1 the effect of milling time on aluminum- silicon carbide...

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THE EFFECT OF MILLING TIME ON ALUMINUM- SILICON

CARBIDE COMPOSITE

MUSTAFA KHALEEL IBRAHIM

UNIVERSITI TEKNOLOGI MALAYSIA

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THE EFFECT OF MILLING TIME ON ALUMINUM- SILICON

CARBIDE COMPOSITE

MUSTAFA KHALEEL IBRAHIM

A project report submitted in partial fulfilment of the

requirements for the award of the degree of

Master of Engineering (Materials Engineering)

Faculty of Mechanical Engineering

Universiti Teknologi Malaysia

JUNE 2014

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To my beloved family

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ACKNOWLEDGEMENT

In the name of God, the most Gracious, the most Merciful.

I wish to express my sincere appreciation to my supervisor, Prof. Dr.

Jamaliah Idris for her guidance and advice.

Special thanks to all the technicians in faculty of Mechanical Engineering,

UTM who involved directly or indirectly in the accomplishment of this research.

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ABSTRACT

Silicon carbide particle reinforced aluminum matrix composites have been

developed over past few decades, owing to their excellent properties like light

weight, wear resistance and high elastic modulus. Thus, the silicon carbide particle

reinforced aluminum matrix composites are expected to have many applications in

aerospace, automobile, aircraft and electronic industries. In this study, aluminum

metal matrix composites contains two weight percentages of reinforcement particles

were prepared by mechanical alloying. The main steps in mechanical alloying are

milling, compacting and sintering. The experiments were performed on two

composition of silicon carbide powder in the composite. The study presents the

results of the influence of milling time on aluminum- silicon carbide composite and

the effect of different weight percentage of silicon carbide in composite on hardness

and microstructure of the composite. Aluminum and silicon carbide particles are

mixed of different milling times 0, 40, 80, 120 minute. Digital image analyzer was

used to characterize the composites. The effect of weight percentage of silicon

carbide on hardness of composites was investigated by using Vickers hardness Test.

Hardness of the composites increased with increasing silicon carbide addition in it.

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ABSTRAK

Matriks komposit aluminum yang diperkukuh dengan zarah silikon karbida

telah dibangunkan sejak beberapa dekad lalu kerana kecemerlangan sifat-sifat seperti

ringan, tahan rintang dan modulus elastik yang tinggi. Oleh itu, matriks komposit

aluminum yang diperkukuh dengan zarah silikon karbida dijangka mempunyai

banyak aplikasi dalam aeroangkasa, kereta, kapal terbang dan industri elektronik.

Dalam kajian ini, komposit matriks logam aluminium mengandungi dua peratusan

berat zarah pengukuhan telah disediakan melalui pengaloian mekanikal. Langkah-

langkah utama dalam pengaloian mekanikal ialah penghancuran, mampatan dan

pensinteran. Eksperimen dijalankan ke atas dua komposisi serbuk silikon karbida

dalam komposit. Kajian ini membentangkan hasil pengaruh masa pengisaran

terhadap komposit aluminium-silikon karbida dan kesan peratusan berat yang

berbeza daripada silikon karbida dalam komposit pada kekerasan dan struktur mikro

yang telah dikaji. Zarah aluminium dan silikon karbida dicampur pada masa

pengisaran yang berbeza; 0, 40, 80, 120 minit. Penganalisis imej digital digunakan

untuk mencirikan komposit. Kesan peratusan berat silikon karbida pada kekerasan

komposit dikaji menggunakan kekerasan Ujian Vickers. Kekerasan komposit

meningkat dengan peningkatan silikon karbida di dalamnya.

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TABLE OF CONTENTS

CHAPTER TITLE PAGE

DECLARATION ii

DEDICATION iii

ACKNOWLEDGEMENT iv

ABSTRACT v

ABSTRAK vi

TABLE OF CONTENTS vii

LIST OF TABLES xi

LIST OF FIGURES xiii

1 INTRODUCTION 1

1.1 Project Background 1

1.2 Metal Matrix Composite 2

1.2.1 Metal Matrix Composite Definitions 2

1.2.2 Metal Matrix Composite

Applications

2

1.3 Problem Statement 3

1.4 Research Objectives 4

1.5 Research Significance 4

1.6 Research Scope 4

1.7 Research Organization 5

2 LITERATURE REVIEWS 6

2.1 Introduction 6

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2.1.1 AMCs Applications 7

2.2 Mechanical Alloying 7

2.2.1 Milling Objectives and Limits 9

2.2.2 Grinding Machine and Process 10

2.2.3 Factors Affecting Grinding Process 13

2.3 Materials and Applications 15

2.3.1 Aluminum (Al) 15

2.3.2 SiC 17

2.3.3 Al SiC 20

2.3.4 Al2O3 SiC 27

2.4 Nano Composites Fabrication Methods 31

2.4.1 Spark Plasma Sintering 31

2.4.2 High-Pressure Sintering 32

2.4.3 Hot Press Sintering 32

3 RESEARCH METHODOLOGY 33

3.1 Introduction 33

3.2 Research Design 34

3.3 Materials 35

3.4 Milling Device 36

3.5 Experiment Design 37

3.6 Measurement 37

3.7 Hydraulic Press 38

3.8 Sintering 40

3.9 Mounting 41

3.10 Grinding and Polishing 42

3.11 Summary 42

4 RESULTS AND DISCUSSION 43

4.1 Introduction 43

4.2 Aluminum 44

4.3 Silicon Carbide 46

4.4 Aluminum- Silicon Carbide 48

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4.5 Hardness Test 73

4.5 Compression Test 74

5 CONCLUSION 82

5.1 Conclusion 82

5.2 Recommendations 83

REFERENCES 84

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LIST OF TABLES

TABLE NO TITLE PAGE

2.1 Milling media in high-energy milling 11

3.1 Milling time 37

4.1 Milling parameters for mixing aluminum and

silicon carbide powders

44

4.2 Compressive test parameters 75

4.3 Maximum data 76

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LIST OF FIGURES

FIGURE NO TITLE PAGE

2.1 Impact Event at a Time of Maximum Impacting

Force

8

2.2 (a) Ball milling, (b) High energy ball milling, (c)

Grinder

11

2.3 An overview of the main factors to be considered

in the milling process

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2.4 Different SiC Particle Sizes: [17] 10 µm and (b) 40

µm

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2.5 Variation of Hardness as a Function of Vol. % SiC

Particulates

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2.6 Microstructure of Al – wt 10 % with milling time

(a) 0 hour, (b) 2 hours, (c) 5 hours, (d) 10 hours

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2.7 Relationship between hardness and milling time 22

2.8 SEM images of (a) as-received Al powder, (b) 12

lm SiC powder, (c) 16 lm SiC powder and the Al–

10%SiC–12 lm powder mechanically alloyed for

(d) 4 h and (e) 8 h (lamellar structure of one of

powder particles is shown in higher magnification)

and (f) 12 h

23

2.9 SEM images of (a) Al–5%SiC–16 lm, (b) Al–

10%SiC–16 lm and (c) Al–20%SiC–16 lm, after 12

h of milling time (the right column is same as the

left but in higher magnification).

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2.10 Powder structure development after attritor- (A1–

A5) and planetary ball milling (B2–B5) of pure Al

and with 1 vol.%, 5 vol.%, 10 vol.% and 20 vol.%

reinforcement. The scale is the same for all the

micrographs except for B2 with mm-sized granules

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2.11 Microstructure of Monolithic Al2O3 and ASx

Samples: (a) Monolithic Al2O3, (b) AS1, (c) AS2,

and (d) AS5

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3.1 The Research Design 34

3.2 Ball Mill 36

3.3 Weight Scale 38

3.4 Hydraulic press mould 39

3.5 Hydraulic press machine 39

3.6 Sintering furnace 40

3.7 The samples after sintering 40

3.8 Mounting machine 41

3.9 Mounted samples 41

3.10 Grinding and polishing machine 42

4.1(a) SEM of aluminum powder before milling 44

4.1(b) X- RAY diffraction (XRD) showed the meeting of

the analysis peaks with aluminum peaks

45

4.1(c) Energy dispersive X-RAY analysis (EDX) showed

the chemical composition of aluminum

46

4.2(a) SEM of silicon carbide powder before milling 46

4.2(b) X- RAY diffraction (XRD) showed the meeting of

the analysis peaks with silicon carbide peaks

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4.2(c) Energy dispersive X-RAY analysis (EDX) showed

the chemical composition of silicon carbide

48

4.3 (a) SEM images of 5%Sic- Al powder composite, at

milling time (a) 0 minute, (b) 40 minute, (c) 80

minute, (d) 120 minute, of 500x magnification

49

4.3 (b) SEM images of 5%Sic- Al powder composite, at


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minute, (d) 120 minute, of 1,00kx magnification 50

4.4 (a) SEM images of 10%Sic- Al powder composite, at


minute, (d) 120 minute, of 500x magnification

51

4.4 (b) SEM images of 10%Sic- Al powder composite, at


minute, (d) 120 minute, of 1,00kx magnification

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4.5 X-RAY diffraction (XRD) of aluminum 53

4.6 X-RAY diffraction (XRD) of silicon carbide 53

4.7 X-RAY diffraction (XRD) of 5%Sic-Al powder

composite

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4.8 X-RAY diffraction (XRD) of 10%Sic-Al powder

composite

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4.9 Energy dispersive X-RAY analysis (EDX) showed

the chemical composition of 5%sSic- Al powder

composite, at 0 minute milling time

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56




57




58




59




60



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composite, at 80 minute milling time 61

4.16 Energy dispersive X-RAY analyses (EDX) showed



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4.17 Optical microscope images of 5%Sic- Al samples

after hydraulic press and sintering of 550c for 5

hours, at milling time of pressed powder (a) 0

minute, (b) 40 minute, (c) 80 minute, (d) 120

minute.

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4.18 Optical microscope images of 10%Sic- Al samples

after hydraulic press and sintering of 550c for 5

hours, at milling time of pressed powder (a) 0

minute, (b) 40 minute, (c) 80 minute, (d) 120

minute

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4.19 Scanning electron microscope image of 5%Sic- Al

samples after hydraulic press and sintering of 550c

for 5 hours, at 0 minute milling time and 500x

magnification

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sample after hydraulic press and sintering of 550c


magnification

65




magnification

66




magnification

66




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magnification 67




magnification

67




magnification

68


samples after hydraulic press and sintering of 550c


magnification

68

4.27 Scanning electron microscope image of 10%Sic-

Al sample after hydraulic press and sintering of

550c for 5 hours, at 0 minute milling time and 500x

magnification

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550c for 5 hours, at 40 minute milling time and

500x magnification

69




500x magnification

70




500x magnification

70




1000x magnification

71

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1000x magnification

71




1000x magnification

72




1000x magnification

72

4.35 Relationship between hardness and milling time of

Al- 10% SiC composite

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4.36 Relationship between hardness and milling time of

Al- 10% SiC composite

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4.37 Compression test of aluminum- silicon carbide

composites

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4.38 5%SicC –Al composite sample, and 0 minute

milling time. Shows even in presence of the cracks

the ultimate stress is still high because of the

orientation of the cracks horizontal to the applied

load. Also may be due to high ductility

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4.39 5%SiC- Al composite sample, and 40 minute

milling time shows lower ultimate stress (73) Mpa

due to the presence of cracks with orientation

vertical to applied load. And the value 513 Mpa

refers to the machine strain not to the sample

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4.40 5%SiC –Al composite, and 80 minute milling time 77

4.41 5%SiC –Al composite, and 120 minute miliing

time. Shows decreasing in ultimate stress may be

because of decreasing of ductility of composite.

78

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4.42 10%SiC- Al composite, and o minute milling time 78

4.43 10%SiC- Al composite, and 40 minute milling time 79

4.44 10%SiC- Al composite, and 80 minute milling time 79

4.45 10%SiC- Al composite, and 120 minute milling

time

80

4.46 5% SiC –Al composite 80

4.47 10% SiC –Al composite 81

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CHAPTER 1

INTRODUCTION

1.1 Project Background

A composite material is a ‘material system’ composed of a combination of

two or more micro or macro constituents that differ in form, chemical composition

and which are essentially insoluble in each other. Aluminum-matrix composites are

not a single material but a family of materials whose stiffness, strength, density,

thermal and electrical properties can be tailored. The matrix alloy, reinforcement

material, volume and shape of the reinforcement, location of the reinforcement and

fabrication method can all be varied to achieve required properties. The aim

involved in designing metal matrix composite materials is to combine the desirable

attributes of metals and ceramics. One of the major challenges when processing

MMCs is achieving a homogeneous distribution of reinforcement in the matrix as it

has a strong impact on the properties and the quality of the material (Mares, 2001).

2

1.2 Metal Matrix Composite

1.2.1 Metal Matrix Composite Definitions

A composite material is made by combining two or more materials – often

ones that have very different properties. The two materials work together to give the

composite unique properties. However, within the composite you can easily tell the

different materials apart as they do not dissolve or blend into each other.

Composite material is a mixture of two or more materials or phases of the

same material, insoluble in one another, possessing properties which are superior to

any of the component materials (Vencl & Rac, 2004).

1.2.2 Metal Matrix Composite Applications

Metal matrix composite (MMC) is engineered combination of the metal

(Matrix) and hard particle/ceramic (Reinforcement) to get tailored properties.

MMC’s are either in use or prototyping for the space shuttle, commercial airliners,

electronic substrates, bicycles, automobiles, golf clubs, and a variety of other

applications (Singla, et al., 2009).

3

1.3 Problem Statement

There are many methods used to reduce the size of materials to become

powder but not all types can achieve the desirable size of fine powder. The common

methods such as jaw crusher or hammering method, sometimes results in the material

losses of its characteristics during size reduction process. High quality ball mills are

potentially expensive and can grind mixture particles to as small as 0.0001 mm,

enormously increasing surface area and reaction rates. However, normal ball mill is

inexpensive and simple process, but it suffer from some defects such as occurring of

wear, principally from the balls, but partially from the casing and this may result in

the product being contaminated. Also soft or sticky materials may cause problems

by caking on the sides of the mill or by holding the balls in aggregates (Bhatt &

Agrawal, 2007).

In milling process, there are many different process variables that can be

tuned in order to obtain a product with well-established properties: milling time,

milling speed, size of grinding media, ball-to-powder ratio, controlled atmosphere,

and so on. This fabrication method is thus simple but not trivial and it can be an

attractive technology in nano-powder production (Russo et al., 2011; Singla et al.,

2009).

Generally, nanoparticles synthesis requires the use of a device or process that

handles these problems (Horikoshi & Serpone, 2013):

• Control of particle size, size distribution, shape, crystal structure and

composition distribution

• Improvement of the purity of particles (lower impurities)

• Control of aggregation

• Stabilization of physical properties, structures and reactants

• Higher reproducibility

• Higher mass production, scale-up and lower costs

4

1.4 Research Objectives

1. To obtain (Aluminum -Silicon carbide) composite from mixing of the two

powders and to study the effect of the milling time on particles size and

distribution.

2. To study the effect of milling time on microstructure and mechanical

properties of (Aluminum –Silicon carbide) composites.

1.5 Research Significance

Raw materials and often occur in sizes that are too big to be used, and

therefore, there must be a reduction or changing in size however if the milled raw

material is too fine and the dispersion of reinforcement material is not good.

Different raw materials vary in shape and size, fragility and durability, and the

product may vary from coarse powder for ease in different industries for different

purposes. Fabrications of fine particles are being investigated increasingly in industry

and academic research because of the applications on a large scale in all the fields of

science and production.

1.6 Research Scope

The research aims to study the effect of ball milling on two selected

materials. Different quantities of powder of Aluminum (Al) and Silicon Carbide

(SiC) will be used to achieve the research goals. The ball mill machine PM 400 will

5

be used in the research experiments. The machine is designed to fabricate a small

powder size estimated in hundreds of grams.

1.7 Research Organization

This research is organized into five chapters as follows. Chapter 2 explores

the literature review. Chapter 3 explains the research methodology. The results and

discussion are demonstrated in Chapter 4, while conclusions and recommendations

are in chapter 5.

84

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