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EXPERIMENTAL INVESTIGATION OF

MECHANICAL BEHAVIOUR OF PMMA BASED


COMPOSITES

A PROJECT REPORT

Submitted by
BALAKUMARAN J (412514114042)
RAJA G (412514114149)
SHYAM V S (412514114182)
SRIRAMA DURGESH M (412514114194)

in partial fulfillment for the award of the degree

of

BACHELOR OF ENGINEERING
in
MECHANICAL ENGINEERING

SRI SAIRAM ENGINEERING COLLEGE, CHENNAI 600 044


ANNA UNIVERSITY : CHENNAI 600 025

APRIL 2018

i
ANNA UNIVERSITY : CHENNAI 600 025

BONAFIDE CERTIFICATE

Certified that this project report titled “EXPERIMENTAL


INVESTIGATION OF MECHANICAL BEHAVIOUR OF PMMA BASED
COMPOSITES” is the bonafide work of

BALAKUMARAN J (412514114042)

RAJA G (412514114149)

SHYAM V S (412514114182)

SRIRAMA DURGESH M (412514114194)

who carried out the project work under my supervision.

SIGNATURE SIGNATURE
DR. A. RAJENDRA PRASAD MR. V. RAVI RAJ
HEAD OF THE DEPARTMENT SUPERVISOR
Assistant Professor
Department of Mechanical Engineering Department of Mechanical Engineering
Sri Sairam Engineering College Sri Sairam Engineering College
Chennai- 600 044 Chennai- 600 044

Submitted for University Project Examination held on ........................………….


at Sri Sairam Engineering College, Chennai-600 044.

INTERNAL EXAMINER EXTERNAL EXAMINER

ii
ACKNOWLEDGEMENT

We hereby acknowledge our sincere gratitude to our beloved chairman


THIRU. MJF. LN. LEO MUTHU for the blessing and provided us with large
facilities.

We are thankful to our beloved Chief Executive officer,


Mr. J. SAI PRAKASH for providing the opportunity to showcase our skills
and knowledge.

We express our heartfelt thanks to Dr. C.V. JAYAKUMAR, our


principal for giving us spontaneous and whole hearted support for completing
the project.

We are grateful to Dr. A. RAJENDRA PRASAD, Head of the


Department and Dean R&D for his encouragement and support, throughout the
project.

We are greatly indebted to Mr. M. SURESH, our project coordinator,


Professor, Department of Mechanical Engineering and Mr. V. RAVIRAJ, our
project guide, Assistant Professor, Department of Mechanical Engineering for
his valuable guidance and suggestions during the entire course of our project.

We owe our special gratitude to Mr. RAMAMORTHY, who constantly


lent his knowledge and experience in the field of Composites, which proved
vital for our project completion.

We wish to thank all the faculty members of Mechanical Engineering


Department for their continuous support and encouragement. We would also
like to thank all the non-Teaching staff members of our Department for
extending their support to us.

iii
ABSTRACT

With the increasing dependence on metals, it has become the need of the

situation to revert innovations on materials that are not on the verge of

annihilations. Metals have been proven earnest for their exceptional properties

of being lustrous, high density, high tensile strength, and high melting point and

also possessing good conductive properties. But they have their own downfalls,

from an engineering point of view. Despite the revolution in metallurgies, it is

indisputably corrosive, limiting its applications in diverse fields. Peeking to the

other spectrum, we have the polymers, revolutionizing material industries and

their reliance to metals. Polymers have princely properties that outstood in

materials paradigm. They are chemically resistant, acts as a good insulator and

they are light in weight. Garnishing our interest is the ability of the polymers to

form composites, as metals do (metal-metal matrix). To revoke the detrimental

properties, such as Low Density, eminent have come out with ideas of suffusing

abrasive materials resulting in improved mechanical strengths. Microscopic

investigation has ascertained the enhancements in the strength to weight ratio.

The focus of our present venture is to give comprehensive review of high

performance plastic materials and their applications. By reinforcing Silicon

Carbide with PMMA, mechanical properties of the materials get enhanced and

sustain intermittent loads.

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TABLE OF CONTENTS

CHAPTER NO. TITLE PAGE NO.

ABSTRACT iv

LIST OF FIGURES x

LIST OF TABLES xii

LIST OF ABBREVATIONS

1. INTRODUCTION 01
1.1 POLYMER MATRIX COMPOSITES 01
1.2 PROCESSING OF PMCs 01

1.3 PROCESSING PROCEDURES 02

1.3.1 Spray Techniques 02


1.3.2 Filament Winding 02

1.3.3 Pultrusion 05

1.3.4 Resin Transfer Moulding (RTM) 06

1.3.5 Fibre Placement systems 07


1.4 INTERFACES IN PMCs 09

1.4.1 Glass Fibre 09

1.4.2 Aramid Fibre 10

1.4.3 Polyethylene Fibre 11

v
1.5 PROPERTIES OF PMCs 11
1.5.1 Mechanical Behaviour 11

1.5.1.1 Environmental Effects 12

1.5.1.2 Frracture

1.5.2 Structural Defects in PMCs 13

1.6 APPLICATIONS 13

2. LITERATURE REVIEW 15

2.1 LITERATURE 15

2.1.1 Development Objectives 23

2.1.2 Reinforcementing composites 23


2.1.3 Manufacturing methods 24

2.2 SUMMARY 24

2.3 AIM OF THE PRESENT WORK 31

3. MATERIAL SELECTION 32

3.1 SELECTION OF CERAMICS 32

3.1.1 Silicon Carbide 34

3.1.2 Types of SiC 34

3.1.2.1 Natural Occurrence 35

3.1.3 Wide scale production 36

3.1.4 Manufacturing method 36

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3.1.5 Structure of SiC polytypes 38
3.1.6 Properties of SiC polytypes 39
3.2 SELECTION OF POLYMER 40

3.2.1 Comparison of PMMA 43

3.2.2 Poly(methyl methacrylate) 44

3.2.3 Advantages of PMMA 45

3.2.4 Synthesis of PMMA 45

3.2.4.1 Processing – Handling 45

3.2.5 Properties of PMMA 47

3.2.6 Modification of properties 48

4. FABRICATION OF LAMINATES 49

4.1 INJECTION MOULDING 49

4.1.1 Equipment Description 50

4.1.2 Injection Moulding process 51

4.1.3 Applications 51

4.1.4 Examples for Injection Moulding 51

4.2 COMPRESSION MOULDING 52

4.2.1 Materials used 54

4.2.2 Applications 55

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4.3 HAND LAY-UP 56

4.3.1 Mould 56

4.3.1.1 Film or Layer 56

4.3.1.2 Gel Coat 57

4.3.1.3 Surface Mat Layer 57

4.3.1.4 Laminates of GFRP 57


4.3.1.5 Resin Coat 57
4 .3.1.6 Surface Mat Layer 58

4.3.1.7 Lay-up of laminates 58

4.3.2 Preparation of Resin Mix

4.3.3 Colour Fibre Mat-prep 59


4.3.4 Lamination Procedure 60

4.3.5 Advantages of Hand Lay-up 60

4.3.6 Cutting of Plates 61

4.3.7 Water Jet Cutting 61

4.3.7.1 Operation 61

5. TESTING OF SPECIMEN 63
5.1 TESTS PERFORMED 63

5.1.1 Tensile Test 63

5.1.2 Purpose of Tensile Test 63

5.1.3 Bend Test 64

5.1.4 Purpose of Bend Test 64

5.1.5 Flexural Test 64

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5.1.6 Purpose of Flexural Test 64

5.1.7 Charpy Impact Test 65

5.1.8 Purpose of Impact test 65


5.2 ASME STANDARD SHAPE 65

5.2.1 Tensile Test specimen 65

5.2.2 Flexural Test specimen 66

5.2.3 Impact Test specimen 66

6. COST ANALYSIS 77

6.1 MATERIALS USED 77

6.2 COST ANALYSIS 78

6.2.1 Material Cost 78

6.2.2 Machining Cost 79

6.3 TOTAL COST 79

7. COROLLARIES PERTAINING TO 80
EXPERIMENT

8. CONCLUSION 81

REFERENCES 82

ix
LIST OF FIGURES

FIG. NO. TITLE PAGE NO.

SCHEMATIC OF A FILAMENT WINDING


1.1(a) 03
PROCESS

SCHEMATIC OF A FILAMENT WOUND


1.1(b) PRESSURE VESSEL WITH A LINER; HELICAL 03
AND HOOP

1.2(a) HAND LAY UP 04

1.2(b) SPRAY LAY UP 04

1.3 SCHEMATIC OF PULTRUSION PROCESS 06

SCHEMATIC OF FIBRE PLACEMENT


1.4 08
PROCESS

1.5 FUNCTION OF SILANE COUPLING AGENT 10

3.1 MOISSANITE SINGLE CRYSTAL 35

3.2 SYNTHETIC SiC CRYSTALS 37

3.3 SYNTHETIC SiC LELY CRYSTALS 37

3.4 STRUCTURE OF SiC POLYTYPES 38

COMPARISON OF PMMA OVER OTHER


3.5 43
POLYMERS

SKELETAL STRUCTURE OF METHYL


3.6 47
METHACRYLATE

4.1 INJECTION MOULDING MACHINE 49

x
4.2 INJECTION MOULD MAKING 49

DIAGRAMMATIC REPRESENTATION OF
4.3 52
COMPRESSION MOULDING MACHINE

4.4 COMPRESSION MOULDING CYCLE 53

4.5 COMPRESSION MOULDING MACHINE 55

4.6 HAND LAY-UP 56

4.7 WATER JET CUTTING 62

5.1 TENSILE TEST SPECIMEN 65

5.2 FLEXURAL TEST SPECIMEN 66

5.3 IMPACT TEST SPECIMEN 66

xi
LIST OF TABLES

TABLE TITLE PAGE NO.


NO.

3.1 PROPERTIES OF CERAMICS 34

3.2 PROPERIES OF MAJOR SiC POLYTYPES 39

6.1 MATERIALS USED 77

6.2 MATERIAL COST 78

6.3 MACHINING COST 79

xii
CHAPTER 1

INTRODUCTION

1.1 POLYMER MATRIX COMPOSITES

Polymer matrix composites (PMCs) have established themselves as engineering


structural materials, not just as laboratory curiosities or cheap stuff for making
chairs and tables. This came about not only because of the introduction of high-
performance fibres such as carbon, boron, and aramid, but also because of some
new and improved matrix materials. Nevertheless, glass fibre reinforced
polymers represent the largest class of PMCs. Carbon fibre reinforced PMCs are
perhaps the most important structural composites.

1.2 PROCESSING OF PMCs

Many techniques, originally developed for making glass fibre reinforced


polymer matrix composites can also be used with other fibres. Glass fibre
reinforced polymer composites represent the largest class of PMCs. Polymeric
matrix materials can be conveniently classified as thermosets and
thermoplastics. Recall that thermosets harden on curing.

Curing or cross linking occurs in thermosets by appropriate chemical agents


and/or application of heat and pressure. Conventionally, thermal energy (heating
to 200°C or above) is provided for this purpose. This process, however, brings
in the problems of thermal gradients, residual stresses, and long curing times.
Residual stresses can cause serious problems in non- symmetrical or very thick
PMC laminates, where they may be relieved by warping of the laminate, fibre
waviness, matrix micro cracking, and ply delamination. Electron beam curing
offers an alternative that avoids these problems. It is a non- thermal curing

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process that requires much shorter time cure cycles. Curing by electron beam
occurs by electron-initiated reactions at a selectable cure temperature.

1.3 PROCESSING PROCEDURES

There are many processing methods for composites with therrnoset matrix
materials including epoxy, unsaturated polyester, and vinyl ester.

1.3.1 Hand Lay-up and Spray Techniques

Hand Lay-up and spray techniques are perhaps the simplest polymer-processing
techniques. Fibres can be laid onto a mold by hand and the resin (unsaturated
polyester is one of the most common) is sprayed or brushed on. Frequently,
resin and fibres (chopped) are sprayed together onto the mold surface. In both
cases, the deposited layers are densified with roller. Figure 2.2 shows
schematics of these processes. Accelerators and catalysts are frequently used.
Curing may be done at room temperature or at a moderately high temperature in
an oven.

1.3.2 Filament Winding

Filament winding is another very versatile technique in which continuous tow


or roving is passed through a resin impregnation bath and wound over a
rotating or stationary mandrel. A roving consists of thousands of individual
filaments. Figure 1.1a shows a schematic of this process, while Figure 1.1b
shows a pressure vessel made by filament winding. The winding of roving can
be polar (hoop) or helical. In polar winding, the fibre tows do not cross over,
while in the helical they do. The fibres are, of course, laid on the mandrel in a
helical fashion in both polar and helical windings; the helix angle depends on
the shape of the object to be made. Successive layers are laid on at a constant
or varying angle until the desired thickness is attained. Curing of the
thermosetting resin is done at an elevated temperature and the mandrel is
removed. Very large cylindrical (e.g., pipes) and spherical (e.g., for chemical

2
storage) vessels are built by filament winding. Glass, carbon, and aramid fibres
are routinely used with epoxy, polyester, and vinyl ester resins for producing
filament wound shapes.

There are two types of filament winding processes: wet winding and prepreg
winding. In wet winding, low-viscosity resin is applied to the filaments during
the winding process. Polyesters and epoxies with viscosity less than 2 Pa 5
(2000 centipoise) are used in wet winding. In prepreg winding, a hot-melt or
solvent-dip process is used to preimpregnate the fibres. Rigid amines, novolacs,
polyimides, and higher-viscosity epoxies are generally used for this process. In
filament winding, the most probable void sites are roving cross-overs and
regions between layers with different fibre orientations.

Fig. 1.1(a) Schematic of a filament winding process.

Fig. 1.1( b) Schematic of a filament wound pressure vessel with a liner; helical
and hoop winding are shown.

3
Fig. 1.2( a) In Hand Lay-up, fibres are laid onto a mould by hand, and the
resin is sprayed or brushed on.

Fig. 1.2 ( b) In spray-up, resin and fibres (chopped) are sprayed together onto
the mould surface.

4
1.3.3 Pultrusion

In this process continuous sections of polymer matrix composites with fibres


oriented mainly axially are produced. Figure 1.3 shows a schematic of this
process. Continuous fibre tows come from various creels. Mat or biaxial fabric
may be added to these to provide some transverse strength. These are passed
through a resin bath containing a catalyst. After this, the resin-impregnated
fibres pass through a series of wipers to remove any excess polymer and then
through a collimator before entering the heated die. Athorough wet-out of the
rovings is very important. Stripped excess resin is recirculated to the resin bath.
The heated die has the shape of the finished component to be produced. The
resin is cured in the die and the composite is pulled out. At the end of the line
the part is cut by a flying saw to a fixed length. Typically, the process can
produce continuously at a rate of 10 to 200 cm/min. The exact Speed depends
on the resin type and the cross-sectional thickness of the part being produced.
Pultruded profiles as wide as 1.25 m with more than 60% fibre volume fraction
can be made routinely. The pultrusion process has a continuous Moulding cycle,
this requires that the fibre distribution be constant and that the cross-sectional
shapes not vary, i.e., no bends or tapers are allowed. Main advantages of the
process are low labor cost and product consistency. Shapes such as rods,
channels, and angle and flat stock are easily produced. Fibrous reinforcements
in different forms can be used. Roving, i.e., continuous, fibres are most
commonly used. Continuous strand mat consisting of continuous fibre lengths
with random orientation can also be used. They are used to obtain reinforcement
action in the transverse direction. Other forms of materials used include
chopped strand mat consisting of short (chopped) fibres that can be bonded or
stitched to a carrier material, commonly a unidirectional tape, and woven fabrics
and braided tapes. Common resins used in pultrusion are polyester, vinyl ester,
and epoxy.

5
Fig 1.3 Schematic of the Pultrusion Process

1.3.4 Resin Transfer Moulding (RTM)

This is a closed-mold, low-pressure process. A preform made of the desired


fibre (carbon, glass, or aramid) is placed inside a mold, and liquid resin such as
epoxy or polyester is injected into the mold by means of a pump.
Reinforcements can be stitched, but more commonly they are made into a
preform that maintains its shape during injection of the polymer matrix. The
resin is allowed to cure and form a solid composite. The polymer viscosity
should be low (<1 Pa 5) enough for the fibres to be wetted easily. Additives to
enhance the surface finish, flame retardancy, weather resistance, curing speed,
etc. may be added to the resin. Thermoplastics have too high a melting point
and too high viscosities (>l Pa 5 or 1000 cp) to be processed with RTM. Among
the advantages of RTM, one can cite the following:

 Large, complex shapes can be obtained.


 The level of automation is higher than in other processes.
 Lay-up is simpler than in manual operations.
 Complex shapes and curvatures can be made easily.
 It take less time to produce.

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 With the aid of woven, stitched, or braided preforms, fibre volume
fractions as high as 60% can be achieved.
 The process involves a closed mold; therefore styrene emissions can be
reduced to a minimum.

Mold design is a critical element in the RTM process. Generally, the fibrous
preform is preheated and the mold has built-in heating elements to accelerate
the process of the resin. Resin flow into the mold and the heat transfer are
analyzed numerically to obtain an optimal mold design. The automotive
industry has found that the RTM can be a cost-effective, high-volume process
for large-scale processing.

1.3.5 Fibre Placement Systems

Automation can result in large productivity gains alternatively to manual


operations. A completely automated process, with no human being involved,
has a great attraction for use in radioactive or clean environments. In the area of
fabrication of composites this has led to processing techniques such as
automatic tape-laying. Another significant advantage is that rather large
structures can be made by this process. The Hand Lay-up process is limited by
the extent of a worker’s reach. Such a restriction would be absent in any
automatic process. The principle of operation is as follows. The customer's
computer aided design (CAD) is the starting point. Using the CAD system, the
product or component to be manufactured, for example, a curved part, is
developed mathematically onto a flat surface. This is broken down into layers to
be fabricated by tape strips laid side by side. Sophisticated software is used to
translate strips in each layer via a series of numerical control steps to the final
product shape. A spool of fibre tape, preimpregnated with a thermosetting resin
and covered with a protective paper on top and protective film underneath, is
unwound. The film and paper are peeled off, and the fibre tape, suspended in

7
midair, is cut to the correct shape by cutting blades. The cutting blades can
make 6000 cuts per minute. The cut pieces of tape are caught between two new
rolls of paper and film and rewound onto a new spool, called a cassette. The
cassette is then taken to the second machine for lay-up. A laser beam in the
tape-laying head is used to accurately lay the tape on the mold.

In fibre placement techniques, individual prepreg tows from spools are fed into
the fibre placement head, where they are collimated into a single fibre band and
laminated onto the work surface. Each tow is about a 3-mm-wide strand of
continuous fibres. A strand, in turn, consists of 12,000 individual filaments
impregnated with an epoxy resin. Different tows can be delivered at different
speeds, allowing a conformation of a complex structure. A compaction roller or
shoe consolidates the tape, pressing it onto the work surface. This pressing
action serves to remove any trapped air and any minor gaps between individual
tows. Figure 1.4 shows a schematic of the fibre placement process.

Fig 1.4 Schematic of the Fibre Placement Process

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1.4 INTERFACES IN PMCs
Below are the summary of some important features of the interface region in
PMCs with glass, aramid, and polyethylene fibres.

1.4.1 Glass Fibre

Silica-based glasses are analogous to many organic polymers, in that they are
amorphous. Crystalline silica melts at 1800°C and can be worked in the range of
1600-1800 °C. However, by adding some metal oxides, one can break the Si-O
bonds and obtain a series of amorphous glasses with low glass transition
temperatures so that they can be processed at much lower temperatures than
pure silica. In general, the atomic or molecular arrangement in any material is
different at the surface than in the interior. In particular, in the case of silica-
based glasses containing a variety of oxides, a complex hydroxyl layer is
formed rather easily. Non hygroscopic oxides absorb water as hydroxyl groups
while hygroscopic oxides become hydrated. The activity of a glass surface is
thus a function of the hydroxyl content and the cations just below the surface.
That is, the surface activity of E-glass will be different from that of fused silica.
Invariably, glass fibres are surface treated by applying a size on the freshly
drawn glass fibres to protect them from the environment, for handling ease, and
to avoid introducing surface defects. Common sizes are starch gum,
hydrogenated vegetable oil, gelatin, polyvinyl alcohol (PVA), and a variety of
nonionic emulsifiers. The size is generally incompatible with the matrix resin
and is therefore removed before putting the glass fibres in a resin matrix by heat
cleaning at ~ 350°C for 15 to 20 hours in air, followed by washing with
detergent or solvent and drying. After cleaning, organometallic or organosilane
coupling agents are applied; an aqueous solution of silane is commonly used for
this purpose. Examples of coupling agents commonly used are organometallic
or organosilane complexes. During the drying of sized glass fibres, water is

9
removed and a condensation reaction occurs between silanol and the glass
surface and between adjacent silanol molecules on the glass surface, leading to a
polysiloxane layer bonded to the glass surface.

Fig 1.5 Function of a Silane Coupling Agent

1.4.2 Aramid Fibre/Polymer Interface

Most polymers show rather poor adhesion to aramid fibres. This is evidenced by
the generally poor interlaminar shear strength and transverse tensile strength
values obtained with aramid reinforced PMCs. Typically, aramid/epoxy
interfacial strengths are about half of the interfacial strengths of glass/epoxy or
carbon/epoxy composites. A highly oriented chain micro-structure and skin/core
heterogeneity are responsible for this low, poor interfacial strength. This may
not be a disadvantage in aramid/polymer composites used to make impact-
resistant items such as helmets or body armor, where ease of delamination may
be an advantage. However, in high-strength and high-stiffness composites, poor
interfacial adhesion can be a disadvantage. Various fibre surface treatments
have been tried to alleviate this problem.

10
1.4.3 Polyethylene Fibre/Polymer Interface

Ultra-high-molecular-weight polyethylene (UHMWPE) fibre is another


chemically very inert fibre, and therefore it does not adhere very well to
polymeric matrix materials. High-modulus polyethylene fibres such as Spectra
or Dyneema are hard to bond with any polymeric matrix. Some kind of surface
treatment must be given to the polyethylene fibre to bond with resins such as
epoxy, PMMA. By far the most successful surface treatment involves a cold gas
(such as air, ammonia, or argon) plasma. When the polyethylene, or any other
fibre, is treated with plasma, surface modification occurs by removal of any
surface contaminants and highly oriented surface layers, addition of polar and
functional groups on the surface, and introduction of surface roughness, all
these factors contribute to an enhanced fibre/matrix interfacial strength. An
exposure of just a few minutes to the plasma is sufficient to do the job.

Chemical treatment with chromic acid and plasma etching in the presence of
oxygen are two treatments that are commonly used to modify the surface
characteristics of polyethelene fibre with a view to improve their adhesion to
polymeric matrix materials.

1.5 STRUCTURAL PROPERTIES OF PMCs

The properties of a composite will depend on the matrix type, fibre type,
amount or volume fraction of matrix (or that of the fibre), fabrication process,
and the orientation

1.5.1 Mechanical Behaviour

Most thermoset matrix composites show elastic behavior right up to fracture,


i.e., there is no yield point or plasticity. The strain-to-failure values are rather
low, typically, less than 0.5%. Consequently, the work done during fracture is

11
also small. Aramid fibre has superior impact characteristics; therefore, aramid
fibre-based polymer composites will show better ballistic resistance against
impact resistance in general. Similar observations can be made regarding
strength characteristics of the polymer matrix composites. High damping or the
ability to reduce vibrations can be very important in many applications.

1.5.1.1 Environmental Effects

Environmental moisture can penetrate organic materials by a diffusion process.


Typically, moisture works as a plasticizer for a polymer, i.e., properties such as
stillness, strength, and glass transition temperature decrease with the ingress of
moisture in a polymer. It is now well recognized that the problem of moisture
absorption in polymer matrix composites is a very important one. The epoxy
resins commonly employed as matrices in the composites meant for use in the
aerospace industry are fairly impervious to the range of fluids commonly
encountered.

There are, however, two fundamental effects that must be taken into account
when designing components made of PMCs, namely, temperature and humidity.
The combined effect of these two, that is, hygrothermal effects, can result in a
considerable degradation in the mechanical characteristics of the PMCs.
Degradation owing to ultraviolet radiation is another important environmental
effect breaking the covalent bonds in organic polymers results in a slight
increase in strength, followed by a gradual loss of strength due to laminate
surface degradation.

1.5.1.2 Fracture

At low temperatures, the fracture of a PMC involves a brittle failure of the


polymeric matrix accompanied by pull-out of the fibres transverse to the crack
plane. At room temperature, the same polymeric matrix (PET) deforms locally
in a plastic manner.

12
Generally, stiffness and strength of a PMC increase with the amount of stiff and
strong matrix introduced in a polymer. The same cannot be said unequivocally
for the fracture toughness. The toughness of the matrix and several micro
structural factors related to the fibres and the fibre/matrix interface have a
strong influence on the fracture toughness of the composite.

1.5.2 Structural Defects in PMCs

The final stage in any PMC fabrication is called debulking, which serves to
reduce the number of voids. Nevertheless, there are some common structural
defects in PMCs. Following is a list of these:

1. Resin-rich (fibre-poor) regions.


2. Voids (e.g., at roving crossovers in filament winding and between
layershaving different fibre orientations, in general). This is a very
serious problem; a low void content is necessary for improved
interlaminar shear strength.
3. Microcracks and Variations in fibre alignment.
4. Debonded and delaminated regions.

1.6 APPLICATIONS
PMMA is an economical, versatile general purpose material. Various types of
acrylics are used in a wide variety of fields and applications, including:

1. Optics: Dust covers for Hi-fi equipment, sunglasses, watch glasses,


lenses, magnifying glasses;

2. Vehicles: Rear lights, indicators, tachometer covers, warning


triangles;

3. Electrical engineering: Lamp covers, switch parts, dials, control


buttons;

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4. Office equipment: Writing and drawing instruments, pens;

5. Medicine: Packaging for tablets, pills, capsules, suppositories, urine


containers, sterilisable equipment;

6. Others: Leaflet dispensers, shatter‐resistant glazing, shower cubicles,


transparent pipelines, illuminated signs, toys.

14
CHAPTER 2

LITERATURE REVIEW

2.1 LITERATURE :

This chapter covers the literature review of results obtained from Experimental
Investigation of mechanical behaviour of Poly Methyl methacrylate (PMMA)
based polymer composites with Silicon Carbide (SiC). Apart from the polymer
composite, reinforcement used, manufacturing methods, this survey includes the
developments in the mechanical behaviour of polymer based composites at
different compositions of SiC reinforcements.

Polymer-based composites, especially PMMA-based composites, have gained


substantial attentions as a new branch of materials due to their superb
mechanical properties, high durability, impact resistance and light weight since
firstly heralded in the 1960s. A series of potential applications in magneto-
electric, biomedical, chemical engineering, automobile and optical field can be
realized through appropriate tailoring. It is well recognized that the type of
polymer matrix and its properties have a great influence on the performance of
composites. However, the composites must withstand high mechanical loads in
various conditions, so it is necessary to enhance mechanical properties using
reinforced materials for special applications, such as in military and aerospace
industry. In general, addition of rigid particles or fibres in polymer matrix can
produce a number of desirable effects, such as increased stiffness, reduced
coefficient of thermal expansion, improved creep resistance and enhanced
fracture toughness. Previous studies have shown that inorganic materials
including nano-zinc oxide, nanosilica, carbon nanotube (CNT), graphene,
aluminum trihydroxide (ATH) have been successfully employed as enhancing
materials in the synthesis of polymer-based composites.

15
Chao Shi et.al (2013) discussed about the synthesis of a polymer based
composite with an inorganic reinforcement with the help of free radical
polymerization in batch technique. -Si3N4 fibres, PMMA were selected as the
inorganic reinforcement constitution and polymer matrix, respectively. Free
radical polymerization in batch was the main method to synthesis composite by
utilizing azodiisobutyronitrile (AIBN) as the initiator, with the advantages of
simple productive process, free of post-process and high purity. Before that,
Si3N4 fibres were modified with g-methacryloxypropyltrimethoxysilane (g-
MPS) to ensure the uniformly distribution in the PMMA matrix. The influence
of surface modification on the molecular level and mechanical properties was
investigated through FTIR, TG-DSC and nano indentation. The results showed
that silane coupling agent facilitated the linkage between Si3N4 fibres and
PMMA matrix, with an obviously increase of elastic modulus and micro-
hardness.

Diwakar Padalia et.al (2013), discussed about the fabrication and


characterization of Cerium doped Barium Titanate / PMMA nano composites as
a kind of suitable materials for integral thin film capacitors and electric stress
control devices. BaTiO3 system by cerium doping was tailored to achieve low
loss and fine grains. On the other hand, the insulating PMMA shell around the
BaTiO3 nano particles could retard the movement of charge carriers in the nano
composites and thus has the potential to surpass conventional composites to
produce low dielectric loss. Different polymer nano composites were made by
solvent evaporation method while cerium doped BaTiO 3 nano fillers were
obtained via solid state reaction. In all polymer nano composites the filling level
was 30% w/w and all of them were treated by micro waves (2.4 GHz). The
results show that the thermal and dielectric behavior of the resulting nano
composites can be improved by varying the Ce-doping in BaTiO3 nano filler.

16
The effect of microwave heating on thermal stability of polymer nanocomposite
was also been studied.

Leslie Banks-Sills et.al (2016), studied about the Experimental determination of


mechanical properties of PMMA reinforced with functionalized Carbon
nanotubes (CNTs). Carbon nanotubes (CNTs) are one of the strongest materials
known to man. This material is a carbon allotrope like graphite, diamond and
fullerene. Early references to carbon structures date back to the 1970s; but it
was not until the discovery of CNTs in and the investigations that followed in
the early 1990s that carbon nanotubes were produced and their potential was
understood. Unfortunately, although CNTs possess excellent mechanical,
thermal and electrical properties, they usually cannot be used by themselves.
Nevertheless, CNTs have the potential to be used in composites of different
matrices. The goal of this investigation is to determine the mechanical
properties of a PMMA matrix reinforced with functionalized CNTs and to
compare the results obtained with the same material containing CNTs which
were not functionalized. The CNTs were functionalized by two methods. Hence,
the determined mechanical properties are also compared for the two
functionalization methods. The evaluation of the mechanical properties was
determined by means of tensile tests conducted on dog-bone specimens. The
composite material was manufactured using a twin screw extruder. The
specimens were produced by means of an injection Moulding (IM) procedure.

Tetsuya Yamamoto et.al (2017), in his study, came up with a conclusion to


improve mechanical properties of adsorbed particulate PMMA by Dispersion,
diffusion and surface adhesion of recycled carbon fibre fillers from CFRP.
Carbon fibre reinforced plastics (CFRP) are light, strong, and one of the most
well-known composite materials used in industrial fields, especially the space
industry. composite materials were fabricated using the thermoplastic resin
poly(methyl methacrylate) (PMMA) and recycled carbon fibres obtained by

17
pulverizing carbon fibre reinforced plastics (CFRP). PMMA particles were
adsorbed on the carbon fibre surfaces via electrostatic interactions, to promote
the interfacial adhesion between the carbon fibres and the PMMA resin and
thereby improve the dispersion of the fibres in the resin. This enhanced the
mechanical properties of the composites; the yield stress and elastic modulus of
the composite.

Prashant Jindal et.al (2015), did an extensive study on Mechanical


characterization of PMMA/MWCNT composites under static and dynamic
loading conditions. PMMA is a light weight mouldable polymer which is
widely used for several engineering applications. However, its usage in
applications gets restricted due to its low mechanical strength especially when
exposed to heavy external static and dynamic loading. Therefore, in order to
enhance the strength of PMMA, composites with stronger filler materials can be
fabricated and characterized. MWCNTs are such filler materials which possess
unique structural and mechanical properties. Therefore, changes in the static and
dynamic mechanical properties (elastic modulus and hardness) were
investigated for various compositions of as synthesized/untreated MWCNTs in
PMMA by employing nano indentation techniques without any additional
component or surface modification in the composite fabrication.

He Runqin et.al (2017), investigated the effect of TiO 2 fillers on the mechanical
properties of CNT/PMMA composites. Different types of polymers show
different mechanical behaviour. However, neat polymer is very rarely used as
bearing materials and wear resistant materials because of unmodified polymer
could not satisfy the demands arising from the situations where in a
combination of good mechanical properties is required. The bidirectional fabric
reinforcement offered a unique solution to the ever-increasing demands on the
advanced materials in terms of better performance and ease in processing.

18
Eduard A. Stefanescu et.al (2011), investigated the Fibreglass-reinforced
polymer composites for potential use as structural dielectrics in multifunctional
capacitors that require simultaneous excellent mechanical properties and good
energy storage characteristics. In recent years substantial efforts have been
dedicated to finding new alternatives for performance, weight and volume
improvements in batteries and capacitors. While commercial ceramic capacitors
are typically employed where small sizes along with high capacitances and
insulation resistances are required, they are not intended for precision
applications due to high variations in the capacitance with temperature. In
contrast, polymer film capacitors are predominantly used in applications
requiring low dielectric absorption and loss factors over a wide temperature
range. However, polymer film capacitors are characterized by smaller
capacitances due to their lower dielectric constants compared to the ceramic
counterparts. PMMA-fibreglass structural dielectrics containing neat or
PEDOT:PSS-coated BaTiO3 particles was focused, for potential use in
multifunctional capacitors that require superior stiffness and energy storage
characteristics. The multifunctional capacitors could be potentially employed as
substitutes for static load-carrying components in traditional structures (e.g.,
hybrid vehicles or airplanes) with the purpose of reducing the overall system
weight and/or volume.

Garima Mittal et.al (2016), came out with a research study of processing
PMMA/polyimide (PI)/hexagonal boron nitride (hBN) composites by
incorporating PI and hBN powder into the PMMA matrix. Hexagonal boron
nitride (hBN), also known as white graphite, is a layered ceramic compound
that is an isoelectric analog to graphite, with an identical hexagonal lattice
structure. Due to its very close similarity with graphite, it shows remarkable
thermal and chemical stability along with the same favorable mechanical
properties that facilitate applications in high temperature equipment. Among all

19
the boron nitrides, the hexagonal form is the most stable and is soft enough to
be used in lubrication. PMMA/PI polymer composites reinforced with silane-
functionalized hBN powder possesses a special position because of very good
environmental stability like, moisture resistance, UV resistance, scratch
resistance etc. Along with these PMMA possesses good mechanical properties,
optical clarity, low friction coefficient. Polyimide (PI) is considered as high
performance thermoplastic material because it owns unique structure due to the
formation of charge transferring complex within the molecules that gives rise to
ordered intermolecular stacking. Consequently, it displays outstanding thermal
and mechanical properties along with the good chemical and radiation
resistance and electronic properties.

H. Varela-Rizo et.al (2011), studied the effect of different functional groups and
processing techniques in the properties of CNF/poly(methyl methacrylate)
(CNF/PMMA) composites. Carbon nanofibres (CNFs) emerged as an
economical alternative to carbon nanotubes (CNTs) with similar characteristics:
high aspect ratio and combination of unique mechanical and electrical
properties. Therefore, all these carbon nanofilaments have been considered for
enhancing polymer properties in nanocomposites, providing conductivity and
reinforcement. Modification of CNF and CNT surface through functionalization
has been a common way of improving dispersion and providing effective
compatibility with the matrix. Melt-compounding, solvent casting and in situ
polymerization in PMMA composites containing pristine, carboxylated and
amino-functionalized CNFs were compared. Mechanical properties and
rheological behavior of the composites revealed a strong filler–polymer
interface interaction in the in situ polymerized composites, even through
covalent binding.

Jialiang Wang et.al (2012), investigated about the Solvent exfoliated graphene
for reinforcement of PMMA composites prepared by in situ polymerization.

20
Graphene (GP), a two-dimensional platelet consisting of sp2-hybridized carbon
atoms arranged in a perfect honeycomb lattice, has triggered enormous research
interest in both fundamental and applied science communities. Due to its
excellent electrical, thermal and mechanical properties, GP has great potential in
applications of sensors, super capacitors, thin conductive films, rechargeable
lithium ion batteries, and polymer composites. Graphene (GP)-based polymer
nano composites have attracted considerable scientific attention due to its
pronounced improvement in mechanical, thermal and electrical properties
compared with pure polymers. to direct exfoliation of graphite in NMP and
covalently functionalizing GP with PMMA (GPMMA) via in- situ free radical
polymerization, and the density of grafted PMMA can be tuned by changing the
feed ratio of GP and methyl meth-acrylate (MMA). GPMMA is of high-quality
with few defects since it is absent from violent and complicated modification
(compared with GO or CMG), and such a perfect structure renders GPMMA an
outstanding reinforcing agent. Additionally, after grafting with PMMA chains,
the functionalized GP is soluble in various solvents (such as NMP, THF and
DMF) and remains stable for a long period of time (over one month), which
also facilitates preparing different kinds of composites.

Jun-long Wang et.al (2009) et.al, did a study on SiO 2/PMMA/CE tri-component
interpenetrating polymer network composites. The interpenetrating polymer
network (IPN) is a unique polymer blend that is formed by two or more
crosslinked polymers through interpenetrating and winding. It is disordered
crosslinked networks in which at least one polymer network forms crosslinked
framework after another has already been formed. IPN is actually a concrete
structure form of macromolecule alloy metals or a special combination mode
among different polymers. CE was modified by CTC-IPN and interface
conjugated interpenetration. A conjugated tri-component penetrating polymer
composite was prepared, in which CE was used as the public network and it was

21
interpenetrated and winded with PMMA and nanometer SiO 2 one another. The
microstructure of the composite was characterized by infrared spectroscopy (IR)
and transmission electron microscopy (TEM). The mechanical properties were
measured in German-made DL-1000B and XCL-40 universal material test
machines, respectively.

A. Akinci et.al (2013), realized the friction and wear performance of pure poly
(methyl methacrylate) (PMMA) and zirconium oxide (ZrO 2) filled PMMA
composites under dry sliding conditions. PMMA resin exhibits better impact
and mechanical and physical properties than other polymer materials. However,
the material possesses poor mechanical and physical properties when used
alone, where it is easily broken into parts during an accident, or when a patient
applies high mastication force on the denture base. Zirconium dioxide possesses
excellent properties like: high strength, high fracture toughness, excellent wear
resistance, high hardness, and excellent chemical resistance. Hence, ZrO 2-
nanoparticles appear as an attractive option to be used as reinforcement of
polymers, in order to produce composites with enhanced performance.

Poomali et.al (2008), worked on mechanical and three-body wear behaviour of


PMMA/TPU blends. Polymers are extensively used in tribological components
such as gears, cams, wheels, brakes, seals, and bushings because of their self-
lubricating properties, lower coefficient of friction and better wear resistance.
However, neat polymer is very rarely used as bearing materials and wear-
resistant materials because of unmodified polymer could not satisfy the
demands arising from the situations wherein a combination of good mechanical
and tribological properties is required. They attempted to understand the three-
body abrasive wear behaviour of PMMA/TPU blends at 22 N load and for four
different abrading distances at 200 rpm.

22
2.1.1 Development Objectives

The development objectives for polymer composite materials are:

• Increase in yield strength and tensile strength at room temperature

• Increase in fatigue strength, especially at higher temperatures

• Improvement of thermal shock resistance

• Improvement of corrosion resistance

• Increase in Young’s modulus

An improvement in the weight specific properties can result, offering the


possibilities of extending the application area, substitution of common materials
and optimisation of component properties. With functional materials there is
another objective, the precondition of maintaining the appropriate function of
the material.

For other applications different development objectives are given, which differ
from those mentioned before. For example, in medical technology, mechanical
properties, like extreme corrosion resistance and low degradation as well as
biocompatibility are expected. Although increasing development activities have
led to system solutions using composite materials, the use of especially
innovative systems, particularly in the area of polymers, has not been realised.
The reason for this is insufficient process stability and reliability, combined
with production and processing problems and inadequate economic efficiency.

2.1.2 Reinforcements used

Generally, the following are the requirements for reinforcement: low density,
compatibility with polymer composite, chemical compatibility, thermal
stability, high compression and tensile strength, economic efficiency. Most of
the previous work is focused on nano-zinc oxide, nanosilica, carbon nanotube

23
(CNT), graphene, aluminum trihydroxide (ATH). Silicon Carbide (SiC) can be
used as reinforcement due to Low Density, High Strength, Low thermal
expansion, High thermal conductivity, low reactivity as well as the robustness
that make this possible to be used in structural applications. Silicon Carbide also
cost effective compared to other reinforcements like Boron Carbide and the
result being a reasonably priced final product.

2.1.3 Manufacturing methods

Two common methods for Polymer Composite manufacture Twin screw


Injection moulding and Compression moulding. Twin screw Injection moulding
and Hand Lay-up methods were the most preferred methods for production of
PMMA based polymer composites with ceramic reinforcement. However,
literature has shown that several modifications are possible in the melting and
casting practice in order to produce high-quality castings from a composite.

2.2 LITERATURE SUMMARY

A detailed literature survey was undertaken on polymer composites with


emphasis on reinforcements, process, characterization and correlation between
the microstructure and the properties like hardness, tensile strength properties as
well as statistical modeling studies. Based on the literature survey, the following
areas have been identified for further research.

PMMA-SiC alloy is not yet to be tried as polymer composite material. This one
is easy to fabricate by means of Injection moulding or Hand Layup process due
to it is better casting qualities. In particle reinforced composites, the properties
of the PMMA composites was observed to depend on reinforcement type,
reinforcement particle size, nature of interface, volume fraction of
reinforcement. Silicon Carbide (SiC) can be used as reinforcement due to Low
Density, High Strength, Low thermal expansion, High thermal conductivity,

24
low reactivity and also SiC is cost effective when compared to the similar
property ceramic like Boron Carbide.

Chao Shi et.al (2013) works summarises that PMMA-based composites


reinforced by surface modified -Si3N4 fibre were synthesized through free
radical polymerization in batch and its mechanical properties were demonstrated
in this work. g-MPS was identified as a linkage between Si3N4 and PMMA
through methacrylate and alkoxy groups, grafting to hydroxylated Si3N4 fibres
and copolymerized with the PMMA monomer through C55C bonds,
respectively. The thermal stability of Si3N4–PMMA was raised with an increase
in thermal decomposition and glass transition temperature. The composite with
super mechanical properties and thermal stability may have potential
applications in aerospace industry and civil engineering fields.

Diwakar Padalia et.al (2013) works concluded (BaTiO 3:Ce)/PMMA


nanocomposites were successfully prepared by solvent evaporation method. The
lattice parameters increase as the doping percent of cerium increases. The glass
transition temperature and thus thermal stability of polymers and related
composites could be improved by microwave treatment. In addition, glass
transition temperature is also affected by particle size of filler. Lower is the
particle size higher is the glass transition temperature. Dielectric measurements
revealed that the nano composites not only showed significantly increased
dielectric constants when compared with pure PMMA, but also showed the
inherent low loss of the base polymer in a wide range of frequencies and
temperatures.

Leslie Banks-Sills et.al (2016) works summarises that Carboxylated CNTs were
further functionalized by the grafting from (GF) and the grafting to (GT)
methods. The effect of these functionalization methods on the CNTs is
evaluated through measurement of effective mechanical properties of a

25
composite containing them, as well as, through a comparison to a previous
investigation, in which non-functionalized (NF) CNTs were employed. it was
seen that the addition of a weight percent higher than 3 of CNTs to a PMMA
matrix increases the elastic modulus of the composite. It was shown that
functionalization of the CNTs prior to their introduction into the matrix
decreases the weight percent of CNTs needed to produce the same increase in
the elastic modulus for non-functionalized CNTs. Low CNT content, both
functionalized and non-functionalized, may cause a decrease in the elastic
modulus or produce a similar value as that of the matrix.

Tetsuya Yamamoto et.al (2017), in their work PMMA composites were


synthesized using a PMMA resin and recycled carbon fibre fillers, concludes
that the recycled carbon fibres were obtained by the pulverization of the CFRP.
In order to enhance of the mechanical properties of the composite materials, the
adhesion properties of the fillers were improved by the adsorption of PMMA
particles on their surfaces through electrostatic interactions. Shorter recycled
carbon fibres were found to diffuse through the entire PMMA resin owing to
their surface modification with the PMMA particles. The good dispersion and
diffusion of the carbon fibres in the PMMA resin combined with the improved
surface adhesion of the fibres to the resin contributed significantly to the
improvement in the mechanical properties, such as the yield stress and elastic
modulus, of the composites.

Prashant Jindal et.al (2015) evaluated quasi-static and dynamic mechanical


properties of Poly (methyl methacrylate)(PMMA)/Multi Walled Carbon
Nanotubes (MWCNTs) composites for different compositions of MWCNTs in
PMMA by using nano-scale characterization technique. It was observed that
hardness and modulus for 5wt% MWCNT composition in PMMA/MWCNT
composites were enhanced by 44% and 27% respectively in comparison to pure
PMMA. However, hardness and elastic modulus for 10wt% PMMA/MWCNT
26
composites reduced by nearly 28% and 23% respectively in comparison to
5wt% PMMA/MWCNT composite. The visco-elastic nature of
PMMA/MWCNT composites was also investigated by using Dynamic
Mechanical Analysis(DMA). Complex storage modulus for 5wt%
PMMA/MWCNT composite and pure PMMA specimen was compared in
dynamic mode for a frequency range between 50Hz and 210Hz. It was observed
that modulus for 5% wt PMMA/MWCNT composite increased for the complete
loading frequency range.

He Runqin et.al (2017), from the studies of the tensile properties, concluded that
the optimum fibre loading was at 20 vol% for CNT/PMMA composite. The
flexural strength of the composites increases with increasing TiO 2 content in the
CNT/PMMA composite. The results show that the addition of TiO 2 helps to
improve the fibre–matrix adhesion leading to higher flexural properties.
Appropriate amount of TiO2 arrive the high-impact strength for the 20 vol %
CNT/PMMA composite. It is observed that addition of CNT and TiO 2 seems to
be beneficial in increasing mechanical strength via increasing the interface
dispersed phase.

Eduard A. Stefanescu et.al (2011), showed that PMMA-fibreglass structural


dielectrics containing neat and PEDOT:PSS-coated BaTiO3 are valuable
potential dielectric candidates for multifunctional capacitor applications.
Addition of PEDOT:PSS-coated BaTiO3 particles was found to elevate the
dielectric constant relative to that of the composites containing similar amounts
of neat BaTiO3. The presence of the ceramic filler was found to also improve
(increase) the decomposition temperature and glass-transition temperature of the
polymeric matrix in PMMA-fibreglass composites. The polymer-based
composite dielectrics described here may be useful in environments where the
temperature fluctuates anywhere between 50 °C and 100 °C, particularly when

27
utilized in high frequency alternating currents (AC) or direct current (DC)
applications.

Garima Mittal et.al (2016), found from the FTIR data that the silane moieties
were attached onto the hBN particles after surface treatment. From FE-SEM and
HR-TEM images, it was observed that multilayer stacking was reduced after
functionalization, and the TGA-DSC curve also validated the attachment of the
silane moieties. Additionally,the thermal and tribological properties of the
composites were compared. It was found that after silanization, the interactions
between hBN and the polymer matrix increased, yielding more homogeneous
dispersion into the polymer matrix, giving rise to the superior thermal and
tribological properties of PMMA/PI/hBN composites.

H. Varela-Rizo et.al (2011) evaluated and compared the properties of


CNF/PMMA nanocomposites, prepared by three different common techniques
in the thermoplastic polymer processing, considering also the effect of CNF
functionalization. The mechanical properties were evaluated considering the
dispersion and possible interactions with the matrix. Covalent bonds were
detected in the in situ polymerized composites by the FTIR analysis and
confirmed by further techniques. Elastic modulus was enhanced with the
dispersion and the functionalization. There was no increase in melt-
compounding, but there was in solvent processing and in situ polymerization,
and even improved with the treated CNFs. In melt-compounding or solvent
processing, the increase of the elongation by the addition of the CNFs was
noticed, enhancing tenacity. In the case of a strong interface interaction, like in
in situ polymerization, elongation was reduced and the material became stiffer.
the changes in the rheological behavior were more significant in the in situ
polymerized samples, in which the addition of the CNFs advanced the polymer
transition to the solid-like behaviour.

28
Jialiang Wang et.al (2012) have demonstrated an efficient approach to
covalently grafting PMMA onto the GP sheets. GP was obtained by direct
exfoliation of graphite in NMP and the polymerization was carried out in the
well-dispersed GP solution. Various methods were used to characterize the
PMMA functionalized GP, Compared with other functionalized GO or RGO,
the obtained GPMMA has a perfect structure with fewer defects which enables
the excellent reinforcement to the composites. Furthermore, GPMMA is well-
dispersed in organic solvents and this facilitates the preparation of a variety of
composites. With the addition of only 0.5 wt% GPMMA, the resulting
PMMA/GPMMA composite film exhibits a prominent enhancement of
mechanical properties, 151% and 115% increases in Young’s modulus and
tensile strength (relative to the pure PMMA film), respectively. Moreover, the
thermal stability is also improved due to the strong interfacial adhesion and
good dispersion in the PMMA matrix.

Jun-long Wang et.al (2009) et.al work summarises that the CE can be modified
by CTC-IPN technology. The mechanical properties of the modified CE are
better than those of pure CE. When the weight ratio of CE/PMMA was 80/20,
the maximum values of the mechanical properties occurred. The impact strength
was enhanced by 2.37 times that of pure CE and the flexural strength increased
by 1.31 times, respectively. SiO2 can improve the loading ability of the
polymer. Compared with the mechanical properties of IPN without SiO 2, the
impact strength of IPN was increased by 29.96% and the flexural strength by
20.05% after nanometer SiO2 was added.

A. Akinci et.al (2013) drawn conclusions from their study that Increase in the
applied loads, sliding speeds and increase in ZrO 2 filler content in the sliding
tests resulted to increase in coefficient of friction of the pure PMMA and ZrO 2
filled PMMA composites. Wear rates of ZrO 2 filled PMMA composites
decrease with increase in ZrO2 content up to 30%wt and increase in the applied
29
loads and sliding speeds. The more the ZrO2 contents of the PMMA + ZrO2
composite, the lower the wear rate resulted. ZrO2 filled PMMA composites
show that the worn surface morphologies of the 10% ZrO 2 and 30% ZrO2
PMMA composites were smooth and include some tiny abrasive grooves.
Increase in the ZrO2 content cause to increase in the smoothness of the worn
surfaces.

Poomali et.al (2008) concluded that a marginal reduction in tensile strength and
tensile modulus and significant improvement in percentage elongation at break
was noticed with an increase in the TPU content in the blends. The lowest wear
volume loss is obtained for neat PMMA and the highest wear volume is for the
80/20 PMMA/TPU blend. Better correlation between selected mechanical
properties and wear volume is obtained for neat PMMA and 95/5 PMMA/TPU
blend. Even though TPU is the best wear resistance material, inclusion of this
polymer with PMMA by blending is not beneficial for improved abrasion
resistance. SEM micrographs of TPU-filled PMMA blends showed deep
furrows, wider cracks and more debris during the abrasion process.

30
2.3 AIM OF THE PRESENT WORK:

The following objectives were identified for present work, after extensive
literature survey:

1. To fabricate the following by Hand Lay-up method:

a. PMMA – SiC polymer composite.

i. 95% wt of PMMA - 5% wt of Silicon Carbide (SiC).

ii. 90% wt of PMMA - 10% wt of Silicon Carbide (SiC).

2. To fabricate the ASTM Standard plates with Poly Methyl Methacrylate


(PMMA) as matrix and SiC as reinforcement, in different proportions.

3. To cut various sizes of ASTM Standard specimen from the fabricated plate
by using Water Jet Machining (WJM) process.

4. To evaluate the mechanical behaviour of the ASTM standard specimen by


performing various mechanical testing over the existing specimen of various
proportions.

5. To study and evaluate the microstructure, density, hardness, and tensile


strength of the above specimen and defining the change in properties occurred
in comparison with a Pure PMMA.

31
CHAPTER 3

MATERIAL SELECTION

Material selection is the foundation of all engineering applications and


design. The possible materials are simply the only materials that can be used in
the application. Possible Materials are defined by the application requirements.

Physical principles are methods of changing a material that are learned through
material science techniques. Using material science physical principles we can
change material properties. Three common physical principles we can use for
functional material strengthening are densification, composites, and alloying.
There many manufacturing techniques used to strengthen and form materials as
well.
Densification is the most common and necessary way to strengthen any
material. In general, this increases the tensile strength by reducing the porosity
of the material.
The standard composite rule of mixtures is when the standard matrix is
soft/pliable and the reinforcing material is tensile strong. One the major reasons
for the prevalent use of composite materials in construction is the adaptability of
the composite to many kinds of applications. The selection of mixture
proportions can be aimed to achieve optimum mechanical behavior of the
harden product. Selection can result in the change of the strength, consistency,
density, appearance, and durability.

3.1 SELECTION OF CERAMICS


“Advanced ceramics”, “technical ceramics”, and “engineered ceramics” are all
terms that encompass a subset of ceramics that offer high-performance
mechanical, thermal, and/or electrical properties. Their highly specialized

32
properties make them desirable for very specific applications that involve
extreme temperatures, high voltages, or high friction/compressive loads. The
vast majorities of these materials are based upon the nitrides, Carbides, and
oxides of different elements and must be produced with very specialized
equipment.
This tool provides a general overview of the properties of the most common
technical ceramics. Because technical ceramics are used in such a wide variety
of applications, it is useful to understand the relative properties of each material.
If you require more in-depth information, please refer to the relevant material
page where you will find detailed engineering properties.
Since the properties of Silicon Carbide over other ceramics are so good that we
chose Silicon Carbide as one of the material of our composite.
Key strength of SiC over other ceramics:
 Low density
 High strength
 Low thermal expansion
 High thermal conductivity
 High hardness
 High elastic modulus
 Excellent thermal shock resistance
 Superior chemical inertness

33
The below table lists the different properties of ceramics:

Table 3.1 Properties of Ceramics

3.1.1 Silicon Carbide

Silicon Carbide is a semiconductor containing Silicon and carbon with chemical


formula SiC. It occurs in nature as the extremely rare mineral moissanite.
Synthetic Silicon Carbide powder has been mass-produced since 1893 for use as
an abrasive. Grains of Silicon Carbide can be bonded together by sintering to
form very hard ceramics that are widely used in applications requiring high
endurance, such as car brakes, car clutches and ceramic plates in bulletproof
vests.

3.1.2 Types of SiC

Silicon Carbide (SiC) is a hard covalently bonded material predominantly


produced by the carbothermal reduction of silica (typically using the Acheson
process). Depending on the exact reaction conditions the resulting Silicon

34
Carbide is either a fine powder or a bonded mass that requires crushing and
milling to produce a usable feedstock.

Several hundred structures of Silicon Carbide (polytypes) have been identified


which have different stacking arrangements for the Silicon and carbon
atoms. The simplest structure is a diamond structure which is designated β-SiC.
Other structures are either hexagonal or rhombic and are referred to as α-SiC.

3.1.2.1 Natural occurrence

Fig 3.1 Moissanite single crystal (≈1 mm in size)

Naturally occurring moissanite is found in only minute quantities in certain


types of meteorite and in corundum deposits and kimberlite. Natural moissanite
was first found in 1893 as a small component of the Canyon Diablo
meteorite in Arizona by Dr. Ferdinand Henri Moissan, after whom the material
was named in 1905. Moissan's discovery of naturally occurring SiC was initially
disputed because his sample may have been contaminated by Silicon
Carbide saw blades that were already on the market at that time .

While rare on Earth, Silicon Carbide is remarkably common in space. It is a


common form of stardust found around carbon-rich stars, and examples of this
stardust have been found in pristine condition in primitive (unaltered)
meteorites. The Silicon Carbide found in space and in meteorites is almost
exclusively the beta-polymorph. Analysis of SiC grains found in the Murchison
35
meteorite, a carbonaceous chondritemeteorite, has revealed anomalous isotopic
ratios of carbon and Silicon, indicating that these grains originated outside the
solar system.

3.1.3 Wide scale production

Wide-scale production is credited to Edward Goodrich Acheson in 1890 .


Acheson was attempting to prepare artificial diamonds when he heated a
mixture of clay (Aluminium Silicate) and powdered coke (carbon) in an iron
bowl. He called the blue crystals that formed carborundum, believing it to be a
new compound of carbon and aluminium, similar to corundum. Acheson
patented the method for making Silicon Carbide powder on February 28, 1893.
Acheson also developed the electric batch furnace by which SiC is still made
today and formed the Carborundum Company to manufacture bulk SiC, initially
for use as an abrasive. In 1900 the company settled with the Electric Smelting
and Aluminum Company when a judge's decision gave "priority broadly" to its
founders "for reducing ores and other substances by the incandescent method".
It is said that Acheson was trying to dissolve carbon in
molten corundum (alumina) and discovered the presence of hard, blue-black
crystals which he believed to be a compound of carbon and corundum: hence
carborundum. It may be that he named the material "carborundum" by analogy
to corundum, which is another very hard substance (9 on the Mohs scale).The
first use of SiC was as an abrasive.

3.1.4 Manufacturing method

Because natural moissanite is extremely scarce, most Silicon Carbide is


synthetic. Silicon Carbide is used as an abrasive, as well as
a semiconductor and diamond simulant of gem quality. The simplest process to
manufacture Silicon Carbide is to combine silica sand and carbon in an Acheson
graphite electric resistance furnace at a high temperature, between 1,600 °C

36
(2,910 °F) and 2,500 °C (4,530 °F). Fine SiO2 particles in plant material (e.g.
rice husks) can be converted to SiC by heating in the excess carbon from the
organic material. The silica fume, which is a byproduct of producing Silicon
metal and ferroSilicon alloys, also can be converted to SiC by heating with
graphite at 1,500 °C (2,730 °F).

Fig 3.2 Synthetic SiC crystals (~3 mm in diameter)

Fig 3.3 Synthetic SiC Lely crystals

The material formed in the Acheson furnace varies in purity, according to its
distance from the graphite resistor heat source. Colorless, pale yellow and green
crystals have the highest purity and are found closest to the resistor. The color
changes to blue and black at greater distance from the resistor, and these darker
crystals are less pure. Nitrogen and aluminium are common impurities, and they
affect the electrical conductivity of SiC.

Pure Silicon Carbide can be made by the Lely process, in which SiC powder is
sublimated into high-temperature species of Silicon, carbon, Silicon diCarbide
(SiC2), and diSilicon Carbide (Si2C) in an argon gas ambient at 2500 °C and
37
redeposited into flake-like single crystals, sized up to 2×2 cm, at a slightly
colder substrate. This process yields high-quality single crystals, mostly of 6H-
SiC phase (because of high growth temperature). A modified Lely process
involving induction heating in graphite crucibles yields even larger single
crystals of 4 inches (10 cm) in diameter, having a section 81 times larger
compared to the conventional Lely process. Cubic SiC is usually grown by the
more expensive process of chemical vapor deposition (CVD). Homoepitaxial
and heteroepitaxial SiC layers can be grown employing both gas and liquid
phase approaches. Pure Silicon Carbide can also be prepared by the thermal
decomposition of a polymer, poly(methylsilyne), under an inert atmosphere at
low temperatures. Relative to the CVD process, the pyrolysis method is
advantageous because the polymer can be formed into various shapes prior to
thermalization into the ceramic.

3.1.5 Structure of SiC polytypes

(β)3C-SiC 4H-SiC (α)6H-SiC

Fig 3.4 Structure of SiC Polytypes

Silicon Carbide exists in about 250 crystalline forms. The polymorphism of SiC
is characterized by a large family of similar crystalline structures called
polytypes. They are variations of the same chemical compound that are identical
in two dimensions and differ in the third. Thus, they can be viewed as layers

38
stacked in a certain sequence. Alpha Silicon Carbide (α-SiC) is the most
commonly encountered polymorph; it is formed at temperatures greater than
1700 °C and has a hexagonal crystal structure (similar to Wurtzite). The beta
modification (β-SiC), with a zinc blende crystal structure (similar to diamond),
is formed at temperatures below 1700 °C. Until recently, the beta form has had
relatively few commercial uses, although there is now increasing interest in its
use as a support for heterogeneous catalysts, owing to its higher surface area
compared to the alpha form.

3.1.6 Properties of SiC polytypes

Polytype 3C (β) 4H 6H (α)

Crystal structure Zinc blende (cubic) Hexagonal Hexagonal

Space group T2d-F43m C46v-P63mc C46v-P63mc

Pearson symbol cF8 hP8 hP12

Lattice constants (Å) 4.3596 3.0730; 10.053 3.0810; 15.12

Density (g/cm3) 3.21 3.21 3.21

Bandgap (eV) 2.36 3.23 3.05

Bulk modulus (GPa) 250 220 220

Thermal Conductivity 360 370 490

Table 3.2 Properties of major SiC Polytypes

39
Pure SiC is colorless. The brown to black color of the industrial product results
from iron impurities. The rainbow-like luster of the crystals is caused by
a passivation layer of Silicon dioxide that forms on the surface.

The high sublimation temperature of SiC (approximately 2700 °C) makes it


useful for bearings and furnace parts. Silicon Carbide does not melt at any
known temperature. It is also highly inert chemically. There is currently much
interest in its use as a semiconductor material in electronics, where its high
thermal conductivity, high electric field breakdown strength and high
maximum current density make it more promising than Silicon for high-
powered devices. SiC also has a very low coefficient of thermal expansion
(4.0 × 10−6/K) and experiences no phase transitions that would cause
discontinuities in thermal expansion.

3.2 SELECTION OF POLYMER

For proper material selection, careful planning, a thorough understanding of


plastic materials, and reasonable prototype testing are required. Plastics are
viscoelastic materials. Viscoelasticity is defined as the tendency of plastics to
respond to stress as if they were are combination of elastic solids and viscous
fluids. This property possessed by all plastics to some degree, dictates that while
plastics have solid-like characteristics such as elasticity, strength, and form
stability, they also have liquid-like characteristics such as flow depending on
time, temperature, rate, and amount of loading. This also means that unlike
metals, ceramics and other traditional materials, plastics do not exhibit a linear
stress -strain relationship. Designers accustomed to working with metals and
other materials often make the mistake of selecting and specifying incorrect
plastic materials. It is this non-linear relationship for plastics that makes an
understanding of creep, stress relaxation, and fatigue properties extremely
important. In an application that demands high-impact resistance, a high-impact
material must be specified. Typically, for most designers the material selection

40
process begins by reviewing the plastic material data sheets generally provided
by the material suppliers. A misinterpretation of the data sheets is one of the
most common reasons for selecting and specifying the wrong material, for a
given application. First it is important to understand the purpose of a data sheet.
Data sheets are useful only for comparing property values of different plastic
materials such as the tensile strength of nylon versus polycarbonate or the
impact strength of polystyrene versus ABS. Data sheets should be used for
initial screenings of various materials. For example, if a designer is looking for
a material that is strong and tough, he may start out by selecting materials
whose reported values are higher than 7,000 psi tensile strength and impact
strength values of better than 1.0 ft F lb/in and eliminating material such as
general purpose polystyrene, polypropylene, and polyethylene. Data sheets are
never meant to be used for engineering design and final or ultimate material
selections. First, the reported data is generally derived from the short term tests.
Short term tests, as the name suggests, are the tests conducted without
consideration of time, and the values derived are instantaneous. Tensile test,
izod impact test, and Heat Distortion Temperature, are the examples of such
short term tests. Data reported on data sheets are also derived from single point
measurements. These tests do not take into account the effect of time,
temperature, environment, and chemicals, etc. A single number representing one
point on a stress-strain curve cannot begin to convey plastics’ behavior over a
range of conditions. The standardized tests used to measure data sheet
properties contain data measured in a laboratory under ideal conditions (as
specified by ASTM or ISO standards) on standardized test specimens that bear
little resemblance to the geometry of real-world parts. These tests likewise take
place at temperatures, stress and strain rates that rarely corresponds to the real-
world conditions.

41
The proper use of multi-point data for selecting the most appropriate plastic
materials for the applications cannot be over emphasized. This point is well
illustrated in a classic example of misinterpretation of published test data and
the true meaning and usefulness of Heat Distortion Temperature (HDT) values.
The Heat Distortion Temperature test is a short-term test conducted using
standard test bars and laboratory conditions. The temperature values derived
from this test for a particular plastic material is simply an indication of the
temperature at which the test bar shall deform .010 in. under a specified load.
The reported values are further distorted by factors such as residual stresses in
the test bars, amount of load, and specimen thickness. This reported value is of
limited practical importance and should not be used to select materials for
applications requiring continuous exposure at elevated temperatures.
Continuous use temperature data such as UL temperature index is a better
indication of how plastic materials will perform for extended period at elevated
temperatures. Key considerations are mechanical properties:

• Tensile strength and Modulus


• Flexural strength and Modulus
• Impact strength
• Compressive strength
• Fatigue endurance
• Creep
• Stress-relaxation

42
3.2.1 Comparison of PMMA

Fig 3.5 Comparison of PMMA over other polymers

PMMA is an economical alternative to polycarbonate (PC) when tensile


strength, flexural strength, transparency, polishability, and UV tolerance are
more important than impact strength, chemical resistance and heat
resistance.Additionally, PMMA does not contain the potentially
harmful bisphenol-A subunits found in polycarbonate. It is often preferred
because of its moderate properties, easy handling and processing, and low cost.
Non-modified PMMA behaves in a brittle manner when under load, especially
under an impact force, and is more prone to scratching than conventional
inorganic glass, but modified PMMA is sometimes able to achieve high scratch
and impact resistance. Since the properties of PMMA over other polymers is
so good we choosed Silicon Carbide as one of the material for our composite.

43
3.2.2 Poly(methyl methacrylate)

A transparent thermoplastic, Polymethylmethacrylate (PMMA) is a possible


lightweight, shatter-resistent substitute for glass. Often referred to as acrylic glass,
PMMA is a synthetic polymer of the organic compound methyl methacrylate
(MMA). It is seen as a cheap alternative to polycarbonate when high strength is not
necessarily a stringent requirement for the given application. PMMA in its
unmodified form can be brittle with particularly poor impact toughness and has a
lower hardness than conventional glass rendering it prone to scratches. However,
when modified, both of these properties can be significantly improved.
Poly(methyl methacrylate) (PMMA), also known as acrylic or acrylic glass as well
as by the trade names Crylux, Plexiglas, Acrylite, Lucite, and Perspex among
several others is a transparent thermoplastic often used in sheet form as a
lightweight or shatter-resistant alternative to glass. The same material can be used
as a casting resin, in inks and coatings, and has many other uses.

Although not a type of familiar silica-based glass, the substance, like many
thermoplastics, is often technically classified as a type of glass (in that it is a non-
crystalline vitreous substance) hence its occasional historical designation as acrylic
glass. Chemically, it is the synthetic polymer of methyl methacrylate. PMMA is an
economical alternative to polycarbonate (PC) when tensile strength, flexural
strength, transparency, polishability, and UV tolerance are more important
than impact strength, chemical resistance and heat resistance. Additionally,
PMMA does not contain the potentially harmful bisphenol-A subunits found in
polycarbonate. It is often preferred because of its moderate properties, easy
handling and processing, and low cost. Non-modified PMMA behaves in a brittle

44
manner when under load, especially under an impact force, and is more prone to
scratching than conventional inorganic glass, but modified PMMA is sometimes
able to achieve high scratch and impact resistance.

3.2.3 Advantages of PMMA

There are a number of advantages to using PMMA:

 Outstanding weathering and resistance to UV radiation

 Transparent

 High gloss and hardness (when modified)

 Good rigidity

 Dimensionally stable

 Good abrasion resistance - surface scratches can be polished out

(when modified)

3.2.4 Synthesis of PMMA

PMMA is routinely produced by emulsion polymerization, solution


polymerization, and bulk polymerization. Generally, radical initiation is used
(including living polymerizationmethods), but anionic polymerization of PMMA
can also be performed. To produce 1 kg (2.2 lb) of PMMA, about 2 kg (4.4 lb)
of petroleum is needed. PMMA produced by radical polymerization (all
commercial PMMA) is atactic and completely amorphous.

3.2.4.1 Processing - Handling

The glass transition temperature (Tg) of atactic PMMA is 105 °C (221 °F).
The Tg values of commercial grades of PMMA range from 85 to 165 °C (185 to

45
329 °F); the range is so wide because of the vast number of commercial
compositions which are copolymers with co-monomers other than methyl
methacrylate. PMMA is thus an organic glass at room temperature; i.e., it is below
its Tg. The forming temperature starts at the glass transition temperature and goes
up from there. All common Moulding processes may be used, including injection
Moulding, compression Moulding, and extrusion. The highest quality PMMA
sheets are produced by cell casting, but in this case, the polymerization and
Moulding steps occur concurrently. The strength of the material is higher than
Moulding grades owing to its extremely high molecular mass. Rubber
toughening has been used to increase the toughness of PMMA to overcome its
brittle behavior.

PMMA can be joined using cyanoacrylate cement (commonly known


as superglue), with heat (welding), or by using solvents such as di-
or trichloromethane to dissolve the plastic at the joint, which then fuses and sets,
forming an almost invisible weld. Scratches may easily be removed by polishing or
by heating the surface of the material.

Laser cutting may be used to form intricate designs from PMMA sheets. PMMA
vaporizes to gaseous compounds (including its monomers) upon laser cutting, so a
very clean cut is made, and cutting is performed very easily. However, the pulsed
lasercutting introduces high internal stresses along the cut edge, which on exposure
to solvents produce undesirable "stress-crazing" at the cut edge and several
millimetres deep. Even ammonium-based glass-cleaner and almost everything
short of soap-and-water produces similar undesirable crazing, sometimes over the
entire surface of the cut parts, at great distances from the stressed edge. Annealing
the PMMA sheet/parts is therefore an obligatory post-processing step when
intending to chemically bond laser cut parts together.

In the majority of applications, it will not shatter. Rather, it breaks into large dull

46
pieces. Since PMMA is softer and more easily scratched than glass, scratch-
resistant coatings are often added to PMMA sheets to protect it (as well as possible
other functions).

3.2.5 Properties of PMMA

Fig 3.6 Skeletal structure of methyl methacrylate, a constituent monomer of


PMMA

PMMA is a strong, tough, and lightweight material. It has a density of 1.17–


1.20 g/cm3, which is less than half that of glass. It also has good impact strength,
higher than both glass and polystyrene; however, PMMA's impact strength is still
significantly lower than polycarbonate and some engineered polymers. PMMA
ignites at 460 °C (860 °F) and burns, forming carbon dioxide, water, carbon
monoxide and low-molecular-weight compounds, including formaldehyde.

PMMA transmits up to 92% of visible light (3 mm thickness), and gives a


reflection of about 4% from each of its surfaces due to its refractive index (1.4905
at 589.3 nm). It filters ultraviolet (UV) light at wavelengths below about
300 nm(similar to ordinary window glass). Some manufacturers add coatings or
additives to PMMA to improve absorption in the 300–400 nm range. PMMA
passes infrared light of up to 2,800 nm and blocks IR of longer wavelengths up to
25,000 nm. Colored PMMA varieties allow specific IR wavelengths to pass while
blocking visible light (for remote controlor heat sensor applications, for example).

PMMA swells and dissolves in many organic solvents; it also has poor resistance
to many other chemicals due to its easily hydrolyzed ester groups. Nevertheless, its
environmental stability is superior to most other plastics such as polystyrene and

47
polyethylene, and PMMA is therefore often the material of choice for outdoor
applications.

PMMA has a maximum water absorption ratio of 0.3–0.4% by weight. Tensile


strength decreases with increased water absorption. Its coefficient of thermal
expansion is relatively high at (5–10)×10−5 °C−1.

3.2.6 Modification of properties

Pure poly(methyl methacrylate) homopolymer is rarely sold as an end product,


since it is not optimized for most applications. Rather, modified formulations with
varying amounts of other comonomers, additives, and fillers are created for uses
where specific properties are required. For example,

 A small amount of acrylate comonomers are routinely used in PMMA


grades destined for heat processing, since this stabilizes the polymer
to depolymerization ("unzipping") during processing.

 Comonomers such as butyl acrylate are often added to improve impact


strength.

 Comonomers such as methacrylic acid can be added to increase the glass


transition temperature of the polymer for higher temperature use such as in
lighting applications.

 Plasticizers may be added to improve processing properties, lower the glass


transition temperature, or improve impact properties.

 Dyes may be added to give color for decorative applications, or to protect


against (or filter) UV light.

 Fillers may be added to improve cost-effectiveness.

 Being transparent and durable, PMMA is a versatile material and has been
used in a wide range of fields and applications such as rear-lights.

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CHAPTER 4

FABRICATION OF LAMINATES

Laminates are fabricated in the various methods. These methods has different
steps and they involve usage of additives and resins to involve uniform
formation and even distribution of composite (PMMA and SIC). The various
methods used in the process of laminates moulding are

 Injection moulding

 Compression moulding

 Hand Lay-up

4.1 INJECTION MOULDING:

Fig 4.1 Injection Moulding machine

Fig 4.2 Injection Mould making


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Injection moulding is a manufacturing process for producing parts by injecting
molten material into a mould. Injection moulding can be performed with a host
of materials mainly including metals, (for which the process is called die-
casting), glasses, elastomers, confections, and most commonly thermo
plastic and thermosetting polymers. Material for the part is fed into a heated
barrel, mixed (Using a helical shaped screw), and injected (Forced) into a mould
cavity, where it cools and hardens to the configuration of the cavity. After a
product is designed, usually by an industrial designer or an engineer, moulds are
made by a mould-maker (or toolmaker) from metal, usually
either steel or aluminium, and precision-machined to form the features of the
desired part. Injection moulding is widely used for manufacturing a variety of
parts, from the smallest components to entire body panels of cars. Advances
in 3D printing technology, using photopolymers which do not melt during the
injection moulding of some lower temperature thermoplastics, can be used for
some simple injection moulds.

Parts to be injection moulded must be very carefully designed to facilitate the


moulding process; the material used for the part, the desired shape and features
of the part, the material of the mould, and the properties of the moulding
machine must all be taken into account. The versatility of injection moulding is
facilitated by this breadth of design considerations and possibilities.

4.1.1 Equipment Description

Paper clip mould opened in moulding machine; the nozzle is visible at right.
Injection moulding machines consist of a material hopper, an injection ram or
screw-type plunger, and a heating unit. Also known as platens, they hold the
moulds in which the components are shaped. Presses are rated by tonnage,
which expresses the amount of clamping force that the machine can exert. This
force keeps the mould closed during the injection process. Tonnage can vary

50
from less than 5 tons to over 9,000 tons, with the higher figures used in
comparatively few manufacturing operations.

4.1.2 Injection Moulding process

With injection moulding, granular plastic is fed by a forced ram from a hopper
into a heated barrel. As the granules are slowly moved forward by a screw-type
plunger, the plastic is forced into a heated chamber, where it is melted. As the
plunger advances, the melted plastic is forced through a nozzle that rests against
the mould, allowing it to enter the mould cavity through a gate and runner
system. The mould remains cold so the plastic solidifies almost as soon as the
mould is filled.

4.1.3 Applications

Injection moulding is used to create many things such as wire


spools, packaging, bottle caps, automotive parts and components, pocket combs,
some musical instruments (and parts of them), one-piece chairs and small
tables, storage containers, mechanical parts (including gears), and most other
plastic products available today. Injection moulding is the most common
modern method of manufacturing plastic parts; it is ideal for producing high
volumes of the same object.

4.1.4 Examples for Injection Moulding

Most polymers, sometimes referred to as resins, may be used, including


all thermoplastics, some thermosets, and some elastomers. Available materials
include alloys or blends of previously developed materials, so product designers
can choose the material with the best set of properties from a vast selection.
Major criteria for selection of a material are the strength and function required
for the final part, as well as the cost, but also each material has different
parameters for moulding that must be taken into account. Common polymers
like epoxy and phenol are examples of thermosetting plastics while nylon,

51
polyethylene, and polystyrene are thermoplastic. Until comparatively recently,
plastic springs were not possible, but advances in polymer properties make them
now quite practical. Applications include buckles for anchoring and
disconnecting the outdoor-equipment webbing.

4.2 COMPRESSION MOULDING

Fig 4.3 Diagrammatic representation of Compression Moulding Machine

Compression moulding is a well-known technique to develop variety of


composite products. It is a closed moulding process with high pressure
application. In this method, as shown in figure 1, two matched metal moulds are
used to fabricate composite product. In compression moulding base plate is
stationary while upper plate is movable. Reinforcement and matrix are placed in
the metallic mould and the whole assembly is kept in between the compression
moulder.

Heat and pressure is applied as per the requirement of composite for a definite
period of time. The material placed in between the moulding plates flows due to

52
application of pressure and heat and acquires the shape of the mould cavity with
high dimensional accuracy which depends upon mould design. Curing of the
composite may carried out either at room temperature or at some elevated
temperature. After curing, mould is opened and composite product is removed
for further processing. In principle, a compression moulding machine is a kind
of press which is oriented vertically with two moulding halves (top and bottom
halves). Generally, hydraulic mechanism is used for pressure application in
compression moulding.

Fig 4.4 Compression Moulding Cycle

The controlling parameters in compression moulding method to develop


superior and desired properties of the composite. All the three dimensions of the
model (pressure, temperature and time of application) are critical and have to be
optimized effectively to achieve tailored composite product as every dimension
of the model is equally important to other one. If applied pressure is not
sufficient, it will lead to poor interfacial adhesion of fibre and matrix. If
pressure is too high, it may cause fibre breakage, expulsion of enough resin

53
from the composite system. If temperature is too high, properties of fibres and
matrix may get changed.

If temperature is low than desired, fibres may not get properly wetted due to
high viscosity of polymers especially for thermoplastics. If time of application
of these factors (pressure and temperature) is not sufficient (high or low), it may
cause any of defects associated with insufficient pressure or temperature. The
other manufacturing factors such as mould wall heating, closing rate of two
matched plates of the plates and de-moulding time also affect the production
process.

4.2.1 Materials Used

Some of the materials which are commonly used in the compression moulding
are

 “Thermosetting polymers” such as Epoxy, polyester, polyvinyl ester,


phenolic resin, Unsaturated polyester, polyurethane resin, Urea
formaldehyde

 “Thermoplastic polymers” Such as polypropylene (PP), polyethylene


(PE), nylon, polycarbonate (PC), polyvinyl chloride (PVC), cellulose
acetate, polyether ether ketone (PEEK), Acrylonitrile-butadiene-styrene
(ABS), polystyrene (PS) biodegradable polymers such as poly lactic acid
(PLA), poly vinyl alcohol (PVA), soy based plastic, starch based
polymers

 Reinforcement such as Glass fibre, carbon fibre, aramid fibre, natural


plant fibres (sisal, banana, nettle, hemp, flax etc.) (All these fibres may be
in the form of unidirectional mat, bidirectional (woven) mat, stitched into
a fabric form, mat of randomly oriented fibres, short fibres, chopped
fibres)

54
4.2.2 Applications

This method is equally applicable for both thermosetting and thermoplastic


polymer based composites. Application includes very wide spectrum ranging
from kitchen goods to automobiles, toys, electrical items and airplane parts etc.

Typical products include automobile panels, roof, life gates, battery trays,
fenders, hoods, bumpers, spoilers, air deflectors, furniture kitchen bowls and
trays, dinnerware, buttons, large containers, recreational vehicle body panels,
medical equipment (ultrasound equipment).

Fig 4.5 Compression Moulding Machine

55
4.3 HAND LAY-UP

It is the oldest moulding method for making composite products. It requires no


technical skill and no machinery. It is a low volume, labour intensive method
suited especially for large components, such as boat hulls. A male and female
half of the mould is commonly used in the Hand Lay-up process.

Fig 4.6 Hand Lay-up

4.3.1 Mould

The mould will have the shape of the product. In order to have a glossy or
texture finish on the surface of the product, the mould surface also should have
the respective finish. If the outer surface of the product to be smooth, the
product is made inside a female mould. Likewise, if the inner side has to be
smooth, the moulding is done over a male mould. The mould should be free
from defects, since the imprint of any defect will be formed on the product.
Release

4.3.1.1 Film or layer:

Since, the resins used are highly adhesive, the product may get stuck to the
mould. So, a proper releasing mechanism should be incorporated. The release of

56
the product can be affected by the use of a release layer of wax or polyvinyl
alcohol (PVA). By using a thin film like polyester film (Mylar). Since, the
Mylar sheet has to be fit into the mould profile, this method is not used for
complex shapes.

4.3.1.2 Gel coat

The gel coat gives the required finish of the product. It is usually a thin layer of
resin about mm thickness applied on the outer surface of the product. The
colour is obtained by adding appropriate pigments to the resin. The gel coat
forms a protective layer that protects the glass fibre getting in contact with water
and chemicals. If the gel coat is too thin, the fibre pattern will become visible. If
it is too thick, crazing and star crack can appear on the gel coat.

4.3.1.3 Surface Mat Layer

A surface mat layer will be placed beneath the gel coat layer. The fibres of the
mat will not give high strength like reinforcement fibres, but the mat provides
crack resistance and impact strength to the resin rich layer. It is an optional layer
used only in specific cases.

4.3.1.4 Laminates of GFRP

The glass fibre layer wetted with resin is laid up one after another to the
required thickness and this finished material is called the laminate. The laminate
gives the strength and rigidity to the product. Glass fibre in the chopped strand
mat (CSM) is commonly used to get composite products. Woven roving,
unidirectional and bi-directional mats are also used to get high strength
composite products.

4.3.1.5 Resin coat

The glass fibre laminate provides a rough surface finish. In order to get a
smoother surface, a surface mat layer or resin coat may be applied over.

57
For the selection of Hand Lay-up as a fabrication process, the following
conditions should favour:

 Only one side need to have good smooth finish.

 The product is large in size and very complex in shape.

 Only a few numbers of mouldings are required.

4.3.1.6 Surface mat layer

The surface mat layer must be applied only after the gel coat is cured. Otherwise
the surface finish will be affected. The surface layer can be any one of the
following.  Glass fibre surface tissue mat.  Polyester woven cloth of fine
thickness  Nylon woven cloth of fine thickness A thin layer of resin is applied
over the surface and the mat is wetted with brush. It may also be lightly rolled
with roller to remove the air bubbles.

4.3.1.7 Lay-up of laminates

The lay-up should start as soon as the gel coat layer is cured. The lamination
should satisfy the following requirements:

 The fibre layers should be uniformly placed and they should fit correctly
into the contour of the product.

 The fibre should not be damaged during lay-up.

 The fibre to resin ratio should be correctly maintained.

4.3.2 Preparation of the Resin Mix

The resin mix can be prepared at least one day ahead so that the entrapment of
air bubbles escape before the lay-up begins. The mix consists of the resin,
accelerator, fillers, and additives if any. The addition of accelerator to resin will
not cause any cross linking until catalyst is added. The mixing can be done by

58
either manually using a paddle or by using an air operated mixer. Vigorous
stirring can cause entrapment of air bubbles therefore; mixing should be done at
a very low rpm. The container in which resin mix is stored may be closed air
tight to minimize the vaporization and loss of styrene.

4.3.3 Colour Fibre Mat Preparation

The required number layers to obtain the thickness can be determined by taking
into account the mat density and the glass-to-resin ratio by weight. The
following points must be taken into account while preparing the mat:

 Wherever joints are there, there should be a minimum overlap of 25 mm,


in case of chopped strand and a 50 mm overlap is required in the case of
woven roving mat.

 Whenever, there is change in thickness the thickness must not abruptly


change and instead it must gradually change.

1) Tools for Lay-up:

 Weighing balance - to weigh the chemicals.

 Brushes - to apply resin for both gel coat application and for lamination.

 Rollers - to remove the air bubbles and also for applying resin.

Long rollers are used to consolidate large areas but short rollers are used for
corners and curved surfaces. Mugs and small bowls - for taking the resin mix
for lay-up.

2) Solvents:

Solvents are required for cleaning the rollers and brushes during or after the lay-
up sequence is over. Acetone or Nitrocellulose thinner can be used as solvents.

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4.3.4 Lamination Procedure

In the process of lamination a thin layer of resin is applied on the gel coat layer.
Then, a chopped strand mat is placed over it. The resin is again applied over the
mat by using brush to wet the mat. By using the roller the air bubbles are
removed.

After the first layer is laid up, subsequent layers are laid in a similar manner.
More than 4 layers of resin and glass mat should not be applied without
allowing the resin to cure at a time. When WRM is laid up, CSM is used in
between in order to increase the inter-laminar shear strength.

The lay-up procedure for WRM and CSM are identical except that the resin
used for WRM is half the quantity of that is needed for CSM. Curing of Resin:
The curing of resin process undergoes through four stages:

1) Gelation Stage: It is the stage at which the resin becomes tack free and
unworkable. It depends on the percentage of catalyst and accelerator
added. Normally, it takes 15 to 30 minutes to gel.

2) Green Stage: This is the stage at which the resin resembles to hard cheese
which when pressed with the thumb it breaks up. The resin is considered
to be set but not cured.

3) Cured Stage: It is the stage at which more than 90% of the cure is
completed. The product can be released from the mould after this stage.

4) Fully Cured Stage: It is the stage at which the physical properties of the
moulding are developed. Normally, it takes 5 to 10 days.

4.3.5 Advantages of Hand Lay-up Method

 It is a Low Volume, Labourious method suited for many products such as


boat manufacturing, automotive components, ducts, tanks, furniture,
corrosion resistant equipment etc.

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 No costly machinery is required.

 Nearly all shapes and sizes can be made.

 Fine Colour and texture finish can be obtained by this Hand Lay-up
method.

4.3.6 Cutting of plates:

Plates created using hand layup method is to be cut into required “ASME
STANDARD SHAPES” so that it can be used for various testing process. In our
project the cutting of plates is done by “Water Jet Cutting” or “Water Jet
Machining” method.

4.3.7 Water Jet Cutting or Water Jet Machining:

The above ASME STANDARD specimen is created using water jet cutting
machining using CNC operated water jet machine. Water Jet Machining (WJM)
also called as water jet cutting is a non-traditional machining process in which
high velocity jet of water is used to remove materials from the surface of the
work piece. WJM can be used to cut softer materials like plastic, rubber or
wood. In order to cut harder materials like metals or granite, an abrasive
material is mixed in the water.

4.3.7.1 Operation

All water jets follow the same principle of using high pressure water focused
into a beam by a nozzle. Most machines accomplish this by first running the
water through a high pressure pump. There are two types of pumps used to
create this high pressure; an intensifier pump and a direct drive or crankshaft
pump. A direct drive pump works much like a car engine, forcing water through
high pressure tubing using plungers attached to a crankshaft. An intensifier
pump creates pressure by using hydraulic oil to move a piston forcing the water
through a tiny hole. The water then travels along the high pressure tubing to the

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nozzle of the water jet. In the nozzle, the water is focused into a thin beam by a
jewel orifice. This beam of water is ejected from the nozzle, cutting through the
material by spraying it with the jet of high-speed water. The process is the same
for abrasive water jets until the water reaches the nozzle. Here abrasives such as
garnet and aluminium oxide are fed into the nozzle via an abrasive inlet. The
abrasive then mixes with the water in a mixing tube and is forced out the end at
high pressure.

Fig 4.7 Water Jet Cutting

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CHAPTER 5

TESTING AND DISCUSSION

5.1 TESTS PERFORMED

After fabrication of the laminate of (PMMA and SIC), the plate is cut into
standard specimen according to ASME standards through water jet cutting
method. Then the specimens are subjected to following four testing which is
performed in micro lab technologies under supervised condition. The end
factors are controlled for the tests and the results are plotted in tables and in
graphs to indicate its results. The tests performed are listed as follows:

 Tensile test

 Bend test

 Flexural test

 Charpy impact test

The brief description about these tests is described as follows.

5.1.1 Tensile test

A tensile test, also known as tension test, is probably the most fundamental type
of mechanical test you can perform on material. Tensile tests are simple,
relatively inexpensive, and fully standardized. By pulling on something, you
will very quickly determine how the material will react to forces being applied
in tension. As the material is being pulled, you will find its strength along with
how much it will elongate.

5.1.2 Purpose of Tensile Test

It is performed to determine the ultimate strength of the fabricated specimen

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It helps in determine the maximum force that the material can withstand without
failure

5.1.3 Bend test:

Bend tests deform the test material at the midpoint causing a concave surface or
a bend to form without the occurrence of fracture and are typically performed to
determine the ductility or resistance to fracture by deforming the sample into a
specific shape. The test sample is loaded in a way that creates a concave surface
at the midpoint with a specified radius of curvature.

5.1.4 Purpose of Bend Test

The main purpose of the Bend testing is to determine the ductility, bend
strength, fracture strength and resistance to fracture of the specimen. It is used
to determine the characteristics of a material which it will fail under pressure.

5.1.5 Flexural test

The flexure test method measures behaviour of materials subjected to simple


beam loading. It is also called a transverse beam test with some
materials. Maximum fibre stress and maximum strain are calculated for
increments of load. Results are plotted in a stress-strain diagram. Flexural
strength is defined as the maximum stress in the outermost fibre. This is
calculated at the surface of the specimen on the convex or tension side.

5.1.6 Purpose of Flexural Test

A flexural specimen simply rests on two supports and is loaded at one or two
points along its length, making the test very easy to perform. Thus this test is
involved with ceramic-matrix composites and bulk ceramics.

In a flexural test, the stress state is neither pure (it varies from tension on one
surface to compression on the other, with shear present as well), nor uniform (it

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varies along the length of the specimen). So a composite material is best suited
to this testing.

5.1.7 Charpy Impact Test

Destructive mechanical test in which a pendulum hammer fractures a standard


size notched piece of material with one blow. It indicates how the material will
respond to suddenly applied shock (stress) by measuring the energy absorbed in
breaking the piece. The Charpy test subjects a small beam, with a 55-mm/2.17-
inch long and 10-mm/0.39-inch square cross- section, to a three-point flexural
impact loading induced by a swinging pendulum .The test specimen contains a
45° included-angle notch, which is 2-mm/0.079-inch deep, on the tensile side to
induce failure at that point. The test results are expressed in foot-pounds or
kilojoules.

5.1.8 Purpose of Impact Test

To investigate the effect of the ratio of the support-span length to thickness l/t
on impact characteristics for both unidirectional. Charpy test rig were
conducted in order to identify key parameters influencing the impact damage
resistance of composite structures.

5.2 ASME STANDARD SHAPE

5.2.1 Tensile Test specimen (ASTM D638-03)

Fig 5.1 Tensile Test specimen


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5.2.2 Flexural Test specimen (ASTM D790)

Fig 5.2 Flexural Test specimen

5.2.3 Impact Test specimen (ASTM D256)

Fig 5.3 Impact Test specimen

The various analysis and testings were carried out to determine the tensile
strength, bend test, flexural test and charpy impact test. These values are shown
in the report given below:

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67
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The reports yielded information pertaining to tensile test, wear test, flexural test
and charpy impact test. These result are presented in an chart format for better
understanding: (values are in MPa)

TENSILE TEST(PMMA+SiC+GFRP)
50
45
40
35
30
25
20
15
10
5
0
SiC 5% SiC 10%

ID-1 ID-2 ID-3

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70
Based on the results obtained, the following are the conclusions reaped, when
PMMA is reinforced with Glass Fibre Mat and varying percentages of Silicon
carbide:

 On increasing Silicon carbide percentage, the tensile test results casted an


increasing gradient, thus proving that SiC has an considerable influence
on the yield strength of the specimen.

 Bend test which is performed to access the ductility and soundness of the
polymer, resulted such that, on increasing the Silicon Carbide percent, the
specimen were susceptible to improved ductility.

 The results from impact test indicated that, specimens with higher
concentration of Silicon Carbide were able to withstand higher rates of
loading and thereby 9+proving its improved service life.

To summarize the results obtained, we were able to witness improved yield


strength, ductility and load withstanding capabilities on increasing the
concentration of Silicon Carbide in pure PMMA-laminated with Glass fibres.

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On comparing these properties with pure PMMA, it was signified that the
tensile strength of reinforced polymers were deprived. This on the contrary
improved the hardness properties of the specimen, thereby levitating the surface
hardness.

With improved surface hardness properties, the specimen could bear extended
scratch exposures. Silicon Carbide, on reinforcing with PMMA showcased an
improved melting range, therefore instituting its application on fields
demanding polymers sustenance on higher temperatures.

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73
74
75
The morphology of different composition of polymer matrix composite are
observed and analyzed in Scanning Electron Microscope(SEM) are shown:

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CHAPTER 6

COST ANALYSIS

6.1 MATERIALS USED

S.No MATERIALS QUANTITY

1. PMMA 600 gms

2. Silicon Carbide 180 gms

3. GFRP 6 sheets

4. Epoxy Rexin and 500 ml


Hardener

Table 6.1 Materials Used

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6.2 COST ANALYSIS

6.2.1 Material Cost

S.No MATERIALS COST(Rs)

1. PMMA 210

2. Silicon Carbide 360

3. GFRP 600

4. Epoxy Resin and 1200


Hardener

5. TOTAL 2370

Table 6.2 Material Cost

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6.2.2 Machining Cost

S.No. TESTING AND MACHINING COST(Rs.)


OPERATION

1. Hand Lay-Up process 7200

2. Cutting Process(Water Jet Cutting) 1000

4. Testing of specimens 4800


(Tensile, Impact, Wear and Hardness)

5. SEM Analysis 1000

TOTAL COST 14000

Table 6.3 Machining Cost

6.3 TOTAL COST

Material Cost = Rs. 2370/-


Machining Cost = Rs. 14000/-
Miscellaneous Expenses = Rs. 2500/-

TOTAL COST = Rs. 18870/-

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CHAPTER 7

COROLLARIES PERTAINING TO EXPERIMENT

Based on the inferences obtained from TENSILE, WEAR, HARDNESS and


IMPACT tests performed on the specimens, the following are the corollaries:

 On comparison of pure PMMA with reinforced counterparts, the later


exhibited better Tensile strength (60MPa) than our experimented
specimen.

 This holds good for our conclusion. PMMA reinforced with 10% Silicon
Carbide exhibited a tensile strength of 43MPa. There is a converse
relationship between tensile strength and hardness, which factualizes that
Tensile strength and Hardness are inversely proportional.

 Increase in hardness stripped a newer regime wherein the material


possessed better indentation capabilities and scratch resistance. Improved
scratch resistance paves plot for its use in CERAMIC INDUSTRIES.

 The decrease in Flexural strength was as foreseen, emphasizing the


hypothesis that, homogeneous materials exhibited flexural strength in par
with the tensile strength. But it’s not the case when materials get
reinforced and hence the decrease in flexural strength.

 Outputs from Impact test showed an ascending gradient; embracing our


cognizance. The absorbed energy is a measure of
material's notch toughness and acted as a tool to study temperature-
dependent ductile-brittle transition.

To summarize, reinforced PMMA revealed better surface hardness properties


and temperature with-holding characteristics on correlation with pure PMMA.

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CHAPTER 8

CONCLUSION

Polymers, which have been lately sensationalized for its alluring properties, has
an potential to attract global dependence. Metals conventionally used pose
concerns as they can’t be relied indefinitely due to this present exhaustion rates.
Polymers on the other hand can be synthesized by polymerization lending in
inarticulate ways of reliance. Polymer parts are lighter and therefore provide
immense advantages over metals by offering lower lifetime freight costs for
equipment that is regularly transported or handled over the product’s lifetime.
The low frictional properties provide for less wear as well. The lower wear rates
allow for less maintenance-related downtime. Not only are polymers lighter, but
they’re also less expensive than many raw metal materials used for parts.
Polymers are produced in faster cycles than metals which helps keep
manufacturing costs down as well. Corrosion due to moisture or even dissimilar
metals in close contact is also a major concern with metal components, but
polymer and composite materials are impervious to chemicals. Polymers and
composites are both thermally and electrically insulating. Metallic components
require special secondary processing and coating in order to achieve any sort of
insulating properties. These components are also naturally corrosion resistant
and experience no galvanic effects in a dissimilar metal scenario that require
sheathing. All these advantages make polymers dominate the throne of metals.
The growth in the fields of composite makes it imminent that future is certainly
“polymer reliant”. To abreast this, constant evolvements are being done to
further enhance the properties of polymers, by either synthesizing novel
polymers or reinforcing with characteristic materials. Our research, on
reinforcing PMMA with SiC has shown valuable outcomes, thereby enlisting
this composite as a viable alternative.

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