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Major Project Report - 1602100054
Major Project Report - 1602100054
ON
B. TECH
In
Submitted By:
ODISHA
JULY 2020
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DECLARATION
I, Swagat Suman Naik (Regd. No.-1602100054), a student of B. Tech (Semester- VIII)
of the Veer Surendra Sai University of Technology, Odisha hereby declare that the major project
report entitled “Synthesize & Characterization of Planetary Milled Alumina/Epoxy
Composite” is an original work and data provided in the study is authentic to the best of our
knowledge. This report has not been submitted to any other institute for the award of any degree.
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ACKNOWLEDGEMENT
It is our pleasure to be indebted to various people, who directly or indirectly contribute to the
development of this work and who influenced our thinking, behavior and acts during the course
of study.
I am thankful to Dr. B. B. Pani and Mr. Dinesh Kumar Mishra for their support, co-operation
and motivation provided to me during the major project for constant inspiration, presence and
blessings.
I would like to thank Dr. Pinaki Chatterjee from Laboratory of Advanced Research in
Polymeric Materials (LARPM), CIPET, Bhubaneswar to guide me through the fabrication of
Epoxy- Alumina Composites of varied composition through hand lay-up method.
I also extend our appreciation to the faculties of our department who provided their valuable
suggestions and precious time in accomplishing my major project report.
Lastly, I would like to thank the almighty and our parents for their moral support and our friends
with whom I shared my day-to day experience and received lots of suggestions that my quality
of work.
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VEER SURENDRA SAI UNIVERSITY OF TECHNOLOGY:
ODISHA
CERTIFICATE
This is to certify that the major project report entitled “Synthesize & Characterization of
Planetary Milled Alumina/Epoxy Composite” submitted by SWAGAT SUMAN NAIK
(1602100054) in the partial fulfilment of the requirement for the award of the degree of
Bachelor of Technology from the Department of Metallurgical & Materials Engineering, Veer
Surendra Sai University of Technology, is a record of candidate’s own work carried out by
them. The matter embodied in this report has not been submitted in part or full to any other
university or institute for the award of any degree.
This is to certify that above statement made by the candidate is correct to the best of our
knowledge.
Approved by:
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CONTENTS
1. INTRODUCTION 08
2. THEORY 10-18
2.1 Composite 10
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3. LITERATURE REVIEW 19
6. CONCLUSION 30
7. FUTURE WORK 31
8. REFERENCE 32
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LIST OF FIGURES:
Fig. 4.4 Resin mixed ingredients are infused on the surface to spread on the whole mould
Fig. 4.5 Roller for removal of trapped air bubbles and the excess of polymer
Fig. 5.2 55 wt.% Epoxy- 45 wt.% Alumina Composition (Milling Time- 5 Hours)
Fig. 5.4 55 wt.% Epoxy- 45 wt.% Alumina Composition (Milling Time- 0 Hour)
Fig. 5.5 65 wt.% Epoxy- 35 wt.% Alumina Composition (Milling Time- 0 Hour)
Fig. 5.6 65 wt.% Epoxy- 35 wt.% Alumina Composition (Milling Time- 5 Hours)
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1. INTRODUCTION
Epoxy is the most common type of matrix used in a ceramic matrix composite. It refers
to any of the basic components or cured end products of epoxy resins, as well as a
colloquial name for the epoxide functional group.
Resins have excellent processability, low cost, low density, and good chemical
resistance but some of its limitations like low stiffness and strength, low impact
resistance, and poor resistance to crack propagation restrict their usage in high
performance applications.
Epoxies are commonly modified by the inclusion of inorganic- particulate fillers, such
as silica, alumina, mica or talc. Fillers are added to epoxy resins to improve fracture
toughness and electrical or heat transfer properties, to increase resin stiffness, flame
retardance, and wear resistance, and to reduce the coefficient of thermal expansion.
The resulting composite specimens have applications as automobile parts, dental
restoratives, and electronic packaging/underfill for circuit cards. Many variables (e.g.
resin crosslink density, particle type, size, size distribution, and filler loading) can affect
the composite's thermal, electrical, mechanical and fracture properties.
Rubber fillers increase fracture toughness with cracks propagating via cavitation and
shear yielding phenomena, but decrease the flexural and Young's moduli.
Alumina is a well-known ceramic material with low cost, nontoxic, stable, inert, high
corrosion, and high temperature resistance. Because of these properties alumina was
chosen as the reinforcing phase in epoxy matrix. So, epoxy alumina composites counter
the negatives of each individual component.
As we know that, with the decrease in particle size, strength increases due to decrease
in the surface area. As per Hall-Petch equation,
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1.1. OBJECTIVES & APPLICATIONS
OBJECTIVES:
Development of polymer-based composites with simultaneously high thermal conductivity and
breakdown strength has attracted considerable attention owing to their important applications
in both electronic and electric industries.
In this study, we successfully design novel epoxy-based composites with epoxy alumina
composite layer sandwiched between micro-epoxy alumina epoxy composite layers, which
how synergistically and significantly enhanced thermal conductivity and breakdown strength.
APPLICATIONS:
The excellent overall properties of SiO2/Al2O3 filled epoxy composites may opens up avenues of
new applications of epoxy composites.
Innovative product development for automotive industry, electronics, coatings and many other
applications are promising applications for these composites.
In this research investigation, the properties of various polymeric insulation containing certain
weight fraction of SiO2/Al2O3/ZnO in epoxy resin can be considered.
While designing the base board of insulated gate bipolar transistor, it is necessary to optimize both
the breakdown strength of the gate dielectric and the electric field distribution in the device. In the
field of more conventional electrical insulation, it seems possible to generate composites
exhibiting a dielectric constant and dissipation factor that are lower than that of either of the
constituent components. It has been suggested that this counterintuitive result is due to polymer
chain immobilization at the interfaces.
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2. THEORY
2.1 COMPOSITE
A Composite is a combination of two materials in which one of the materials, called the
reinforcing phase, is in the form of fibers, sheets, or particles, and is embedded in the other
materials called the matrix phase. The reinforcing material and the matrix material can be
metal, ceramic, or polymer.
Merits of Composite-
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HAND LAY-UP-
Hand lay-up is the most common and least expensive open-molding method because it
requires the least amount of equipment. Fiber reinforcements are placed by hand in a mold and
resin is applied with a brush or roller. This process is used to make both large and small items,
including boats, storage tanks, tubs and shower.
SPRAY-UP-
Spray-up is similar to hand lay-up but uses special equipment—most notably a chopper
gun—to cut reinforcement material into short fibers, add them to resin and deposit the mixture
(called chop) onto a molding surface. Spray-up is more automated than hand lay-up and is
typically used to produce large quantities.
FILAMENT WINDING-
Resin transfer molding (RTM), sometimes called liquid molding, is a closed-molding method in
which reinforcement material is loaded into a closed mold, the mold is clamped, and resin is pumped
in (through injection ports) under pressure.
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COMPRESSION MOLDING-
Compression molding is a manufacturing process in which composite materials are sandwiched
between two matching molds under intense pressure and heat (from 250° to 400° F) until the part cures.
PULTRUSION-
Pultrusion is used to form composites into long, consistent shapes like rods or bars. Continuous
strands of reinforcement are pulled through a resin bath to saturate them, then pulled through heated
steel molds that sculpt the composites into continuous lengths.
CENTRIFUGAL CASTING -
In centrifugal casting, reinforcements and resin are deposited against the inside surface of a rotating
mold. Centrifugal force holds them in place until the material cures or hardens.
FILAMENT WINDING -
Filament winding is an automated process that applies resin-saturated, continuous strands
of fiber reinforcements over a rotating cylindrical mold. It’s used for creating hollow products like
rocket motor casings, pipes, stacks, and chemical storage tanks. Filament winding is less labor-intense
than other open-molding processes.
Gel coat is a specialized polyester resin that is formulated to provide a cosmetic outer
surface on a composite product, and to provide weather-ability for outdoor products. Gel coat
consists of a base resin and additives.
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SOLID SURFACE MOLDING -
Solid surface products (also known as densified products) consist of a cast matrix without a gel-coated
surface. A vacuum can be used to remove entrapped air in the matrix. Solid surface products offer limitless
design styles.
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2.6 OPTICAL MICROSCOPY
The optical microscope is also called the light microscope, uses a combination of light and lenses
to magnify an image.
Optical microscope are used in the viewing of small objects such as cells. This type of microscope
does not offer the highest magnification and so when viewing a cell has limited structures.
Optical microscopy is extensively used in microelectronics, nanophysics, biotechnology,
pharmaceutic research and mineralogy.
The major imaging principle of optical microscope is that an objective lens with very short focal
length is used to form a highly magnified real image of the object.
The best resolution for an optical microscope is about 0.2 microns= 200nm
Although, optical microscopy has a long established characterized technique. These involve higher
resolution, higher speed of data, acquisition, more quantitative results or more sensitive detection.
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2.7 FTIR SPECTROSCOPY
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2.8 TERMINOLOGIES:
2.8.2 RESINS
The matrix of the composite to ‘bind’ the composite
materials together and transfer the component stresses that
may act on the part to the fibers in the composite. In this lab,
a two-part epoxy and hardener (accelerator) resin system will
be used.
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2.8.4 WORK STATION PREPARATION
Initial preparation of materials and tools is standard
procedure when working with composites. Once resin and
hardener are mixed, the “working time” – amount of time
an epoxy remains viscous enough that it can be still be easily
applied, prior to the resin mix curing - is limited by the speed
of the hardener chemically reacting with the epoxy
producing an exothermic reaction. Student must prepare
ALL materials and supplies, and set up before proceeding.
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2.8.7 RESIN STARVED
Localized area lacking enough resin to wet
out the fiber.
2.8.8 DELAMINATION
Separation of the laminate, along the
layers.
Fig.2.10 Delamination
2.8.9 VOID
Air trapped and cured in the laminate. Voids
will not allow the transmission of stresses to the load
and can result in premature failure of the part that
could be catastrophic failure.
Fig. 2.11
Void
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CHAPTER 3
LITERATURE REVIEW
3.1. Devaraj.Eand et.al. worked on study of mechanical and wear behaviour of carbon fiber
reinforced epoxy resin composites with alumina filler additions and found that 4% alumina
filler content display better tensile characteristic and 2% filler content has highest surface
mechanical performance of epoxy/glass fiber hybrid composites” and found that the hardness
and impact energy increases as compared to other modifiers. Procedia Materials Science6
(2014) 1359-1364.
3.3. Oladapo A Akinyede et.al worked on static and dynamic loading behaviour of hybrid
epoxy composite with alumina nanoparticles and found that there is an increase of 18% to 29%
fracture toughness for the resin and fibre over the traditional epoxy composite. (2007/01/01).
A. Tessema, D. Zhao, J. Moll et.al worked on effect of filler loading, geometry, dispersion and
temperature on thermal conductivity of polymer nanocomposites, polymer testing and found that
the effective thermal conductivity (Ke), of the polymer nanocomposites increases with increase
& the effective thermal conductivity as a function of temperature for epoxy silica composites.
The effective thermal conductivity increses linearly with temperature. Vol. 57, 1011062017
(2017).
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CHAPTER 4
EXPERIMENTAL PROCEDURE
(a) Alumina (Al2O3) (b) Epoxy: LY556 (c) Hardener: HY951 (d) Tissue Paper (e) Zip tie
(f) Cotton (g) Toluene (Methyl Benzene- C7 H8) (h) Silicon oil.
Used to obtain Nano crystalline structure from either single phase or multiphase
materials. It uses steels or refractory balls.
It is applicable for synthesis of ceramic or metallic nanomaterial.
When the ball rotator at a particular RPM, the necessary energy is transformed to the
powder, which in turn reduces the powder of coarse grain size structure to ultrafine
grain structure.
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The energy transformed to the powder from the ball depends on many factor.
Such as-
a) Rotation speed of the ball
b) Size of the ball
c) Number of balls
d) Milling time
e) Ratio of ball to powder
f) Milling medium or Atmosphere
e.g. - Liquid Nitrogen, Cryogenic atmosphere
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4.4 HAND LAY-UP TECHNIQUE
Fig. 4.2
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Then, a thin plastic sheet is applied at the top &
bottom of the molld plate to get a smooth surface
of the product. The layers of woven
reinforcement are cut to required shapes and
placed on the surface of the mould.
Fig. 4.3
Fig. 4.4
Fig. 4.5
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A load of 20kg is applied. The mould is then
closed and pressure is released to obtain a single
mat.
Fig. 4.6
Fig. 4.7
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CHAPTER 5
5.1 RESULTS
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Fig. 5.4 Optical images of 55 wt.% epoxy- 45 wt.% Alumina Composition
(Milling Time- 0 Hour)
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Fig. 5.6 Optical images of 65 wt.% Epoxy- 35 wt.% Alumina Composition
(Milling Time- 5 Hours)
5.2 DISCUSSIONS
In general, a more rough fracture surface with evidence of crack-tip pinning and bowing indicates
that more energy is absorbed during fracture, and it could also be seen as a confirmation of the
higher mechanical properties.
It should be noted, however, that the resolution of the scanning electron micrographs is too low to
detect any energy absorbing mechanisms.
Testing revealed that the stiffness, or the modulus, of the epoxy polymer was improved when
alumina was added, even at very low concentrations of alumina. This effect was observed also
when agglomerates of the Al2O3 were present in the composites. The resolution of the micrographs
is too low to detect individual whiskers or particles, but the agglomeration indicates that relatively
strong intermolecular forces are acting between the whiskers.
This is expected to represent a challenge with respect to the dispersion of alumina in a given
solvent, e.g. epoxy curing agents, as large forces are required to separate the particles from one
another. In fact, difficulties to obtain a high degree of dispersion were observed.
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However, it seems that the removal of the solvent in which the surface treatment was conducted
may have led to some re-agglomeration of the alumina as relatively large clumps, or agglomerates,
were observed. Nevertheless, after dispersion in the anhydride, these agglomerates were no longer
observed in the alumina/anhydride dispersions, indicating weaker interfacial interactions between
the particles after surface-modification.
The fracture surface of the neat epoxy polymer was relatively smooth around the crack initiation
site, and rougher and more three-dimensional towards the opposite side of the specimen. This
corresponds well to previously reported fracture surfaces of unfilled epoxies with blunt pre-cracks.
Also, debonding between the agglomerated whiskers and the epoxy was observed.
When it comes to the thermal dispersion problem, these composites cannot meet the requirements
in the aerospace electrical and electronic components due to their poor thermal conductivity and
weak resistance to high temperature.
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CHAPTER 6
CONLUSION
This study has demonstrated a novel approach to improve the thermal properties of epoxy
composites. It is an important class of thermoset polymer, which is widely used in polymer
composites.
Epoxy composites of varied Al2O3 composition with optimized mechanical properties can be used
in wide range of applications.
The investigated Al2O3 act differently on the complex permittivity of the composite resin.
Compared to the reference neat resins the non-porous alumina tend to increase the relative
permittivity values, while the porous Al2O3 fillers tend to reduce them.
Factors that affect the properties of composites most significantly are observed to be filler loading,
interface between matrix and filler, mechanical loading, etc. It owns to its excellent electrical
insulation, chemical resistance, mechanical properties and low cost
Hence, after the evaluation of phases which can be determined through Scanning Election
Microscopy (SEM), XRD; we can get a brief idea regarding its phase transformation. Then, by
conducting various mechanical tests like tension test, impact test, fractural strength, etc. it's
mechanical properties can be attributed.
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CHAPTER 7
FUTURE WORK
Further research may be required but is not limited to the following areas:
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CHAPTER 8
REFERENCE
[1] Oladapo A Akinyede, Ram Mohan, Ajit Kelkar, Jagannathan Sankar. “Static And
Dynamic Loading Behaviour Of Hybrid Epoxy Composite With Alumina Nanoparticles”. 16th
[2] Ramesh K. Nayak, Alina Dash and B.C.Ray.” Effect of epoxy modifiers
[3] M.T. Tilbrook, R.J. Moon, M. Hoffman∗.”On the mechanical properties of alumina–
epoxy composites with an Interpenetrating network structure”. School of Materials Science and
Received 17 June 2004; received in revised form 4 October 2004; accepted 4 October 2004.
[4] G.X. Glenis, G. Papalabris, Th.G. Argyropoulos and C.T. Dervos.” Dielectric
[5] Wisnom M. R.: Nonlinear analysis of misaligned unidirectional carbon fibre-epoxy compression
DOI: 10.1016/0961-9526(93)90051-K.
mechanical properties of Al2O3/ polymer laminate composite. Composite Science and Technology.
[7] Gillespie J W, T.M., McKnight S H, Palmese G R. Use of silane coupling agents to enhance the