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STUDY OF THE MEDIUM DENSITY POLYETHYLENE MECHANICAL
MILLED WITH THE GRAPHITE POWDER
CHEAH WOI LEONG
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TABLE OF CONTENTS
Pages
TITLE PAGE i
TABLE OF CONTENTS ii
LIST OF TABLES iiiLIST OF FIGURES iv
LIST OF APPENDIX v
LIST OF ABBREVIATIONS vi
CHAPTER 1 INTRODUCTION
1.1 Research Background 1
1.2 Problem Statement 2
1.3 Objectives 2
CHAPTER 2 LITERATURE REVIEW
2.1 Polyethylene-graphite nanocomposite 3
2.2 Graphite 4
2.3 Polyethylene (PE) 4
2.4 Medium Density Polyethylene (MDPE) 6
2.5 Mechanical Milling Method 8
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LIST OF TABLES
Tables No. Page
3.1 Instruments and method 9
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LIST OF FIGURES
Figures No. Page
2.1 Polyethylene chain with side branches 6
3.1 Condition for constructive interference 11
3.2 Sample preparation and etching process 13
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LIST OF APPENDIX
Tables No. Page
A1 commercially produced metallocenes 17
A2 Gantt chart proposal 2010 20
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LIST OF ABBREVIATIONS
Abbreviations
DENT Double Edge Notched Tensile
FNCT Full Notched Creep Tensile
FTIR Fourier Transform Infrared Spectroscopy
HDPE high density polyethylene
IUPAC International Union of Pure and Applied Chemistry
MA Mechanical Alloying
MD Mechanical Disordering
MDPE Medium Density Polyethylenemf mass at the end of temperature, T
MG Mechanical Grinding
ML percentage loss of mass
MM Mechanical Milling
ms mass at the start, before heating
PE Polyethylene
PE100 PE water pipes ISO 4427, an HDPE material
PMC P l M i C i
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CHAPTER 1
INTRODUCTION
1.1 Research Background
Many researchers do relate the conductivity to polymer matrices with respect to the
presence of polymer groups, polymer surface tension and different blends of polymer.
One influencing factor that has not been dealt with is the compatibility of polymer
t i ith d ti fill hi h d h b t ti l ff t d ti it
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diffraction (XRD), Scanning electron microscope (SEM), and Thermogravimetry
(TGA).
1.2 Problem Statement
According to the research of Hamouda et al. (2006). Creep fracture by slow crack
growth is studied in a medium density polyethylene at 60 C and 80 C. Whereas
elasticplastic fracture mechanics load parameters fail to provide a unique
temperature-independent correlation, that of the fracture mechanics for creeping solids
is proved to be relevant since this parameter correlates very well with the time to
failure.
Slow crack growth (SCG) behaviour has been investigated under creep conditions in a
medium density ethylenebutene copolymer (MDPE) on both axisymmetrical Full
Notched Creep Tensile (FNCT) and Double Edge Notched Tensile (DENT) samples
tested at 60 C. Fracture Mechanics for Creeping Solids approach was attempted for
the present medium density polyethylene used for gas-pipe networks. The creep load
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Chapter 2
LITERATURE REVIEW
2.1 Polyethylene-graphite Nanocomposite
This research conducted a mixture of both a new and modified research. The research
will carry out the characterization of the MDPE-graphite composite and determine the
chemical properties and mechanical properties. Some of the researchers have also
t ti t d i th ff t f th th l t i it f h i l
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2.2 Graphite
In recent years, The raw materials most frequently used in graphite manufacturing are
some types of coke, carbon black and natural graphite, which are ground, sieved and
added to a binder. The paste at this stage is homogenized and placed in molds or
passed through drawing frames, sufficiently compacted. The material is then baked
slowly, protected by coke powder, at a temperature of at least 1000 C for complete
elimination of volatile particles from the binder and to transform the remaining
particles into coke.
In principle, graphite is normally classified by grain size. The grain size is used as a
criteria because most of the other properties and characteristics of graphite are related
directly or indirectly to the grain size and orientation. Nowadays, the market offers
graphite classes with average grain sizes under 1m up to 20m.
Due to its low mechanical strength, graphite is considered to be easily machined.
However, complications arise in the cutting of this material due to the layered
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Polyethylene (PE) is a natural, organic, thermoplastic homopolymer which does not
melt at one particular temperature into a clean liquid. Instead it becomes increasingly
soft and ultimately turns into a very viscous, tacky molten mass. It has a low Tg as
strong intermolecular cohesive forces are absent and the substituent group (CH2)
present in it is not bulky. PE is a polymer consisting of long chains of the monomer
ethylene (IUPAC name ethene). Polyethylene is classified into several different
categories based mostly on its density and branching. The mechanical properties of PE
depend on variables such as the extent and type of branching, the crystal structure, and
the molecular weight. (Kosuri et al. , 2008)
Some classifications of PE include:
Ultra high molecular weight PE (UHMWPE)
High density PE (HDPE)
Cross-linked PE (PEX)
Medium density PE (MDPE)
Linear low density PE (LLDPE)
Low density PE (LDPE)
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2.4 Medium Density Polyethylene (MDPE)
Medium-density polyethylene, MDPE, is a semi-crystalline thermoplastic polymer
which has been increasingly used for fabrication of plastic pipes for water and gas
distribution systems. (Peres et al. , 2010)
MDPE viscoelastic characteristics at room temperature, it is susceptible to long term
creep fracture by means of a slow stable crack growth mechanism. (Brown, 2007)
According to the research of Mohammad (2008), he investigated the sole effect of
each parameter and their combination on maximum stress produced in MDPE gas
pipes and their sockets which are made from PE100. MDPE can be used for water
pipe, gas pipe, MDPE plastic pipe and so on. It is known that MDPE pipes offer many
advantages over traditional ductile iron and steel pipes. These advantages include
flexibility, coilability, high ductility, light weight, corrosion resistance, and reduced
installation costs. These features provide both performance and economic benefits
which in turn have made MDPE pipes popular in ploughing-in and trenchless
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Figure 2.1 shows a schematic picture of such a side branching chain; the branches
radiate three-dimensionally, just as the branches of a tree point in all directions from
various places along the trunk. The presence of such side branches is a reason for
variations in a number of important physical properties (such as density, hardness,
flexibility or melt viscosity), which distinguish polyethylene resins. Chain branches
also become points in the molecular network where oxidation may take place. (Wan et
al. , 2006)
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Chapter 3
METHODOLOGY
3.1 Location of research
The research will be conducted at Laboratory of Basic Physics (MFA) in Department
of Physical Sciences, Faculty of Science and Technology, University Malaysia
Terengganu (UMT).
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3.2.2 Characterization
Every 20 hours alternate of ball milling, little grain size of powder will be taken out
and do the characterization by using the X-ray diffraction (XRD) to determine the
crystalline size and using the Scanning electron microscope (SEM) to determine the
graphite morphology.
3.2.3 Compounding process (composite)
In this process, MDPE will mix with the graphite by using the HAAKE Polylab
system. The blending process will carry out 5 samples; each sample will use 0wt%,
1wt %, 2wt%, 3wt%, 4wt% mix with the MDPE. The materials were compounded
into different mixture ratios of graphite content in MDPE. The MDPE will compound
at 180 and 170RPM for 20 min. Firstly, the MDPE will add to the mixer until the
MDPE fully melt and be liquid, and then the graphite powder is added until the
mixing torque become stabilized.
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3.2.5 Analysis
Lastly, MDPE-graphite composite be produced. Testing and analysis were perform on
this stage. Table below shows several characterizations method and description in this
research.
Table3.1 : Instruments and method
Method Description
Thermogravimetry (TGA) Determine change of weight in relation of
the change of temperature
X-ray diffraction (XRD) Investigation of the fine structure of matter
Fourier Transform InfraredSpectroscopy (FTIR)
Determine the type of bonds which arepresent in a compound
Testometric MODEL 350/500 Tensile test
Four Point Probe Determine the conductivity
3 3 I t t
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ML =msmf
ms 100%
TGA measurements were carried out in a TGA 6 Perkin-Elmer analyzer under a
nitrogen atmosphere. Around 10 mg of sample was used. The measurements were
performed from 50-800C at a heating rate of 10C/ min. (Kosuri et al. , 2008)
3.3.2 X-Ray Diffraction
X-ray diffraction is a tool for the investigation of the fine structure of matter. This
technique had its beginnings in von Laues discovery in 1912 that crystals diffract
Xrays, the manner of the diffraction revealing the structure of the crystal. At first, x-
ray diffraction was used only for the determination of the crystal structure. Later on,
however, other uses were developed and today the method is applied not only to
structure determination but to such diverse problems as chemical analysis and stress
measurement, to the study of phase equilibria and the measurement of particle size, to
the determination of the orientation of one crystal or the ensemble of orientations in
polycrystalline aggregate.
(3.1)
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Braggs law states the essential condition which must be met if diffraction is to occur.
N is called the order of reflection, it may take on any integral value consistent with
sin not exceeding unity and is equal to the number of wavelengths in the path
difference between rays scattered by adjacent planes. Therefore, for fixed values of
and d, there may be several angles of incidence 1, 2, 3 at which the diffraction
may occur corresponding to n=1,2,3
Debye Scherrers formula is used to calculate the crystallite lamella size. Scherrers
equation is given as Crystallite Lamella size= 0.9 /(B cos ) Where, B is ful l width
half maxima in nm. (Kosuri et al. ,2008)
3.3.3 Fourier Transform Infrared Spectroscopy (FTIR)
Fourier transform infrared spectroscopy is another form of infrared spectroscopy
which does not bombard the samples using infrared radiation of individual
wavelengths. Instead, FTIR uses sends out a pulse of beam which contains the
information of all infrared wavelengths. The beam is transmitted through the sample,
and the transmitted beam results in an interferogram. The interferogram is then
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3.3.4 Testometric Model 350/500
Testometric Model 350/500 design and manufacture a comprehensive range of
materials testing machines and software for evaluating the mechanical properties and
performance of materials. It has two type of this model, there are AT range of stand-
alone universal strength testing machines and the CT range of universal strength
testing machines. Testometric machine can done the testing including tensile test, wet
strength and puncture of tissue, board tests include flat, ring edge and the etc.
Accessories for paper testing include a wide range of grips and fixtures for paper
testing and all are compliant to international standards.
3.3.5 Four Point Probe
Four point probes method is a simple apparatus for measuring the resistivity of
semiconductor samples. By passing a current through two outer probes and measuring
the voltage through the inner probes allows the measurement of the substrate
resistivity. The sheet resistivity of the top emitter layer is very easy to measure
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3.4 Process Flow Chart
Preparation of samples-mill graphite (20, 40, 60, 80,100 hr)
Characterization graphite
SEM
XRD
Compounding process
MDPE
MDPE
+
1wt%
graphite
MDPE
+
2wt%
graphite
MDPE
+
3wt%
graphite
MDPE
+
4wt%
graphite
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Chapter 4
EXPECTED RESULTS
Graphite transforms to an amorphous phase by ball milling, the average size reachfrom 3nm to 8nm after 60 hour milling.
When MDPE mix with the graphite, crystallinity will increase and structure will be
more close packing. When crystallinity increases, hardness will increase. Tensile
d l i i f 1 9 3 2 G h il h ill i f 16
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REFERENCES
Peres, M. F. , Schn, C.G. & Tarpani, J.R. 2010 Effect of precracking method on KIcresults for medium-density polyethylene tested under cryogenic condition.
Journal of Polymer Testing 29 : 667673
Brown, N. Intrinsic lifetime of polyethylene pipelines. 2007. Polymer Engineering
and Science. doi:10.1002/pen :477480
Mohammad Shishesaz1 & Mohammad Reza Shishesaz . 2008. Applicability of
Medium Density Polyethylene Gas Pipes in Hot Climate Areas of South-west
Iran. Iranian Polymer Journal. 17 (7), 503-517
Zhang , W. , Dehghani-Sanij , A. A. & Blackburn, R.S. 2007 Carbon based
conductive polymer composites.J Mater Sci. 42: 34083418
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Wolak, J. E. 2005. Polyolefin miscibility: Solid-state NMR investigation of phase
behavior in saturated hydrocarbon blends. Dissertation Degree of Doctor of
Philosophy. North Carolina State University.
Dhoot, S.N. , B.S. & M.S. 2004. Sorption And Transport Of Gases And Organic
Vapors In Poly(Ethylene Terephthalate). Dissertation Degree of Doctor of
Philosophy. University of Texas, Austin.
Suryanarayana, C . 2001. Mechanical alloying and milling. Journal of Progress in
Materials Science, 46: 1-184
Wan Aizan & Rahman, W.A. 2006. Design of silane crosslinkable high density
polyethylene compounds for automotive fuel tank application. Thesis of
project IRPA. Faculty of Chemical and Natural Resource Engineering,
Universiti Teknologi Malaysia
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APPENDIX
Table A1: commercially produced metallocenes
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20
Table A2: Gantt Chart for FYP
No. Task
Month
2010 2011
JUL AUG SEP OCT NOV DEC JAN FEB MAR APR
1 Literature Review
2 Title Selection & Submission
3 Writing Proposal
4 Proposal Submission
5 Proposal Presentation
6 Lab work 1 (Preparation)
7 Lab work 2 (Compounding)
8 Writing Progress Report 1
9 Writing Progress Report 2
10 Thesis Writing
11 Submit Final Draft
12 Final Presentation
13 Thesis Submission