ALLOYING OF ALUMINIUM SURFACE WITH Q-SWITCHED Nd:YAG...

ALLOYING OF ALUMINIUM SURFACE WITH

Q-SWITCHED Nd:YAG LASER

MOHD SHAFIQ BIN SHAHARIN

UNIVERSITI TEKNOLOGI MALAYSIA

ALLOYING OF ALUMINIUM SURFACE WITH

Q-SWITCHED Nd:YAG LASER

MOHD SHAFIQ BIN SHAHARIN

A thesis submitted in fulfillment of the

requirements for the award of degree of

Master of Science (Physic)

Faculty of Science

Universiti Teknologi Malaysia

APRIL 2015

iii

Dedicate, with love,

To my beloved family especially my parents

Wan Zaharah binti Wan Ab Rahman & Shaharin bin Hj Mohammed

To all my lovely my friends,

Thank you for understanding and support through my endeavour till

the end.

iv

ACKNOWLEDGEMENT

Alhamdulillah. First and foremost, I am grateful to Allah SWT for His mercy,

has given me the strength and health to complete this master study. I wish to express

my deepest and sincere gratitude to my master degree supervisor, Prof. Dr. Noriah

Bidin toward the successful completion of this study. Thank you for her expertise,

sincerity, valuable guidance and encouragement extended to me.

My sincere thanks and appreciation go to Dr Waskito, Fakaruddin, Ganesan,

Mundzir, Aiza, Hanum, Radhiana, Hida, Syuhada and Saleha for theirs assistance

and guidance during my lab works. My warm thanks to my colleague and friends

Luqman, Junaidi, Amirul, Mustakim, Ahmad, Syamsul and others for their thoughts,

opinions, cooperation’s and friendships throughout completing this research.

I owe my loving thanks to my parents and my family members. Thank you

for their patience, support and motivation all the way from the beginning of this

research. Last but not least, I take this opportunity to record my sincere thanks to all

who, directly or indirectly, have lent their helping hands in this venture.

v

ABSTRACT

In surface modification, laser has been used as a tool to improve and enhance

the surface properties of metallic alloys through laser alloying technique. Therefore,

the aim of this study is to modify aluminium surface with iron (Fe) and copper (Cu)

by Q-switched Nd:YAG laser. The Q-switched Nd:YAG laser is operating at a

fundamental wavelength of 1064 nm with 10 ns pulse duration. The laser optimized

parameters in this work are focus distance, pulse width and pulse energy. The target

consists of a pure aluminium plate and the two alloying elements used are iron (Fe)

and copper (Cu) powders. The alloying elements were well mixed and prepared in

four different ratios (Fe:Cu) of (1:0), (1:1), (2:1), and (3:1). The surface alloying

process was carried out by varying the laser output energy delivered to the targets

from 67 to 331 mJ per pulse. The modified surfaces were characterized by using

three types of analysis; structural elemental, and mechanical analysis. The results

from field emission scanning electron microscopy (FESEM) showed that the surface

microstructures change significantly compared to the untreated surface. The

formation of alloyed layer due to the rapid melting and solidification processes of

alloying elements with aluminium substrate was observed. In addition, all the treated

surfaces show less porosity and are free from any cracks. X-ray diffraction (XRD)

analysis of the treated surface showed the formation of new compounds which

comprise AlCu, AlFe, CuFe and AlFeCu. The maximum hardness of the treated

surfaces as measured using microhardness tester is 86.2 HV which is two times

higher than that of the untreated surface. The formation of intermetallic phases and

the change in the surface microstructures are responsible for the increase in the

surface hardness compared to untreated one.

vi

ABSTRAK

Dalam pengubahsuaian permukaan, laser telah digunakan sebagai alat untuk

memperbaiki dan meningkatkan sifat-sifat permukaan aloi metalik melalui teknik

pengaloian laser. Oleh itu, tujuan kajian ini adalah untuk mengubah suai permukaan

aluminium dengan menggunakan besi (Fe) dan kuprum (Cu) dengan melalui laser

Nd:YAG bersuis-Q. Laser Nd:YAG bersuis-Q ini beroperasi pada panjang

gelombang asas 1064 nm dengan tempoh denyutan 10 ns. Parameter-parameter laser

yang dioptimumkan dalam kerja ini adalah jarak fokus, lebar denyut dan tenaga

denyut. Sasaran merupakan kepingan aluminium tulen dan dua bahan pengaloian

digunakan adalah serbuk besi (Fe) dan kuprum (Cu). Bahan-bahan pengaloian

dicampurkan dengan sekata dan disediakan dalam empat nisbah yang berbeza

(Fe:Cu) iaitu (1:0), (1:1), (2:1), dan (3:1). Proses pengaloian permukaan telah

dijalankan dengan mengubah tenaga keluaran laser kepada sasaran bermula 67

hingga 331 mJ per denyut. Permukaan yang diubahsuai telah dicirikan dengan

menggunakan tiga jenis analisis; analisis struktur unsur dan mekanikal. Keputusan

daripada mikroskopi elektron imbasan medan pancaran (FESEM) menunjukkan

mikrostruktur permukaan telah berubah secara ketara berbanding permukaan yang

tidak diubahsuai. Pembentukan lapisan aloi disebabkan oleh proses peleburan dan

pemejalan yang laju berlaku antara bahan aloi dengan substrat aluminium telah

diperhatikan. Tambahan pula, semua permukaan yang diubahsuai menunjukkan

bilangan liang yang kurang dan bebas dari sebarang keretakan. Analisis pembelauan

sinar x (XRD) pada permukaan yang diubahsuai menunjukkan pembentukan sebatian

baru yang terdiri daripada AlCu, AlFe, CuFe dan AlFeCu. Kekerasan maksimum

permukaan yang diubahsuai diukur menggunakan penguji kekerasan mikro adalah

86.2 HV yang mana dua kali lebih tinggi berbanding permukaan yang tidak

diubahsuai. Pembentukan fasa-fasa intermetalik dan perubahan pada mikrostruktur

permukaan bertanggungjawab terhadap peningkatan pada kekerasan permukaan

berbanding yang tidak diubahsuai.

vii

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

LIST OF SYMBOLS xvii

ABBREVIATIONS xix

1 INTRODUCTION

1

1.1 Background Information 1

1.2 Problem Statement 3

1.3 Research Objective 3

1.4 Scope of the Study 4

1.5 Thesis Outline 4

viii

2 LITERATURE REVIEW

6

2.1 Introduction 6

2.2 Aluminium 6

2.3 Laser Technology in Material Processing 8

2.4 Laser Surface Treatment 10

2.5 Laser Surface Alloying Technique 13

2.5.1 Effect of Laser Energy During Laser

Alloying

2.5.2 Effect of Laser Beam Spot Size During

Laser Alloying

2.5.3 Effect of Shielding Gas During Laser

Alloying

2.5.4 Effect of Powder Particle Size During

Laser Alloying

2.6 Metastable Phase Formation

15

15

17

17

17

2.7 Laser Surface Alloying Mechanisms 18

2.8 Advantages and Disadvantages of Laser Surface

Alloying

19

2.9 Hardness 19

2.8.1 Vickers Hardness Test

20

3 RESEARCH METHODOLOGY

22

3.1 Background Information 22

3.2 Materials and Sample Preparation

3.2.1 Samples Preparation

3.2.2 Alloying Element

3.2.3 Surface Preparation

24

24

26

27

3.3 Laser Surface Modification

3.3.1 Q-Switched Nd:YAG Laser

3.3.2 Laser Calibration

29

29

30

ix

3.3.3 Laser Surface Alloying Process 35

3.4 Microstructure Characterization Techniques

3.4.1 Microscopy Analysis

3.4.2 Hardness Analysis

37

37

38

4 RESULT AND DISCUSSION

39

4.1 Introduction 39

4.2 Sample Location and Labeling

4.2.1 Sample Location

4.2.2 Sample Labeling

40

40

40

4.3 Modified Surface Sample Characterization

4.3.1 Sample A

4.3.1.1 XRD Analysis

4.3.1.2 FESEM and EDXS Analysis

4.3.1.3 Microhardness Measurement

4.3.2 Sample B




4.3.3 Sample C




4.3.4 Sample D




4.4 Effect of Laser Surface Modification to the

Surface Hardness

41

42

42

44

48

50

50

52

56

58

58

60

64

66

66

68

72

74

x

5 CONCLUSION

77

5.1 Summary 77

5.2 Recommendations 79

REFERENCES 80

APPENDICES

79

PAPERS & PRESENTATIONS

92

xi

LIST OF TABLES

TABLE NO TITLE PAGE

2.1 Physical properties of aluminium 7

2.2 Lasers properties in material processing 9

3.1 Physical properties of the alloyed materials 27

3.2 Q-switched Nd:YAG laser calibration 30

3.3 Beam spot size and beam density upon displacement 32

3.4 Surface hardness testing 34

4.1 Sample label specification 40

4.2 List of peaks observed on the spectrum A 42

4.3 The element and compound present on the treated

sample A

43

4.4 Surface hardness of modified sample A 48

4.5 List of peaks observed on the spectrum B 50

4.6 The element and compound present on the treated

sample B

51

4.7 Surface hardness of modified sample B 56

4.8 List of peaks observed on the spectrum C 58

4.9

The element and compound present on the treated

sample C

59

4.10 Surface hardness of modified sample C 64

4.11 List of peaks observed on the spectrum D 66

xii

4.12

The element and compound present on the treated

sample D

67

4.13 Surface hardness of modified sample D 72

xiii

LIST OF FIGURES

FIGURE NO TITLE PAGE

2.1 Summary of laser surface treatment 10

2.2 Range of laser process in surface modification 12

2.3 Schematic diagram of laser alloying process 13

2.4 Gaussian beam with curved wavefronts 16

2.5 Vickers hardness indenter 20

3.1 Overview of the experiment process flowchart 22

3.2 Original aluminium metal plate 25

3.3 Aluminium metal plate after cutting process 25

3.4 Grinding and polishing machine 25

3.5 Aluminium metal plate in ultrasonic cleaning 25

3.6 Aluminium metal plate during drying process 26

3.7 Aluminium metal plate ready for pre-coated process 26

3.8 Powders of alloying element (A) iron and (B) copper 26

3.9 Pure aluminium metal plate for pre-coating 28

3.10 Pre-coating process 28

3.11 Pre-coating sample during sintering process 28

3.12 Pre-coating sample ready for surface modification 28

3.13 AL-114 Q-Switched Nd:YAG laser 29

3.14 Output laser energy versus applied energy 31

xiv

3.15 Laser beam spot along the Rayleigh region 31

3.16 Beam density versus displacement 33

3.17 Displacement versus surface hardness 34

3.18 Schematic diagram of the experiment set-up 35

3.19 Experimental set-up of laser surface alloying 36

3.20 Plasma formation 36

3.21 FESEM analysis instrument 37

3.22 Shimadzu micro-vickers hardness tester 38

4.1 Treated aluminium surface 41

4.2 X-ray diffraction pattern of Sample A alloyed surface 43

4.3 Microstructure of sample A alloyed surface with

magnification of X400

44



45



46

4.6 EDXS qualitative analysis of spectrum 1 for Sample A

alloyed surface

47


alloyed surface

47


alloyed surface

47

4.9 Graph of sample A surface hardness 49

4.10 X-ray diffraction pattern of Sample B alloyed surface 51

4.11 Microstructure of sample B alloyed surface with


52

4.12 Microstructure of sample B alloyed surface with


53



54

4.14 EDXS qualitative analysis of spectrum 1 for Sample B

alloyed surface

55

xv


alloyed surface

55


alloyed surface

55

4.17 Graph of sample B surface microhardness 57

4.18 X-ray diffraction pattern of Sample C alloyed surface 59

4.19 Microstructure of sample C alloyed surface with


60



61



62

4.22 EDXS qualitative analysis of spectrum 1 for Sample C

alloyed surface

63


alloyed surface

63


alloyed surface

63

4.25 Graph of sample C surface microhardness 65

4.26 X-ray diffraction pattern of Sample D alloyed surface 67

4.27 Microstructure of sample D alloyed surface with


68



69



70

4.30 EDXS qualitative analysis of spectrum 1 for Sample D

alloyed surface

71


alloyed surface

71


alloyed surface

71

4.33 Graph of sample D surface microhardness 73

xvi

4.34

Graph of surface hardness with different types of

samples

74

xvii

LIST OF SYMBOLS

cm - Centimeter

g - Gram

oC - Celsius

W - Watt

m - meter

K - Kelvin

J - Joule

kg - Kilogram

Ω - Ohm

MPa - Megapascal

mm - Millimeter

ns - nanosecond

ms - millisecond

Ed - Energy density

d - Diameter

E - Energy

HV - Vickers Hardness Number

F - Load

V - Volt

% - Percentages

Hz - Hertz

xviii

d

-

Diagonal length

θ - Angle between opposite face of the diamond

xix

ABBREVIATIONS

FESEM - Field Emission Scanning Electron Microscopy

XRD - X-ray diffraction

EDXS - Energy-dispersive X-ray spectroscopy

LSA - Laser Surface Alloying

Nd:YAG - Neodymium-doped yttrium aluminium garnet

CO2 - Carbon dioxide

Ti - Titanium

Nb - Niobium

Fe - Iron

Cu - Copper

Cr - Chromium

Ni - Nickel

CHAPTER 1

INTRODUCTION

1.1 Background Information

Aluminium is extensively used in industry due to its excellent in conductivity

for both thermal and electrical, high mechanical strength, low specific weight, good

formability, and relatively low cost (Tomida and Nakata, 2003). Within excellent

characteristic, poor surface properties such as hardness and wear resistance have

limited it in application range. These limitations might be overcome if the surface

properties could be improved while retaining the bulk properties. There are a few

metallurgical techniques that may be utilized to improve surface properties, for

example, flame spraying, plasma spraying and electroplating. However, these

techniques are not usually applied because of the poor metallurgical bonding to the

base material (Katipelli et al., 2000). Due to the rapid advancement in the field of

surface engineering, conventional techniques for surface treatment have been

replaced by techniques using advanced heat sources such as plasma, laser, ion, and

electron.

For many years, lasers are practically well-known as a powerful tool that can

be used for many applications such as cutting, welding, drilling and surface

2

modification. Many research works have been conducted to enhance the surface

properties of the material through laser material processing. Laser has many

excellent features and one of them is the effective processes in surface treatment of

the metallic substrates. Laser treatment is new and have various number of

advantages in relation to processing and the most interesting one is the possibility of

producing surface alloys or structures which not attainable by other methods.

Usually, laser material processing involve a thermal process where the

absorption of large number of photons heats the metallic material to achieve the

surface modification. Previous studies show that laser surface treatment and coating

could be an ideal technique to protect die surfaces from thermal fatigue and extend

die life by reducing the damage at contact surfaces (Jiang et al., 2001). Laser surface

modification offers a solution to enhance the surface properties of metallic alloys

(Almeida et al., 1995). The electromagnetic radiation of laser beam has been fully

utilized as a part of thermal processes to modify the microstructure of the surface

layer to enhance the surface properties in comparison with the material original

properties. Within laser beam, the applied energy can be delivered precisely on the

surface of an opaque material that is enabling in increasing the temperature of

substrate material above the melting point.

Among the various surface modification techniques, laser surface alloying is

considered to be the most effective technique to modify the surface properties of

aluminium since previous studies by various authors have shown positive results

(Tomida and Nakata, 2003; Jiang and Molian, 2001; Almeida et al., 1995; Tomida et

al., 2001; Das, 2004; Ravi et al., 2000). The most important advantage of this process

is the possibility of modifying the properties and composition within a thin surface

layer without affecting the properties of the bulk material.

3

1.2 Problem Statement

Aluminum is currently receiving a great deal of attention from several

industries such as aircraft, automotive and household appliance due to its unique and

excellent properties. However, its tribological characteristics such as hardness, wear

and corrosion resistance are poor in comparison to steel. Research on the aluminum

has been carried out actively in the past few decades by laser alloying with various

elements such as Cu, Nb, Ti, Fe, Cr and Ni (Tomida and Nakata, 2003; Katipelli et

al., 2000; Man et al., 2007; Almeida et al., 1995; Das, 2004). Mostly, lasers used in

surface modification are high energy, high power, continuous and long wavelength

like CO2 laser that reach up to 10 m. However, it is not suitable and easy task to

modify a localized area. Therefore, this work will be carried out in order to alloying

aluminum by using Q-switched Nd:YAG laser. This versatile surface treatment

technique utilized such laser with only low-level energy, faster, great precision,

localized treatment and controllable with number of pulses.

1.3 Research Objectives

The main objective of this study is to alloy aluminum surface with Iron (Fe) and

Copper (Cu) by a Q-switched Nd:YAG laser. In attempt to achieve this goal, the

following works are performed:

1. To optimize laser ablation parameters in alloying process

2. To analyze the composition of new composite on alloy surface

3. To characterize the surface hardness of the alloy

4

1.4 Scope of the Study

In this study, a Q-switched Nd:YAG laser with a fundamental wavelength of

1064 nm and pulse duration of 10 ns was employed as a source of energy. The laser

was focused by a biconvex lens with focal length of 10 cm. The target comprised of a

pure aluminum plate that stand as a substrate material. The chosen alloying elements

to alloy the aluminum substrate were iron (Fe) powder and copper (Cu) powder.

Both powders was mixed (Fe:Cu) with ratios of 1:0, 1:1, 2:1 and 3:1. Bostik contact

bond glue was selected as an adhesive material to bond between substrate and

alloying element. The aluminum surface was painted with glue prior pre-coated with

alloying element. The samples target were placed at the focal point in order to obtain

the optimum energy density from the laser to ensure maximum melting at the coated

surface. The alloying process was carried out by exposing the pre-coated sample to

energy in the range of 66.88 mJ to 331.25 mJ. The modified sample was examined

using the metallurgical techniques including FESEM (Field Emission Scanning

Electron Microscopy), EDX (Energy Dispersive X-ray Spectroscopy) and XRD (X-

ray Diffraction). The strength of the modified surface is measured by using a Vickers

hardness tester.

1.5 Thesis Outline

The entire research was documented in the thesis, and it consists of five main

chapters. Chapter 1 describes the introduction and background information of the

thesis, problem statement, a list of the research objective and the scope of the

research.

Chapter 2 is on the complete theory of the laser surface modification. It

explains the basic process of alloying technique, the effect of laser parameter and its

5

mechanism. The basic properties of aluminium and working principle of hardness

tester also explained in this chapter.

Chapter 3 explains the methodology of the research. In this chapter, the

sample preparation, experimental setups, and its process are discussed. The laser

calibration such as laser output, beam density and sample target location were

measured. Several characterization techniques involved in this project were also

included.

Chapter 4 discuss the microstructure characterization and hardness evaluation

in detail. All the results were presented and discussed in this chapter. This includes

the analysis of microstructure alloyed surface and its elemental composition via

FESEM and EDXS. Then followed by XRD analysis to determined the phase

formation on alloyed surface. The hardness measurements of alloyed surface were

also presented.

Finally, all the works are concluded in Chapter 5. This includes the summary

of the results achieved from the experiment works together with some

recommendations for future study.

.

80

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