layered manufacturing of polymer matrix composites (pmc) materials...
TRANSCRIPT
LAYERED MANUFACTURING OF POLYMER
MATRIX COMPOSITES (PMC) MATERIALS VIA
FUSED DEPOSITION MODELING (FDM)
NASUHA BIN SA’UDE
UNIVERSITI TUN HUSSEIN ONN MALAYSIA
i
LAYERED MANUFACTURING OF POLYMER MATRIX COMPOSITES (PMC)
MATERIALS VIA FUSED DEPOSITION MODELING (FDM)
NASUHA BIN SA’UDE
A thesis submitted in
Fulfilment of the requirement for the award of the
Doctoral of Philosophy
Faculty of Mechanical and Manufacturing Engineering
Universiti Tun Hussein Onn Malaysia
AUGUST 2016
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DEDICATION
Assalamualaikum w.b.t
In the name of Allah, The Most Generous and The Most Merciful
Especially dedicated to my lovingly families,
My father; Mr. Sa’ude Bin Nokek
My Mother; Madam Zaharah Binti Abdullah
Special thanks to:
My Wife; Madam Nur Ezreen Binti Sanusi
My Sons; Mohammad Naufal Wafiq, Muhammad Nuqman Hakimi, Muhammad
Darwisy Sanusi, Muhammad Khalis Thaqif and Muhammad Umar Irshad
My Daughters; Nur Damia Widad, Nur Kaisah Maisarah
My Brothers; Mr Mohd Yusof Bin Sa’ude, Mr. Mohd Isa Bin Sa’ude, Mr Jaafar Bin
Sa’ude, Mr Mohd Saifulizam Bin Sa’ude, Mr Mohd Khairulnizam Bin Sa’ude and Mr
Mohd Hamiyuddin Bin Sa’ude.
My Sisters; Madam Norainon Binti Sa’ude, Madam Norisa Binti Sa’ude, Madam
Norhayati Binti Sa’ude and Madam Noraini Binti Sa’ude.
for their support from early stage of my study until completed.
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ACKNOWLEDGMENT
Assalamualaikum w.b.t
In the name of Allah, The Most Generous and The Most Merciful
I would like to express my profound gratitude to the supervisor, Assoc. Prof. Dr
Mustaffa Bin Ibrahim and Assoc. Prof. Dr. Mohd Halim Irwan Bin Ibrahim for their
valuable support, encouragement, supervision and useful suggestion throughout this
research work. Their moral support and continuous guidance enabled me to complete
my work successfully.
Special thanks to my wife; Nur Ezreen Binti Sanusi, my daughters; Nur Damia
Widad and Nur Kaisah Maisarah, my sons; Muhammad Naufal Wafiq, Muhammad
Nuqman Hakimi, Muhammad Darwisy Sanusi, Muhammad Khalis Thaqif and
Muhammad Umar Irshad for their support from early stage of my study until completed.
I am also thankful to the technician in UTHM, Mr. Fazlanuddin and Mr Shahrul
(Polymer and Ceramic Lab), Mr. Mokhtar (Advanced Manufacturing and Material
Center), special thanks to Mr Kamaruddin Bin Kamdani, Mr. Azriszul Bin Mohd Amin
and Mr. Rosli Bin Asmawi for their moral support and providing me the experimental
facilities and their valuable suggestion throughout this study.
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ABSTRACT
This research present the mechanical properties, Melt Flow Index (MFI) and Melt Flow
Rate (MFR) of an ABS-Copper filament through the Fused Deposition Modelling
(FDM) machine. The main objectives of this study are to investigate and analyze the
influences of the componding ratio and process parameters of polymer matrix
composite (PMC) filament wire material on the mechanical properties, melt flow index
(MFI) and melt flow rate (MFR) by FDM machine. In this study, the effect MFR of
10% -40 % copper filled in 52 % - 85% % ABS filament material by volume percentage
(vol. %) was investigated experimentally based on the melting temperature and feedrate
with the nozzle size 0.4 mm and 0.6 mm in diameter through the FDM heated liquefied
head. The mechanical properties of ABS-Copper filament through the injection
molding machine and Melt Flow Rate by the FDM liquefied head was investigated in
experimental for the mechanical properties and MFR. Based on the result obtained, it
was found that, increment of 30 %(vol. %) copper filled in ABS filament material
increase the mechanical properties and MFR (velocity and length) of PMC filament
material through the FDM machine. It can be concluded that, highest temperature and
feed rate are needed to extrude polymer matrix composite (PMC) filament compared to
ABS filament material in FDM machine.
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ABSTRAK
Kajian ini membentangkan tentang sifat-sifat mekanikal, Melt Flow Index (MFI) dan
Melt Flow Rate (MFR) filament ABS-Copper melalui mesin Fused Deposition
Modelling (FDM). Objektif utama kajian adalah untuk menyiasat dan menganalisis
pengaruh nisbah campuran dan parameter proses polymer matrix composite (PMC)
bahan wayar filament terhadap sifat-sifat mekanikal, MFI dan MFR dari mesin FDM.
Dalam kajian ini, kesan MFR 10 % - 40% kuprum di tambah dalam 52 % - 85 % bahan
filamen ABS mengikut peratusan isipadu (vol. %) telah di siasat melalui ujikaji
berdasarkan pada suhu lebur dan kadar suapan dengan ukurlilit size muncung 0.4 mm
dan 0.6 mm melalui kepala pemanas FDM. Sifat-sifat mekanikal filamen ABS-
kuprum melalui mesin suntikan acuan dan MFR dari kepala pemanas FDM telah di
siasat melalui ujikaji untuk komposisi kejuruteraan dan MFR. Berdasarkan keputusan
yang diperolehi, di dapati bahawa, kenaikan 30 % serbuk kuprum dalam filament ABS
meningkatkan sifat-sifat mekanikal dan MFR (halaju dan panjang) PMC filamen
melalui mesin FDM. Ini boleh di simpulkan bahawa, suhu dan kadar suapan yang
tinggi diperlukan untuk penyemperitan filamen PMC berbanding filamen ABS
melalui mesin FDM.
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CONTENTS
TITLE i
DECLARATION ii
DEDICATION iii
ACKNOWLEDGMENT iv
ABSTRACT v
ABSTRAK v
CONTENTS vi
LIST OF FIGURES xi
LIST OF TABLES xiv
LIST OF SYMBOLS AND ABBREVIATIONS xvi
CHAPTER 1 INTRODUCTION 1
1.1 Background of Study 3
1.2 Problem Statement 5
1.3 Objectives 8
1.4 Scope of Study 9
1.5 Significant of Study 9
1.6 Organization of thesis 10
CHAPTER 2 OVERVIEW OF MATERIALS IN ADDITIVE
MANUFACTURING 12
2.1 Introduction 13
2.2 Overview of AM Process 13
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2.2.1 Material in FDM 14
2.2.2 Acrylonitrile Butadiene Styrene (ABS) 14
2.2.3 Binder and Surfactant 16
2.2.3.1 Binder in Injection Molding 17
2.2.3.2 Binder in FDM 18
2.2.4 Polymer Matrix Composites in Injection Molding 19
2.2.4.1 Powder Loading (PL) of Feedstock 19
2.2.5 Polymer Matrix composites in FDM 20
2.3 Material Issues in Mixing 21
2.3.1 Mixing and Compounding 22
2.3.2 Melting and Thermal Degradation Temperature 22
2.3.3 Surface Tension 25
2.3.4 Melt Flow Index (MFI) 27
2.4. Layered Manufacturing (LM) by FDM Machine 28
2.4.1 FDM Parameter 28
2.4.2 PMC Simulation in FDM 29
2.4.3 Packing Fraction (PF) of Feedstock 30
2.4.4 PMC Filament Composition in Layered Manufacturing 33
2.5 Research Direction in FDM Process 38
2.6 Summary 38
CHAPTER 3 DEVELOPMENT OF A NEW ABS-COPPER
FILAMENT COMPOSITES FOR FUSED DEPOSITION
MODELING (FDM) PROCESS 40
3.1 Introduction 40
3.2 Characterization and Selection of Material 42
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3.2.1 Acrylonitrile Butadiene Styrene (ABS) 43
3.2.2 Copper Powder 44
3.2.3 Binder and Surfactant 45
3.2.3.1 Thermal Degradation of Palm Stearin 46
3.2.3.2 Thermal Degradation of Calcium Stearate 47
3.3 Processing and Compounding a New ABS-Copper
Composites by Injection Machine for Mechanical
Properties Test 48
3.3.1 Compounding and Mixing Ratio of the PMC
Feedstock Material 48
3.3.2 Brabender Plastograph Mixer 53
3.3.3 Crusher Machine 55
3.3.4 Injected PMC Feedstock Material by Injection
Molding Machine 56
3.3.5 Extruder Wire Filament 57
3.3.6 Preparation of ABS-Copper Composite by Melt
Indexer Machine for Melt Flow Index (MFI) 58
3.4 Fabrication of Wire Filament 58
3.5 Type of Testing 60
3.5.1 Dynamic Mechanical Properties 60
3.5.2 Differential Scanning Calorimetry (DSC) 60
3.5.3 Thermo Gravimetric Analysis (TGA) 61
3.6 Morphological properties of ABS-Copper 62
3.6.1 Surface Tension 62
3.6.2 Melt Flow Index (MFI) 63
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3.6.3 Density Test 64
3.6.4 Scanning Electron Microscope (SEM) 66
3.7 Mechanical Properties Test 67
3.8 Experimantal Setup of a New ABS-Copper
Filament Composites by FDM Machine 68
3.8.1 Machine Setup 68
3.8.2 Machine Parameter 68
3.8.3 Nozzle Tip Diameter 69
3.8.4 FDM Hardware 70
3.8.4.1 Circuit Board 71
3.8.5 Firmware Setup 73
3.9 Summary 74
CHAPTER 4 RESULTS AND DISCUSSIONS 75
4.1 Introduction 75
4.2 Thermal Mechanical Properties 75
4.2.1 Dynamic Mechanical Properties 75
4.2.2 Differential Scanning Calorimetry (DSC) Results 78
4.3 Morphological Properties of ABS-Copper 80
4.3.1 Surface Tension 80
4.3.2 Melt Flow Index (MFI) 82
4.3.3 Density Results 83
4.3.4 Scanning Electron Microscope (SEM) 86
4.4 Mechanical Properties Results 88
4.4.1 Flexural Strength Results 88
4.5 Results on Extrusion ABS-Copper Filament
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through FDM Machine 90
4.5.1 Extrusion ABS Filament with different size of
The Nozzle Diameter by FDM Machine 91
4.5.2 Extrusion ABS-Copper Filament with different
size of The Nozzle Diameter by FDM Machine 92
4.5.3 Comparison Result of Melt Flow Rate (MFR)
ABS and ABS-Copper Filament by FDM Machine 93
4.5.4 Part Fabrication of ABS-Copper Filament in
Layered Manufacturing 98
4.6 Summary 99
CHAPTER 5 CONCLUSION AND RECOMMENDATION 100
5.1 Introduction 100
5.2 Conclusion 100
5.3 Recommendation 102
REFERENCES 104
APPENDIX A 113
APPENDIX B 126
APPENDIX C 131
APPENDIX D 133
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LIST OF FIGURES
Figure 1.1 : The hardware in the FDM Machine Model Prusa I3 3
Figure 1.2 : The schematic of the FDM process 4
Figure 2.1 : The schematic diagram of The FDM filament 13
Figure 2.2 : The TGA curve shows the decomposition of ABS polymer 16
Figure 2.3 : The curve of the feedstock with 95 wt. % copper powder 17
Figure 2.4 : TGA curve for ABS terpolymer at a heating rate of 20 °C/min 24
Figure 2.5 : Dynamic mechanical properties of virgin ABS and 10%
iron-powder filled ABS 24
Figure 2.6 : Contact angle of a solid surface by a water 25
Figure 2.7 : Contact angle of a solid surface by a water 26
Figure 2.8 : Metal Surface Modification 27
Figure 2.9 : Melts Flow Indexer Machine 31
Figure 2.10 : Crystal structure Copper in Haxagonal close-packed (HCP) 29
Figure 3.1 : The research methodology flow chart for entire project study 41
Figure 3.2 : ABS Filament 43
Figure 3.3 : Copper Powder 45
Figure 3.4 : Grain particle size of copper powder 45
Figure 3.5 : The TGA curve shows the decomposition of palm stearin 47
Figure 3.6 : The degradation temperature of calcium stearate 47
Figure 3.7 : Brabender Plastograph Mixer 54
Figure 3.8 : (a) The feedstock material mix by Brabender Plastograph
Mixer, (b) Feedstock after crushed in a pallet form 54
Figure 3.9 : Crusher Machine 55
Figure 3.10 : Zone temperature in injection molding machine 56
Figure 3.11 : Injection molding machine 57
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Figure 3.12 : Single Screw Extruder Machine 59
Figure 3.13: Copper ABS Wire Filament by Single Screw Extruder
Machine 56
Figure 3.14 : Linseis Thermobalance Machine for TGA Test 62
Figure 3.15 : Surface tension measurement system 63
Figure 3.16 : The melt flow index machine 64
Figure 3.17 : Mettler toledo for density test 65
Figure 3.18 : Scanning Electron Microscope 66
Figure 3.19 : Flexural Strength Equipment 67
Figure 3.20 : ABS from Injection Molding 68
Figure 3.21 : Copper filled in ABS by Injection Molding 68
Figure 3.22 : Size of Nozzle in 0.4 mm and 0.6 mm in diameter 69
Figure 3.23 : 3D Printer Model Prusa I3 70
Figure 3.24 : 3D Printer System with Stainless Steel Extruder 71
Figure 3.25 : Arduino MEGA 2560 board 72
Figure 3.26 : RAMPS plugged into Arduino 72
Figure 3.27 : Firmware and Power Supply Connection 73
Figure 3.28 : Pronterface Software 73
Figure 4.1 : Dynamic Mechanical Properties of 20% copper powder
filled ABS 78
Figure 4.2 : Glass transition temperature (Tg) of pure ABS 79
Figure 4.3 : Glass transition temperature (Tg) of 70% copper filled in
30% ABS 80
Figure 4.4 : Melt flow index results in weight percentage (wt. %) of ABS,
Copper and Binder Material 85
Figure 4.5 : Density Results by Experimental 81
Figure 4.6 : Density Results by Formula and Experimental 86
Figure 4.7 : Wire filament of Copper-ABS for sample 8 86
Figure 4.8 : Consistency of 3 mm wire filament in diameter 87
Figure 4.9 : Inconsistency of 3 mm wire filament in diameter 87
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Figure 4.10 : SEM Image of 3 mm wire filament in diameter 88
Figure 4.11 : Flexural Strength Results 90
Figure 4.12 : Length (mm) of ABS Filament by Different Nozzle
Diameter 91
Figure 4.13 : Velocity (mm/s) of ABS Filament by Different Nozzle
Diameter 92
Figure 4.14 : Length (mm) of ABS-Copper Filament by Different Nozzle
Diameter 93
Figure 4.15 : Velocity (mm/s) of ABS-Copper Filament by Different Nozzle
Diameter 94
Figure 4.16 : Length (mm) of ABS and ABS-Copper Filament by Different
Nozzle Diameter 95
Figure 4.17 : Velocity (mm/s) of ABS and ABS-Copper Filament by
Different Nozzle Diameter 96
Figure 4.18 : Comparison velocity of ABS and ABS-Copper filament based
on varieties feed rate value with different size of nozzle diameter 97
Figure 4.19 : Comparison velocity and length of ABS and ABS-Copper
filament based on varieties temperature value with different
size of nozzle diameter 98
Figure 4.20: The fabrication sample from ABS-Copper filament by FDM
Machine 99
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LIST OF TABLES
Table 2.1 : Value of critical network formation (Cp) of various systems 32
Table 2.2 : Value of packing fraction (PF) for various systems 33
Table 2.3 : Overall references from previous study 35
Table 3.1 : The Properties of ABS polymer material 43
Table 3.2 : Properties of Copper Powder 44
Table 3.3 : Properties of palm stearin material 46
Table 3.4 : Properties of calcium stearate material 46
Table 3.5 : Characteristic of compounding Copper, ABS and surfactant
material 48
Table 3.6 : Mixing ratio of Copper, ABS, Calcium Stearate and Palm
Stearin material by volume percentage (vol. %) 50
Table 3.7 : Mixing ratio of Copper, ABS, Calcium Stearate and Palm
Stearin Material by volume (cm³) 51
Table 3.8 : Mixing ratio of copper, ABS and calcium stearate material
by weight percentage (W %) 52
Table 3.9 : Mixing ratio of copper, ABS and calcium stearate material
by weight (gram) 52
Table 3.10 : Parameter Setting of Copper ABS Wire Filament by Single
Screw Extruder 60
Table 3.11 : Input Parameters for TGA 61
Table 4.1 : Storage Modulus and Tangent Delta of Composites with
20 % copper filled ABS 76
Table 4.2 : Storage Modulus and Tangent Delta of Composites with
30 % copper filled ABS 77
Table 4.3 : Effect of copper filled in ABS on the Tg 79
xv
Table 4.4 : Surface Tension with Varieties Liquid 81
Table 4.5 : Critical Surface Tension of PMC Samples by Distiller Water 82
Table 4.6 : Melt Flow Index Test 82
Table 4.7 : Average result on density by experimental 84
Table 4.8 : Density of copper filled in abs composites 84
Table 4.9 : Flexural strength results on maximum stress and strain 89
Table 4.10 : Comparison length of ABS and ABS-Copper filament based
on varieties temperature and feed rate value with different
size of nozzle diameter 94
Table 4.11 : Comparison velocity of ABS and ABS-Copper filament
based on varieties temperature and feed rate value with
different size of nozzle diameter 95
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LIST OF SYMBOLS AND ABBREVIATION
LM Layered Manufacturing
AM Additive Manufacturing
RP Rapid Prototyping
ASTM American Society for Testing and Material
ABS Acrylonitrile Butadiene Styrene
PS Palm Stearin
PP Polypropylene
PMMA Poly-Methyl Methacrylate
EEA Ethylene Ethyl Acrylate
EVA Ethylene Vinyl Acetate
PW Parafin Wax
CW Carnauba Wax
BW Bees Wax
OB Organic Binder
SA Stearic Acid
PEG Polyethylene Glycol
LDPE Low Density Polyethylene
HDPE High Density Polyethylene
PE Polyethhlene
PLA Polylactide
PA Polyamide
SAN styrene acrylonitrile copolymer
SFF Solid Freeform Fabrication
TGA Thermogravimetric Analysis
DMA Dynamic mechanical Analysis
AF Additive Fabrication
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2D Two Dimensional
MIM Metal Injection Molding
3DP Three Dimensional Printing
FF Freeform Fabrication
FDM Fused Deposition Modeling
FDC Fused Deposition Ceramic
FDMet Fused Deposition Metals
PMC Polymer Matrix Composite
MMC Metal Matrix Composite
CMC Ceramic Matrix Composite
RDPC Rapid Deposition Polymer Composite
CAD Computer Aided Design
SLA Stereolithography
SLS Selective Laser Sintering
LOM Laminated Object Manufacturing
MFI Melt Flow Index
MFR Melt Flow Rate
LMT Layer Manufacturing Technology
ECG Electro Ceramic Group
PL Powder Loading
SS Stainless Steel
IPA Isopropyl alcohol
MMA Methyl-methacrylate
MO Mineral Oil
AT Acetone
DMSO Dimethyl Sulfoxide
EG Ethylene Glycol
GR Glycerol
DW Distilled Water
DSC Differential Scanning Calorimeter
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SEM Scanning Electron Microscope
Φ Contact Angle
g/10 min Gram per 10 minutes
W/g Weight per Gram
g/cm3 Gram per Centimeter Cube
mm/s Milimeter per Seconds
°C Celcius
% Percentage
vol. Volume
wt. Weight
kg Kilogram
g gram
L Length
d density
t Time
V Extruded Volume
δ Viscoelastic
𝜃 Wettable
GPa Gega Pascal
MPa Mega Pascal
Tg Glass Transition Temperature
cm Centimeter
mm Milimeter
N Newton
E’ Storage Modulus
E’’ Loss Modulus
E* Complex Modulus
Ф Contact angle
𝛾𝑔𝑠 Gas/solid interfacial tension
𝛾𝑙𝑠 Liquid/solid interfacial tension
𝛾𝑙𝑔 Liquid/gas interfacial tension
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𝑁𝑎𝑡𝑜𝑚 Number of atoms
𝑉𝑎𝑡𝑜𝑚 Volume of an atom
𝑉𝑢𝑛𝑖𝑡𝑐𝑒𝑙𝑙 Volume Unit Cell
𝑃𝑐 Critical loading of network formation
𝐶𝑝 Random dispersion of spheres
Z Maximum number of possible contact
PF Packing Fraction
CHAPTER 1
INTRODUCTION
Layered manufacturing (LM) or additive manufacturing (AM) technologies is an
evolution of rapid prototyping (RP) techniques, where a part is built in a layered
process on the heated platform. AM is defined by the American Society for Testing
and Material (ASTM) as the process of joining materials to make object from 3D
model data in a layer by a layer process (Noort, 2012). There are several names used
for LM such as solid freeform fabrication (SFF), additive fabrication (AF), rapid
prototyping (RP), rapid manufacturing, 3D-printing (3DP) and freeform fabrication
(FF) (Petrovic et al., 2011). The first patterns in plastic AM were proposed by Ross
Housholder since in 1981 and assigned to DTM Corporation (Goa et al., 2015). Rapid
LM technology growth on the laser source on liquid melts was develop by Charles
Hull since 1984 to 1986. The invention of LM technology is capable to transform the
imagination or idea into the reality product without involving with re-tooling and the
printed parts will be customized without additional cost (Campbell et al., 2011a).
Currently, others available technologies in part fabrication or manufacturing
process involving with high cost of tooling, mold making some of those technology
is required the secondary process in finished part such as machining, injection
molding, casting, forming and extrusion processes. All those technologies are
“subtractive” techniques and each process involving with removing material and
waste material was occur during fabrication process (Campbell et al., 2012b). Any
changes on the design required more cost on tooling, mold modification and the
wasted material will be increased extremely (Boothroid et al., 2002).
In contrast, AM technology an alternative “additive” process could be
explored to gain the same target in part fabrication or manufacturing process with
fastest process, low cost on material and machine, the waste material could be reduced
2
proportionally with high production rate without additional cost and worker. The
equipment is becoming competitive with traditional manufacturing techniques in
terms of price, speed, reliability, and cost of use (Kochan et al., 1999, Noort, 2012).
Among of AM technologies is the fused deposition modeling (FDM) have
been able to deposit only thermoplastic filament in a layer by a layer process as long
as the material can be made in filament wire. The filaments or wire from spool will
flow through the heated liquefied head and nozzle and the melt material will deposited
on the FDM heated platform or bed. These technology was developed by S. Scott
Crump since 1980s and it was commercialized in early 1990 (Noort, 2012).
Fused Deposition Modeling (FDM) and others related printing technology in
layered manufacturing could be used in direct PMC part fabrication and rapid
manufacturing process. These technologies will offer a possibility combination of
varieties material from ceramic and metallic material for continues improvement on
internal structure, mechanical and thermal properties, as long as the material in a
filament wire. Continued growth on a new PMC filament will enhance the mechanical
properties, smoothest material flow on conductive and functional graded material
deposition on the printed platform through the heated liquefied head and nozzle tips
in layered manufacturing processes. Noort (2012), was mentioned that, the available
material and the transition from prototypes to functional devices will begin to play a
much bigger role.
A similarly statement was mentioned by Diegel et al., (2010), a new possibility
to print directly the complex parts with conductive electronic track by layered
deposition process. Furthermore, Anzalone et al., (2013) mentioned that, the
limitation of open source metal 3D printer development in layered manufacturing
because of high capital investment. A development of advanced new filament material
will be apply in several manufacturing product such as medical part, conductive
electric and electronic components, safety and consumer product without involving
with tooling equipment in the manufacturing process. Therefore, the PMC filament
material will be deposited layer by a layer process by FDM machine and the product
development times, the production cost, the tool and die fabrication will be reduced.
The deposition process by FDM involved with added material in a layer by a layer
process and the wasted material will significantly reduce with additive manufacturing
process via rapid deposition polymer composite (RDPC) process in manufacturing
processes.
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1.1 Background of Study
Additive Manufacturing (AM) is a technique in manufacturing in which a solid
physical model of a part is made directly from a three-dimensional computer-aided
design (CAD) file. There are several RP techniques are available. Some of the most
common RP techniques include Stereolithography (SLA), Selective Laser Sintering
(SLS), Fused Deposition Modelling (FDM), 3-D Printing and Laminated Object
Manufacturing (LOM) (Campbell et al., 2012b). FDM is the RP technique used in this
study. FDM, a solid-based RP technique, is commercialized by Stratasys Inc. and an
extrusion-based layered manufacturing process in which semi-solid thermoplastic
polymers gets deposited on a platform through a nozzle fitted into a heated liquefier
controlled in X and Y directions.
The hardware in the FDM machine Model Prusa I3 is represented in Figure
1.1. At the early stage the filament wire will be fitted and drived from the spool by
stepper motor in the FDM heated head. The filament will flow through the heated
nozzle and with controlled by outsource software to transform the solid filament in to
a semi-molten state during deposition process on the heated platform. The head is then
moved around in the X-Y plane and deposits material according to the part
requirements from the STL file. The head is then moved vertically in the Z plane to
begin depositing a new layer when the previous one is completed. After a period of
time, usually several hours, the head will have deposited a full physical representation
of the original CAD file.
Figure 1.1 The hardware in the FDM machine Model Prusa I3
Heated Head
Stepper Motor
Filament
Nozzle Tips
Platform
4
Among the parameters in FDM are included of traveling table speed, feed rate
of X-Y axis, melt temperature, platform temperature and material melt flow rate.
Commercially available materials for FDM include wax, ABS and nylon (Mostafa et
al., 2009a, Mostafa et al., 2011b). Therefore, the quality of part fabrication is
controlled by outsource software, software parameters of layered process, extrusion
rate and the nozzle temperature and feeding speed of filament in FDM machine. The
schematic of the FDM process is shown in Figure 1.2.
Figure 1.2 The schematic of the FDM process (Sidambe,2014)
The basic principle of FDM process offers a great potential for a range of other
materials, including metals and composites to be developed. New material can be
produced in feed stock filament form of required size, strength and properties. Zhong
et al., (2001) was mentioned that, the key mechanical properties of the filament
material must have a good strength, stiffness, ductility and flexible. In order to achieve
a good flexibility of the filament wire in the matrix material, the composition need to
added some of a binder or surfactant material. The function of flexible filament is an
easier to flow from the spool through the heated liquified head during deposition
process on the machine platform (Masood and Song, 2005c; Mostafa et al., 2009a and
Mostafa et al., 2011b). The polymeric binder systems have several advantages over
wax/polymer binders, including improved flow properties, mechanical properties and
better shape retention after debinding process (Omar et al., 2010). The binder acts as
5
a temporary vehicle for homogeneously packing a powder into desired shape and
holding the particles in that shape until the beginning of debinding and sintering
method (Omar et al., 2010).
1.2 Problem Statement
Customer needs and requirement of the product customization and continued demand
for low cost product and time savings have been generated a renewed interest in AM
technology. The Fused Deposition Modelling (FDM) has been identified as the focus
of this research because of its potential versatility in the choice of materials and
deposition configuration. This innovative approach allows for designing and
implementing highly complex internal architectures into parts through deposition of
different materials in a variety of configurations in such a way that the finished
product meet the performance requirements. This implies that, in principle, one can
tailor-make the assembly of materials and structures as per specifications of an
optimum design.
Development of a new filament material in AM especially using FDM will be
apply in several industries with low volume product with minimum of cost. The
development cost of automotive, internal functionality part in aerospace and 3D
medical imaging can be converted in solid objects (Campbell et al., 2012b). There are
five (5) major issues in this research which are (1) The mixing or compounding (2)
The feedstock preparation (3) The injected specimen via injection molding (4) The
fabrication filament via extruder machine (5) Layered Manufacturing of Polymer
Matrix Composite (PMC) via FDM machine
Firstly, the major issues in mixing material are the homogeneous
compounding material and bonding. It involved with the method and procedure in
compounding of varieties material and each materials there have their own melting
temperature. Most important criteria in the material compounding are the selection of
melting temperature. The degradation on the material will occur when the temperature
selection over the melting temperature and some of the material weight will be
reduced and vaporized. Moballegh et al., (2005), concluded that the thermal
degradation properties of copper feedstock with 95 wt%, degrading of paraffin wax
occur from 170 to 350 °C and 350 – 500 °C for polyethylene. The binder degradation
will start at 171 °C. The temperature on mixing and injection molding process must
6
be lower than the binder degradation temperature. Masood et al., (2004b) was
mentioned that, the homogenous mix of iron filler into ABS polymer with the metal
particle size of 200 µm to 500 µm approximately using the tumble mixer in 2 hour.
Secondly, the feedstock compounding ratio of varieties material such as the
matrix material, conductive filler, binder and surfactant will provide a continuous
linkages and effective concentration for conductive composite material in continuous
network (Sancaktar, 2011). The continuous linkage of varieties compounding material
will provide a good inter connection between matrix and filler material in order to
maintain the conductive portion in filament fabrication with good flexibility, stiffness,
and viscosity. A similarly observation was done by Qu et al., (2003), where the
conductivity of carbon fibre filler dramatically increase around 8 % to 10 % by volume
percentage. Therefore the selection of compounding ratio will be effected on the
filament viscosity and conductive potion in PMC feedstock material.
Thirdly, due to a varieties compounding and viscosity on the feedstock
material used in the injection molding machine, the material was burned inside the
barrel screw and compounding material of the certain ratio could not be processed at
identical settings. The suitable selection parameter on the temperature and pressure
are most important criteria and must take as a main consideration in order to achieve
a good viscosity and flowability. In the injection molding process consists of four
zones of temperature and with different temperature setting will affect the mechanical
properties of the specimen fabrication. Unsuitable melt temperature zone in injection
machine will creates a stacking problems on mold and it’s involve with melts flow
rate of a new PMC material. In order to minimize the melt issues and stacking at the
screw, the barrel temperature was started from low to high temperature. The injected
specimen was used for flexural strength, melt flow index, surface tension and density
using the injection molding machine.
Fourthly, the material selection and method of compounding process to
produce the filament are most important for enhance the material performance and
application in the FDM. An understanding of the dynamic and solidification effect on
filament and layered process are most critical in freeform fabrication (Tseng &
Tanaka, 2001). The suitable selection of melting temperature and the solidification
effect are needed to explore extensively for successful in the deposited material on the
FDM platform. Inconsistency of melt temperature will creates some problems on the
filament motion and sticking in the nozzle during extrusion melts flow of composite
7
filament in layered process (Mostaffa et al., 2009a and Mostaffa et al., 2011b). The
properties of the mixed feedstock filament meet the flexibility, stiffness, and viscosity
required for successful FDM processing (Masood, 2005). An important criteria in the
filament fabrication is homogenous mixing and bonding material. The distribution of
metal filled in polymer matrix shall be constant and these will be effected on the
conductive portion with constant viscosity in the fabrication filament. The highly
metal material filled in matrix material will provide a brittle material and it’s difficult
to produce the filament in wire form. In order to minimize the brittles material, some
of binder and surfactant will be added in matrix material for smooth material flow in
the fabrication filament (Masood, 1996, Wu et al., 2002, Masood and Song, 2005,
Mostaffa et al., 2009a, Mostaffa et. al., 2011).
Finally, the major limitation of AM are speed, accuracy, nonlinearity
(resolution XYZ axes and wall thickness), material properties and system cost
(Campbell et al., 2012b). A significant issue in the layered manufacturing is the feed
rate and melt temperature of composite wire filament in layered process on FDM
platform. Due to the highly metal filled in polymer matrix, will be effected on the feed
rate of the composite filament during melt flow extrusion by FDM machine (Wu et
al., 2002, Masood and Song, 2005, Mostaffa et al., 2011). An important parameters
involve in layered manufacturing process, which are the filament grips, gap between
nozzle tips and platform, constant the feed rate of filament flow, constant travelling
feed rate and constant temperature on FDM platform during PMC deposition. Those
parameters was effected the printing consistency in a layer by a layer process for
especially for a new PMC filament material in FDM machine.
Nevertheless, there are limited data/research available particularly dealing
with the deposition of PMC through the heated liquefied nozzle. Layered of rapid
deposition polymer composites (RPDC) with highly filled metal powder in the
polymer matrix may offer the possibility of introducing new composite material in
FDM. There are no published reports and other commercially claim are available on
the velocity behavior and melts temperature of ABS-Copper filament in layered
manufacturing. It was expected that, this need some of knowledge, methods, material
transition phase and behavior from solid to semi solid and effect of temperature, melt
flow and the feed rate during deposition material in layer by a layer manufacturing
process. Thus the FDM process offers the potential composite material to produce the
functional parts directly via deposition process for rapid tooling.
8
The intention of this study is to fabricate the composite filament with copper
filled in ABS polymer by single extruder machine and deposited via layered
manufacturing processes by FDM machine. An investigation of optimum composition
will be explored on the mixing ratio of constituent material by the Brabender mixer
machine. A suitable binder and surfactant material has been added as lubricant agent
for smoothest melt flow of composites materials in wire filament form for used in
FDM machine in layered manufacturing process. In order to accomplish a
homogeneous mixing, the compounding procedure, methods, mixing ratio and time
shall be followed in wire filament fabrication to ensure the constant diameter in 3 mm
approximately.
1.3 Objectives
Generally, the main objectives of this study are to evaluate the PMC filament wire
material by FDM machine and the influences of the process parameters on mechanical
properties, surface tension, melt flow index (MFI) and melt flow rate (MFR). Detail
objectives that have to be fulfilled, which are;
i) To investigate and analyze the effect of Copper filled in ABS matrix
material on the mechanical properties, melt flow index, surface tension
and density.
ii) To fabricate ABS-Copper specimen by the injection molding machine
and tested on the flexural strength.
iii) To fabricate a new ABS-Copper filament wire with 3 mm in diameter
using single screw extruder machine.
iv) To analyze the effect parameters (melts temperature and feed rate) of
ABS-Copper filament in the melts extrusion by FDM machine.
v) To apply and deposited a new ABS-Copper filament material on in a
layer by a layer process by FDM machine.
1.4 Scope of Study
The research objectives can be achieved through the experimental process on material
behavior. Studies are conducted in the following categories:
9
i) Material preparation and the compounding of an ABS-Copper filament
with suitable melting temperature, screw speed, mixing time by the
Brabender plastograph mixer (Model: W50).
ii) The fabrication of ABS-Copper specimens(Flexural Strength) with
various melting temperature, pressure, fives (5) zone temperature
(Feeding, Rear 2, Rear 1, Middle, Nozzle) and cooling times using
injection moulding machine (Model:NP7-1F)
iii) Development a new ABS-Copper filament wire (diameter: 2.00 mm ~ 3.00
mm) with different melting temperature (feeding, middle, front, die) by the
single extruder machine (Model: Y100).
iv) Extrusion of a new ABS-Copper filament (diameter: 3 mm) on the melts
analysis through the FDM heated liquefied head.
v) The fabrication of sample on layered manufacturing of ABS-Copper
filament in a layer by a layer process by the FDM machine.
vi) Type of the Specimen Testing: Flexural strength (ASTM D790), surface
tension, melt flow index (MFI), melt flow rate (MFR).
1.5 Significant of Study
In this dissertation, research reported has focused on the development of a new PMC
filament material and performance in the thermal, mechanical, dynamic and
morphological properties. The PMC filament has been applied and deposited in the
FDM machine platform via additive manufacturing process and the details are ;
The thesis writing was focused on PMC filament fabrication for FDM machine.
i) Material characteristic and development, degradation of a new PMC
filament, mixing and compounding process through experimental testing.
ii) Development a good flowability PMC filament through the melt flow
indexer machine and deposit PMC filament on the FDM machine platform
through the heated liquefied head.
The results obtained on a new PMC filament developed will provided as:
10
i) Guideline on the development of a new PMC filament by single screw
extruder machine, the performance material on MFI, thermal and
mechanical properties with a good flowability in the layered process.
ii) Obtained the best melt flow rate (MFR), velocity and feed rate of highly
filled metal in polymer composites filament in additive manufacturing
process.
The deposition of a new PMC filament in a layer by a layer process was successfully
done and achieved to enhance the material performance, with a good material
performance on flowability, MFI, velocity, density, thermal and mechanical
properties especially with highly metal filled in ABS matrix in FDM machine.
Moreover, a new PMC for FDM filament was successfully develop as an alternative
PMC filament material in additive manufacturing process.
1.6 Organization of Thesis
In this section has contribute the detail contents of thesis writing on five (5) chapter.
In chapter 1 presents the introduction of the additive manufacturing process, problem
statement, objectives, scopes and significant of study.
In chapter 2 presents an overview of materials and process in additive
manufacturing, materials issues in the mixing and compounding, melting and thermal
degradation temperature. Furthermore, the finding data from previous researcher on
the FDM parameters, powder loading of feedstock, polymer matrix composites
(PMC) simulation in FDM, packing fraction of feedstock, PMC filament composition
in layered manufacturing and research direction.
In chapter 3 presents the development of a new abs-copper filament
composites for FDM process, selection of material, processing and compounding a
new abs-copper composites, FDM filament fabrication, type of testing, morphological
properties and experimental setup.
In chapter 4 discusses the results on the thermal, mechanical, dynamic and
morphological properties, and analysis on MFI, density, extrusion of the PMC
filament with different sizes of the nozzle diameter and comparison results on MFI
and PMC filament by FDM.
11
In chapter 5 presents a comprehensive summary, emphasizing the
achievements on the functionally graded material through the layered manufacturing
process and recommendation on the future work.
CHAPTER 2
OVERVIEW OF MATERIALS IN ADDITIVE MANUFACTURING
2.1 Introduction
Layer Manufacturing Technology (LMT) or Additive Manufacturing (AM), is based
on the principle of adding material in two dimensional (2D) layers to build a complete
3D-model. In the early 1990s, Kruth (1991) was categorized AM in three (3) types
material which is liquid based, powder based and solid based material with different
types of technology on melts material either drop on demand binder in powder based,
laser tracer on liquid based and heated liquefied head by solid based material (Goa et
al., 2015). There are several names of layer manufacturing such as Rapid prototyping
(RP), 3D-printing, solid freeform fabrication (SFF), freeform fabrication (FF) and
additive manufacturing.
Traditionally, the LM systems have been able to fabricate parts either from the
solid, liquids or powder material. Currently, Each AM process involved with either
plastic, wax, metal, metal matrix composite (MMC), polymer matrix composite
(PMC) and ceramic matrix composite (CMC) material. Material plays an important
factor to produce an economic part or component by AM processes. The application
of composites material in AM are mainly for the inter discipline area in optical,
electronic and those area not yet been extensively explore and investigated (Kumar &
Kruth, 2010). Among the AM process is the fused deposition modeling (FDM)
process, which is involved with plastic filament wire or feedstock wire form, and the
fabrication wire is from the extrusion machine. The process involves layer-by layer
deposition of extruded material through a liquefied nozzle using feedstock filaments
from a spool.
This section has been discussed on the research review from previous
researchers in term of material issues and research direction in AM. The direction of
13
research was focused on layered manufacturing of metal filled in polymer matrix
material in FDM filament wire form. However, varieties material used in AM such as
polymer, reinforced polymer, wood, ceramic, composite, bio material and sustainable
material, but it beyond our research direction and therefore some finding was not
reviewed in this chapter.
2.2 Overview of AM Process
AM technology is a new technique for part fabrication in layers by a layer process
(Petrovic et al., 2011). Normally, previous RP applications focused on build a final
product for fitting and testing. Customer needs for the end used product and continued
demand for low-cost and time saving have generated a renewed interest in AM. A
shift from prototyping to manufacturing of the final product will give an alternative
selection with different material choice, low cost part fabrication and achieving the
necessary mechanical properties (Ning et al., 2015). One of the RP technologies
available today is Fused Deposition Modelling (FDM), which involves extrusion of
plastic filament wire as feedstock material (Dudek, 2013). Existing FDM machine
have been able to deposit only thermoplastic filament through the heated liquefied
nozzle (Masood, 1996). Figure 2.1 shows the schematic diagram of the FDM filament
through heated liquefied nozzle.
Figure 2.1 The schematic diagram of FDM filament (Mostaffa et al., 2009a;
Mostaffa et al., 2011b)
14
2.2.1 Material in FDM
The fused deposition modeling (FDM) technique is one of the most widely used rapid
prototyping (RP) systems in the part fabrications. The main reasons behind the RP
selection are a simple fabrication process, reliability, safe and low cost of material,
and the availability of variety's thermoplastics material (Petrovic et al., 2011).
Varieties types of materials are compatible in FDM machine such as metal, ceramic
and composites for the part fabrication in a layer by a layer process as long as the
material can be solidified and extruded. Normally, this filament will drive by the FDM
machine spool and flow through the heated liquefied head and solidified. The material
were heated from solid stage to semi solid stage and the material were solidified
during deposition process in a layer by a layer process.
2.2.2 Acrylonitrile Butadiene Styrene (ABS)
Acrylonitrile butadiene styrene (ABS) is one of the most successful engineering
thermoplastics material with high performance in the engineering application. These
material are widely used in the automotive industry, telecommunication, business
machines and consumer markets. It consists of styrene acrylonitrile copolymer (SAN)
mixed with and to some extent grafted to polybutadiene rubber (Boldizer & Moller,
2003). ABS has a desirable properties which is good mechanical properties, chemical
resistance and easy processing characteristic (Wang et al., 2002).
An ABS has a good mechanical properties and fluidity, desirable flexibility
and stiffness (Mostafa et al., 2009a and Mostafa et al., 2011b). Furthermore, ABS is
a commercial material with a good mechanical properties, chemical resistance, good
processing characteristics and low cost material approximately (Owen & Harper 1999,
Salamone, 1999 and Dong et al., 2001). A similarly mentioned by Qu et al. (2003),
where the characteristic of ABS polymer is high electrical resistance and as act an
insulator in more engineering application.
Most of previous researcher has been used ABS filament material in the rapid
prototyping parts especially by the FDM machine (Masood, 1996a, Masood et al.,
2004b, Masood & Song, 2005b, Zhong et al., 2001, Tyberg & Bohn, 1999, Anitha et
al., 2001, Rodriguez et al., 2001, Ahn et al., 2002, Anna et al., 2004, Lee et al., 2005,
15
Ma et al., 2007, Jin et al., 2009, Sood et al., 2009, Mostaffa et al., 2009a, Mostaffa et
al., 2011b, Arivazhagan et al., 2012
Masood & Song, 2005 has successfully produced a new filament with a strong,
flexible feedstock filament material for rapid tooling application. The flexible
feedstock filament has been used for producing the functional parts and tooling by the
FDM machine. Zhong et al., (2001) has been done to study the ABS filament material
on the softening point of ABS of 100 ̊C approximately, which accomplish the heat
resistant requirement in the FDM deposition process. The ABS polymer begin to flow
at 200 ̊C and decomposition temperature at 250 ̊C approximately. Meaning, that the
heated temperature must not beyond that temperature in order to prevent the
decomposition material.
The mechanical properties of thermoplastic polymer material are significantly
affected by the molecular orientation between ABS filaments (Rodriguez et al., 2001).
The orientation in extruded ABS depends on the extrusion temperature and extrusion
rate. Meaning that, an important criteria of ABS filament material used for deposition
process depends on the melt temperature and deposition feed rate in a layer by a layer
process.
The most important of material properties is the thermal degradation or
decomposition of ABS polymer used in mixing and compounding process. When the
temperature achieved at degradation temperature, some of the material weight
percentage were loss and some of the material will vaporize. According to Ma et al.,
(2007), the thermal degradation of ABS polymer is around 350 °C to 500 °C using
nitrogen gas. The thermal degradation of ABS polymer are shown in Figure 2.2. The
determination of degradation temperature shall be finalize at early stage before mixing
and compounding process with varieties material. In the experimental, the TGA curve
shows the decomposition of ABS polymer are degrading from 366 °C to 450 °C
respectively.
16
Figure 2.2 The TGA curve shows the decomposition of ABS polymer (Ma et al.,
2007)
2.2.3 Binder or Surfactant
Binder and surfactant material is used as a lubricant and release agent in the polymer
matrix composites material. Binder will be acts as temporary vehicle for
homogeneous packing a powder in desired shape (Omar et. al., 2010). The binder
composition of palm stearin of 50 % to 80 % and polyethylene of 20 % to 50 % in
weight percentage Furthermore, the binder system with palm stearin will gave better
rheological properties, bio natural source and environmental friendly in MIM (Subuki,
et al., 2005 and Omar et al., 2010). One of the main consideration in the binder
selection are an easier to find the material with good material characteristic and
rheological properties. Omar et al., (2010) was mentioned that, the bio-polymer like
a palm stearin binder gave a natural source, environmental friendly and better
rheological properties. Meaning that the some of the natural source binder will gave
a good followability when added into polymer matrix.
Surfactant powder is normally organic compound as a lubricant agent used in
polymer matrix composite. It consists of both hydrophobic groups and hydrophilic
groups. The surfactant contains a water soluble component and it will diffuse in water
and absorb at interfaces between air and water. By adding the surfactant in polymer
matrix will modified the surface properties with good interconnection bonding and
17
concentration. Surfactant also reduce the surface tension of water by adsorbing at the
liquids-gas interface.
Moballegh et al., (2005) was mentioned that the thermal degradation
properties of paraffin wax and polyethylene are degrading from 170 °C to 350 °C and
350 °C to 500 °C respectively where the feedstock content with 95 wt. % copper
powder. The binder degradation starts at 171 °C and in order to prevent the binder
degradation, the processing temperature of mixing and injected part in injection
molding must be lower than the degradation temperature. Figure 2.3 shown the
degradation temperature of paraffin wax and polyethylene binder.
Figure 2.3 TGA Curve of the feedstock with 95 wt. % copper powder (Moballegh et
al., 2005)
2.2.3.1 Binder in Injection Molding
Injection molding process has been well known in the plastic part fabrication with
mass production. The process involve with the mold making, injection machine and
system and polymer pallet material. Several polymers that have been used
wax/polymer as a binders which are polyethylene (Huang et al., 2003, Ganster et al.,
2006, Moballegh et al., 2005, Omar et al.. 2010 and Ahn et al.,2009). With 30 % by
18
weight percentage of polyethylene binder in injection molding gave better results for
flow behavior and viscosity Moballegh et al., 2005).
Li et al., (2007) and Huang et al., (2003) studied the rheology of several Fe-Ni
based wax/polymers feedstock with binders contained paraffin wax, EVA, HDPE and
PP. The binder composition in weight percentage of paraffin wax 65 %, poly ethylene
vinyl acetate 30 % and stearic acid 5 % in metal injection molding process. Binders
containing PW/EVA, PW/HDPE, PW/PP and PW/HDPE/PP wt % were prepared and
tested in the capillary rheometer. The results indicate that PW/PP binder was useless
because of binder separation in the capillary flow. On the other hand, the binder based
on PW/HDPE/PP showed the best flow behavior having the lowest shear sensitivity
and the lowest activation energy in flow.
Ma et al., (2007) was investigated the mechanical and thermal properties of
epoxy loaded with metal, ceramic or mineral salt powder. Aluminum, alumina, silicon
nitride and calcium sulphate dehydrate powder were selected as epoxy based
composites in weight %, which is 10 %, 20 %, 30 % and 40 %. Resin and hardener
material was a diglycidyl ether polymer and hardener aliphatic and cycloaliphatic
polyamine. The standard type of hardness is ASTM D2240-97 with specimen size
Ø16 mm, height 6.4mm, the compression is ASTM D695-96 with specimen size 12.7
mm x 12.7 mm x 25.4 mm, the thermal expension is ASTM E831-93 with specimen
size Ø5 mm and height 6 mm, wear rate ASTM G99-95a with specimen size Ø30 mm
and height 8 mm.
2.2.3.2 Binder in FDM
FDM machine has been well known in the rapid prototyping technology on a layer by
a layer process as long as the material in a filament wire. Normally, filament wire
material are from ABS, PLA, PP, PC and this plastic material will flow from spool
through the heated liquefied head on FDM machine. Some additive material act as
lubricant will be added in polymer matrix in compounding and mixing for filament
wire fabrication. The polymer-based binders, consists of blends of two or more
polymers. Masood et al. (2004) mentioned that, the function of plasticizer or binder
as a lubricant agent, increase the homogeneous dispersion and to reduce the
intermolecular friction between each particles distribution in the composites material.
19
2.2.4 Polymer Matrix Composites in Injection Molding
Various kinds of metal material used in injection molding process such as nickel by
Huang et al. (2003), alloys by Tseng & Tanaka (2001), Hartwig et al. (1998), copper
by Moballegh et al. (2005), iron by Gungor (2007), Huang et al. (2003), Ahn et al.
(2009) and Lam et al. (2003), stainless steel by Omar et al. (2010), Amin et al. (2009),
Ibrahim et al. (2009), Ahn et al. (2009), Hartwig et al. (1998) and Li et al. (2007),
titanium by Hartwig et al., (1998).
In the present work, the most common composites material used in injection
moulding are basalt-LDPE Akinci (2009), iron-HDPE Gungor (2007), Ahn et al.
(2009), iron, nickel-HDPE Huang et al. (2003), zirconia-PE Merz et al. (2002),
copper-PE Moballegh et al. (2005), stainless steel-PE Omar et al. (2010); Ahn et al.
(2009), stainless steel-PEG, PMMA Amin et al. (2009), Ibrahim et al. (2009), iron-
PP, EVA Ahn et al. (2009) and stainless steel-EVA Li et al. (2007).
The selection compounding of stainless steel powder in injection molding by
volume percentage is 65 % by Omar et al., (2010), 62 % to 64 % by Yulis et al.,
(2008), 60 % to 72 % by Li et al., (2007), 61.5 % to 62.5 % by Ibrahim et al., (2009).
Solid loading of stainless steel and iron powder in injection molding of 50 % to 64 %
in volume percentage by Ahn et al., (2009). Huang et al., (2003) was used 58 %
volume percentage of iron and nickel powder in metal injection molding process. A
similar finding was obtained by Merz et al., (2002), where the best compounding
zirconia powder in the injection molding of 50 % to 60 % by volume percentage with
average particle size 100 µm to 500 µm. Akinci (2009) was used 10 5 to 70 % in
weight percentage of basalt filler by injection molding process for mechanical
properties test of composites material.
2.2.4.1 Powder Loading (PL) of Feedstock
The volume ratio of solid powder to the total volume of powder and binder is defined
as the powder loading (Li et al., 2007). He has mentioned that, with higher powder
loading will lead to high viscosity and feedstock failure in injection. From the result
obtained it was concluded that, with higher powder loading the lower flowability of
feedstock. With 68 % to 72 % powder loading of SS is the best powder binder ratio
for metal injection feedstock with lowest compact distortion frequency. Moballegh et
20
al., (2005) concluded that the increasing of copper powder loading to significantly
increase the viscosity. The feedstock with 66.2 vol. % or 95 wt. % powder loading,
which has suitable viscosity and higher powder loading is prepared. The mixing and
injection molding temperatures must be lower in order to maintain binder degradation
where by binder degradation starts at 171 °C.
Several researchers were investigated the rheological properties of stainless
steel powder with binder contained polyethelene glycol (PEG), polymethyl
methacrilate (PMMA), stearic acid (SA) by variation of powder loading
concentration. The results indicate that 61.5 % powder loading gives the highest
rheological index with the lowest viscosity, easier flowability and low value of a flow
behavior exponent Ibrahim et al. (2009).
Gungor (2207) studied the mechanical properties of Fe powder fillers in the
HDPE polymer matrix based on vol. % (5, 10, 15vol. %). They concluded that an
additional 5 vol. % of Fe was reduced the impact strength of HDPE 40% and reduced
90% of elongation respectively. When vol. % Fe increase 10 and 15 vol. %, the impact
strength and % elongation values decrease proportionally. Additional 5 vol. % Fe
composite in HDPE, the modulus of elasticity was 31% higher than unfilled HDPE.
2.2.5 Polymer Matrix Composites in FDM
Currently, the most common composites' material used in layer by layer deposition
and FDM process deposition are HDPE-steatite ceramic by Karatas et al. (2004),
ABS-Iron Mostafa et al. (2009a), Mostafa et al. (2011b), Masood & Song (2004a),
Masood & Song (2005b), fibre glass Diegel et al. (2010). The compounding ratio of
iron and copper powder in the filament wire fabrication are from 5% to 40 % by
volume percentage (Mostaffa et al., 2011b) and 30 % to 40 % by volume percentage
(Masood et al., 2004a). Mostafa et al., (2009a) was mentioned that, due to the high
metal powder loading in the polymer matrix will increase the viscosity of composites
and dispersion of filament wire become worse.
An important characteristic of the powdered metal are particle size, particle
size distribution, particle shape and grain size of particles. Jing et al., (2000) was
mentioned that, the smallest particles size will create a higher possibility contact of
particles distribution in the composites material. A similarly procedure was made by
Guillet et al., (2009), where the copper or polymer composites annealing in primary
21
vacuum to minimize the oxidation. Mireles et al., (2012), has been noticed that, alloys
have a possibility to oxidize during the build process and the environment needs to be
controlled in order to minimize the oxidation. Copper remain as commercial metal in
engineering with excellent electrical conductivity, thermal conductivity, outstanding
resistance to corrosion, easy on fabrication, good strength and fatigue resistance
(Devis, 2001).
Some researcher was investigated the reproducibility and accuracy of
compounded stainless steel, electro ceramic group (ECG2) binder and stearic acid
using fused deposition of the metal (FDMet) process (Wu et al., 2002). The
QuickSlice 2.0 software was used to create the tool path and control the material
deposition rate and liquefied x-y position. Basic parameters are consisted of main
flow, preflow, start distance, start delay, shutoff distance, speed, acceleration and roll
back. Fine metal powders are preferred for eliminate the nozzle clog and a spherical
powder with average particle size 22µm. The stearic acid (SA) was selected as a
surfactant to reduce the inter-particle forces and to lubricate the powder. The 58 vol.%
SS17-4 powder compounded with 10% ,20%, 30% and 40% ECG2, 2 hour mixing
time. The extrusion temperature was 80-100, 1.78 mm nozzle size, 1 hour holding
time and extrusion speed 1mm/min during filament fabrication.
2.3 Material Issues in Mixing
Normally, material issues in mixing of varieties material are the melting temperature
during compounding below the degradation temperature. Each material they have
their own melt temperature and some of material will degrade at low temperature.
Application of FDM material requires a good mechanical properties and stiffness
toward rapid manufacturing in a layer by a layer process. Campbell et al., (2012) was
mention that a key development of part fabrication in direct manufacturing should be
incorporate with additives material in polymer matrix to enhance the mechanical
properties. Pure metal is unsuitable for deposit through the heated liquefied head by
FDM machine because of higher melting temperature and viscosity (Sa’ude et al.,
2014a). Layered of rapid deposition polymer composites (RDPC) with highly filled
metal powder in the polymer matrix may offer the possibility of introducing new
composite material in FDM.
22
2.3.1 Mixing and Compounding
Wu et al., 2002, have investigated the development of stainless steel-ECG2 ceramic
composite for time and cost saving using Fused Deposition Ceramic (FDC). It was
mentioned that, the compounding is a very critical process to provide homogenous
powder polymer mixture of stainless steel filament. The fabrication of ABS-Iron
filament wire for FDM machine has been done by Masood (1996); Masood and Song
(2005) and Mostafa et al. (2009a) and Mostafa et al. (2011b), with proper formulation
and mixing processes. They mentioned that, a very small percentage by weight of a
plasticizer and surfactant material was added in the ABS polymer matrix to improve
the flow and dispersion material and both material to act as a lubricant for reducing
intermolecular or friction between molecules polymer.
Furthermore, Mostafa et al. (2011b) have investigated the thermo mechanical
properties of a highly filled polymeric composites for FDM. The selection of metal
filler are 5%, 10%, 20%, 30% and 40% in volume percentage (vol. %). The metal
filler particles size is 45 µm with 99.7 % in metal purity. It was mentioned that, the
coated surfactant powder on the metal particles will reduces the high free energy
surfaces of the metal filler with lower interfacial tension between composite particles
in the melting stage.
2.3.2 Melting and Thermal Degradation Temperature
The physical and chemical of polymeric materials will be changes when heat is
applied during the compounding or mixing process in manufacturing processes.
Thermal degradation can present an upper limit to the service temperature of plastics
as much as the possibility of mechanical property loss. Thermal degradation is “a
process of the action or elevated temperature on a material, product or assembly
causes a loss physical, mechanical or electrical properties (Beyler & Hirschler, 2002).
The degradation temperature is an important criteria for finalize the weight
loss at early stage in the compounding process when the materials involve with heat.
The best selection temperature is to ensure the material will sustain the mechanical
and chemical properties in the compounding process without vaporize.
Thermogravimetric Analysis (TGA) measures the amount and rate of change
in the weight of a material as a function of temperature or time in a controlled
23
atmosphere. Measurements are used primarily to determine the composition of
materials and to predict their thermal stability at temperatures up to 1000 °C with a
scanning rate of 10 °C/min. The technique can characterize materials that exhibit
weight loss or gain due to decomposition, oxidation, or degradation. The TGA curve
for the degradation of ABS begins at 360 °C and the heating rate of 20 °C/min (Suzuki
et al., 1994), 340 °C for heating rate 10 °C/min (Wang et. al. , 2002), 450 °C for
heating rate 10 °C/min (Brebu et al., 2004). Figure 2.4 shows the TGA curve for ABS
terpolymer at a heating rate of 20 °C/min.
According to Mostaffa et al., (2011b) it was found that the glass transition
temperature increased proportionally with an increment of 10% iron in ABS. On the
peak glass transition temperature (Tg), the loss modules' value of 10% iron filled in
ABS is 368 MPa and the storage modulus value is 1700 MPa approximately.
Therefore, the Tangent delta will be calculated based on the loss modules divide by
storage modulus value. The value of viscoelastic material of 10% iron filled ABS is
61.5°. According to Figure 2.5, the Tangent delta value of 10% iron filled in ABS is
1.84. Therefore, the value of viscoelastic of virgin ABS is 64.8° approximately.
Meaning that the compounding material is in viscoelastic reagent at Tangent delta
peak (126 °C). The best value of viscoelastic material of the DMA should be in range
0 < tan delta < 90. The phase lag will be 0° for purely elastic material and 90° for
purely viscous material. Meaning that, in early stage on the FDM filament
development should in viscoelastic region for stiffness issues rather than brittles FDM
filament. Therefore, one of the important criteria of FDM filament must be good
stiffness and easily to flow through the heated liquefied head without break during
deposition process on the FDM platform.
24
Figure 2.4 TGA curve for ABS terpolymer at a heating rate of 20 °C/min (Suzuki &
Wilkie, 1994)
Figure 2.5 Dynamic mechanical properties of virgin ABS and 10% iron-powder
filled ABS (Mostafa et al., 2011b)
Dynamic mechanical Analysis (DMA) is a technique used to measure the
mechanical properties of an elastic, inelastic and viscous material. Normally, DMA
works in the linear viscoelastic range, and it is more sensitive to structure. In dynamic
mechanical test, the material stiffness and the loss modulus was measured. The
Sto
rag
e M
od
ulu
s
(MP
a)
Lo
ss M
od
ulu
s (M
Pa
)
118.93 °C
126
_____ 10% filled
ABS …….. Unfilled ABS
104
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