraulic press at a pressure of 0.5 MPa and was allowed to cure for a day
at room temperature. Subsequently, post curing was done at a temperature of
70 ± 5°C for 3 hours in a hot air circulated furnace. The panel thus prepared
has a size 500 mm × 500 mm × 3 mm. Figure 3.3 shows the flow chart of
processes involved in the composite preparation. To prepare the silane-treated
SiC filled C-E composites, silane-treated SiC filler was mixed with a known
amount of epoxy resin. The particulars of the composites made are shown in
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Table 3.4. The test samples as per ASTM standard were prepared from the
laminate using a diamond tipped cutter. Densities of the composites were
determined with the help of a high precision electronic balance (Make:
Mettler Toledo, Accuracy: 0.0001g) using Archimedes principle.

Bi-directional
Carbon fabric
Hand layup
technique Compression Curing Composite
technique molding laminate
Epoxy resin
+
Silane-treated
SiC particulates

Figure 3.3 Processes involved in the preparation of composite laminate

Table 3.4 Composites selected for the present study

Density
Material Matrix Filler
Fiber (wt.%) (g/cm3)
(Designation) (wt.%) (wt.%)
ASTM D792
Carbon-epoxy (C-E) Carbon Epoxy --- 1.42
(60±2) (40±2)
5% SiC filled carbon- Carbon Epoxy SiC (5) 1.48
epoxy (60±2) (35±2)
(5SiC-C-E)
10% SiC filled carbon- Carbon Epoxy SiC (10) 1.52
epoxy (60±2) (30±2)
(10SiC-C-E)

3.4 EXPERIMENTAL SETUP USED FOR MECHANICAL

TESTS

The mechanical tests involved in this present study are explained in

the following sections.
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3.4.1 Hardness test and Tensile test

The mechanical properties such as tensile and hardness properties

were investigated using Instron testing machine (ASTM D638) and
Durometer(ASTM D2240) respectively.

As per the ASTM D2240, Durometer (Hiroshima make Hardness

tester) was used to measure Shore hardness of the samples. On different
places of the samples, six readings were taken and the average value was
recorded for each materials.

Uniaxial tensile test was conducted using an Instron testing

machine according to ASTM D638. The tensile tests were performed at a
crosshead speed of 5 mm/min (quasistatic). Five samples were tested for each
composition of the composites. The results reported are thus the average of
five readings, and the relative deviations in mechanical properties were below
8%. Both the load and cross head displacements were recorded using a
software and a data acquisition computer. Mechanical properties such as
tensile strength, modulus and elongation were determined. The dimensions of
the test specimen as per ASTM D638, type M-I are listed below.

All dimensions are in mm

3.4.2 Flexural Test

Flexural test was conducted on an Instron universal testing machine

using centre-loading flexure fixture according to ASTM D790 standard three
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point bending method. The flexure tests were performed at crosshead speed of
2.4 mm/min. Five samples were tested for each composition of the
composites. The dimensions of the test specimen as per the ASTM D790 are
90 mm × 12.7 mm × 3 mm. Both the load and cross-head displacements were
recorded using software and a data acquisition computer.

3.5 EXPERIMENTAL SETUP USED FOR DRY SLIDING WEAR

TEST

A pin-on-disk setup (Make: DUCOM ASTM G-99 standard,

TR-20-M26 was used for the dry sliding wear tests and schematic diagram
and the photo graphic view of the same is shown in Figures 3.4 and 3.5
respectively.

Figure 3.4 Schematic diagram of the Pin-On-Disc wear test rig

indicating the various parts of the wear setup
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Figure 3.5 Photographic view of the Pin-On-Disc wear test rig

A surface (6 mm × 6 mm × 3 mm) of the composite specimen glued

to a pin of 6 mm diameter and 22 mm length has contact with a hardened
alloy steel disc with a hardness value of 62 HRC and surface roughness (Ra)
of 0.25–0.30 µm, as shown in Figure 3.6.

Figure 3.6 Composite sample with pin assembly and the steel
countersurface on which sliding takes place
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The summary of the experimental conditions used for this study are
listed in Table 3.5. The test samples were polished against a 600 grade SiC
paper to ensure proper contact with the countersurface. The surfaces of both
the samples and the disc were cleaned with a soft paper soaked in acetone and
thoroughly dried before the test. The pin assembly was initially weighed to an
accuracy of 0.0001 g in an electronic balance (Mettler Toledo). The difference
between the initial and final weights is the measure of the sliding wear loss.

In general, the sliding process can be divided into two stages

namely; a running-in stage and a steady wear stage. In most cases, the sliding
behavior in the steady stage is a matter of primary concern as it determines
the wear life and thus, the overall applicability of the component. Therefore,
in this study, the values of friction coefficient and weight loss refer to the
mean values in the steady stage. Also, each result is an average value from at
least three repeated tests. The results reported are thus the average of three
readings, and the relative deviation in wear loss was observed to be below
12%. The wear was measured by loss in weight, which was then converted
into wear volume using measured density data. The specific wear rate (ks) was
calculated through the following equation:

Ks
V
LuD
 m3 / Nm  (3.1)

where V is the volume loss (m3), L is the applied load (N) and D is the sliding
distance (m).
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Table 3.5 Details of the dry sliding wear conditions selected for this study

I-Group test for different loads &sliding distances

Sliding Sliding
Load Number of
Materials S.No velocity Distances
(N) tests
(m/s) (m)
1 25 2 1000
2 25 2 2000
3 25 2 3000
4 25 2 4000
C-E 5 25 2 5000
5 SiC-C-E
6 25 2 6000
10 SiC-C-E 42 number of
7 25 2 7000 tests
8 25 2 8000
9 25 2 5000
10 25 3 5000
11 50 2 5000
12 50 3 5000
13 75 2 5000
14 75 3 5000
II-Group test for different loads and sliding velocities
1 25 2 5000
2 25 3 5000
C-E 3 50 2 5000 18 number of
5 SiC-C-E tests
4 50 3 5000
10 SiC-C-E 5 75 2 5000
6 75 3 5000
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3.6 EXPERIMENTAL SETUP USED FOR ABRASIVE WEAR

TEST

3.6.1 Two-Body Abrasion

Two-body abrasive wear tests were performed using a Pin-on-disc

wear test rig according to ASTM-G 99 standards. Test samples were prepared
after proper cutting and polishing to 6mm x 6mm x 3mm size. Prior to testing,
the test samples were polished against a 600 grade SiC paper to ensure proper
contact with the countersurface. The composite sample was abraded against
the water silicon carbide (SiC) abrasive papers of 150 and 320 grit size at 10
and 20 N loads for abrading distances of 75,150 and 225 m in multi pass
condition. Figure 3.7 shows the photographic view of the two-body abrasive
wear process on Pin-on-Disc wear test rig. Figures 3.8 (a) and (b) shows the
SEM images of the abrasive particles embedded on the abrasive paper
(150 and 320 grit size) before the test. The embedded hard SiC particles
abrade the test samples.

During the test, the sample is so placed in such a way that the fibers
are parallel and anti-parallel with respect to abrading direction and the
abrading plane. The weight loss measurements were carried out for three
abrading distance of 75,150 and 225 m. Before and after the test, the test
samples were cleaned by soft paper immersed in acetone and thoroughly
dried. The weight loss of the sample was measured using the electronic
balance with the accuracy of 0.0001g (Mettler Toledo). The wear was
measured by the loss in weight, which was then converted in to wear volume
using the measured density data. The specific wear rate was calculated from
the Equation (3.1). The detail of testing conditions for this study is shown in
Table 3.6.
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Sample holder Sample

with Pin

Abrasive sheet with

rotating disc

Figure 3.7 Photographic view of the two-body abrasive wear process

a b

SiC particles SiC particles

(150 grit size) (320 grit size)

Figure 3.8 (a) 150 grit and (b) 320 grit SiC papers used before abrasion test

Table 3.6 The details of the two-body wear test conditions followed for
this study

Varying load Varying abrading

Conditions/experiments
conditions distance (m) conditions
Applied load (N) 10 and 20 75,150 and 225 m
Speed (RPM) 200 200
Abrasive paper 150 grit size 320 grit size
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3.6.2 Three-Body Abrasion

Three-body abrasive wear test was conducted using the ASTM

G-65 standard, rubber wheel abrasive wear tester (Magnum Engineers,
Bangalore). The schematic diagram and the photographic view of the rubber
wheel abrasive wear tester are shown in Figures 3.9 and 3.10 respectively.
The abrasive test samples as per the ASTM G65 of size 70 mm × 27 mm × 3
mm were also prepared from the plate using the diamond tipped cutter.
Details of the three-body wear test conditions employed for this study is
shown in Table 3.7.

Figure 3.9 Schematic diagram of three body rubber wheel abrasive

wear tester
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Figure 3.10 Photographic views of the rubber wheel abrasive wear tester
rig

For this test, AFS 60 grade silica sand have been used as abrasive
particles with sharp edges and angular in shape (200–250 µm) and its SEM
image as shown in Figure 3.11. The abrasive particles were fed in between the
contact surfaces of rotating wheel and the sample.

Figure 3.11 SEM image of the abrasive particles (Silica sand)

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Before the test, the samples were cleaned using acetone liquid and
dried; further, the initial weight of the samples was measured using a digital
electronic balance (Mettler, Toledo) with a high accuracy of 0.1 mg. The
samples were then fitted in the sample holder. The silica sand of AFS 60
grade was introduced between the sample and the rotating rubber wheel
(constant speed 200 rpm) prepared by chlorobutyl rubber tyre (hardness:
Durometer-A 58-62) with the feed rate of 255 ± 5 g/min. The load by the way
of lever arm exerts the force on the specimen holder and the specimen where
it is pressed against the rotating wheel while the controlled flow of the sand
particles abrades the sample surface.

The rotation of the abrasive rubber wheel rotates such that its
contacting surface rotates in the direction of the sand flow. The lever arm
which holds the sample at one end and carries the load at other end makes the
sample position approximately tangential to the outer diameter of the rubber
wheel and normal to the load applied. For each test condition, three tests were
performed and the average values obtained were recorded. The tests were
conducted for the abrading distances in the steps of 160, 320 and 480 m. The
tests were also repeated for two different loads (25 and 35 N). After the test,
the samples were again cleaned by acetone and dried. The final weight of the
samples was measured using a digital electronic balance. The differences
between the initial and final weights of the samples give the value of wear
loss. The wear loss obtained from the above method was converted to wear
volume loss using the measured density data of the samples. The specific
wear rate (Ks) was calculated using the Equation (3.1).
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Table 3.7 The details of three-body wear test conditions employed for
this study

S.No Parameters Details

1 Applied load (N) 25 and 35
2 Abrading distances (m) 160,320 and 480
3 Speed (RPM) 200

3.7 EXPERIMENTAL SETUP FOR DYNAMIC MECHANICAL

ANALYSIS

Dynamic Mechanical Analysis (DMA) was carried out as per the

standard ASTM D4065-01 using test setup DMA Q800 V 7.4 (TA
Instruments, USA). The schematic diagram of the DMA Q800 is shown in
Figure 3.12. DMA 800 is a controlled stress with combined motor and
transducer machine, in which motor applies force and displacement sensor
measures strain. The signals of force and amplitude were recorded by the
machine; the stiffness is obtained from force and amplitude. The storage
modulus is obtained using the stiffness data.

Figure 3.12 DMA Q800 instrument

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The DMA instrument was operated in the single cantilever clamp

mode which is used to test the SiC-filled and unfilled C–E samples. DMA
instrument operates at a frequency of 1 HZ and strain at an amplitude of 25
µm. The test was performed in the temperature range of 25°C to 250°C and
at a temperature ramp of 2°C per minute. From each material, three samples
with the size of 90 mm × 12 mm × 3 mm were prepared using the diamond
tipped cutter. The DMA test was conducted for all samples. Also, the storage
modulus and glass transition temperatures were recorded and revealed.

3.8 VISUAL MACRO OBSERVATION

Hardness, Tensile, flexural and impact tested samples were first

subject to observation using the regular photography technique. This method
came in handy during the characterization of failures, especially in tension
failed samples in different stages of crack propagation.

3.9 SCANNING ELECTRON MICROSCOPY

Wear characterization of the worn surfaces of unfilled C–E

composite and silane-treated SiC-filled C–E hybrid composites samples were
studied using the scanning electronic microscope (JEOL, model JSM 840A),
which is shown in Figure 3.13.

Figure 3.13 Scanning Electron Microscopy

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Before the examination, a thin gold film was coated on the worn
out surface by sputtering to get a conducting layer.

Figure 3.14 shows the experimental flow chart which lists all the
tests conducted to characterize the mechanical and tribological properties of
the composite.

Fabrication of composites
Mechanical
study Tribological study

Adhesive wear Abrasive wear

Mechanical Dynamic
properties mechanical
(hardness, tensile properties
and flexural Dry sliding
Two-body Three-body
strength) wear test
wear test wear test

Viscoelastic properties, Effect of load, Effect of applied load,

(glass transition sliding velocity, abrading distance,
temperature, storage sliding distance abrasive grit size and
modulus, loss modulus and filler wt. % filler wt. %
and tandelta)

Effect of applied load,

abrading distance and
filler wt. %
Fractographic
analysis Worn surface
using SEM morphology Worn surface
using SEM morphology
using SEM

Results and discussion

Conclusions

Figure 3.14 Experimental flow chart