EVALUATION OF NICKEL ELECTROLESS PLATING ON MILD STEEL MOHD RIDZWAN BIN ADNAN Thesis submitted in fulfillment of the requirements for the award of the degree of Bachelor of Mechanical Engineering Faculty of Mechanical Engineering UNIVERSITI MALAYSIA PAHANG DECEMBER 2010
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EVALUATION OF NICKEL ELECTROLESS PLATING ON MILD STEEL
MOHD RIDZWAN BIN ADNAN
Thesis submitted in fulfillment of the requirements
for the award of the degree of Bachelor of Mechanical Engineering
Faculty of Mechanical Engineering
UNIVERSITI MALAYSIA PAHANG
DECEMBER 2010
ii
UNIVERSITI MALAYSIA PAHANG
FACULTY OF MECHANICAL ENGINEERING
I certify that the thesis entitled “Evaluation of Nickel Electroless Plating on Mild Steel”
is written by Mohd Ridzwan Bin Adnan. I have examined the final copy of this thesis
and in my opinion; it is fully adequate in terms of scope and quality for the award of the
degree of Bachelor of Mechanical Engineering. I herewith recommend that it be
accepted in fulfillment of the requirements for the degree of Bachelor of Mechanical
Engineering.
LUQMAN HAKIM BIN AHMAD SHAH
Examiner: Signature
iii
SUPERVISOR’S DECLARATION
I hereby declare that I have checked this project and in my opinion, this project is
adequate in terms of scope and quality for the award of the degree of Bachelor of
Mechanical Engineering.
Signature:
Name of Supervisor: DAYANGKU NOORFAZIDAH BINTI AWANG SH’RI
Position: LECTURER
Date: 06 DECEMBER 2010
iv
STUDENT’S DECLARATION
I hereby declare that the work in this project is my own except for quotations and
summaries which have been duly acknowledged. The project has not been accepted for
any degree and is not concurrently submitted for award of other degree.
Signature:
Name: MOHD RIDZWAN BIN ADNAN
ID Number: MA08007
Date: 06 DECEMBER 2010
vi
ACKNOWLEDGEMENTS
I am grateful and would like to express my sincere gratitude to my supervisor
Mrs. Dayangku Noorfazidah binti Awang Sh’ri for her germinal ideas, invaluable
guidance, continuous encouragement and constant support in making this research
possible. She has always impressed me with her outstanding professional conduct, her
strong conviction for science and material, and her belief that a degree program is only a
start of a long-time learning experience. I appreciate her consistent support from the
first day I applied to graduate program to these concluding moments. I am truly grateful
for her progressive vision about my training in science and material, her tolerance of my
naïve mistakes, and her commitment to my future career. I also sincerely thank her for
the time spent proofreading and correcting my many mistakes.
My sincere thanks go to all my labmates and members of the staff of the
Mechanical Engineering Department, UMP, who helped me in many ways and made
my stay at UMP pleasant and unforgettable. Many special thanks go to member science
and material research group for their excellent co-operation, inspirations and supports
during this study.
I acknowledge my sincere indebtedness and gratitude to my parents for their
love, dream and sacrifice throughout my life. I also gratefully acknowledge the
assistance of everybody who helped in the execution of this project in UMP. Special
thanks to Mr. Basirul Subha Bin Alias as the PSM coordinator, who has given some
advice and share his knowledge on this PSM. I would like to acknowledge their
comments and suggestions, which was crucial for the successful completion of this
study.
vii
ABSTRACT
Nickel electroless plating on mild steel is carried out by a chemical reaction and without
the use of an external source of electricity. In nickel electroless plating, nickel chloride
will come as a metallic salt and is reduced by using Sodium hypophosphite as the
reducing agent to nickel metal, which then is deposited on the mild steel. In this
experiment, the effect of solution concentration on thickness and mechanical properties
of nickel plating on mild steel using electroless plating process was investigated. The
solutions used in this experiment were Sodium hypophosphite and nickel chloride.with
varying concentration. Electroless plating were done for 30 days. Then the surface
structure and morphology nickel plating was evaluated using scanning electron
microscopy (SEM), Optical Microscope while its hardness was evaluated using Vickers
hardness test. In electroless plating, anode is the movements of negative ions toward the
positive electrode and the mild steel as the cathode because the movement of positive
ions toward the negative electrode. Electroless plating found the coating thickness by
effected of percentage of concentration of solution, effect of thickness of coating to the
mechanical properties and anode and cathode weight loss in electroless plating. The size
of sample specimen is 0.05 m of length, 0.03 m of width and 0.001 m of thickness for
both of mild steel and nickel sheet metal. The machine that was applied in the
experiment were, shearing machine to cut the mild steel into size, drilling machine to
make a hole to the surface of mild steel and nickel, micro vickers hardness test machine
to get a mechanical properties behavior to mild steel after electroless plating and
scanning electron microscopy (SEM) to get the microstructure observation of sample
after electroless plating. The highest coating thickness is at 252 µm corresponding to
percentage of concentration solution of 22.2 % at sample 8 followed by 19.4 %, 16.7 %,
13.9 %, 11.1 %, 8.3 %, 5.6 %, and 2.8 % for sample 7, 6, 5, 4, 3, 2, and 1. When the
percentage of concentration of solution is increase, the hardness value of mild steel is
decrease while the coating thickness increases. So, the grain size of microstructure will
increase while increase the percentage of concentration of solution.
viii
ABSTRAK
Penyaduran nikel kurang elektro pada keluli tulen (mild steel) dilakukan oleh reaksi
kimia dan tanpa menggunakan sumber tenaga elektrik sebagai agen luar. Dalam
penyaduran nikel kurang elektro, Nikel klorida akan datang sebagai garam metalik dan
dikurangkan dengan menggunakan Natrium hipofosfit sebagai agen pengurangan untuk
logam nikel, yang kemudian disimpan dalam keluli tulen. Pada eksperimen ini,
pengaruh konsentrasi larutan terhadap ketebalan dan sifat mekanik pelapisan nikel pada
keluli tulen dengan menggunakan proses penyaduran atau pelapisan kurang elektro
diselidiki. Serbuk larutan yang digunakan dalam penyaduran ini adalah Natrium
hipofosfit dan nikel klorida dengan pelbagai kepekatan. Penyaduran kurang elektro
dilakukan selama 30 hari. Kemudian struktur permukaan dan morfologi penyaduran
nikel dinilai menggunakan Pengimbasan Mikroskop Elektron (SEM), Mikroskop
optikal manakala kekerasannya dinilai dengan menggunakan ujian kekerasan Vickers.
Dalam penyaduran kurang elektro, Anod adalah pergerakan ion negatif terhadap
elektrod positif dan keluli tulen sebagai katod kerana pergerakan ion positif terhadap
elektrod negatif. Hal ini di sebabkan ketebalan lapisan mempengaruhi peratusan
kepekatan larutan, pengaruh ketebalan lapisan terhadap sifat mekanik dan kehilangan
berat pada katod dan katod pada penyaduran kurang elektro. Saiz sampel spesimen
adalah 0.05 m panjang, 0.03 m lebar dan 0.001 m tebal untuk kedua keluli tulen dan
kepingan logam nikel. Mesin yang digunakan dalam eksperimen adalah, mesin
pemotong untuk memotong keluli tulen mengikut ukuran, mesin gerudi untuk membuat
lubang pada permukaan keluli tulen dan nikel, mesin ujian kekerasan vicker mikro
untuk mendapatkan perilaku sifat mekanik untuk keluli tulen selepas penyaduran kurang
elektro dan Pengimbasan Mikroskop Elektron (SEM) di gunakan untuk mendapatkan
pemerhatian mikrostruktur pada sampel selepas penyaduran kurang elektro. Ketebalan
lapisan tertinggi pada 252 µm sesuai dengan peratusan kepekatan larutan sebanyak 22,2
% pada sampel 8 diikuti oleh 19.4 %, 16,7 %, 13,9 %, 11,1 %, 8,3 %, 5,6 %, dan 2.8 %
untuk sampel 7, 6, 5, 4, 3, 2, dan 1. Apabila peratusan konsentrasi larutan bertambah,
nilai kekerasan untuk keluli tulen akan berkurang sementara meningkatkan ketebalan
lapisan. Jadi, saiz butiran mikro akan meningkat sementara meningkatnya peratusan
kepekatan larutan.
ix
TABLE OF CONTENTS
Page
APPROVAL DOCUMENTS ii
SUPERVISOR’S DECLARATION iii
STUDENT’S DECLARATION iv
DEDICATION v
ACKNOWLEDGEMENTS vi
ABSTRACT vii
ABSTRAK viii
TABLE OF CONTENTS ix
LIST OF TABLES xiii
LIST OF FIGURES xiv
LIST OF SYMBOLS xvii
LIST OF ABBREVIATIONS xviii
CHAPTER 1 INTRODUCTION
1.1 Project Background 1
1.2 Problem Statement 2
1.3 Project Objectives 2
1.4 Project Scope of Work 2
1.5 Significance of The Study 3
1.6 Project Flow Diagram 5
1.7 Project Flow Details 6
1.8 Project Task (Gantt Chart) 7
CHAPTER 2 LITERATURE REVIEW
2.1 Introduction 8
2.2 Current Existing Electroless Plating Sample 9
2.2.1 Origin of Electroless Nickel, History and Basic Theory 9
x
2.2.2 Interpretation of Electroless Plating 10
2.2.3 Electroplating Process 11
2.2.4 Coating Technologies 14
2.2.5 Mechanical Properties of Nickel Electroless Plating 15
2.3 Parameter Included In Nickel Electroless Plating 21
2.3.1 Types of Chemical 21
2.3.2 Type of Material 23
2.3.3 Common Material Plated 23
2.4 Applications of Electroless Nickel Plating 25
2.5 Pretreatment of Parts for Electroless Nickel Plating 26
2.5.1 Advantages of Electroless Nickel Plating 26
2.5.2 Disadvantages of Electroless Nickel Plating 27
2.6 Time Uses In Electroless Nickel Plating 28
2.6.1 For Corrosion Resistance 28
2.6.2 For Wear Resistance in Hard to Reach Areas 28
2.7 Types of Electroless Nickel Plating 28
2.7.1 Nickel Phosphorus Baths 28
2.7.2 Nickel-Boron Baths 29
2.7.3 Polyalloys 30
2.7.4 Composite Coatings 30
2.8 Scanning Electron Microscopy (SEM) 31
2.9 Conclusion 32
CHAPTER 3 RESEARCH METHODOLOGY
3.1 Introduction 33
3.2 Process Flow Diagram 35
3.3 Specimen Preparations 36
3.3.1 Type of Metal that were Used 36
3.3.2 Size of Sheet Metal 37
3.3.3 Quantity Needed in Experiment 38
3.4 Items of Solution 39
3.4.1 Type of Solution that were Used 39
3.4.2 Concentration of Solution 40
3.4.3 Preparation of Solution 41
3.5 Apparatus and Instrument Preparation 41
3.5.1 Apparatus that Apply 41
xi
3.5.2 Instrument Preparations 43
3.6 Overall Experiment Configuration 44
3.7 Design of Experiment (DOE) 46
3.7.1 General Flow of Experiment 46
3.7.2 Step-by-Step of Procedure 47
3.8 Conclusion 57
CHAPTER 4 RESULTS AND DISCUSSION
4.1 Introduction 58
4.2 Before Electroless Plating Process 59
4.2.1 Important Aspect 59
4.2.2 Weight Measurement Process 60
4.3 Anode and Cathode Weight Loss in Electroless Plating 62
4.4 Material Characterization 65
4.5 Microstructure Observation 66
4.5.1 Microstructure Observation for Mild Steel After
Electroless Plating Process
66
4.5.2 Nickel Coating Surface Morphology 67
4.5.3 Grain Boundaries Structure of Mild Steel on The Surface
after Electroless Plating Process
69
4.6 Evaluation of Effect of Percentage of Concentration 70
4.6.1 Effect of Percentage of Concentration of Solution to the
Thickness of Coating
70
4.6.2 Effect of Coating Thickness to the Mechanical properties 77
CHAPTER 5 CONCLUSION AND RECOMMENDATIONS
5.1 Introduction 79
5.2 Conclusions 79
5.3 Recommendation 80
REFERENCES 82
APPENDIXS 84
A Data of important aspect before electroless nickel plating process 84
B Data for measuring the mass of powder before electroless plating
process
85
xii
C Data for mixture of distilled water + sodium hypophosphite +
nickel chloride before electroless plating process
86
D Data for weight after electroless plating process 88
E Data for comparing the reading of Mild Steel and Nickel before
and after electroless plating process
89
F Data for Reading of Mild steel by using Micro Vickers Hardness
Test (HV)
90
G
(a) –(h)
Metallurgical microscope grain boundary structure for specimen 1
until specimen 8
91
H Overall experiment setup for electroless plating process 99
xiii
LIST OF TABLES
Table No. Title Page
2.1 Coating processes used to protect functional surfaces 15
2.2 Properties of sodium phosphinate 22
3.1 The experiment’s essentials in electroless plating 47
4.1 The sample preparation of electroless plating process 59
4.2 Measuring the weight of powder (Sodium Hypophosphite &
Nickel Chloride
60
4.3 Amounts for each sample specimen before electroless plating
process
61
4.4 Comparing the weight of Mild Steel and Nickel before and after
Electroless plating
62
4.5 The percent of weight loss of mild steel and nickel 63
4.6 The thickness of coating with fix of time to plating (30 day) 75
4.7 Reading of mild steel by using micro vickers hardness test (HV) 77
5.1 Etching used for low carbon steel 81
6.1 Data of important aspect before electroless nickel plating process 84
6.2 Data for measuring the mass of powder before electroless plating
process
85
6.3 Data for mixture of distilled water + sodium hypophosphite +
nickel chloride before electroless plating process
86
6.4 Data for weight after electroless plating process 88
6.5 Data for comparing the reading of Mild Steel and Nickel before
and after electroless plating process
89
6.6 Data for Reading of Mild steel by using Micro Vickers Hardness
Test (HV)
90
xiv
LIST OF FIGURES
Figure No. Title Page
1.1 Project flow diagrams 5
1.2 Project gantt chart 7
2.1 Examples of electroformed Microstructures 10
2.2 Schematic of electroplating process 12
2.3 Order in which dissimilar metals produce electromotive-force
(Galvanic) series
13
2.4 Chemical reaction of sodium phosphinate 22
2.5 Evo 50 type of common SEM machine in industries 31
2.6 Schematic diagram of SEM 32
3.1 Process flow diagram 35
3.2 Sample of mild steel sheet metal 36
3.3 Sample of nickel sheet metal 37
3.4 Sketching for Size of specimen 38
3.5 Size of specimen 38
3.6 Sample powder of sodium hypophosphite and
its colour
39
3.7 Sample powder of nickel chloride and its colour 40
3.8 Sample of 500ml glass beaker 42
3.9 Sample of commonly electronic wire 42
3.10 Sample of stick 43
3.11 Evo 50 type of Common SEM machine 44
3.12 Sample 5 during electroless plating 44
3.13 Schematic diagram of nickel electroless plating on mild steel 45
xv
3.14 General flow of experiment 46
3.15 Cutting process 48
3.16 Drilling process 49
3.17 Filing process 49
3.18 Measurement process 50
3.19 The specimens before added to the distilled water 51
3.20 The specimens after added to the distilled water 51
3.21 Vickers hardness test (HV) 52
3.22 Mounting process 53
3.23 Grinding and polishing process 54
3.24 Etching process 55
3.25 Etching time and place to etching process 55
3.26 Observation process by using metallurgical microscope 56
3.27 Observation process by using optical microscope 56
4.1 The weighted loss of mild steel and nickel after electroless plating 64
4.2 The sample 8 of mild steel in electroless plating process, (a)
before; (b) after
65
4.3 The sample of microstructure observation after electroless plating
for sample 1
66
4.4 SEM surface morphology of nickel electroless plating 67
4.5 The surface of mild steel by using metallurgical microscope 68