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CHAPTER 1
INTRODUCTION

A Composite material is a material system composed of two or more macro constituents

that differ in shape and chemical composition and which are insoluble in each other. The
history of composite materials dates back to early 20th century. Poly Ethylene Vinyl Acetate
(PEVA) is a random copolymer synthesized from ethylene monomer and vinyl acetate co-
monomer. This copolymer is often produced by continuous bulk polymerization under high
pressure similar to polyethylene. It is a polymer that approaches elastomeric (“rubber-like”)
materials in flexibility and softness. This is distinct from a thermoplastic, in that the material
is cross-linking, ergo difficult to recycle. The product design, development and
manufacturing process analysis are the essential process for the successful application of any
polymer and polymer composites. An eminent product design is ensured by performing
mechanical and thermal testing of the material used in prior to product design.
The combination of a matrix and strong reinforcing filler is called as composite which
possess all desirable properties that could not be available in either matrix or filler alone. In
order to develop the unique properties of a polymer composite material extensive research
activities are in progress. From the research analysis it has been proved that all polymer
composites show much improved thermal and mechanical properties. Mainly the particle
reinforced composites shows enormous improvement in properties overall. The particles used
for reinforcement due to small size, have a high surface to volume ratio and provides good
strength and high-energy surfaces. The polymer composite technology innovation leads to
improved bonding between polymer and reinforcing media by presenting an improved
polymer composite material. Improving performance is a key challenge enforced to all
manufacturers to meet customer demands and to maintain a dominant place in competition
driven market. The polymer composite technology, induce the manufacturers to introduce
new technologies in process and to announce new lightweight materials for the society. Thus
polymer composite technology improves the size of product performance area mainly due to
discovery of lightweight materials. When compared to steel and aluminum, polymer
composites fare better in terms of weight, thermal expansion, specific stiffness, specific
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strength and fatigue strength. Replacing steel with polymer composite can save from 60% to
80% in weight and can save up to 50% cost when polymer composites are used in place of
aluminum. Metal counter parts could not perform far better than polymer composites.
Polymer composites are extremely lightweight, offer tailor made properties and provides
parts consolidation.
Materials in the field are most commonly represented by ceramics, metals and polymers.
While noted improvements have taken place in the area of ceramics and metals, it is the field
of polymers that has experienced an explosion in progress. Polymers have gone from being
cheap substitutes for natural products to providing high-quality options for a wide variety of
applications. Further improvements and breakthroughs supporting the economy can be
expected in the coming years. Polymers are derived from petroleum, and their cost has its
roots in the abundance of the feedstock, in the ingenuity of the chemical engineers who
devised the processes of manufacture, and in the economics of scale that have come with
increased usage. Less than 5 percentage of the petroleum barrel is used for polymers, and thus
petroleum is likely to remain as the principal raw material for the indefinite future. Polymers
constitute a high value-added part of the petroleum customer base and have led to increasing
international competition in the manufacture of commodity materials as well as engineering
thermoplastics and specialty polymers. Polymers are now produced in great quantity and
variety. Polymers are used as film packaging, solid molded forms for automobile body parts
and TV cabinets, composites for golf clubs and aircraft parts (airframe as well as interior,
foams for coffee cups and refrigerator insulation, fibers for clothing and carpets, adhesives
for attaching anything to anything, rubber for tires and tubing, paints and other coatings to
beautify and prolong the life of other materials, and a myriad to other uses. It would be
impossible to conceive of our modern world without the ubiquitous presence of polymeric
materials. Polymers have become an integral part of our society, serving sophisticated
functions that improve the quality of our life. The unique and valuable properties of polymers
have their origins in the molecular composition of their long chains and in the processing that
is performed in producing products. Both composition (including chemical makeup,
molecular size, branching and cross-linking) and processing (affected by flow and
orientation) are critical to the estimated properties of the final product. The classes of
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polymeric materials and the technical factors that contribute to their usefulness are more. In
spite of the impressive advances that have been made in recent years, there are still
opportunities for further progress, and failure to participate in this development will consign
our nation’s progress to second class.

The familiar categories of materials called plastics, fibers, rubbers and adhesives consist of
a diverse array of synthetic and natural polymers. It is useful to consider these types of
materials together under the general rubric of structural polymers because macroscopic
mechanical behavior is at least a part of their function. Compared with classical structural
materials like metals, the present usage represents a considerable broadening of the term.
Man-made plastics, fibres and rubber accounted for 70 million tons in 2000, and production
has tripled over the last decade. The price received by the original manufacturer ranges from
roughly ten thousands to several thousand per ton, depending on the material. As compared to
barrel value of crude oil cost, polymers cost represents considerable value added. Because
these materials go through several manufacturing steps before reaching the final consumer,
the ultimate impact on the national economy is measured in the hundreds of million rupees
each year. These materials have many different chemical and physical forms, such as cross-
linked versus non-cross-linked, crystalline versus amorphous and rubbery versus glassy.
More recently, structural polymers having liquid crystalline order have become important.
Structural polymers are rarely used in the pure form but often contain additives in small
quantities such as antioxidants, stabilizers, lubricants, processing aids, nucleating agents,
colorants and antistatic agents or in larger quantities, plasticizers of fillers. There is rapid
growth in the areas of blends and composites. In composites, a material of fixed shape, such
as particles (filler) or fibers is dispersed in a polymer matrix. The filler or fiber may be an
inorganic material or another organic polymer. Blends (or alloys) on the other hand consist of
two or more polymers mixed together and differ from composites in that the geometry of the
phases is not predetermined prior to processing. Some polymers are used for many different
purposes. The word “plastic” is frequently used loosely as a synonym for “polymer”, but the
meaning of “polymer” is based on molecular size while “plastic” is defined in terms of
deformability. Plastics are polymeric materials that are formed into a variety of three-
dimensional shapes, often by moulding or melt extrusion processes. They retain their shape
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when the deforming forces are removed, unlike some other polymers such as the elastomers,
which return to their original shape. Plastics are usually categorized as thermoplastics or
thermosets, depending on their thermal processing behaviour. Thermoplastics are polymers
that soften and flow upon heating and become hard again when cooled. This cycle can be
repeated many times, which makes reprocessing during manufacture or recycling after
consumer use possible heat fabrication techniques such as extrusion or moulding. The
polymer chains in thermoplastics are linear or branched and do not become cross-linked as in
the case of thermosets. While there are many different chemical types of thermoplastics,
those made from only four monomers (ethylene, propylene, styrene and vinyl chloride)
account for about 90 percentage of all thermoplastics produced in India. Of these four types,
polypropylene has grown most rapidly in recent years in which production has increased
eightfold over the past decade. Thermoplastic polyesters, primarily PET, are growing even
more rapidly at the present time (driven mainly by packaging applications), with current sales
nearly one-quarter of those for polypropylene. For the long term, the majority of commodity
thermoplastics are expected to follow their traditional growth, with continued opportunities
for both process and product innovation. Future activities will focus strong on recycling. In
the case of PET, recycling can be accomplished by chemical depolymerisation to monomers
or oligomers followed by re-polymerisation to PET or other products. Such processes are
currently in use for products that come into contact with food, while simple reprocessing is
used for less critical products. The so-called engineering thermoplastics, which include the
higher-performance, more expensive polymers such as the polyacetals, polycarbonates,
nylons, polyesters, polysulfones, polyetherimides, some acrylonitrile butadiene styrene
(ABS) materials, and so on, have generally exhibited stronger growth than the commodity
plastics. These materials generally have greater heat resistance and better mechanical
properties than the less expensive commodity thermoplastics and, therefore, are used in more
demanding applications, such as aircraft, automobiles and appliances. A major area of
development is new blends or alloys of engineering plastics that are designed for speciality
market products and are usually quite tough and chemical resistant. New products and
advances in processes have resulted from the ring-opening polymerization of cyclic
oligomers; for example, new developments in polycarbonates are particularly noteworthy.
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Other new products can be expected based on copolymers, and entirely new polymers are
under development. A further category sometimes referred to as high-performance
engineering thermoplastics commands even higher prices for yet higher levels of
performance. These include highly aromatic polymers such as poly (phenylene sulphide),
several new polyamides, Polysulfornes and polyetherketones. Development of new molecular
structures has dominated this sector. Polymer chains with quite rigid backbones have liquid
crystalline order, which offers unique structural properties. Almost one-third are used in
packaging, primarily containers and film.

1.1 POLY ETHYLENE VINYL ACETATE (PEVA)

The material has good clarity and gloss, low-temperature toughness, stress-crack
resistance, hot-melt adhesive, waterproof properties and resistance to UV radiation.
PEVA has a distinctive vinegar-like odor and it is competitive with rubber and vinyl
products in many electrical applications. Its properties can be easily varied by adjusting
the vinyl acetate co-monomer ratio from 10 to 40% with the remainder being ethylene. If
Vinyl acetate ratio is low the EVA obtained has enough ability to crystallize. If Vinyl
acetate ratio is high, it prevents formation of crystal lattice. Thermal exploration of poly
ethylene vinyl acetate (PEVA) and its composites plays a vital role.

Table: 1.1 PEVA Properties

Physical and Chemical Properties
Property Value
Form Pellets
Colour Transparent
Odour None
Melting Point 190˚C
Volatile 0%
Density 0.935 g/cm3
Water solubility Insolubility
Tensile strength 14.7 MPa
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1.2 APPLICATIONS OF PEVA POLYMER

PEVA shows great commercial potential in the packaging industry due to their well-
known good mechanical properties, specifically good process ability and increased stiffness
in molded parts, high resistance to tearing and toughness and significant moisture barrier
properties. The barrier to moisture, oxygen and carbon dioxide in a package system improves
the food product shelf life and improves its quality. Mixing of PEVA with PTFE obtain a
composite exhibiting better flexibility, toughness and high resistance to environmental stress
cracking and improved thermal properties in the application of solar panels. The combination
of transparency and resistance to oils, fats and cleaning agents make PEVA very suitable for
use in the kitchen as mixing bowls and basins and fittings for refrigerators. Hot melt
adhesives, hot glue sticks, and top of the line soccer cleats are usually made from PEVA,
usually with additives like wax and resin. PEVA is also used as a clinginess-enhancing
additive in plastic wraps. Craft foam sheets are made of PEVA and these foam sheets are
popularly used for children's foam stickers. PEVA is also used in biomedical engineering
applications as a drug delivery device. The polymer is dissolved in an organic solvent (e.g.,
dichloromethane). Powdered drug and filler (typically an inert sugar) are added to the liquid
solution and rapidly mixed to obtain a homogeneous mixture. The drug-filler-polymer mix is
then cast into a mould at −80 °C and freeze dried until solid. These devices are used in drug
delivery research to slowly release a compound. While the polymer is not biodegradable
within the body, it is quite inert and causes little or no reaction following implantation.
PEVA is one of the materials popularly known as expanded rubber or foam rubber. PEVA
foam is used as padding in equipment for various sports such as ski boots, bicycle saddles,
hockey pads, boxing and mixed martial arts gloves and helmets, wakeboard boots, water ski
boots, fishing rods and fishing reel handles. It is typically used as a shock absorber in sports
shoes, for example. It is used for the manufacture of floats for commercial fishing gear such
as purse seine (seine fishing) and gillnets. In addition, because of its buoyancy, PEVA has
made its way into non-traditional products such as floating eyewear. It is also used in the
photo-voltaic industry as an encapsulation material for crystalline silicon solar cells in the
manufacture of photovoltaic modules. PEVA slippers and sandals are currently very popular
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because of their properties like light weight, easy to form, odourless, glossy finish, and
economical compared to natural rubber. In fishing rods, it is used to construct handles on the
rod-butt end. PEVA can be used as a substitute for cork in many applications. PEVA
emulsions are polyvinyl acetate copolymers based on vinyl acetate internally plasticized with
vinyl acetate ethylene. PEVA copolymer are adhesives used in packaging, textile,
bookbinding for bonding plastic films, metal surfaces, coated paper, as dispersible powder in
plasters and cement renders. PEVA is used as a solar panel adhesive and encapsulate. PEVA
is also used in coatings formulation of good quality interior water-borne paints at 53%
primary dispersant. PEVA is used in orthotics, fire safe cigarettes (FSC), surfboard and ski-
board traction pads, and for the manufacturing of some artificial flowers. It is used as a cold
flow improver for diesel fuel and a separator in HEPA filters. EVA can easily be cut from
sheets and moulded to shape. It is also used to make thermoplastic mouth guards that soften
in boiling water for a user specific fit. It is also used for impregnation of leather. Additional
uses are in the making of nicotine transdermal patches since the copolymer binds well with
other agents to form gel like substances.
1.3 POLYTETRAFLUROETHYLENE (PTFE)
PTFE was accidentally discovered in 1938 by Roy J. Plunkett while he was working in
New Jersey for DuPont. As Plunkett attempted to make a new chlorofluorocarbon refrigerant,
the Tetrafluro-ethylene gas in its pressure bottle stopped flowing before the bottle's weight
had dropped to the point signaling "empty." Since Plunkett was measuring the amount of gas
used by weighing the bottle, he became curious as to the source of the weight, and finally
resorted to sawing the bottle apart. He found the bottle's interior coated with a waxy white
material that was oddly slippery. Analysis showed that it was polymerized Perfluoroethylene,
with the iron from the inside of the container having acted as a catalyst at high pressure.
Kinetic Chemicals patented the new fluorinated plastic (analogous to the already
known polyethylene) in 1941, and registered the Teflon™ trademark in 1945.

PTFE is produced by free-radical polymerization of Tetrafluoroethylene. The net equation is

n F2C=CF2 → −(F2C−CF2)n−. PTFE is a thermoplastic polymer, which is a white solid at
room temperature, with a density of about 2200 kg/m3. According to Chemours, its melting
point is 600 K. It maintains high strength, toughness and self-lubrication at low temperatures
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down to 5 K and good flexibility at temperatures above 194 K. Processing PTFE can be
difficult and expensive, because the high melting temperature, 327 °C, is above the initial
decomposition temperature, 200 °C. Even when melted, PTFE does not flow, but instead
behaves as a gel due to the absence of crystalline phase and high melt viscosity.

Table: 1.2 PTFE properties

Physical and Chemical Properties
Form Powder

Colour White

Odour None

Melting Point 327-342˚C

Volatile 0%

Density 2200 Kg/m3

Water solubility Insoluble

Tensile strength 3.9 N/mm2

1.4 APPLICATIONS OF PTFE POLYMER

The major application of PTFE, consuming about 50% of production, is for wiring in
aerospace and computer applications (e.g. hookup wire, coaxial cables). This application
exploits the fact that PTFE has excellent dielectric properties, especially at high radio
frequencies, making it suitable for use as an excellent insulator in connector assemblies
and cables, and in printed circuit boards used at microwave frequencies. Combined with its
high melting temperature, this makes it the material of choice as a high-performance
substitute for the weaker and lower-melting-point polyethylene commonly used in low-cost
applications. In industrial applications, owing to its low friction, PTFE is used for plain
bearings, gears, slide plates, seals, gaskets, bushings, and more applications with sliding
action of parts, where it outperforms acetyl and nylon. It’s extremely high
bulk resistivity makes it an ideal material for fabricating long-life electrets,
the electrostatic analogues of permanent magnets. PTFE film is also widely used in the
production of carbon fibre composites as well as fiberglass composites, notably in the
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aerospace industry. PTFE film is used as a barrier between the carbon or fiberglass part being
built, and breather and bagging materials used to encapsulate the bondment when de-bulking
(vacuum removal of air from between layers of laid-up plies of material) and when curing the
composite, usually in an autoclave. The PTFE, used here as a film, prevents the non-
production materials from sticking to the part being built, which is sticky due to the carbon-
graphite or fiberglass plies being pre-pregnated with bismaleimide resin. Non-production
materials such as Teflon™, Air-weave Breather and the bag itself would be considered
F.O.D. (foreign object debris/damage) if left in layup.
Because of its extreme non-reactivity and high temperature rating, PTFE is often used as
the liner in hose assemblies, expansion joints, and in industrial pipe lines, particularly in
applications using acids, alkalis, or other chemicals. Its frictionless qualities allow improved
flow of highly viscous liquids and for uses in applications such as brake hoses.
Gore-Tex is a brand of expanded PTFE (e-PTFE), a material incorporating a
fluoropolymer membrane with micro-pores. The roof of the Hubert H. Humphrey
Metrodome in Minneapolis, US, was one of the largest applications of PTFE coatings. 20
acres (81,000 m2) of the material was used in the creation of the white double-layered PTFE-
coated fiberglass dome. PTFE is often found in musical instrument lubrication product; most
commonly, valve oil. PTFE is used in some aerosol lubricant sprays, including in micronized
and polarized form. It is notable for its extremely low coefficient of friction, its hydrophobia
(which serves to inhibit rust), and for the dry film it forms after application, which allows it to
resist collecting particles that might otherwise form an abrasive paste. PTFE (Teflon™) is
best known for its use in coating non-stick frying pans and other cookware, as it
is hydrophobic and possesses fairly high heat resistance. The sole plates of some clothes irons
are coated with PTFE (Teflon™).
Other niche applications include: It is often found in ski bindings as a non-mechanical
AFD (anti-friction device). It can be stretched to contain small pores of varying sizes and is
then placed between fabric layers to make a waterproof, breathable fabric in outdoor apparel.
It is used widely as a fabric protector to repel stains on formal school-wear, like uniform
blazers. It is used as a film interface patch for sports and medical applications, featuring a
pressure-sensitive adhesive backing, which is installed in strategic high friction areas of
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footwear, insoles, ankle-foot orthosis, and other medical devices to prevent and relieve
friction-induced blisters, calluses and foot ulceration. Expanded PTFE membranes have been
used in trials to assist trabeculectomy eye surgery to treat glaucoma. Powdered PTFE is used
in pyrotechnic compositions as an oxidizer with powdered metals such
as aluminium and magnesium. Upon ignition, these mixtures form carbonaceous soot and the
corresponding metal fluoride, and release large amounts of heat. They are used in infrared
decoy flares and as igniters for solid-fuel rocket propellants. Aluminium and PTFE is also
used in some thermo-baric fuel compositions. Powdered PTFE is used in a suspension with a
low-viscosity, azeotropic mixture of siloxane ethers to create a lubricant for use in twisty
puzzles. In optical radiometry, sheets of PTFE are used as measuring heads in spectra
radiometers and broadband radiometers due to PTFE's capability to diffuse a transmitting
light nearly perfectly. Moreover, optical properties of PTFE stay constant over a wide range
of wavelengths, from UV down to near infrared. In this region, the ratio of its regular
transmittance to diffuse transmittance is negligibly small, so light transmitted through
a diffuser (PTFE sheet) radiates like Lambert's cosine law. Thus PTFE enables co-sinusoidal
angular response for a detector measuring the power of optical radiation at a surface, e.g. in
solar irradiance measurements.
Certain types of bullets are coated with PTFE to reduce wear on the rifling of firearms that
uncoated projectiles would cause. PTFE itself does not give a projectile, an armour piercing
property. Its high corrosion resistance makes PTFE useful in laboratory environments, where
it is used for lining containers, as a coating for magnetic stirrers, and as tubing for highly
corrosive chemicals such as hydrofluoric acid, which will dissolve glass containers. It is used
in containers for storing fluoroantimonic acid, a super acid. PTFE tubes are used in gas-gas
heat exchangers in gas cleaning of waste incinerators. Unit power capacity is typically several
megawatts. PTFE is widely used as a thread seal tape in plumbing applications, largely
replacing paste thread dope. PTFE membrane filters are among the most efficient industrial
air filters. PTFE-coated filters are often used in dust collection systems to collect particulate
matter from air streams in applications involving high temperatures and high particulate loads
such as coal-fired power plants, cement production and steel foundries. PTFE grafts can be
used to bypass steno-tic arteries in peripheral vascular disease if a suitable
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autologous vein graft is not available. Many bicycle lubricants and greases contain PTFE and
are used on chains and other moving parts subjected to frictional forces. PTFE can also be
used for dental fillings, to isolate the contacts of the anterior tooth so the filling materials will
not stick to the adjacent tooth. PTFE sheets are used in the production of butane hash oil due
to its non-stick properties and resistance to non-polar solvents. PTFE, associated with a
slightly textured laminate, makes the plain bearing system of a Dobsonian telescope. PTFE is
widely used as a non-stick coating for food processing equipment; dough hoppers, mixing
bowls, conveyor systems, rollers, and chutes. PTFE can also be reinforced where abrasion is
present – for equipment processing seeded or grainy dough for example. PTFE has been
experimented with for electro-less nickel plating. PTFE tubing is used for Bowden tubing
in 3D printers because its low friction allows the extruder stepper motor to push filament
through it more easily.

1.5 THERMAL PROPERTIES

Generally, a material expands when heated. This property of a material is called
Thermal Expansion. Materials with high thermal conductivity will conduct more
heat than the ones with low conductivity. Thermal properties come under the broader
topic of physical properties of materials. Thermal properties of a material decide how it
reacts when it is subjected to heat fluctuation (excessive heat or very low heat, for
example). The major components of thermal properties are: Heat capacity, Thermal
Expansion, Thermal conductivity and Thermal stress.
In the amorphous region of the polymer, at lower temperature, the molecules of the
polymer are in, say, frozen state, where the molecules can vibrate slightly but are not able to
move significantly. This state is referred as the glassy state. In this state, the polymer is
brittle, hard and rigid analogous to glass, hence the name glassy state. The glassy state is
similar to a super-cooled liquid where the molecular motion is in the frozen state. The glassy
state shows hard, rigid, and brittle nature analogous to a crystalline solid with molecular
disorder as a liquid. Now, when the polymer is heated, the polymer chains are able to wiggle
around each other, and the polymer becomes soft and flexible similar to rubber. This state is
called the rubbery state. The temperature at which the glassy state makes a transition to
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rubbery state is called the glass transition temperature (Tg). Note that the glass transition
occurs only in the amorphous region, and the crystalline region remains unaffected during the
glass transition in the semi-crystalline polymer.
1.5.1 HEAT CAPACITY
Heat capacity of a material can be defined as the amount of heat required to change the
temperature of the material by one degree. The amount of heat is generally expressed in
joules or calories and the temperature in Celsius or Kelvin.
1.5.2 THERMAL CONDUCTIVITY
It is the property of a material to conduct heat through itself. Materials with high thermal
conductivity will conduct more heat than the ones with low conductivity.
1.5.3 THERMAL EXPANSION
When heat is passed through a material, its shape changed. Generally, a material expands
when heated. This property of a material is called Thermal Expansion. There can be change
in area, volume and shape of the material.
1.5.4 THERMAL STRESS
The stress experienced by a body due to either thermal expansion or contraction is called
thermal stress. It can be potentially destructive in nature as it can make the material explode.
1.5.5 INTERMOLECULAR FORCES
Strong intermolecular forces cause higher (Tg). For example, PVC (Tg = 80˚C) has
stronger intermolecular forces than polypropylene (Tg = −18˚C) because of the dipole–dipole
forces from the C—Cl bond.
1.5.6 CHAIN STIFFNESS
The presence of the stiffening groups (such as amide, sulfone, carbonyl, p-phenylene etc.)
in the polymer chain reduces the flexibility of the chain, leading to higher glass transition
temperature. For example, polyethyleneterephthalete is stiffer than polyethylene adipate due
to the presence of benzene ring. Therefore, Tg value is higher for polyethyleneterephthalate.
1.5.7 CROSS-LINKING
The cross-links between chains restrict rotational motion and raise the glass transition
temperature. Hence, higher cross-linked molecule will show higher Tg than that with lower
cross-linked molecule.
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1.6 MECHANICAL PROPERTIES

Strength is a mechanical property that explains about how strong a polymer is? Tensile
strength is important for a material that is going to be stretched. Fibres need good tensile
strength. Compressional strength is important for a material that is going to be compressed.
Concrete is a good example of a material having more compressional strength. Flexural
strength is important for a material that is going to be bent. Similarly, a torsional strength is
important if it is to be twisted. Also impact strength for a material is important if it is
subjected sharp and sudden forces.
To measure the tensile strength of a polymer sample, the sample must be stretched. This
machine simply clamps each end of the sample, then turn it on it stretches the sample. While
it is stretching the sample, it measures the amount of force (F) that it is exerting. When the
force being exerted on the sample, then divide that number by the cross-sectional area (A) of
our sample.

The amount of force and stress are increased naturally, on the sample until it breaks. The
stress needed to break the sample is the tensile strength of the material. Likewise for
compressional and flexural strengths, the strength can be measured by increasing the stress
until it breaks. The tensile stress is the force applied on the sample divided by the cross-
sectional area of the sample; tensile stress and tensile strength are both measured in units of
force divided by units of area (N/cm2). Also 1 MPa = 100 N/cm2.
1.6.1 Elongation or Tensile strength:
A polymer’s mechanical properties are most important than to know how it is strong. The
strength of a polymer reveals about how much stress is needed to break a sample, but it does
not reveal about what happens to a sample when we are trying to break it. Thus it is essential
to study about the elongation or tensile strength of a polymer sample. Elongation is a type of
deformation. Deformation is simply a change in shape of a product that undergoes stress. The
tensile stress is the force required to deform a sample by stretching and becomes longer. The
percentage elongation is the length of the polymer sample after stretched (L), divided by the
original length of the sample (L0), and then multiplied by 100.
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There are a number of things we measure related to elongation. Two important things
measured are ultimate elongation and elastic elongation. Ultimate elongation of a sample is
the amount of stretch the sample undergoes before it breaks. Elastic elongation is the
percentage of elongation obtained without permanently deforming the sample. This is the
percentage of stretch that sample come back to its original length, after releasing the stress on
it.
Maximum tensile stress of a material can withstand before failure (MPa). It is the property
of a material that allows it to deform under tensile loading without breaking under the action
of a load. If the stress is too large, the strain deviates from being proportional to the stress.
The point at which this happens is the yield point because there the material yields,
deforming permanently (plastically). Hooke's law is not valid beyond the yield point. The
stress at the yield point is called yield stress, and is an important measure of the mechanical
properties of materials. In practice, the yield stress is chosen as that causing a permanent
strain of 0.002. When stress continues in the plastic regime, the stress-strain passes through a
maximum, called the tensile strength, and then falls as the material starts to develop a necked
it finally breaks at the fracture point.
1.6.2 Modulus of elasticity:
All plastics do not stretch or deform as they resist deformation. The measurement given by
the sample that resists deformation is called modulus. To measure tensile modulus as like
measuring tensile strength, the stress applied on the sample is slowly increased until the
sample breaks. Then we take a plot of stress versus elongation, like this:
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Fig. 1.1 Stress-strain curve

This plot is called a stress-strain curve. (Strain is any kind of deformation, including
elongation). The height of the curve when the sample breaks is the tensile strength, of course,
and the tensile modulus is the slope of this plot. If the slope is steep, the sample has a high
tensile modulus, which means it resists deformation. If the slope is gentle, then the sample
has a low tensile modulus, which means it is easily deformed. The plastics have medium
tensile modulus. The unit to modulus is N/cm 2. Elastic moduli measure the stiffness of the
material. They are related to the second derivative of the interatomic potential, or the first
derivative of the force vs. inter-nuclear distance. Due to thermal vibrations the elastic
modulus decreases with temperature. E is large for ceramics (stronger ionic bond) and small
for polymers (weak covalent bond). Since the interatomic distances depend on direction in
the crystal, E depends on direction (i.e., it is anisotropic) for single crystals.
1.6.3 Toughness:
The area underneath the stress-strain curve, coloured red in the graph below is called
toughness. Ability of a material to absorb energy (or withstand shock) and plastically deform
without fracturing (or rupturing); a material's resistance to fracture when stressed;
combination of strength and plasticity. This is commonly associated with impact loading. It is
defined as the energy required fracturing a unit volume of material. Generally, the
combination of a high ultimate tensile strength and a high ductility results in a higher
toughness.
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Fig. 1.2 Toughness graph

Toughness is really a measure of the energy a sample can absorb before it breaks. If the
height of the triangle in the plot is strength, and the base of the triangle is strain, then the area
is proportional to strength times strain. Since strength is proportional to the force needed to
break the sample, and strain is measured in units of distance (the distance the sample is
stretched), then strength times strain is proportional is force times distance, also force times
distance is energy.

The strength is the force required to break a sample and toughness is the energy that is
needed to break a sample. A strong material is not tougher. The graph below has three
different plots one blue, one red and one pink.

Fig. 1.3 Strength graph

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The blue plot is the stress-strain curve for a sample that is strong, but not tough also it
takes a lot of force to break this sample, but not much energy, as there isn't much area
underneath the curve. Likewise, this sample can't stretch very far before it breaks. A material
like this which is strong, but can't deform very much before it breaks is called brittle. On the
other hand, the red plot is a stress-strain curve for a sample that is both strong and tough. This
material is not as strong as the sample in the blue plot, but the area underneath its curve is a
lot larger than the area under the blue sample's curve. So it can absorb a lot more energy than
the blue sample can. The red sample elongates a lot more before breaking than the blue
sample does. You see, deformation allows a sample to dissipate energy. If a sample can't
deform, the energy won't be dissipated, and will cause the sample to break. We usually want
materials to be tough and strong. Ideally, it would be nice to have a material that wouldn't
bend or break. The blue sample has a much higher modulus than the red sample. While it's
good for materials in a lot of applications to have high moduli and resist deformation, it's a lot
better for a material to bend than to break, and if bending, stretching or deforming in some
other way prevents the material from breaking, all the better. So when we design new
polymers or new composites, we often sacrifice a little bit of strength in order to make the
material tougher.
The additions of particles in a matrix have very high tensile strength and good flexural
strength as well, but they usually have terrible compressional strength. They also only have
good tensile strength in the direction of the particle orientation.

Fig. 1.4 Fibre orientations

1.6.4 Wear Resistance:

 18

Wear test is performed in three levels, namely, (1) laboratory test, (2) component
simulation test, (3) in-service test.
Stage 1 Laboratory test with small samples are initially carried out under testing conditions
simulated insofar as conveniently possible to determine whether the surface engineering
technology warrants further consideration, and if so, to find out under what treatment
conditions, the highest wear resistance improvement can be achieved.

Stage 2 In the next stage, the optimised surface treatment condition will be used to treat
some real joint parts, e.g. femoral head or cup, which will then be tested in a hip-joint
simulator, with the testing conditions being controlled as close as possible to those for a
real human joint, for example, lubricated with body liquid, temperature around 37°C, and
moving like a human walking or running.

Stage 3 Only when the surface treated parts have survived the simulation tests, and indeed
show considerably improved wear resistance yet without losing other properties (e.g.
corrosion and bio-compatibility), can the in-service tests be carried out. The surface treated
joint parts will be implanted in a human body and tested (monitored) for a pro-longed
period of time if there is no immediate side effect after implantation.
As we can see, simulation test and in-service test produce more reliable results, however,
laboratory test is cheap, safe and quick and thus serve a most useful function.
The Laboratory wear testing methods are as follows: An apparatus for wear testing is
termed as wear tester, tribotester or tribometer. The prefix of "tribo-" refers to wear,
friction and lubrication. A wear tester will always involve two components loaded against
and relatively moving each other. The movement can be driven by a motor or by an electro-
magnetic device. For convenient purpose, the material or component being investigated is
normally referred to as specimen, the other termed as counter face. As examples, the
working principle of three most widely used laboratory wear testers are given below.
 19

Fig. 1.5 An abrasive wear tester

Fig. 1.5 is a schematic of an abrasive wear tester, in which a wheel or a ball is driven by
a motor, rotating and sliding against a fixed sample in the presence of abrasive particles.
The specimen is in the form of a plate or a block. Contact pressure is controlled by dead
weight through a loading lever. The abrasive particles, such as silica, are added through a
nozzle connecting to a hopper above, giving a three-body wear situation. After a set time of
running, the sample is removed, and wear loss is measured. The parameters to be controlled
include contact load, sliding speed, type of abrasive particles and its flow rate.

Fig. 1.6 Schematic of a pin-on-disc-wear test

 20

In a pin-on-disc wear tester, a pin is loaded against a flat rotating disc specimen such
that a circular wear path is described by the machine. The machine can be used to evaluate
wear and friction properties of materials under pure sliding conditions. Either disc or pin
can serve as specimen, while the other as counter face. Pin with various geometries can be
used. A convenient way is to use ball of commercially available materials such as bearing
steel, tungsten carbide or alumina (Al2 O3) as counter face, so that the name of ball-on-disc
is used.
Wear measurement is carried out to determine the amount of materials removed (or
worn away) after a wear test, (and in reality after a part in service for a period of time – 30
minutes). The material worn away can be expressed either as weight (mass) loss, volume
loss, or linear dimension change depending on the purpose of the test, the type of wear, the
geometry and size of the test specimens, and on the availability of a measurement
facility.Common techniques of wear measurement include using a precision balance to
measure the weight (mass) loss, profiling surfaces, or using a microscope to measure the
wear depth or cross-sectional area of a wear track so as to determine the wear volume loss
or linear dimensional change.
To finalize the material for an engineering product/application, we should have the
knowledge of Mechanical properties of materials. The mechanical properties of a material are
those which affect the mechanical strength and ability of a material to be molded in suitable
shape. Mechanical properties including elasticity, yield strength, ultimate tensile strength and
ductility are usually part of material specifications and are obtained by tensile testing.
A material's property (or material property) is an intensive property of some material, i.e.
a physical property that does not depend on the amount of the material. These quantitative
properties may be used as a metric by which the benefits of one material versus another can
be compared, thereby aiding in materials selection.
 21

CHAPTER 2
OBJECTIVE

 To fabricate synthetic polymer matrix with synthetic polymer particle filler using melt
mixing by INJECTION molding method.
 To identify suitable particle reinforcement to improve thermal and mechanical
properties when build with PEVA matrix with composite innovation.
 To study the behavior of PEVA/PTFE composite material samples under varying
temperatures using TGA.
 To study the thermal stability of optimum composite using FTIR, XRD and Optical
Microscopy.
 To study the thermal conductivity for the optimum composite.
 To perform the mechanical testing by conducting tensile, flexural and wear tests.
 22

CHAPTER 3
LITERATURE REVIEW
3.1. BASED ON FILLER
AUGMENTATION OF THERMAL CONDUCTIVITY FOR POLYPROPYLENE /
ETHYLENE VINYL ACETATE BASED COMPOSITES FILLED BY OEGANIC
AND INORGANIC PARTICLES
The reliance of thermal conductivity of composites on the filler loading, filler networking
morphology and on the whole composite structure is also discussed. This work is intended to
design composites for the improvement of thermal conductivity of polypropylene and
ethylene vinyl acetate copolymer with lower filler contents.
AN EXPERIMENTAL STUDY ON MECHANICAL PROPERTIES OF EPOXY-
MATRIX COMPOSITES CONTAINING GRAPHITE FILLER
The current work studies the effect of the incorporation of different amounts of graphite filler
on the mechanical properties of epoxy resin and of carbon filler reinforced epoxy composites.
Graphite-reinforced epoxy-matrix composites were prepared with graphite fractions ranging
from5 to 30 wt.%. The produced material were subjected to tensile and to flexural three point
bending tests.
EFFECT OF FILLER LOADING ON THE TENSILE PROPERTIES OF MULTI-
WALLED CARBON NANOTUBE AND GRAPHENE NANOPOWDER FILLED
EPOXY COMPOSIES
In this work, multi-walled carbon nanotube (MWCNT) and grapheme nanopowders (GNP)
filled epoxy composites were fabricated via ultrasonication and casting method. The
experimental results prove that the strength and modulus of filler filled epoxy composites are
lower as compared to Pristine Epoxy. Thus it indicates that in addition of filler (MWCNT and
GNP) has reduced the mechanical properties of epoxy composites. The reason for this is due
to the high aspect ratio and high Vanderwaal’s attraction of the MWCNT causes
entanglement among nanotube.
IMPROVEMENT OF SCRATCH AND WEAR RESISTANCE OF POLYMERS BY
FILLERS INCLUDING NANOFILLERS
 23

Aluminium nanoparticles as filler are more effective for property improvement than micro
particles at the same overall volumetric concentration. Prevention of local agglomeration of
filler particles is discussed along with a technique to verify the prevention.
EFFECT OF FIBRES AND FILLERS ON MECHANICAL PROPERTIES OF
THERMOPLASTIC COMPOSITES
Thermoplastic copolyester elastomer (TCE) and polyoxy methylene (POM) filled polytetra
fluro ethylene (PTFE) composite, reinforced with short glass fibre (SGF) and different shape
microfillers such as short carbon fibre (SCF), silicon carbide (SiC) and alumina (Al 2O3) were
prepared by melt mixing method using twin screw extruder followed by injection moulding.
LOW-COST CARBON FILLERS TO IMPROVE MECHANICAL PROPERTIES
AND CONDUCTIVITY OF EPOXY COMPOSITES
In recent years, low-cost carbons derived from recycled materials have been gaining attention
for their potentials as filler in composites. The electrical and mechanical properties of
polymer composites can be measured using different percentages and different kind of fillers:
either low cost (eg., carbon black), eco friendly (eg., biochar) or sophisticated (eg., carbon
nanotubes).
STUDY OF THE INFLUENCE OF FILLER ON THE MECHANICAL PROPERTIES
OF COMPOSITES BASED ON POLYIMIDE
Physical and mechanical properties of polymer composite films on the basis of polyimide
filled with high-temperature superconductors (yttrium ceramics) were studied. Calculations
under the catastrophic models were carried out. Exponential and parabolic models show the
best agreement with the experiment.
3.2 BASED ON FABRICATION
PREPARATION AND PROPERTIES OF ETHYLENE VINYL ACETATE / LINEAR
LOW DENSITY POLYETHYLENE / GRAPHENE OXIDE NANOCOMPOSITE
FILMS
Ethylene vinyl acetate based nanocomposites with 18 and 28 wt% vinyl acetate were
prepared via solution casting method. The morphological studies indicated that the graphene
oxide diffraction peak disappeared in all prepared nanocomposites, probably due to its
 24

exfoliation; also proper dispension and good interaction between nanofillers and polymer
matrix were achieved.
DEVELOPMENT AND CHARACTERIZATION OF INJECTION MOULDED ALL-
POLYPROPYLENE COMPOSITES
Prior to injection molding, pre-impregnated pellets were prepared by a three step process
(filament winding, compression molding and pelletizing). A highly oriented polypropylene
multifilament was used as the reinforcement material and a random polypropylene copolymer
(with ethylene) was used as the matrix material. Plaque specimens were injection molded
from the pellets with either a film gate or fan gate.
FABRICATION AND CHARACTERISTICS OF HYDROXYAPATITE
REINFORCED POLYPROPYLENE AS A BONE ANALOGUE BIOMATERIAL
In this investigation, a manufacturing route employing injection molding was established for
producing bone analogue biomaterials. Using this manufacturing technology, a potential bone
replacement material, hydroxyapatite (HA) reinforced polypropylene (PP) composite was
made, with the HA volume percentage being up to 25%
INFLUENCE OF REGRIND OF PROPERTIES OF PLASTICS PRODUCED BY
INJECTION MOULDING
Materials Crastin PBT (with 30% glass fiber) and Celanex 2004-2PBT (without filler) were
used at tests with various percentage of added regrind into basic material. Utilization of
regrind at the production on new molded parts is important from aspect of reduction plastics
waste and pollution abatement of environment.
INJECTION MOULDING OF POLYPROPYLENE HYBRID COMPOSITES
REINFORCED WITH CARBON FIBER AND WOOD FIBER
Incorporating carbon fiber and wood fiber into a polymer matrix to make hybrid composites
through injection molding would be a path to expanded applications for both. This paper
investigated the injection molding of Carbon fiber - Wood fiber / Polypropylene hybrid
composites and their mechanical properties.
MECHANICAL PROPERTIES OF INJECTION MOULDED PRODUCTS
FABRICATIED BY DIRECT FIBER FEEDING INJECTION MOULDING
 25

Direct-Fiber-Feeding Injection Molding (DFFIM) with the improvement of the screw and
cylinder and a fiber-direct-feeding method, is a new way to make short fiber reinforced
composite material from one step by throwing fiber into a formation machine directly, in
which the traditional compounding process can be unnecessary.
ON THE INJECTION MOULDING PROCESSING PARAMETERS OF HDPE-TiO 2
NANOCOMPOSITES
A substantial amount of research has been done in order to design polymeric Nano
composites in a safe and efficient manner. In the present study, the impact of processing
parameters, such as, barrel temperature and residence time on the mechanical and thermal
properties of high density polyethylene (HDPE)-TiO2 Nano composites were investigated.
STYRENE-ACRYLONITRILE (SAN) LAYERED SILICATE NANOCOMPOSITES
PREPARED BY MELT COMPOUNDING
Poly (styrene-co-acrylonitrile) (SAN) nano-composites were successfully made by melt
compounding and exhibited improved thermal stability and reduced flammability.
Flammability of these materials was measured by pulse-combustion flow calorimetry
(PCFC), also known as micro-cone calorimetry.
3.3 BASED ON THERMAL PROPERTIES
THE THERMO-MECHANICAL DEGRADATION OF ETHYLENE VINYL
ACETATE USED AS A SOLAR PANEL ADHESIVE AND ENCAPSULANT
The thermal ageing of a ethylene vinyl acetate polymer used as an adhesive and encapsulant
in a photovoltaic module has been investigated. Using a range of experimental techniques,
including Dynamic Mechanical Analysis, Differential Scanning Calorimetry and Thermo-
gravimetric Analysis, it was possible to show a link between changes in mechanical
properties with both the transient temperature and the degree of long-time thermal ageing.
COMPATIBILIZATION EFFECTS IN THE THERMAL DEGRADATION OF
BLENDS CONTAINING TPR AND EDPM POLYMERS
With plain mixtures of TPR and EDPM, degradation behavior is practically improving
whereas in the case of EPDM-g-TPR lower volatile products are produced. The degradation
process is influenced by the dispersion of the blend components.
 26

CHARACTERIZATION OF NANOCOMPOSITES BY THERMAL ANALYSIS

Thermal analysis is a useful tool to investigate a wide variety of polymers and it can be
applied to polymer Nano composites in order to gain further insight into their structure. This
review illustrates the versatile applications of thermal analysis methods of polymer
nanomaterial research, presenting applications of differential scanning calorimeter (DSC),
Thermogravimetric analysis (TGA), dynamic mechanical thermal analysis (DMTA) and
thermal mechanical analysis (TMA) for the characterization of Nano composite materials.
CHARACTERIZATION OF PANI-PV Ac COMPOSITE THIN FILMS USING XRD
ANALYSIS
Polyaniline (PANI) and Poly (vinyl acetate (PV Ac) composite film were characterized by
XRD technique. This method can be used to show the perfection of PV Ac network structure
in the composite. XRD technique has been used to determine the possible crystallinity in the
composite films. The XRD of all samples was carried in the 20 range from 10 to 100 degree.
THERMAL CHARECTERIZATION OF ORGANICALLY MODIFIED
MONTMORILLONITE
During this study, modern thermal analysis techniques combined with infrared spectroscopy
and mass spectrometry (TGA-FTIR-MS) were used to obtain information on the thermal
stability and degradation products. The effect of chemical variation (alkyl chain length,
number of alkyls and unsaturation) of organic modifiers on the thermal stability of the
organically exchanged montmorillonite are discussed.
EVALUATION OF THERMAL PROPERTIES OF E-GLASS/ EPOXY COMPOSITES
FILLED BY DIFFERENT FILLER MATERIALS
The main aim of this work was to determine the thermal conductivity, thermal expansion
coefficient, time to ignition and flame propagation rate of composites. Experimental results
show that Al2O3 and Mg(OH)2 filled composites exhibited low thermal conductivities.
Composites filled by SiC particles exhibited low thermal expansion coefficient when
compared with other filled composites.
MORPHOLOGY, THERMAL AND MECHANICAL PROPERTIES OF
THERMOPLASTIC RUBBER (TPR)/CLAY NANOCOMPOSITES FROM
ORGANIC-MODIFIED MONTMORILLONITE
 27

The influences of the direct organic modified MMT on the structure and properties of the
TPR/clay Nano composites are investigated by XRD, TEM, HREM, TGA, DMA,
respectively. The results indicate that the TPR cannot intercalate into the interlayers of the
pristine MMIT and results in Micro composites. The thermal stability and the char residue at
700˚C of the TPR/clay Nano composites have remarkably enhancements compared with pure
TPR. DMA measurements show that the silicate clays improve the storage modulus and glass
transition temperature (Tg) of the TPR matrix in the Nano composites.
RESULTS OF THERMAL ANALYSIS ON FIBER REINFORCED PLASTIC
MATRIX COMPOSITE MATERIALS
The materials hardened at room temperature and one group was not cured and the other was
exposed to post-curing process and then, they are tested on Q 800 TA Dynamic Mechanical
Analyzer instrument. Heat Deflection Temperature (HDT) values were determined according
to ASTM E 2092-04 standard while Glass Transition Temperature Tg values were
determined according to ASTM E 1640-04 standard.
MIGRATION OF MULTIWALLED CARBONS IN BLENDS OF THERMO PLASTIC
RUBBER
Multi-walled carbon nanotubes (MWNTs) have been introduced into blends of polycarbonate
(PC) and poly(styrene-acrylonitrile) (TPR) by melt mixing in a micro compounder
DYNAMIC MECHANICAL THERMAL ANALYSIS OF POLYMER COMPOSITES
REINFORCED WITH NATURAL FIBERS
The detailed characterization of the viscoelastic properties is an essential step in the
development process of composites. This review describes the use of Dynamic Mechanical
Thermal Analysis (DTMA) in the viscoelastic characterization of composites and a brief
description about the utility of the DTMA in the study of their structure/properties
relationship is given.
THERMAL AND FLAMMABILITY PROPERTIES OF POLYPROPYLENE/SILICA
AEROGEL COMPOSITES
Polypropylene/Silica aerogel with different weight percent were prepared via melt
compounding method and their thermal and flammability properties were studied. The SEM
images confirmed the homogenous mixing of the components. The measurement of the
 28

thermal conductivities of samples indicated that PP would be a better thermal barrier in the
presence of SA. The TGA results showed that combining the SA into PP increased the
decomposition temperature.
3.4 BASED ON MECHANICAL PROPERTIES
EFFECTS OF ETHYLENE VINYL ACETATE CONTENT ON PHYSICAL AND
MECHANICAL PROPERTIES OF WOOD-PLASTIC COMPOSITES
To investigate the effects of different ethylene vinyl acetate (EVA) contents on the
performance of wood plastic composites (WPCs) made from poplar wood flour (PWF) and
high density polyethylene (HDPE), physical property tests, mechanical property tests and
scanning electron microscope (SEM) tests were employed. This research suggests that the
flexibility and mechanical properties of WPCs could be improved by adding EVA. The best
condition of EVA content could be 15%.
FABRICATION AND TESTING OF FIBER REINFORCED POLYMER
COMPOSITES MATERIAL
In this study, Sisal-glass fiber reinforced epoxy composite is developed and their mechanical
properties such as tensile strength, compression strength, flexural strength and impact
strength are evaluated. The interfacial properties, internal cracks and internal structure of the
fractured surfaces are evaluated using travelling microscope.
IMPROVEMENT OF SCRATCH AND WEAR RESISTANCE OF POLYMERS BY
FILLERS INCLUDING NANOFILLERS
Polymers have lower resistance to scratching and wear than metals. The inclusion of fillers
like micro particles or nano-particles shows improvement of tribological properties of
polymers. For example aluminum nano particles as fillers are more effective than
microparticles at the same overall volumetric concentration.
MECHANICAL CHARACTERIZATION OF THE TENSILE PROPERTIES OF
GLASS FIBER AND ITS REINFORCED POLYMER (GFRP) COMPOSITE UNDER
VARYING STRAIN RATES AND TEMPERATURES
Unidirectional glass fiber reinforced polymer (GFRP) is tested at four initial strain rates (25,
50, 100, 200 s-1) and six temperatures (-25, 0, 25, 50, 75 and 100˚C) on a servo-hydraulic
 29

high-rate testing system to investigate any possible effects on their mechanical properties and
failure patterns.
MECHANICAL TESTING OF HYBRID COMPOSITE MATERIAL (SISAL AND
COIR)
Evaluation of mechanical properties such as tensile strength, flexural strength and impact
strength for different fiber length and fiber volume fraction for Specimen 1 sisal 25% - coir
15%, Specimen 2 sisal 20% - coir 20%, Specimen 3 sisal 15% - coir 25%. Sisal and coir
fibers used as reinforcement materials with matrix of Epoxy resin to manufacturing of
composite plate by hand lay-up process and cut into that as per ASTM for testing of
materials.
PHYSICO-MECHANICAL BEHAVIOR OF THERMOPLASTIC CO-POLYESTER
ELASTOMER/ POLYTETRAFLUROETHYLENE COMPOSITE WITH SHORT
FIBERS AND MICROFILLERS
Short fibers and particulate fillers are known to enhance the mechanical properties of the
polymers. The influence of these fibers and fillers on the tensile, flexural, and impact
properties was investigated. All composite samples were fabricated using twin-screw extruder
followed by injection molding.
TESTING AND ANALYSIS OF MECHANICAL PROPERTIES OF E-GLASS FIBER
REINFORCED EPOXY POLYMER COMPOSITES
The present project works aims to prepare E-glass fiber based composite with percentage
variation of glass fiber content like 1%, 2% and 3% with using a bisphenol A as matrix
material and conducting the mechanical (tensile, compressive and flexural) testing on the
composite.
A PHYSICALLY-BASED ABRASIVE WEAR MODEL FOR COMPOSITE
MATERIALS
The size of this non-contributing portion (NCP) of reinforcement is estimated by modeling
three primary wear mechanisms, specifically, plowing, cracking at the matrix/reinforcement
interface or in the reinforcement, and particle removal. Critical variables describing the role
of the reinforcement, such as relative size, fracture toughness and the nature of the
matrix/reinforcement interface, are characterized by a single contribution coefficient,
 30

Predictions are compared with the results of experimental two-body (pin-on-drum) abrasive
wear tests performed on a model aluminum particulate-reinforced epoxy-matrix composite
material.
 31

CHAPTER 4
RESEARCH METHODOLOGY

Fig.4.1 Research Methodology Flow Chart

 32

CHAPTER 5
EXPERIMENTAL DETAILS
5.1 MATERIALS AND COMPOSITE PREPARATION
Poly Ethylene Vinyl Acetate containing 18% ethylene vinyl acetate copolymer resin,
designed for a variety of foam moulding application; manufactured by IPC an affiliate of
Sipchem in The Kingdom of Saudi Arabiausing an Exxon-Mobil high-pressuretubular
process. EVA 2518 CO exhibits low melting temperature, excellent processability, thermal
and mechancial properties. Vinyl acetate content is 18 by weight percentage is an injection
moulding grade and Profile extrusion grade. PEVA was procured from Speciality Polymer
Solutions, Chennai in granular form. Polytetrafluroethylene in fine powder form obtained
from Modoplast Company, Taltala, Kolkata. PTFE powder moulded by compression
moulding, free flow, Carbon 25%, Bronze 40 and 60%, Glass 25 and 40% and MOS2.
5.2 INJECTION MOLDING PROCESS
Injection Molding is a process in which molten polymer is forced under high pressure into
a mold cavity through an opening called sprue. Polymer material PEVA in form of pellets
and PTFE in form of particles are fed into an Injection Molding machine through a hopper.
Injection molding is a manufacturing process for producing parts by injecting molten material
into a mold. Material for the part is fed into a heated barrel, mixed (Using a helical shaped
screw), and injected (Forced) into a mold cavity, where it cools and hardens to the
configuration of the cavity. The whole injection molding process usual lasts from 2 seconds
to 2 minutes. There are four stages in the cycle. These stages are the clamping, injection,
cooling and ejection stages. Injection moulding machine is similar to Extruder. The main
difference between the two machines is in screw operation. In extruder screw rotates
continuously providing output of continuous long product (pipe, rod and sheet). Screw of
injection moulding machine is called reciprocating screw since it not only rotates but also
moves forward and backward according to the steps of the moulding cycle.
 33

Figure 5.1 Injection Moulding Machine

It acts as a ram in the filling step when the molten polymer is injected into the mould and
then it retracts backward in the moulding step. Heating elements, placed over the barrel,
soften and melt the polymer. The mould is equipped with a cooling system providing
controlled cooling and solidification of the material. The polymer is held in the mould until
solidification and then the mould opens and the part is removed from the mould by ejector
pins. Injection moulding machine is used mainly for manufacturing products made up of
Thermoplastics but Elastomers and Thermosets are also may be extruded. In this case cross-
linking occurs during heating and melting of the material in the heated barrel.
5.3 THERMAL PROPERTY TESTS
Thermal analysis and testing of polymers and plastics across the polymer supply chain
and lifecycle is a powerful means of measuring physical properties, transitions, ageing
processes, the effect of additives and the influence of0 diverse production conditions on
materials. Across many industries, it is essential that the properties of polymers, raw
materials and finished products are well understood as they are integral to enhancing the
performance of materials to meet specifications for the desired end-use, and within the
remit of product failure analysis. Our thermal analysis deploy a range of thermal
 34

techniques to reveal detailed understanding of polymer formulations, the impact of

processing and final physical properties of materials, accelerating your product
development process and delivering the insight you need to make decisions regarding
quality control, research and development or to address failure.
5.3.1 THERMAL CONDUCTIVITY MEASUREMENT

In general, steady-state techniques perform a measurement when the temperature of the

material measured does not change with time. This makes the signal analysis straightforward
(steady state implies constant signals). The disadvantage is that a well-engineered
experimental setup is usually needed. There are various modifications to these devices
depending on the temperatures and pressures needed as well as sample sizes. A sample of
unknown conductivity is placed between two samples of known conductivity (usually brass
plates). The setup is usually vertical with the hot brass plate at the top, the sample in between
then the cold brass plate at the bottom. Heat is supplied at the top and made to move
downwards to stop any convection within the sample. Measurements are taken after the
sample has reached to the steady state (with zero heat gradient or constant heat over entire
sample), this usually takes about 30 minutes and over.

5.3.2 OTHER THERMAL TESTS

Abbrevation Technique Response Measured

XRD X-ray diffraction Material structure

FTIR Fourier transform infrared Molecular finger prints
TGA Thermograivimetric analysis Weight change
___________________________________________________________________________
Table: 5.1 Common thermo analysis techniques.
5.3.2.1 X-RRAY DIFFRACTION (XRD)
To investigate the structure and degree of dispersion of prepared PEVA/PTFE composites,
a Bruker ECO D8 ADVANCE wide angle X-ray diffraction system (40 kW, 30 mA) was
utilized. The spacing was obtained according to Bragg’s law: d = nλ/2sinθ, where d is the
spacing between layers, λ is the wave length of X-ray (equals to 0.154 mm), θ is the angle
 35

wherein first peak in spectra takes place, and n corresponds to the order of diffraction, which
is assumed as 1 in calculations.
5.3.2.3 FOURIER TRANSFORM INFRA RED (FTIR)
Fourier Transform Infrared Spectroscopy, also known as FTIR Analysis or FTIR
Spectroscopy, is an analytical technique used to identify organic, polymeric, and, in some
cases, inorganic materials. The FTIR analysis method uses infrared light to scan test samples
and observe chemical properties. The FTIR instrument sends infrared radiation of about
10,000 to 100 cm-1 through a sample, with some radiation absorbed and some passed
through. The absorbed radiation is converted into rotational and/or vibrational energy by the
sample molecules. The resulting signal at the detector presents as a spectrum, typically from
4000 cm-1 to 400cm-1, representing a molecular fingerprint of the sample. Each molecule or
chemical structure will produce a unique spectral fingerprint, making FTIR analysis a great
tool for chemical identification.
5.3.2.4 THERMOGRAVIMETRIC ANALYSIS (TGA)
Thermo-gravimetric analysis (TGA) is a thermal analysis technique which measures the
amount and rate of change in the weight of a material as a function of temperature of time in
a controlled atmosphere. TGA measurements are particularly powerful when coupled with
knowledge of the chemistry of the sample, as one can then correlate changes in the weight of
the subject with its chemical state. All experiments were conducted in an inert atmosphere
with nitrogen atmosphere 100ml/min with a TA instruments Perkin Elmer thermal analysis
and heat rates 10˚C/min; recording mass loss and the rate of mass loss as a function of
temperature. Samples were cut into powder form and experiments were carried out in
platinum pans.
5.4 MECHANICAL PROPERTY TESTS
The physical and mechanical testing of polymers is a vital part of the product development
and production process. Mechanical, thermal, optical, rheological behavior and climate
testing allow the developers to understand their product better and introduce stronger quality
control. Physical and mechanical testing of polymers ensures that the material complies with
industry specifications. This applies to the aerospace, automotive, consumer, medical and
defense industries, amongst others. With the vast array of product types and additives
 36

available, understanding the capabilities and limitations of a material is a key concern to

suppliers, manufacturers and product developers on every level of the polymer industry.
Physical testing can help raw material suppliers and manufacturers to determine the
properties of their products through vast range of testing methods. Knowing when to apply
the most relevant technique to obtain the data needed requires specialist insight, knowledge
and experience. When a material or additive does not meet the user’s specifications, expert
interpretation and advice are highly required. The breadth of physical and mechanical testing
capability is vast and includes ASTM standards using industry specific methods.
5.4.1 TENSILE TEST
Prepared samples were cut into rectangular shape specimens along longitudinal direction.
The specimen had a gauge length of 250mm and a width of 25mm and a thickness 3mm. The
tensile tests were performed using a Hounsfield-H10KS machine with a load cell of 100 N.
The tensile speed was 5 mm/min.
5.4.2 FLEXURAL TEST
The flexural test measures the force required to bend a beam under three point loading
conditions. The data is often used to select materials for parts that will support loads without
flexing. Flexural modulus is used as an indication of a material’s stiffness when flexed. Since
the physical properties of many materials (especially thermoplastics) can vary depending on
ambient temperature, it is sometimes appropriate to test materials at temperatures that
simulate the intended end use environment. Most commonly the specimen lies on a support
span and the load is applied to the centre by the loading nose producing three points bending
at a specified rate. The parameters for this test are the support span, the speed of the loading,
and the maximum deflection for the test. These parameters are based on the test specimen
thickness and are defined differently by ASTM. For ASTM D790, the test is stopped when
the specimen reaches 5% deflection or the specimen breaks before 5%. If the specimen does
not break, the test is continued as far a possible and the stress at 3.5% (conventional
deflection) is reported.

5.4.3 OPTICAL MICROSCOPY TEST

 37

Microscopy analysis of polymers provides a means to study and characterize the micro
and nano-structural features of polymers, composites and products. The magnification offered
by optical or electron microscopy can be used to obtain chemical information.
The magnification is obtained via a two-lens system, referred to as the objective and the
eyepiece, respectively. The maximum magnification obtained is about 2000x. Surface
topography is studied in reflected light mode. Bulk structure is studied with the light
transmitted through the specimen – More often used for polymers – Sample thickness
important, usually 5-40 mm.
5.3.4 WEAR TEST

Wear test is carried out to predict the wear performance and to investigate the wear
mechanism. From a material point of view, the test is performed to evaluate the wear
property of a material so as to determine whether the material is adequate for a specific
wear application. From a surface engineering point of view, wear test is carried out to
evaluate the potential of using a certain surface engineering technology to reduce wear for a
specific application, and to investigate the effect of treatment conditions (processing
parameters) on the wear performance, so that optimised surface treatment conditions can be
realised.
Coefficient of friction test (Static and kinetic) as per ASTM D 1894 were performed. This
test method covers a laboratory procedure for determining the wear of plastic composite
materials during sliding using a pin-on-disk setup. Materials are tested in pairs under
nominally non-abrasive conditions. For the pin-on-disk wear test, two specimens are
required. One, a pin or ball that is positioned perpendicular to the other, usually a flat circular
disk. The tester causes stationary pin/ball to press against the rotating disk at a known force
and speed. During the test COF, friction, wear etc. parameters are measured and reported.
The volume addresses the complex nature of plastic composite wear, from various
mechanisms by which polymer composites can wear and factors that influence these modes,
to the influence of contact and environmental conditions on wear. The results presented
clearly indicate that useful and effective wear tests exist and that they can be developed for a
given application.
 38

Wear measurement is carried out to determine the amount of materials removed (or worn
away) after a wear test, (and in reality after a part in service for a period of time – 30
minutes). The material worn away can be expressed either as weight (mass) loss, volume
loss, or linear dimension change depending on the purpose of the test, the type of wear, the
geometry and size of the test specimens, and on the availability of a measurement facility.
Common techniques of wear measurement include using a precision balance to measure the
weight (mass) loss, profiling surfaces, or using a microscope to measure the wear depth or
cross-sectional area of a wear track so as to determine the wear volume loss or linear
dimensional change.
Mass loss measurement by a precision balance is a convenient method for wear
measurement, especially when the worn surface is irregular and unsymmetrical in shape.
Sample to be measured is carefully cleaned, and the weight is measured before and after a
wear test. The difference in weight before and after test represents the weight loss caused by
wear. The unit can be gram (g) or milligram (µg).
Wear volume is normally calculated from the wear track (scar) depth, length, width
and/or scar profile according to the geometry of the wear track/scar. A surface profilometer,
e.g. a stylus type, or sometimes a microscope with scale is used for the measurement. The
reporting unit of wear volume loss is mm3 or µm3. Wear volume loss enables a better
comparison of wear among materials having different densities. However, it is not easy to
measure volume loss when a wear track is irregular. In this case, mass loss may be measured
first, and the volume loss is calculated if the material is uniform and its density is known.
Measuring wear by linear dimension change is very useful in many engineering
situations, where certain dimension such as length, thickness or diameter is more critical to
the normal function of the system. A surface profilometer, e.g. a stylus type, a micrometer or
a microscope can be used. The unit for linear dimension loss can be µm or mm.
 39

CHAPTER 6
REPORT ON THE PRESENT INVESTIGATION
6.1 THERMAL CONDUCTIVITY REPORT

The thermal conductivity ‘k’, values obtained from Lee’s disc apparatus in W/mK for the
different samples under steady state condition with mean temperature 55˚C of heat flow from
the top of the specimen was obtained from Central Institute of Plastics Engineering and
Technology were given as bar chart. The ‘k’ value for Sample 1 – PEVA is 0.201 W/mK and
‘k’ value for Sample 2 – PEVA+10%PTFE is 0.211 W/mK, which has improvement of 5%
and ‘k’ value for Sample 3 – PEVA+20%PTFE is 0.226 W/mK which has improvement for
12.5% (Rasheed Al Mizan and Md. Aminul Islam, 2018).

Table 6.1 Comparison of Thermal Conductivity

Composite materials Thermal Conductivity (W/m˚K)
PEVA 0.201
PEVA+10%PTFE 0.211
PEVA+20%PTFE 0.226

Fig. 6.1 Thermal conductivity for different composition of composite

materials
 40

6.2 FTIR report

RAMAN spectroscopy was used in our studies for baseline chemical characterization
and monitoring changes related to age. The key areas of interest, namely the double bonds,
are usually expressed as strong absorption peaks within 1500-1900 cm-1. In comparison, the
carbonyls show relatively weak signals within 1680-1820 cm-1. Figure provides a summary
of the results from RAMAN spectroscopy. This shows the carbonyl signals which are
typically weak responses in RAMAN. The method is however; highly sensitive to unsaturated
double bonds and our studies suggest that these species are not present within the base resin
and not produced through ageing of the resins at temperature up to 75˚C. Figure show the
chemical changes on heating the unfilled material to temperatures exceeding 270˚C. Under
such conditions, the material undergoes significant changes in the carbon skeleton with
reduction of acetate groups (C=O) and a small but significant reduction in the main chain
polyethylene (–CH2-) signal arising presumably through oxidative degradation of the
polyethylene segments of the EVA. A key observation is the production of unsaturated
double bond species within the backbone. The generation of these species from poly
(ethylene-vinyl acetate) and/or poly (vinyl alcohol) materials is explained in the open
literature by de-acetylation and dehydration mechanisms. These elimination reactions result
in the loss of acetic acid and moisture and the production of conjugated polyenes and non-
conjugated polyenes species of the type depicted in Figure.
 41

Fig 6.2 FTIR graph

6.3 X-RAY DIFFRACTOMETER (XRD) Report

This thermal property determination test performed at VIT-Vellore. The test specimens used
for this are in the powder form obtained by hacksawing. The XRD data were collected on a
Bruker AXS diffractometer using Cu Kα radiation (λ = 0.1505945 mm) with a 0.02 2θ step
size and a 2s count time. Samples used for XRD were hacksawed to a particle size of <40 μm
and placed in a horizontal configuration (reflection) for collection of XRD data. All PEVA
and PEVA/PTFE composite samples were analyzed in synchronous rotation mode. The X-ray
diffraction (XRD) analysis is a very useful method used to describe the extent of intercalation
and exfoliation of the composite having layered structure.
 42

Fig 6.3 XRD graph for Sample 1, 2 and 3

6.5 THERMOGRAVIMETRIC ANALYSER (TGA)

The TGA report obtained from Sophisticated Analytical Instruments Facility, STIC,
Cochin University, raw data are analyzed and curves are drawn using the experimental values
conducted at a range of increasing temperature values 10˚C/min. as origin graph and plotted
below. For PEVA there is an evidence for the thermal degradation in two-steps [8]. The first
stage completed at around 390˚C, with long radius of curvature suggests a slow rate of
degradation process with high thermal stability. The second stage has sharp bend with less
radius of curvature and degradation process ends at fast rate (within the interval of 465-550˚
C). It is evident from the graph that due to the addition of PTFE particle and curve appears to
be three-step thermal degradation process. For composites PEVA+10%PTFE and
PEVA+20%PTFE degradation process increases up to 610˚C and 625˚C respectively for zero
percentage weight loss.
 43

Fig. 6.4 TGA test report of PEVA & PEVA Composites

From the Table 6.1 given below it was observed that the 5% weight loss degradation
temperatures for all the three samples are same. It was also noticed that 50% weight loss
temperature and peak temperature values obtained during degradation are more for
composites blended with PTFE powder samples. The same ratio of percentage weight loss
prevails till 75% and beyond that composite with 10%PTFE and 20%PTFE withstands alone
at very high degradation temperature of 610˚C and 625˚C respectively.

Table 6.2. The TGA data for PEVA and PEVA/PTFE particle composites
Samples T-5 wt% degradation T-50 wt% degradation Tmax
(˚C) (˚C) (˚C)
Sample 1 PEVA 390 465 550
Sample 2 PEVA+10% PTFE 390 480 610
Sample 3 PEVA+20% PTFE 390 480 625

6.6 TENSILE STRENGTH REPORT

Tensile strength is the property describing a material’s ability to withstand maximum load
until its failure condition. It is well known that tensile strength of the composite is dependent
on such factors as Polymer-filler interaction and filler characteristic, namely type and shape
of filler. From the obtained results it is observed that composites filled by (10% Wt.) PTFE
exhibited maximum tensile strength. From the literature review we can observed that PTFE
particles having good tensile strength property because PTFE powder enhances the bonding
strength. It is also observed that composites filled by (20% Wt.) PTFE exhibited good tensile
strength than Sample 1 pure PEVA.
 44

Table 6.3 Comparison of Tensile strength

Composite materials Tensile strength(N/mm2) Elongation (%)
PEVA 4.33 373.13
PEVA+10%PTFE 4.47 237.31
PEVA+20%PTFE 3.18 116.67

Fig. 6.5 Tensile strength for different composition of composite materials

6.7 FLEXURAL STRENGTH TEST REPORT

From the experimental results it is observed that increase the addition of PTFE to SAN
decreases the flexural strength, here the filler PTFE binds the matrix and prevents it from
expanding as much as it would on its own. Subsequently, this would affect the bending
strength of the composite system. The many studies have shown that materials with filler
content leads to a lower flexural strength. Composites filled by (10% Vol.) exhibited low
flexural strength when compared with other (20% Vol.) composites this is due to that 10%
PTFE having reduced bending strength and good dimensional stability. 10% PTFE filled
composites exhibited good bending strength.
 45

Table 6.4 Comparison of flexural strength of TPR composites

Composite materials Flexural Strength
(N/mm2)
PEVA 0.86
PEVA+10%PTFE 0.89
PEVA+20%PTFE 0.76

Fig. 6.6 Flexural strength for different composition of composite materials

6.8 Optical Microscopy Test
The Optical microscopy analysis was done by Motic optical microscope at
International Research Centre, KARE, India were presented as images, which
described the composite innovation technology effectively utilized to disperse the
PTFE particles in the PEVA matrix. The particle distribution was effective and
achieved successfully on behalf of melt mixing to obtain tailor made composite
samples by Injection molding technique.
 46

Fig. 6.7 Images of PEVA matrix

Fig. 6.8 Images of 10% PTFE particle fillers in PEVA matrix

Fig. 6.9 Images of 20% PTFE particle fillers in PEVA matrix

6.9 WEAR TEST REPORT

An apparatus for wear testing is termed as wear tester, tribotester or tribometer. The
prefix of "tribo-" refers to wear, friction and lubrication. Many, probably more than several
 47

hundreds, different wear testing arrangements and procedures are used in laboratories
around the world and described in technical literature. However big difference of one
arrangement as compared with another, a wear tester will always involve two components
loaded against and relatively moving each other. The movement can be driven by a motor
or by an electro-magnetic device. For convenient purpose, the material or component being
investigated is normally referred to as specimen, the other termed as counter face. The load
applied on the counter face and sliding distance is found to be 500m as per calculation by
taking diameter of disc 120mm and velocity 2.3 m/s.
Table 6.5 Comparison of Wear Resistance of SAN composites
Composite materials Weight Wear Specific COF
Loss Volume Loss Wear rate
(gms) (mm3) (mm3/Nm)
Sample 1 PEVA 0.08 142 0.0071 0.284
Sample 2 PEVA + 10% PTFE 0.07 155 0.0155 0.31
Sample 3 PEVA + 20% PTFE 0.09 153 0.0153 0.306

From the results obtained sample 2 (10%PTFE blended by wt.%) composite having more
wear resistance property, i.e., mass loss during the test is very low, when compared with
other two samples given in table. Sample 3 (20%PTFE blended by wt.%) also performs
better result in wear resistance, when compared with pure PEVA. The specific wear rate W s
of the specimens were calculated by using the equation,

Ws = (∆m)/ρ. FN. L (mm3/Nm)

Where ∆m is the mass loss, ρ is the density of the specimen, F N is the normal load applied
and L is the distance travelled by sliding.

CHAPTER 7
RESULTS AND DISCUSSIONS
 48

From the obtained results it is observed that composites filled by (10% weight) PTFE
exhibited maximum thermal conductivity. From the literature review we can observed that
PTFE particles having good thermal conductivity property because PTFE powder enhances
the heat transfer rate. It is also observed that composites filled by (20% weight) PTFE
exhibited good thermal conductivity than Sample 1 PEVA

From the obtained results it is observed that composites filled by (10% weight) PTFE
exhibited good mechanical properties. From the literature review we can observed that PTFE
particles having good tensile property because PTFE powder enhances the elongation rate. It
is also observed that composites filled by (20% weight) PTFE exhibited good impact strength
than Sample 1 PEVA.

From the experimental results it is observed that increase the addition of PTFE to PEVA
decreases the flexural or bending strength, here the filler PTFE binds the matrix and prevents
it from bending as much as it would on its own. Subsequently, this would affect the flexural
strength of the composite system. The many studies have shown that materials with filler
content leads to a lower wear resistance. Composites filled by (10% by weight) exhibited low
wear resistance when compared with other (20% by weight) composites this is due to that
10% PTFE having reduced wear strength and good dimensional stability. 10% PTFE filled
composites exhibited good wear resistance.

CHAPTER 8
CONCLUSION
 49

From the obtained results it is observed that composites filled by (10% by weight)
PTFE exhibited maximum thermal conductivity. From the literature review we can observed
that PTFE particles having good thermal conductivity property because PTFE powder
enhances the heat transfer rate. It is also observed that composites filled by (20% by weight)
PTFE exhibited good thermal conductivity than Sample 1 PEVA.
From the obtained results it is observed that composites filled by (10% by weight)
PTFE exhibited maximum tensile strength. From the literature review we can observed that
PTFE particles having good tensile strength property because PTFE powder enhances the
elongation rate. It is also observed that composites filled by (20% by weight) PTFE exhibited
good flexural strength than Sample 1 PEVA.
From the experimental results it is observed that increase the addition of PTFE to
PEVA decreases the wear property, here the filler PTFE binds the matrix and prevents it from
wear as much as it would on its own. Subsequently, this would affect the wear resistance of
the composite system. The many studies have shown that materials with filler content leads to
a higher impact strength. Composites filled by (10% by weight) exhibited high impact
strength when compared with other (20% by weight) composites this is due to that 10% PTFE
having improved wear resistance and good dimensional stability. 10% PTFE filled
composites exhibited good mechanical properties.

CHAPTER 9
 50

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