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EFFECTS OF HEAT TREATMENT ON THE MICROSTRUCTURES AND ELECTROCHEMICAL BEHAVIOR OF STAINLESS STEEL
NUR HASMISHA BINTI HASLAN
A thesis submitted in partial fulfillment of the requirements for the award of degree of
Master of Engineering (Mechanical-Materials)
Faculty of Mechanical Engineering Universiti Teknologi Malaysia
JANUARY 2013
v
ACKNOWLEDGEMENTS
I wish to express my sincere appreciation to my supervisor, Professor Dr
Esah Hamzah for her constant guidance and advice comments throughout the
completion of this work.
Thanks a lot to all the technicians of Material Science Lab in Faculty of
Mechanical Engineering for their willingness to guide and help me to do my thesis
experiments using all available facilities.
Very special thanks go to my mother Mrs. Ruslina Binti Dollah, my father
Haslan Bin H.Abdullah and my husband Mohd Hafiz Bin Harun for their support and
dedication.
Finally, I would like to thank all for their encouragement and constructive
advice.
vi
ABSTRACT
The objective of this project is to investigate the effects of heat treatment
parameters on corrosion resistance and phase transformation in relation to the
microstructures and electrochemical behaviors of austenitic 304 and martensitic 420
stainlesssteel. In this project, there are several heat treatment parameters under
investigation namely annealing at temperature 900 °C and 1000°C and normalizing with
difference soaking times. Other heat treatment process carried out on martensitic
stainless steel only is quench and temper. Corrosion test was conducted on non-treated
and heat treated samples according to British Standard (BS ISO 17475:2005) for
electrochemical test (Tafel test). Hardness test was also carried out on the non-treated
and heat treated samples using Vickers hardness test. Microstructure analysis was
performed on the samples using characterization equipment such as Glow Discharge
Spectroscope (GDS), Optical Microscope (OM), Scanning Electron Microscope (SEM),
Energy Dispersive X-ray (EDX) and X-ray Diffraction (XRD). The results shows that
heat treatment affect the microstructures and electrochemical behaviors of stainless
steel. It was also found that higher temperature gives lower hardness. From the corrosion
test results, it can be concluded that higher austenization temperatures and higher
normalizing soaking times improved the corrosion resistance of stainless steel due to
increase in grain size and less in formation of carbides. These carbides will contribute to
the corrosion whereby it provides sites for anodic and cathodic reaction to occur
between the carbide and the matrix phases.
vii
ABSTRAK
Objektif projek ini adalah untuk mengkaji kesan parameter rawatan haba ke atas
rintangan kakisan dan penjelmaan fasa dalam hubungan dengan mikrostruktur dan
tingkah laku elektrokimia 304 austenit dan martensit 420 keluli tahan karat. Di dalam
projek ini, terdapat dua parameter rawatan haba yang dikaji iaitu suhu austenit bersuhu
900°C dan 1000 °C dan menormalkan dengan perbezaan masa merendam. Lain-lain
proses rawatan haba yang dijalankan pada keluli tahan karat martensit sahaja iaitu
pelinkejutan dan pembajaan. Ujian kakisan telah dilakukan ke atas sampel-sampel yang
belum dirawat dan telah dirawat haba berdasarkan Piawaian British (BS ISO
17475:2005) untuk ujian elektrokimia. Ujian kekerasan juga telah dilakukan ke atas
sampel-sampel belum dirawat dan yang telah dirawat haba menggunakan ujian
kekerasan Vickers. Analisis mikrostruktur telah dilakukan ke atas sampel-sampel
menggunakan peralatan pencirian seperti Spektroskopi Nyahcas Bara (GDS),Mikroskop
Optik (OM), Mikroskop Imbasan Elektron (SEM), Sinar-X Serakan Tenaga (EDX) dan
Pembelauan Sinar-X (XRD). Keputusan kajian menunjukkan rawatan haba menjejaskan
mikrostruktur dan tingkah laku elektrokimia keluli tahan karat. Ia juga didapati bahawa
suhu yang lebih tinggi memberikan kekerasan yang lebih rendah. Daripada hasil ujian
kakisan, dapat disimpulkan bahawa suhu austenit dan lebih tinggi masa rendaman
penormalan meningkatkan rintangan kakisan keluli tahan karat disebabkan oleh
peningkatan dalam saiz bijian dan pengurangan pembentukan karbida.. Karbida ini akan
viii
menyumbang kepada kakisan di mana ia menyediakan laman untuk reaksi anodic dan
katod berlaku antara karbida dan fasa matriks.
viii
TABLE OF CONTENTS
CHAPTER TITLE PAGE
TITLE PAGE i
DECLARATION iii
DEDICATION iv
ACKNOWLEDGEMENT v
ABCTRACT vi
ABSTRAK vii
TABLE OF CONTENTS viii
LIST OF TABLES xiii
LIST OF FIGURES xiv
LIST OF ABBREVIATIONS xxi
1 INTRODUCTION 1
1.1 Background 1
1.2 Objectives of The Research 3
1.3 Statement of Research Problems 3
1.4 Scopes of Study 4
2 LITERATURE REVIEW 5
2.1 Introduction 5
2.2 Stainless Steel 5
2.3 Basic elements in Stainless steel 6
2.4 Types of Stainless steel 8
2.4.1 Austenitic Stainless Steel 10
2.4.2 Martensitic Stainless Steel 11
ix
CHAPTER TITLE PAGE
2.5 Heat Treatment 11
2.5.1 Heat Treatment Process for
Austenitic Stainless Steel 12
2.5.1.1 Annealing 12
2.5.1.2 Normalizing 14
2.5.1.3 Effect of Microstructure and
Mechanical Properties after
Annealing and Normalizing 14
2.5.2 Heat Treatment Process for
Martensitic Stainless Steel. 17
2.5.2.1 Effect of Microstructure and
Mechanical Properties after
Annealing and Normalizing 18
2.5.2.2 Effect of Microstructure and
Mechanical Properties after
Quenched and Tempered 19
2.5.2.3 Effect of Hardness on
Martensitic Stainless Steel
after Heat Treatment 23
2.6 Electrochemical Behavior of Stainless Steel 26
2.6.1 Electrochemical test 27
2.6.2 Effect of Heat Treatment on the
Electrochemical Behavior on
Martensitic Stainless Steel 29
3 RESEARCH METHODOLOGY 33
3.1 Introduction 33
3.2 Materials 35
3.2.1 Samples preparation 36
x
CHAPTER TITLE PAGE
3.3 Heat Treatment Processes 40
3.4 Metallographic Investigation 42
3.4.1 Determination of Grain Size 42
3.4.2 Microstructure Observation by
Using Optical Microscope 43
3.4.3 Microstructure Observation by
Using Scanning Electron
Microscope (SEM) 44
3.5 Materials Characterization 45
3.5.1 Energy Dispersive X-Ray Analysis
(EDX) 45
3.5.2 X-Ray Diffraction (XRD) 47
3.6 Hardness Test 48
3.7 Electrochemical Test 49
4 RESULTS AND DISCUSSION 53
4.1 Introduction 53
4.2 Microstructural Characterization of
As-Received Materials 53
4.2.1 Chemical Composition of AISI 304
Austenitic Stainless Steel and AISI 420
Martensitic Stainless Steel. 54
4.2.2 Microstructure Analysis of Austenitic
Stainless Steel 54
4.2.2.1 Optical Microscopy Analysis 54
4.2.2.2 Scanning Electron Microscope
and Energy Dipersive X-Ray
Analysis of As-received Sample 55
4.2.2.3 X-Ray Diffraction Analysis of
As-received sample 57
xi
CHAPTER TITLE PAGE
4.2.3 Microstructure Analysis of Martensitic
Stainless Steel 57
4.2.3.1 Optical Microscopy Analysis 58
4.2.3.2 Scanning Electron Microscope
and Energy Dipersive X-Ray
Analysis of As-received Sample 58
4.2.3.3 X-Ray Diffraction Analysis of
As-received Martensitic
Stainless Steel Sample. 60
4.3 Microstructural Characterization of
Heat Treated Samples 61
4.3.1 Austenitic Stainless Steel after
Annealing Process 61
4.3.2 Austenitic Stainless Steel after
Normalizing Process 63
4.3.3 Martensitic Stainless Steel after
Annealing Process 66
4.3.4 Martensitic Stainless Steel after
Normalizing Process 67
4.3.5 Martensitic Stainless Steel after
Quench and Temper Process 70
4.3.6 Effect of Grain Size on Heat
Treated Austenitic Stainless Steel 71
4.3.7 XRD Analysis on Heat Treated
Stainless Steel 73
4.3.7.1 Austenitic Stainless Steel after
Annealing Process 73
4.3.7.2 Austenitic Stainless Steel after
Normalizing Process 74
4.3.7.3 Martensitic Stainless Steel after
Annealing Process 76
xii
CHAPTER TITLE PAGE
4.3.7.4 Martensitic Stainless Steel after
Normalizing Process 77
4.3.7.5 Martensitic Stainless Steel after
Quench and Temper Process 78
4.4 Mechanical Property – Hardness 80
4.5 Electrochemical Behavior after Heat Treatment 82
5 CONCLUSIONS 89
5.1 Conclusions 89
5.2 Recommendation for future work 90
REFERENCES 91
APPENDICES 97
xiii
LIST OF TABLES
TABLE NO. TITLE PAGE
2.1 Allotropes of Iron (Rivlin and Raynor, 1980) 6
2.2 Atomic sizes of Fe, Cr and Ni (Rivlin and Raynor, 1980) 7
2.3 304 stainless steel chemical compositions [wt%] 10
2.4 Grain sizes of austenite crystal at different quenching
temperatures (Liu Yu-rong, 2011) 19
3.1 Chemical Composition (wt%) of materials used 35
3.2 Parameters for X-Ray Diffraction (XRD) Measurement 47
4.1 Results of chemical composition of the as-received
stainless steel 54
xiv
LIST OF FIGURES
FIGURE NO. TITLE PAGE
2.1 Three dimentional view of the Fe-Cr-Ni equilibrium 8
diagram. (H.J.Eckstein, 1990)
2.2 Equilibrium diagram for Fe-Cr alloys (without carbon
content) (L. Colombier and J. Hochman, 1967). 9
2.3 900 °C isotherm of Cr-Fe-Ni system. (Rivlin, V.G.
and Raynor, G.V.1980) 13
2.4 1000 °C isotherm of Cr-Fe-Ni system. (Rivlin, V.G.
and Raynor, G.V.1980) 13
2.5 Optical micrograph of the solution annealed material
consisting of equiaxed austenite grains
(J. Ka¨llqvist, 1999) 15
2.6 Grain boundary M23C6 precipitates in a austenitic
stainless steel observed using transmission electron
microscopy (A. F. Padilha and P.R.Rios, 2006) 15
2.7 Optical micrographs paired with representative maps
of the modified 316LN alloy in the (a and d)
as-received, (b and e) 20 hours and (c and f) 100 hours
annealed conditions, respectively
(S. Downey II, P.N. Kalu, K. Han, 2008) 16
xv
2.8 SEM micrographs of M316LN in the (a) 100 hours
annealed and (b) as-received conditions (S. Downey
II, P.N. Kalu, K. Han, 2008) 17
2.9 Microstructure of tested steel quenched at 1050 °C
(a) Steel 1, (b) Steel 2 (Liu Yu-rong, 2011) 20
2.10 Microstructure of the heat treated AISI 420,
(a) 1050 °C, (b) 1015 °C, (c) 980 °C
(A. N. Isfahany, 2011) 21
2.11 EDS analysis of specimens tempered at (a) 200 °C,
(b) 500 °C, (c) 700 °C. (A. N. Isfahany, 2011) 22
2.12 The relationship between the carbon content and
the hardness of martensite (Wei Du, 2011) 24
2.13 Effect of austenitizing time and temperature on
Hardness (A. N. Isfahany, 2011) 25
2.14 Hardness versus tempering temperature
(A. N. Isfahany, 2011) 26
2.15 Potentiodynamic plot of austenitic stainless steel
sample at different tempering times and tempering
temperature of (a) 150 °C and (b) 250 °C
(Ayo Afolabi, 2011) 30
2.16 Comparison between 980◦C and 1050◦C potensiostatic
curves in AISI 420 (A. N. Isfahany, 2011) 32
3.1 Research Methodology 34
xvi
3.2 LECO GDS850A Glow Discharge Atomic
Spectrometer (GDS) 35
3.3 Schematic drawings of shapes and dimensions of the
(a) Austenitic and (b) Martensitic stainless steel
were sectioned respectively 37
3.4 Mecatome T255/300 Cutter Machine 38
3.5 Buehler Rool Grinder 38
3.6 Metaserv Polishing Machine 39
3.7 Buehler Electromet 4 Electro Etching Machine 39
3.8 Schematic heat treatment path for annealing process 41
3.9 Schematic heat treatment path for normalizing process 41
3.10 Schematic heat treatment path for quench and
temper process 42
3.11 Research Microscope (manufactured by Nikon in 1995) 44
3.12 Phillips XL40 scanning electron microscope 45
3.13 Schematic Drawing of X-Ray Detector for
EDX Analysis 46
3.14 X-Ray Diffractometer 47
3.15 Matsuzawa Seiki Vickers Hardness 48
3.16 The samples cold mounted in plastic moulds 50
xvii
3.17 Working electrode (mounted samples and
copper wire enclosed in glass tube) 50
3.18 Potentiostat/ galvanostat Corrosion Test Machine
(Parstat-2263) 51
3.19 Sample in all-glass cell of (a) an actual preparation
and (b) schematic drawing according to
ASTM Standard G-5 51
3.20 The anodic and cathodic polarization curves in
E vs. I / (A/cm2) 52
4.1 Optical micrograph of as-received austenitic
stainless steel (etched with oxalic acid solution, 200x) 55
4.2 (a) Scanning Electron Micrograph of as-received
austenitic stainless steel at magnification 2000x;
(b), (c), (d), and (e) EDX results to verify element
content on microstructure 56
4.3 XRD results of as-received austenitic stainless steel 57
4.4 Optical micrograph of as-received martensitic
stainless steel (etched with oxalic acid solution, 200x) 58
4.5 SEM micrograph of as-received martensitic
stainless steel (etched with oxalic acid solution, 2000x) 59
4.6 (a) SEM micrograph of as-received martensitic
stainless steel at magnification 2000x, (b), (c), (d),
and (e) EDX results to verify element content
on microstructure 59
xviii
4.7 XRD results of as-received martensitic stainless steel 61
4.8 Optical micrographs of the annealed austenitic
stainless steel at (a) 900 ° C and (b) 1000 °C
consisting of equiaxed austenite grains (etched with
oxalic acid solution, 200x) 62
4.9 Optical micrographs of the austenitic stainless steel
normalized at 900 ° C for (a) 1 hour and (b) 2 hours
consisting of equiaxed austenite grains (etched with
oxalic acid solution, 200x) 63
4.10 SEM micrograph of the austenitic stainless steel
normalized at 900 ° C for (a) 1 hour and (b) 2 hours
(c) 8 hours consisting of equiaxed austenite grains,
Spot A = at dark area, Spot B = at grain boundary,
Spot C = at matrix of the surface 65
4.11 Optical micrographs of the martensitic stainless steel
annealed at (a) 900 ° C and (b) 1000 °C
(etched with oxalic acid solution, 200x) 67
4.12 Optical micrographs of the martensitic stainless steel
normalized at 900 ° C for (a) 1 hour, (b) 2 hours and
(c) 8 hours (etched with oxalic acid solution, 200x) 68
4.13 Scanning electron micrographs of the martensitic
Stainless steel normalized at 900 ° C for (a) 1 hour
and (b) 2 hours (1000x) and (c) 8 hours (1000x) 69
4.14 Optical micrographs of the martensitic stainless steel
austenizing at 980 °C for (a) 1 hour and (b) 2 hours
and tempered at 200 °C for 1 hour (etched with oxalic
acid solution, 200x) 70
xix
4.15 Result of hardness (grain size vs temperature and
soaking time) on (a) annealed samples and
(b) normalized samples respectively 71
4.16 XRD Analysis on the Austenitic Stainless Steel
Annealed at (a) 900°C and (b) 1000°C 72
4.17 XRD Analysis on the Austenitic Stainless Steel
Normalized at 900°C for (a) 1hour, (b) 2 hours
and (c) 8 hours soaking times 74
4.18 XRD Analysis on the Martensitic Stainless Steel
Annealed at (a) 900°C and (b) 1000°C 75
4.19 XRD Analysis on the Martensitic Stainless Steel
Normalized at 900°C for (a) 1hour ,
(b) 2 hours and (c) 8 hours soaking times 76
4.20 XRD Analysis on the Martensitic Stainless Steel
Austenized at 980°C for (a) 1hour and (b) 2 hours
soaking times 78
4.21 Hardness (Hv) of Annealed Stainless Steel 79
4.22 Hardness (Hv) of Normalized Stainless Steel 79
4.23 Hardness (Hv) of Quenched and Tempered Stainless Steel 80
4.24 Tafel graph E vs A/cm2 results in water medium for
Annealed 304 Stainless Steel at (a) 900°C, (b) 1000°C 81
xx
4.25 Tefal graph E vs log (I) results in water medium on
the Austenitic Stainless Steel Normalized at 900°C
for (a) 1hour, and (b) 2 hours soaking times and
(c) 8 hours soaking times 82
4.26 Tafel graph E vs log (I) results in 3.5% NaCl solution
as a medium for Annealed 304 Stainless Steel at
(a) 900°C and (b) 1000°C 84
4.27 Tefal graph E vs log (I) results in 3.5% NaCl medium
on the Austenitic Stainless Steel Normalized at 900°C
for (a) 1hour, and (b) 2 hours soaking times and
(c) 8 hours soaking times 85
4.28 The corrosion rate (mpy) of annealed austenitic
stainless steel in water medium and 3.5% NaCl solution 87
4.29 The corrosion rate (mpy) of normalized austenitic
stainless steel in water medium and 3.5% NaCl solution 87
4.30 Tefal graph E vs log (I) results in water medium on
the Martensitic Stainless Steel Quench and Temper
for (a) 1hour and (b) hours soaking times 88
xxi
LIST OF ABBREVIATIONS
1
CHAPTER 1
INTRODUCTION
1.1 Background
Stainless steels form part of the great section cut through history by the
development of iron alloys, beginning about 1400 B.C. with the first man-made iron.
The so-called industrial revolution was made possible only through Cort’s improvement
in iron making methods and his introduction of mills to produced rolled sections (J.
Gordon Parr, 1971). As a class of materials, stainless steels stand apart and are
considered the backbone of modern industry since they find wide applications in
chemicals, petrochemicals, off-shore, power generation, allied industries (Maurer E. and
Strauss B, 1920).
With the mass production of steel came a scientific interest in the material. Of
course, there were brilliant examples of earlier research. But it is not until about 1890
that the constitution and properties of steels were methodically investigated. By 1920
2
metallurgist were applying methods of x-rays diffraction to the study of metallic
properties (J. Gordon Parr, 1971).
Satisfactory and economical heat treatment plays and important role in the
selection and development of engineering materials, and stainless steel are no exception.
Such steels are normally favored for engineering applications requiring good strength at
moderate temperatures and high corrosion resistance. Most grades of stainless steels are
usually low in carbon (0.05 to 0.20%) but contain 4 to 18% chromium along with other
alloying elements (M. I. Qureshi and M. Mujahid, 2000). In the industry, the component
that used stainless steel will expose to the high temperature environment and at the long
time exposure. That will result in changing mechanical properties or microstructures of
the stainless steel due to the failure. Many researches had been conducted to investigate
the effect of the heat treatment on the stainless steels.
Besides the favorable corrosion properties of stainless steels, the good
mechanical properties make these materials very interesting for mechanical engineering
applications. They are used in demanding applications as, for instance, in the processing
and power industry (Henrik Sieurin, 2006).
Austenitic stainless steels of the AISI 304 and 316 types, amongst other hundred
types of stainless steels available in the market, are the most frequently used ones
worldwide. They are selected for numerous applications due to their favorable
combination of characteristics such as low price, moderate to good corrosion resistance,
excellent ductility and toughness along with good weldability (C.Herrera, 2007).
3
Martensitic stainless steels are commonly used to manufacturing components
with excellent mechanical properties and moderate corrosion resistance, so that they can
work under high and low temperatures. Unlike other stainless steel, their properties
could be changed by heat treatments hence these steels usually are used for a wide range
of applications such as steam generators, pressure vessels, cutting tools, and offshore
platforms for oil extraction (J.-Y. Park and Y.-S. Park, 2006).
1.2 Objectives of The Research
The objectives of the research are as follows:
1. To characterize the microstructures of stainless steels after various heat
treatments.
2. To determine the electrochemical behavior of heat treated stainless steels.
1.3 Statement of Research Problems
Microstructures of stainless steel can be varied by heat treatment. Variation in
microstructures is expected to affect the mechanical properties and electrochemical
behavior of the steels. The heat treatment may enhance the steel properties but it may
also gives poor performance. Therefore, selection of correct heat treatment is paramount
in order to have stainless steel with better mechanical and electrochemical properties.
4
1.4 Scopes of Study
The scopes of the study are as follows:
a) Initial investigation on as-received martensitic and austenitic stainless
steels in terms of chemical composition, microstructures and properties
b) Selection of heat treatment methods that can vary the microstructures and
properties: Annealing, normalizing, quench and temper.
c) Detail investigation on the heat treated samples by using optical
microscope, SEM, EDX and XRD.
d) Electrochemical test (Tafel) on heat treated samples to relate between
variation in microstructures due to heat treatment and the corrosion
resistance of the steels.
91
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