The Eect of Phase Morphology and Volume Fraction of Retained Austenite on the Formability of Transformation Induced Plasticity Steels

by

Jerey Benjamin Rutter Lawrence

A thesis submitted to the Department of Mechanical and Materials Engineering in conformity with the requirements for the degree of Masters of Applied Science

Queens University Kingston, Ontario, Canada January 2010

Copyright Jerey Benjamin Rutter Lawrence, 2010

Abstract
Transformation induced plasticity (TRIP) steels are a class of steels with exceptional formability properties, due mainly to the presence of meta-stable retained austenite which transforms to martensite under loading, locally hardening the steel. The volume fraction and mechanical stability of the retained austenite play an important role in producing the high formabilities of TRIP steels. In this thesis, two separate morphologies of retained austenite, equiaxed versus lamellar, have been produced through thermo-mechanical processing of a single common TRIP steel chemistry. The sheet formability characteristics of these two microstructures were examined, with varying volume fractions of retained austenite, through uniaxial tensile and in-plane planestrain (IPPS) testing. It was found that higher levels of retained austenite produced better formability properties for both microstructures and strain paths. In uniaxial tension it was seen that the the lamellar microstructure attained higher strains at maximum load, and exhibited more sustained instantaneous n values than the equiaxed structure, despite having a lower volume fraction of retained austenite. IPPS testing was performed using an optical measurement of local strain and a comparative forming limit based on dierences in strain rate between a developing neck and the surrounding material. It was found that the lamellar microstructure performed better than the equiaxed microstructure for this strain path, achieving higher strains before reaching the comparative forming limit.

For Rachel, without whose love and support this thesis would not have been possible.

ii

Acknowledgements
I would like to acknowledge: My supervisors Dr. Keith Pilkey and Dr. Doug Boyd, for their great help, support, expertise, and friendship which was invaluable in all aspects of completing this thesis. Dr. Thomas Krause of RMC for the very generous use of equipment as well as his time and knowledge of magnetic testing methods, along with Brian Judd for his technical help and support of the same. Jasmine Chiang whose exemplary work as a summer student greatly helped in the completion of this thesis. Dr. Alison Mark whose Ph.D work this thesis extends, for her availability in answering questions about all things TRIP. The Mechanical and Materials Engineering Department technicians at Queens uUiversity, namely Charlie Cooney, Chris Gabryel, Joyce Cooley and the sta of the Mechanical Engineering machine shop for their technical skill and patient explanations. CANMET for manufacturing and supplying the steel used in this thesis. The nancial support of Queens University, the STELCO graduate fellowship and AUTO21 Canadian automotive research group. iii

Contents
Contents List of Figures List of Tables List of Nomenclature Chapter 1: 1.1 1.2 Introduction i v ix xi 1 1 2 4 4 5 7 10 17 22 22 23 24 27

Motivation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Research Objective . . . . . . . . . . . . . . . . . . . . . . . . . . . . Literature Review

Chapter 2: 2.1

TRIP Steel Microstructure . . . . . . . . . . . . . . . . . . . . . . . . 2.1.1 2.1.2 2.1.3 2.1.4 Chemistry . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Processing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . The Bainite Transformation . . . . . . . . . . . . . . . . . . . Retained Austenite Stability . . . . . . . . . . . . . . . . . . .

2.2

TRIP Steel Properties . . . . . . . . . . . . . . . . . . . . . . . . . . 2.2.1 2.2.2 2.2.3 2.2.4 Tensile Properties . . . . . . . . . . . . . . . . . . . . . . . . . Hardening Rate . . . . . . . . . . . . . . . . . . . . . . . . . . Sheet Formability Testing . . . . . . . . . . . . . . . . . . . . IPPS Testing . . . . . . . . . . . . . . . . . . . . . . . . . . . iv

Contents 2.2.5 2.3 TRIP Steels and Forming Path . . . . . . . . . . . . . . . . .

v 28 30 30 32 34 36 36 36 37 43 43 43 44 52 52 56 56 57 58 58 59 60 60 63 64 65

TRIP Steel Characterization . . . . . . . . . . . . . . . . . . . . . . . 2.3.1 2.3.2 X-Ray Diraction . . . . . . . . . . . . . . . . . . . . . . . . . Magnetic Saturation . . . . . . . . . . . . . . . . . . . . . . .

2.4

Literature Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . Experimental Methods

Chapter 3: 3.1

Heat Treatments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3.1.1 3.1.2 The As-Received Condition . . . . . . . . . . . . . . . . . . . TRIP Steel Heat Treatments . . . . . . . . . . . . . . . . . . .

3.2

Magnetic Saturation Measurements . . . . . . . . . . . . . . . . . . . 3.2.1 3.2.2 3.2.3 Magnetic Theory . . . . . . . . . . . . . . . . . . . . . . . . . Magnetic Sample Preparation . . . . . . . . . . . . . . . . . . Magnetic Testing Conditions . . . . . . . . . . . . . . . . . . .

3.3

X-Ray Diraction Measurements . . . . . . . . . . . . . . . . . . . . 3.3.1 3.3.2 X-Ray Diraction Theory . . . . . . . . . . . . . . . . . . . . X-Ray Diraction Sample Preparation . . . . . . . . . . . . .

3.4

Optical Microscopy . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3.4.1 Optical Sample Preparation . . . . . . . . . . . . . . . . . . .

3.5

Uniaxial Tensile Testing . . . . . . . . . . . . . . . . . . . . . . . . . 3.5.1 3.5.2 3.5.3 Sample Preparation and Dimensions . . . . . . . . . . . . . . Testing Equipment and Conditions . . . . . . . . . . . . . . . Data Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . .

3.6

In-Plane Plane-Strain Testing . . . . . . . . . . . . . . . . . . . . . . 3.6.1 3.6.2 3.6.3 Sample Preparation and Geometry . . . . . . . . . . . . . . . Testing Equipment and Conditions . . . . . . . . . . . . . . . Data Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . .

Contents Chapter 4: 4.1 Results

vi 67

Characterization and Validation of the Magnetic Determination of Retained Austenite . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4.1.1 4.1.2 4.1.3 Vibrating Sample Magnetometer Setup and Results . . . . . . X-Ray Diraction Results . . . . . . . . . . . . . . . . . . . . Optical Analysis . . . . . . . . . . . . . . . . . . . . . . . . . 67 67 67 69 70 70 72 75 77 77 82 83 83 87 90 93 94 95 99 99

4.2

Heat Treatments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4.2.1 4.2.2 4.2.3 4.2.4 4.2.5 4.2.6 Equiaxed and Lamellar Microstructures . . . . . . . . . . . . . Investigation of the Bainite Hold . . . . . . . . . . . . . . . . Equiaxed Tensile Samples . . . . . . . . . . . . . . . . . . . . Equiaxed IPPS . . . . . . . . . . . . . . . . . . . . . . . . . . Lamellar Tensile . . . . . . . . . . . . . . . . . . . . . . . . . Lamellar IPPS . . . . . . . . . . . . . . . . . . . . . . . . . .

4.3

Tensile Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4.3.1 4.3.2 4.3.3 Equiaxed Stress Strain Analysis . . . . . . . . . . . . . . . . . Lamellar Stress Strain Analysis . . . . . . . . . . . . . . . . . Instantaneous n Values . . . . . . . . . . . . . . . . . . . . . .

4.4

In-Plane Plane-Strain Testing . . . . . . . . . . . . . . . . . . . . . . 4.4.1 4.4.2 Strain in Cells . . . . . . . . . . . . . . . . . . . . . . . . . . . Comparative Forming Limits . . . . . . . . . . . . . . . . . . . Discussion

Chapter 5: 5.1

Characterization of TRIP steels . . . . . . . . . . . . . . . . . . . . . 5.1.1 Use of Magnetic Saturation for the Measurement of Volume Percent of Retained Austenite . . . . . . . . . . . . . . . . . . 5.1.2 X-Ray Diraction Measurements of Volume Percent of Retained

99

Austenite . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101 5.1.3 Microscopy and the Determination of TRIP Steel Microstructures103

Contents 5.2

vii

Microstructural Evolution . . . . . . . . . . . . . . . . . . . . . . . . 104 5.2.1 5.2.2 5.2.3 5.2.4 Initial Microstructures . . . . . . . . . . . . . . . . . . . . . . 104 The Inter-critical Hold . . . . . . . . . . . . . . . . . . . . . . 105 The Bainite Hold Curve . . . . . . . . . . . . . . . . . . . . . 106 Temperature and Heating Rate Dependance of Microstructure 108

5.3

Role of Retained Austenite in Formability . . . . . . . . . . . . . . . 109 5.3.1 5.3.2 5.3.3 Retained Austenite in Uniaxial Tension . . . . . . . . . . . . . 109 Eect of Retained Austenite on Material Hardening . . . . . . 109 Retained Austenite in IPPS . . . . . . . . . . . . . . . . . . . 110

5.4

Aect of Phase Morphology on Performance of TRIP Steel . . . . . . 111 5.4.1 5.4.2 5.4.3 5.4.4 Dierences in Morphology . . . . . . . . . . . . . . . . . . . . 111 Dierences in Mechanical Properties . . . . . . . . . . . . . . 112 Dierences in Hardening Behavior . . . . . . . . . . . . . . . . 113 Dierences in IPPS . . . . . . . . . . . . . . . . . . . . . . . . 113 Conclusions and Recommendations 115

Chapter 6: 6.1

Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115 6.1.1 6.1.2 6.1.3 Microstructure . . . . . . . . . . . . . . . . . . . . . . . . . . 115 Mechanical Properties . . . . . . . . . . . . . . . . . . . . . . 116 Characterization . . . . . . . . . . . . . . . . . . . . . . . . . 117

6.2

Recommendations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117 6.2.1 6.2.2 6.2.3 Microstructure . . . . . . . . . . . . . . . . . . . . . . . . . . 118 Mechanical Properties . . . . . . . . . . . . . . . . . . . . . . 118 Characterization . . . . . . . . . . . . . . . . . . . . . . . . . 118 120

References

List of Figures
1.1 Ranges of UTS and total elongation for high-strength steel (HSS) and advanced high-strength steels (AHSS), showing the benets of TRIP steels over HSLA and DP steels . . . . . . . . . . . . . . . . . . . . . 2.1 2.2 The aect of alloying elements on the thermal processing of TRIP steels Schematic representation of the thermo-mechanical treatments applied to TRIP steels, from hot- or cold-rolled material to the two-stage heattreatment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.3 Typical SEM micrograph of equiaxed TRIP structure, phase A is austenite, B is bainite and F is inter-critical ferrite . . . . . . . . . . . 2.4 Sketch of the evolution of the martensite-based TRIP structure from a) martensite laths to b) partially recovered laths + carbon moving to boundaries, c) recovered ferrite laths + austenite and d) recovered ferrite + austenite with bainite . . . . . . . . . . . . . . . . . . . . . 2.5 SEM of martensite-based TRIP steel, light phase is austenite/martensite, dark phase is ferrite/bainite . . . . . . . . . . . . . . . . . . . . . . . 2.6 The growth of a bainite sheaf from primary nucleation at a grain boundary (top) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.7 2.8 Representative T0 and Ae3 lines for a given steel . . . . . . . . . . . . Theoretical relation between the grain size and thermal stability of retained austenite grains . . . . . . . . . . . . . . . . . . . . . . . . . 19 15 16 12 11 9 8 3 6

viii

List of Figures 2.9 Volume fraction of retained austenite measured during tensile testing for four austenite morphologies . . . . . . . . . . . . . . . . . . . . . 2.10 Representative stress-strain curves of DP, TRIP and HSLA steels . . 2.11 Comparison of instantaneous n values calculated for DP, TRIP and HSLA steels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.12 FLCs of HSLA, mild and DP steels, showing strain paths from uniaxial to equi-biaxial tension . . . . . . . . . . . . . . . . . . . . . . . . . . 2.13 Volume fraction of retained austenite with increasing major strain for TRIP steel tested in several strain paths . . . . . . . . . . . . . . . . 2.14 Magnetic hysteresis curve for an austenitic stainless steel after undergoing 55% reduction in thickness to produce 75 vol.% martensite . . . 3.1 Schematic graph of the two-stage heat treatment used to produce the equiaxed microstructure. . . . . . . . . . . . . . . . . . . . . . . . . . 3.2 Coupon dimensions for tensile sample heat treatments showing position of tensile bar and magnetic testing discs, all dimensions in mm. . . . 3.3 Coupon dimensions for IPPS sample heat treatments showing position of IPPS sample and magnetic testing discs, all dimensions in mm. . . 3.4 Schematic graph of the three-stage heat treatment used to produce the lamellar microstructure. . . . . . . . . . . . . . . . . . . . . . . . . . 3.5 VSM showing the dierent parts of the machine, the sample is vibrated vertically through the magnetic eld. . . . . . . . . . . . . . . . . . . 3.6 Magnetic hysteresis loops for pure ferrite (calculated) and sample TE1001 with 13.1 vol.% retained austenite. . . . . . . . . . . . . . . . . . . 3.7 Second derivative of the magnetic hysteresis loop of the equilibriumcooled sample showing peak values at the inection point of the rst derivative. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

ix

21 23

25

26

29

33

39

40

41

42

45

47

49

List of Figures 3.8 Curve-tting results for sample TE100-1 showing the negative approach to saturation. . . . . . . . . . . . . . . . . . . . . . . . . . . . 3.9 Full XRD prole for sample AH60 with 6.4 vol.% R.A. . . . . . . . .

50 53 54

3.10 Full XRD prole for sample AM200 with 11.2 vol.% R.A. . . . . . . . 3.11 Deconvolution of the double copper ferrite (200) peak for sample AL200. The original data is shown with the two Pearson VII curves, background radiation level, the total curve t and the residuals (dotted) . 3.12 Sub-sized tensile sample geometry, sheet thickness of 1 mm, all dimensions in mm. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3.13 Position of the grid dots on the surface of the IPPS samples, dots were centered in the major and minor directions . . . . . . . . . . . . . . . 3.14 Experimental setup for IPPS testing, showing digital camera, Instron with wide grips and digital clock . . . . . . . . . . . . . . . . . . . . . 3.15 Post-processed image of deformed grids showing necked and un-necked rows . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3.16 Geometry of IPPS samples, all dimensions in mm, sheet thickness is 1 mm . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4.1 a) Longitudinal and b) transverse section of sample AM200. Etched with picric/sodium metabisulte, martensite/austenite is light, ferrite/bainite dark. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4.2 Micrographs of sample TL300-2 in a) longitudinal and b) transverse directions. Etched with picric/sodium metabisulte, martensite/austenite is light, ferrite/bainite is dark. . . . . . . . . . . . . . . . . . . . . . . 4.3 The volume percent of RA produced at bainite hold temperatures of 350, 400 and 450 C, as a function of bainite hold time . . . . . . . . 4.4 Volume percent of RA as a function of bainite hold time for TE series heat treatments, employing a bainite hold temperature of 450 C . . .

55

59

61

62

63

64

71

72

74

76

List of Figures 4.5 Volume percent of RA as a function of bainite hold time for IE series heat treatments, employing a bainite hold temperature of 450 C . . . 4.6 Volume percent of RA as a factor of bainite hold time for TL series heat treatments, employing a bainite hold temperature of 450 C . . . 4.7 4.8 Typical engineering stress-strain curves for TE series samples . . . . . Strain at UTS and volume percent RA as a function of bainite hold time for TE series heat treatments, employing a bainite hold temp of 450 C . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4.9 Typical engineering stress-strain curves for TL series heat treatments

xi

79

81 84

86 88 89

4.10 Strain at UTS and volume percent RA for TL series heat treatments 4.11 Instantaneous n as it changes with strain for three TE series heat treatments. TE30-1 - Green, TE100-3 - Blue, TE1800-1 - Red . . . . 4.12 Instantaneous n as it changes with strain for three TL series heat treatments. TL60-1 - Green, TL100-2 - Blue, TL1800-1 - Red . . . . . . . 4.13 Strain proles for the a) beginning, b) middle and c) end of the IPPS testing of sample IE100-3 . . . . . . . . . . . . . . . . . . . . . . . . . 4.14 Curves of the dierence in strain rate for sample IE100-3 between necked and un-necked rows at ve locations across the sample width . 4.15 Strain at relative necking limit for IE and IL series samples plotted against the volume percent of RA in each sample . . . . . . . . . . .

91

92

94

96

98

List of Tables
3.1 Chemistry of the TRIP steel, as received in weight percent, balance is iron 3.2 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37

The measured ferrite and austenite peaks with their corresponding expected diraction angles . . . . . . . . . . . . . . . . . . . . . . . . 53 68

4.1 4.2

Volume percent retained austenite as measured by VSM and XRD . . A-series heat treatment conditions and volume percent retained austenite, as measured by magnetic saturation . . . . . . . . . . . . . . . .

74

4.3

Bainite hold times and measured volume percent retained austenite for equiaxed tensile samples. . . . . . . . . . . . . . . . . . . . . . . . . . 75

4.4

Bainite hold times and average volume percent of retained austenite measured magnetically for equiaxed tensile samples. The A and B samples were taken from either side of the IPPS sample as shown in Figure 3.3. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 78

4.5

Bainite hold times and volume percent of retained austenite measured magnetically for lamellar tensile samples. . . . . . . . . . . . . . . . . 80

4.6

Lamellar IPPS samples with volume percent of retained austenite measured magnetically on either side of the IPPS sample as shown in Figure 3.3, bainite hold time is 100 seconds. . . . . . . . . . . . . . . . . 83 85 88

4.7 4.8

Tensile properties of TE samples

. . . . . . . . . . . . . . . . . . . .

Tensile properties of lamellar tensile samples . . . . . . . . . . . . . .

xii

List of Tables 4.9 Retained austenite and strain at the local necking condition for equiaxed and lamellar IPPS samples . . . . . . . . . . . . . . . . . . . . . . . .

xiii

97

List of Nomenclature
Ae3 Ao d e Fapp H
hkl Ix

Equilibrium carbon concentration in austenite Original cross-sectional area Atomic spacing Engineering strain Applied force Applied magnetic eld Integrated intensity of the hkl plane of phase x Hardening constant Gauge length Original gauge length Change in gauge length Magnetic moment Magnetic saturation Strain hardening exponent Instantaneous n Theoretical intensity ratio for the hkl plane of phase x Engineering stress

k l lo l M Ms n ni
hkl Rx

xiv

List of Nomenclature

xv

T0

Thermodynamic maximum carbon concentration in austenite for the bainite transformation

True stress True strain

Diraction angle Wavelength

Chapter 1

Introduction
1.1 Motivation

Increasing oil prices and environmental consciousness in consumers, along with new environmental legislation have made fuel eciency a top priority of the automotive industry. A straightforward means to increasing a vehicles fuel eciency is to reduce vehicle weight, which often means using new materials to produce lighter vehicle parts without sacricing strength or performance. A reduction of 100 kg in the average weight of a gasoline passenger car has been found to lead to a decrease in fuel consumption of 0.35 liters per 100 km or 700 liters over the vehicles life cycle [1]. The automotive industry has been looking towards plastics, composites and light-weight alloys to replace traditional materials, while at the same time using small amounts of advanced steels to replace larger pieces made of traditional steels. Automotive body parts are commonly stamped out of sheet steels, forming complex structural members from thin sheet. If the strength of the steel were increased, thinner sheet could be used to provide the same strength at a lower weight. It has been estimated that by replacing conventional steel with advanced high-strength steels the overall weight of a standard family car could be reduced by 118 kg [2]. This could result in even larger total weight savings in the vehicle as the size of many components is dependent on the vehicle weight, so that reducing the overall weight of the vehicle allows additional weight savings to be made elsewhere. Assuming one liter of gasoline contains 2.32 kg of CO2 [3], the savings in emissions over the life cycle of a car could be as high 1

Introduction

as 1916 kg of CO2 . Conventional high-strength steels do not possess the formability required to create many of these complex sheet parts using a reduced sheet thickness. Therefore, the challenge is to design a steel which exhibits both high strength for weight reduction and good formability for forming complex structural components. Multi-phase TRansformation Induced Plasticity aided steels, or TRIP steels, are a class of advanced high-strength steels that potentially have the high strength and good formability needed for signicant weight reductions in automotive applications. These steels possess a multi-phase microstructure which includes a meta-stable retained austenite phase which is capable of producing the TRIP eect, along with inter-critical ferrite and bainitic ferrite. When the steel is deformed the austenite transforms into martensite, which helps to absorb energy and locally harden the material. This hardening eect, combined with the volume increase of the martensite transformation, acts to resist necking in the material and postpone failure in sheet forming operations. TRIP steels also incorporate the advantages of the composite structure of a dual-phase steel, containing strong austenite/martensite phases amongst the weaker ferrite and bainite. The macroscopic benets of the TRIP eect can be demonstrated by comparing dierent steels in terms of their ultimate tensile strength and total elongation. A representative plot is shown in Figure 1.1 where the TRIP steels exhibit a much higher total elongation (which is loosly related to formability) than comparable highstrength low-alloy (HSLA) or dual-phase (DP) steels.

1.2

Research Objective

The microstructure of a TRIP steel can greatly alter its mechanical properties. The most important aspects of the TRIP steel microstructure are the volume percent, size and morphology of the retained austenite phase, as these properties directly aect

Introduction

Figure 1.1 Ranges of UTS and total elongation for high-strength steel (HSS) and advanced high-strength steels (AHSS), showing the benets of TRIP steels over HSLA and DP steels [4]

the austenite-to-martensite transformation when the steel is deformed [5, 6]. Previous research has investigated a variety of dierent phase morphologies and the resulting mechanical properties in TRIP steels. In this thesis, the eect of austenite phase morphology on TRIP steel formability is examined by producing two distinct microstructures of retained austenite with a common steel chemistry. To accomplish this objective two groups of steel samples were heat-treated to obtain similar surrounding matrices of ferrite and bainite, but diering morphologies of retained austenite. It was found that the two steel microstructures had very dierent properties, both under uniaxial tensile and in-plane plane-strain testing, and that the mechanical properties of both steels relied heavily on the volume fraction and morphology of the retained austenite phase.

Chapter 2

Literature Review
TRIP steels present a complex class of materials, where the mechanical properties are aected by an evolving, multi-phase microstructure. In order to understand the microstructure and its evolution through processing and service, a range of characterization techniques are needed to analyze these steels. By considering the contribution of each microstructural component to the overall mechanical behavior of the material it is possible to design TRIP steels with a microstructure optimized for the mechanical properties needed to solve real-world problems. In this study, the evolution and morphology of two separate TRIP microstructures are analyzed, and their mechanical properties are evaluated for their use in sheet forming operations. Hence, there are three main areas of interest: the microstructure, the mechanical properties and the characterization of the TRIP steels.

2.1

TRIP Steel Microstructure

The microstructure of TRIP steels revolves around the presence of meta-stable retained austenite which produces the TRIP eect. There are many compositions and microstructures which allow the austenite to be stabilized at room temperature. In this study, low-alloy TRIP steels with austenite stabilized by inter-critical and bainite holds are considered.

Literature Review

2.1.1

Chemistry

There are several ways in which to chemically stabilize austenite at room temperature. The simplest approach is through the addition of nickel as in austenitic stainless steels. The mechanical advantages of the TRIP eect were in fact rst observed in nickelbearing meta-stable austenitic steels in 1967 by Merz et al. [7]. Transformation due to plasticity in austenitic steels is still a major area of interest [8], but the high nickel contents of these steels make them very expensive and so the stabilization of austenite using low levels of alloying elements was developed out of research involving similar dual-phase steels. In low-alloy TRIP steels the austenite is stabilized through its carbon content. The carbon content necessary to stabilize austenite is approximately 1 wt.% [9]. However, carbon content this high prevents the steel from being easily welded, so the overall carbon content of TRIP steels is limited to 0.2 wt.% [10] so that it can be widely used in industry. A complex heat-treatment is therefore employed to concentrate the carbon within the austenite. A common TRIP steel chemistry also contains small additions of other elements to both help in stabilizing the austenite and to aid in the creation of microstructures which partition carbon into the austenite. The most common additions in TRIP steels are 1.5 wt.% of both silicon and manganese. The manganese directly stabilizes the austenite by lowering the martensite start temperature; it will also lower the starttemperature for the formation of cementite, preventing pearlite from forming during cooling [10, 11]. The silicon content of the steel is also important as silicon is highly insoluble in cementite. The silicon will therefore act to greatly delay the formation of carbides, especially during the bainite transformation, as time must be given for the silicon to diuse away from the bainite grain boundaries before cementite can form [10, 12]. The eects of each of these elements, as they apply to TRIP steel processing, are shown in Figure 2.1.

Literature Review

Figure 2.1 The aect of alloying elements on the thermal processing of TRIP steels [10]

Literature Review

The use of silicon in TRIP steels does have one major drawback. It causes serious problems when applying a zinc coating to the surface, as is the case for a standard galvanneal process used in the production of automotive sheet steel [13]. This problem has lead researchers to experiment with other alloying elements in place of the silicon, such as aluminum and phosphorus [14]. Additional alloying elements, such as vanadium, may also be included to precipitation strengthen the ferrite matrix [15].

2.1.2

Processing

Specic processing routes are required to concentrate carbon into the austenite in order to stabilize it at room temperature. The most common method for accomplishing this task in a TRIP steel is to start with a hot-rolled steel, followed by cold rolling in order to deform the microstructure and impart the potential energy needed for ecient recrystallization. The steel is then re-heated to the inter-critical region where the steel recrystallizes, growing small grains of austenite and ferrite. In the inter-critical region the austenite can be enriched in carbon up to the eutectoid chemistry (approximately 0.8 wt.% carbon) by holding it at the bottom of the temperature range. Depending on the amount of prior deformation and the holding temperature this recrystallization to ferrite and austenite can be very fast. Long hold times are avoided in this step to prevent detrimental grain growth. A schematic of the common two-stage TRIP heat treatment is shown in Figure 2.2. After inter-critical annealing the steel is then cooled to the bainite region where it is held for a short length of time. This bainite hold is necessary to further enrich the carbon content of the austenite. The steel is then quenched to room temperature to halt the bainite reaction. The bainite grows into the inter-critical austenite, partitioning carbon to the austenite according to the transformation described in Section 2.1.3. Usually the bainite reaction is accompanied by the formation of carbides

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around the bainitic ferrite, but the addition of silicon prevents this occurrence, and so the carbon is partitioned directly into the austenite [16]. The length of the bainite hold time must be carefully chosen as holds which are too short will not allow enough bainite to grow and the austenite will not be stabilized by enough carbon; hence, the austenite will transform to martensite upon quenching to room temperature. If the bainite hold time is too long the high-carbon austenite will decompose into carbides, reducing the volume percent of austenite retained at room temperature [16].

Figure 2.2 Schematic representation of the thermo-mechanical treatments applied to TRIP steels, from hot- or cold-rolled material to the two-stage heat-treatment [12] The heat treatment described above will produce a structure consisting of ferrite, bainite and austenite, with some martensite or cementite depending on the bainite hold conditions. The ferrite will appear as equiaxed grains that were formed during

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the inter-critical hold. The inter-critical austenite grains will be partly consumed by bainitic ferrite which has grown into them during the bainite hold. The austenite which is retained to room temperature appears in small equiaxed or blocky grains at the boundaries of the ferrite or bainite grains [17]. This structure is shown in Figure 2.3.

Figure 2.3 Typical SEM micrograph of equiaxed TRIP structure, phase A is austenite, B is bainite and F is inter-critical ferrite [17] It is possible to produce dierent microstructures from the one depicted in Figure 2.3 by using the same two-stage heat-treatment but starting with a dierent microstructure. For example, Sugimoto et al. started the heat treatment with a microstructure of ne martensite [6]. In this work, the TRIP steel was rst heated up to the fully austenitic region, and held at this temperature for sucient time to produce a structure of only austenite. The steel was quenched directly to room temperature

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in order to produce ne martensite, and then re-heated up to the inter-critical temperature so that the two-stage TRIP heat treatment could be applied. The highly disordered martensitic structure produces a similar driving force for recrystallization as the plastic deformation from cold rolling in the usual TRIP process. When the martensite is heated to the inter-critical region it transforms into a mixture of ferrite and austenite. Moreover, the high-carbon martensite partitions over short ranges, and so the ferrite and austenite form alternating plates from the original repeating lath structure of the martensite [6]. When the steel is subsequently cooled to the bainite region, the bainite grows into the austenite, stabilizing it with carbon. The nal microstructure consists of a matrix of ferrite grains or sub-grains arranged in thick plates. The retained austenite exists in thin plates between these larger areas of ferrite and bainite [6]. This microstructure was also investigated in the Ph.D. work of Mark [5]. Its evolution is sketched in Figure 2.4, and a representative SEM micrograph is shown in Figure 2.5. The two TRIP steel processing routes described above were examined in this thesis. Each is referred to by the resulting morphology of the retained austenite, such that the common, two-stage heat-treatment TRIP steel microstructure is referred to as equiaxed and the more complex martensite-based microstructure is referred to as lamellar for the thin, plate-like structure of the retained austenite.

2.1.3

The Bainite Transformation

Of the microstructural evolutions in TRIP steel processing, the bainite hold is the most complex and also the most important in the stabilization of the austenite at room temperature. The transformation of austenite into bainite is a complex phenomenon which is a matter of much research and some controversy. In theory, the reaction is a non-equilibrium process that produces many ne lenticular sub-units of supersaturated ferrite which arrange themselves into needle-like structures referred to as

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Figure 2.4 Sketch of the evolution of the martensite-based TRIP structure from a) martensite laths to b) partially recovered laths + carbon moving to boundaries, c) recovered ferrite laths + austenite and d) recovered ferrite + austenite with bainite [5]

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Figure 2.5 SEM of martensite-based TRIP steel, light phase is austenite/martensite, dark phase is ferrite/bainite [5]

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sheaves of bainite. Bainite will nucleate at an austenite grain boundary and grow into the grain. The carbon content of the ferrite is higher than equilibrium, while the remaining carbon is either partitioned to the surrounding austenite or forms carbides which surround the bainite sheaves. The process by which the bainite nucleates and grows into this structure has been a matter of considerable debate. The crux of this debate has been whether bainite grows athermally or through a diusion process. The original theory of diusional bainite growth was developed by Heheman et al. in 1972 [18] and there continues to be kinetic models of bainite growth developed based on diusion processes [19]. These models, however, do not account for the observed kinetics of the bainite transformation which occurs at speeds which are orders of magnitude greater than what has been predicted from diusion models [20]. In the diusionless process proposed by Bhadeshia [21] the bainite nucleates in equilibrium, grows diusionlessly and the excess carbon is subsequently partitioned to the surrounding matrix. This model, based on the thermodynamics of the bainite reaction, accounts for the observed chemistry and shape of the bainite grains and forms the basis of the model adopted in this thesis. Bainite initially nucleates at the boundaries of prior austenite grains [21]. The nuclei will form on pre-existing aws at the grain boundaries such as dislocation networks. These areas are highly disordered, and this high free energy allows the nucleus to form with almost any carbon concentration, allowing larger changes in free energy at nucleation. From a given nucleus the bainite grows quickly and diusionlessly in a martensite-like transformation to form a small sub-unit. This sub-unit is made up of super-saturated ferrite, and its growth must be accommodated plastically by the surrounding austenite, given that the specic volume of ferrite (BCC) is higher than that of austenite (FCC). Plastic accommodation of the bainite sub-unit limits its growth as the austenite strain-hardens around it. The geometric mismatch between the parent austenite and the growing bainite results in growth which is more easily

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accommodated in certain crystallographic directions than others. As with martensite, this anisotropic strain limits the growth of the sub-units perpendicular to the habit plane, which in turn results in their lenticular shape, the aspect ratio of which depends on the formation temperature as well as the carbon and manganese contents of the steel [21]. The newly formed bainite sub-unit is supersaturated in carbon, having the same carbon content as the parent austenite due to its diusionless growth. The temperature at which bainite forms is sucient for this carbon to partition out of the supersaturated ferrite into the surrounding austenite, but is not sucient to allow diusion of substitutional alloying elements. The carbon, therefore, partitions out of the sub-units into the surrounding austenite shortly after formation. Being a diusion process, the concentration and distance of carbon partitioning in the austenite is temperature dependent. The end result is austenite enriched in carbon, and bainite with a chemical composition closer to that of equilibrium ferrite. Once a bainite sub-unit has formed, the total surface area of the austenite grain boundary has been eectively increased by the presence of the boundary between the newly formed sub-unit and the parent austenite. New bainite sub-units can therefore not only form on the existing austenite grain boundaries but also at the tip of the newly-formed sub-units, as shown in Figure 2.6. This additional nucleation site gives rise to the sheaf structure of the bainite sub-units and eectively increases the number of possible nucleation sites for sub-units as the reaction progresses. The bainite transformation will end well before the austenite completely transforms as a result of two factors: the thermodynamic driving force for nucleation decreases as the carbon content of the remaining austenite increases, and the bainite must be plastically accommodated by the austenite which is increasingly strainhardened by the transformation. For reasonably large grains of austenite the thermodynamic limit is more important [22]. The thermodynamic limitations on bainite

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Figure 2.6 The growth of a bainite sheaf from primary nucleation at a grain boundary (top) [21]

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growth place a maximum on the possible carbon content of austenite. This maximum is temperature dependent; that is, decreasing temperatures increase the driving force of the bainite reaction, and will complete with smaller volume fractions of austenite, but the austenite will have a higher carbon content. The line which denes the maximum carbon content for the austenite at any given temperature is known as the T0 line. As can be seen in Figure 2.7, this line lies well below the equilibrium concentration of the austenite dened by the Ae3 line.

Figure 2.7 Representative T0 and Ae3 lines for a given steel [21] The transformation from austenite into bainite is a very complex process, governed by non-equilibrium thermodynamics, having multiple transformation steps and having several ways in which the prior formation of bainite aects further transformation. The microstructures which result from this process in TRIP steels are equally complex, having several phases of dierent properties. The structure is made even more complex by the eect of the dynamic martensitic transformation of the retained austenite which is based on many factors including grain size, stress and strain state, and the composition of the surrounding matrix.

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2.1.4

Retained Austenite Stability

The stability of retained austenite refers to its resistance to transformation with stress, strain and temperature, so that for a given temperature more stable retained austenite will transform to martensite at higher stresses and strains. In this work the stability of austenite will refer to its resistance to transformation with the global strain applied to the steel, as opposed to the micro-mechanical state of the retained austenite grains themselves. There are several factors which aect the stability of retained austenite. The most important of these is the concentration of stabilizing alloying elements in the austentite, usually carbon, silicon and manganese [23]. Of these, carbon is the most important element aecting the stability of austenite in low-alloy TRIP steels [12]. Other important factors which control the stability of the retained austenite are the size of the austenite grains, the nature of the surrounding phases and the morphology of the retained austenite. In a study by Reisner et al. [24] it was found that austenite grains with very low levels of carbon (<0.6 wt.%) transforms at very low strain levels. This early transformation was found to detrimentally aect the total elongation of the steel as the austenite transforms too early so that the hardening supplied by the TRIP eect is used up before failure begins when it is needed most. The opposite problem has also been reported in steels with very high austenite carbon concentrations. De Meyer et al. [25] found that steels with austenite carbon concentrations of over 1.8 wt.% had sizable volumes of retained austenite present in fractured samples, meaning that some of the retained austenite remained untransformed and did not add to the hardening and elongation of the steel. It is therefore clear that there exists an optimal stability of the retained austenite so that it does not transform at too low a strain to prevent local necking, or remain untransformed in the matrix through the deformation. The stability of retained austenite can also be aected by the size of the retained austenite grains. Smaller grains of retained austenite have been found to be more

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stable under deformation, with grains larger than approximately 1m transforming too readily to help improve ductility. The relationship between size and stability of retained austenite grains has been investigated theoretically by Wang and Van Der Zwaag [23]. As the steel is deformed, dislocations build up in the austenite forming potential nucleation sites for the martensite transformation. For a given potential nucleation density small grains of austenite have fewer sites for the nucleation of martensite, and so are less likely to transform than larger grains with more nucleation sites available [23]. This relationship is shown below in Figure 2.8 which shows the theoretical aect of grain size on the martensite start temperature (M s), a measure of the thermal stability of the austenite grains. It has also been suggested that the increase in stability seen in small grains of austenite is partly due to the restriction in martensite variants that can be selected for transformation in small grains of austenite [17]. Only certain martensite variants will be favoured by the stress-strain state of the grain and some of these variants will be geometrically impossible to accommodate. One of the more complex contributions to austenite stability comes from the interaction of the austenite with the surrounding matrix. The size, shape and composition of the phases surrounding the retained austenite grain play a major role in the global level of strain required for transformation. Thinking of the multiphase structure of the TRIP steel as a composite material, it is clear that the mechanical properties of the surrounding matrix will aect the stress and strain carried by the austenite at a given strain level and therefore its transformation behaviour [26]. The strain and stress state of inidividual TRIP phases has been studied by Jacques et al. [17] using in-situ neutron diraction and in-situ SEM tensile tests. It was found that each phase carries a dierent level of stress and strain under loading, with martensite being the strongest followed by bainite and austenite, while ferrite was the weakest. If the austenite phase is surrounded by soft ferrite it experiences more of the global stress and strain than if it were surrounded by bainite. This was found by Jacques et

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Figure 2.8 Theoretical relation between the grain size and thermal stability of retained austenite grains [23]

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al. [16] where TRIP steels with retained austenite which had a lower level of carbon exhibited improved apparent stability due to the stronger surrounding matrix. The nal source of martensite stabilization is the eect of retained austenite phase morphology, which is the topic of this thesis. Retained austenite has been produced and observed to exist in several dierent morphologies within TRIP steels. The simplest of these are the small islands present in a steel with a classic two-stage heat treatment as described in Section 2.1.2. In addition to this morphology researchers have observed retained austenite as thin layers between bainite sheaves [23] or as a thicker lamellar shape as produced by Sugimoto et al. [6]. It has been found that dierent morphologies of retained austenite have dierent mechanical stabilities, as found by Timokhina et al. [26]. It was found that austenite existing as layers between bainite sheaves was much more stable than the retained austenite existing between bainite grains. A direct measurement of the transformation behaviour of dierent austenite morphologies was presented by Mark [5] using in-situ neutron diraction experiments. These experiments provided a direct measure of the volume fraction of retained austenite which existed in the samples at several strain levels during tensile loading. Mark investigated four separate austenite morphologies, two fully bainitic TRIP steels (coarse and ne), one traditional equiaxed structure and one lamellar structure base on the work of Sugimoto et al. [6]. It was found that the ne and coarse bainitic TRIP steels had the most stable morphology of retained austenite showing almost no transformation through the testing. The least stable morphology was found to be the equiaxed samples which transformed quickly at low strains. The lamellar structure showed intermediate stability and steadily transformed throughout the entire test. These results are summarized in Figure 2.9 which shows the measured volume fraction of retained austenite with increasing strain for all four austenite morphologies.

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Figure 2.9 Volume fraction of retained austenite measured during tensile testing for four austenite morphologies [5]

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While the work of Mark and others has shown that there is clearly a relationship between the morphology and austenite stability, the reasons for this improved stability are complex and not well dened. Large changes in the processing conditions are needed to produce these dierent austenite morphologies and so the chemistry, size and surrounding matrix of the retained austenite is necessarily also changed. As shown above, any of these factors can greatly inuence the stability of the austenite and so it is not clear what direct aect a simple change in morphology would have on the stability of the retained austenite. Timokhina et al. [26] suggest that the dierences in stability seen with dierent morphologies in their study is due mainly to the location of the austenite grains in the matrix and their carbon content. In Marks work [5] the high stability of the bainitic TRIP structures is thought to arise from the presence of the strong bainite surrounding the austenite grains and also from the small size of the austenite grains. The equiaxed structure is not constrained in this way, and transforms readily, while the lamellar structure transformation is slightly retarded by the surrounding ferrite phase producing behaviour intermediate between the equiaxed and bainitic structures. A full discussion of the mechanisms of martensite nucleation and all of the factors aecting the TRIP transformation can be found in Marks thesis [5].

2.2
2.2.1

TRIP Steel Properties

Tensile Properties

TRIP steels show major improvements over dual phase and other high-strength steels in their behavior under uniaxial tension [27]. The dynamic transformation of TRIP steels, along with their multi-phase structures, allow them to attain very high uniform elongations, over 20%, and also very high ultimate tensile strengths (UTS) up to 1000MPa [28]. These properties make TRIP steels very attractive for high-strength

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forming operations. A comparison of stress-strain curves for TRIP versus dual phase (DP) steels is plotted in Figure 2.10.

Figure 2.10 Representative stress-strain curves of DP, TRIP and HSLA steels [4] TRIP steels exhibit both an increased elongation and a good UTS, due in part to the sustained hardening of the material that helps suppress the onset of necking [12]. There are several aspects of a stress-strain curve which reveal important information about a given materials formability. The strain at maximum load of a steel presents the onset of plastic instability or diuse necking and is a weak predictor of the formability of the material, but provides a simple measure which is easily determined from the stress-strain data. Better indicators of formability, such as the instantaneous hardening exponent, can also be calculated from the stress-strain data.

2.2.2

Hardening Rate

The rate at which a material hardens, and how this rate changes with strain, is very important with respect to its forming behavior. The hardening of a material is often

Literature Review modeled as a simple power-law relationship, such that: =k

n

24

(2.1)

where k is the hardening constant, and n is the strain-hardening exponent of the material. Equation 2.1 is a simplication of the hardening behavior of a material, but it applies quite well to many metal alloys. A more informative measure of a materials hardening behavior is its instantaneous hardening rate, a value that can be calculated by taking natural logarithms of Equation 2.1 to isolate n. If the stressstrain data is taken as a series of discrete data points, and the hardening constant k is assumed to be constant from point to point, then the instantaneous strain-hardening exponent (ni ) of the material at a given stress (m ) and strain ( ln ln
m (m1)
m (m1)

m)

is dened by:

ni =

(2.2)

A material that exhibits a sustained, high value of ni is expected to be resistant to plastic instability and the onset of necking, producing greater uniform elongations and a more formable material. This is one area in which the martensitic transformation of TRIP steels greatly aids in their mechanical properties. TRIP steels exhibit more sustained levels of hardening than DP and other types of steels, as is evident from the ni values plotted in Figure 2.11.

2.2.3

Sheet Formability Testing

In sheet forming operations the most important quality of a metal is how far it can be stretched along any given strain path before it fails. Failure in sheet forming is dened by the onset of local necking. Local necking appears in a sheet material as a line across the surface of the sheet which has experienced higher strains in the plane

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Figure 2.11 Comparison of instantaneous n values calculated for DP, TRIP and HSLA steels [4]

of the sheet than the surrounding material and has thinned through the thickness of the sheet. Considering uniaxial tension, local necking is a condition which follows the onset of diuse necking or plastic instability, ie. after the material is strained past the point of maximum applied load. If the material is strained beyond this point there will eventually develop an orientation in the sheet which undergoes smaller and smaller increments of strain, approaching zero. This direction of zero strain will dene the local neck in the material. It is possible to calculate the strain at which local necking starts by assuming stress states and hardening behaviours in the material, but in practice the onset of local necking is usually determined experimentally by deforming a sheet in a specic strain path and then dening a criterion (usually visual) for the onset of local necking. Once this criterion is reached the local major and minor strains within the necked (failed) and un-necked (safe) regions are measured. When

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this test is repeated for many dierent strain paths and the results are plotted in terms of major and minor strain, the highest safe and lowest failed strains will dene an upper boundary of safe forming. This method of measuring sheet formability was introduced by Keeler [29] and Goodwin [30] in the 1960s and is widely used and understood in industry. This diagram is known as a forming limit diagram (FLD) and the upper boundary is known as the forming limit curve (FLC). An example FLD with FLCs of HSLA, mild and DP steels is shown in Figure 2.12.

Figure 2.12 FLCs of HSLA, mild and DP steels, showing strain paths from uniaxial to equi-biaxial tension [4] The FLD in Figure 2.12 shows the forming limits for strain paths from negative minor strains on the left (approaching uniaxial tension) through in-plane-plane strain at the vertical axis to equi-biaxial tension on the right. The forming limits of a metal generally follow the shape shown in Figure 2.12, highest in uniaxial tension, lowest in in-plane plane-strain and increasing again in equi-biaxial tension.

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2.2.4

IPPS Testing

The in-plane plane-strain (IPPS) forming path is the strain path of greatest interest for materials in sheet forming applications because it typically produces the lowest level of formability. IPPS represents a forming path where strain is applied to the major direction of the material and strain in the orthogonal minor direction is constrained to zero, usually due to the geometry and gripping of the sample. The sample is therefore free to deform in the major direction and through the thickness, dening a plane of plane-strain. Given that the failure of a sheet material is dened by the visible necking or thinning of the material, and this strain path poses the lowest resistance to necking, IPPS testing measures the lower bound of sheet formability for a given material. This low resistance to necking is due to the fact that one of the criteria for the formation of a neck is the development of a zero-strain direction in the material along which a neck can form. In other strain paths this zero-strain direction takes some time to develop, however in IPPS this criterion is automatically satised by the strain state of the material (zero strain in the minor direction), and so material thinning and necking occur at lower strains as can be seen from Figure 2.12. The development of a local neck can either be dened by the thinning of the material (such as the visible formation of a neck), or through the major strain behaviour of the material. As the material thins locally to form a neck, the material inside the necked region will have an increasing strain rate compared with the material outside the neck which will have a strain rate which decreases towards zero. If a criterion for local necking is established as a limit on the dierence between these two strain rates then the initiation of a local neck can be determined directly from the local major strain rates of the material.

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2.2.5

TRIP Steels and Forming Path

As discussed above, the lowest limit on TRIP steel forming is along the in-plane plane-strain path. This reduction in forming limit has been observed to be more severe in TRIP steels than other grades. The forming limits of several high-strength steels were investigated by Bleck et al. [31] who found that TRIP steels showed the lowest forming limit of all the steels tested in IPPS, but had more comparable levels of forming in stretching (tension-tension) and uniaxial tension. It is suggested, with support from Mamalis et al. [32], that the TRIP steels performed particularly poorly in IPPS because the full benet of the dilatational martensitic transformation is dependent on the hydrostatic stress component of the loading. Not only does the strain path aect the usefulness of the retained austenite transformation, the strain path will also aect how quickly the retained austenite transforms during loading. In order to build a multi-scale mechanical model of TRIP steel behaviour Jacques et al. [17] measured the change in volume fraction of retained austenite as the steel was tested on several strain paths. It was found that the retained austenite transformed at larger strains in uniaxial and equi-biaxial tension, but transformed much more quickly for samples nearer to the plane strain condition. This result is shown for one TRIP steel sample below in Figure 2.13. As discussed in Section 2.1.4, the nature of the TRIP transformation means that there is an optimal level of austenite stability which allows TRIP steels to resist failure and prolong ductility. As shown here, the transformation rate of the austenite is strongly dependant on the strain path. There is therefore no one optimal level of austenite for a TRIP steel, but rather the optimal austenite stability will depend on the strain path applied.

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Figure 2.13 Volume fraction of retained austenite with increasing major strain for TRIP steel tested in several strain paths [17]

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2.3

TRIP Steel Characterization

One of the most important aspects of a TRIP steel microstructure is the volume fraction of retained austenite. While there are several characterization techniques available to perform this analysis, such as metallography, neutron diraction and dilatometry. The two characterization methods employed in this study were X-ray diraction and magnetic saturation analysis.

2.3.1

X-Ray Diraction

X-ray diraction is currently the most commonly used method for determining the volume percent of retained austenite in TRIP steels, as the equipment is widely available [33]. X-ray diraction can distinguish the phases in a material by their variation in atomic spacing. When a beam of X-rays interacts with the surface layer of a material it will be diracted at a specic angle depending on the wave-length of the X-rays ()and the atomic spacing of the material (d) as dened by Braggs Law: = 2d sin(). (2.3)

For a given wavelength of X-rays, the angle at which a diraction peak is detected is related to the atomic spacing of the corresponding phase by Equation 2.5, and the intensity of the peak is related to the volume fraction of that phase. The volume fraction of retained austenite in a TRIP steel can therefore be determined from the intensity of the austenite and ferrite peaks in the material as described in Jatczak [34]. Bainite and martensite have very similar atomic spacings, such that their diraction peaks lie on top of those for ferrite; hence a comparison between the two sets of peaks provides an accurate volume percent of the austenite versus all of the other phases. In rolled sheet material there is always the chance that the material has developed a preferred crystallographic texture, which means it will not diract from

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all orientations equally. All available orientation peaks of each phase must therefore be averaged in order to account for any texture within the sample. The intensity of each peak is divided by its theoretical intensity and averaged with all of the other peak intensities. The volume fraction of a specic phase, namely austenite in this case, can be found using [34]: Va =
n h h 0 (IA kl/RA kl )) n h n h 1 h h 0 (IA kl/RA kl ) + nF 0 (IF kl/RF kl ) 1 nA

1 nA

(2.4)

where nA and nF are the numbers of austenite and ferrite diraction peaks, IA and IF are the integrated peak intensities, and RA and RF are the theoretical intensities of these peaks, which are also listed by Jatczak [34]. Equation 2.4 assumes that the carbide volume fraction is zero and only the ferrite/bainite/martensite and austenite peaks are measured. If the X-ray source is not entirely monochromatic, multiple peaks will appear for each lattice spacing. X-rays created from copper radiation will present two separate peaks, Cu-K1 and Cu-K2 . These peaks will lie within a few degrees of each other, separated by = 2( )tan

(2.5)

where = 0.00382 and = 1.54178 . Therefore, the peaks must be deconvoluted into two separate peaks in order to properly curve-t them and determine the integrated intensity. A method for this deconvolution is outlined by Gupta [35] who employed a Pearson VII t and the assumption that the Cu-K2 peak has a maximum intensity of half of the Cu-K1 peak and a peak shift of , but is otherwise identical. Following this approach if the Cu-K1 curve can be represented by the equation f (x), then the entire intensity prole is t to the equation: y (x) = f (x) + 0.5f (x ) + g (x). (2.6)

Literature Review The Pearson VII t denes the intensity prole of a peak as: f (x) = a 1 + (x d)2 b2
m

32

(2.7)

where (d, a) are the co-ordinates of the peak maximum, exponent m is the shape factor and b is proportional to the full-width at half-maximum. When m = the assuming a linear change in background radiation, is: (x d)2 y (x) = a 1 + b2
m

curve is Gaussian, when m = 1 the shape is Cauchy. The full equation of the curve,

a (x d )2 + 1+ 2 b2

+ (px + q ).

(2.8)

The intensity y (x) can be t to the experimental data using the variables a, b, m, d, p and q [35]. In this way the separate peaks of the copper radiation can be separated and curve t, eliminating noise and background levels of radiation in the experimental data and allowing for easier integration of the individual peaks.

2.3.2

Magnetic Saturation

The second technique used to characterize the volume percent of retained austenite in TRIP steels was based on a measurement of magnetic saturation. The magnetic saturation is the maximum magnetic response of a material under an applied magnetic eld. With an increasing magnetic eld the degree to which the material is magnetized increases, at rst linearly, and then eventually approaching a maximum. If the eld is then decreased back to zero and reversed, the sample will again pass through a linear region before approaching the negative magnetic saturation, as seen in Figure 2.14 which illustrates the hysteresis curves produced in using magnetic saturation for measuring martensitic transformations in austenitic steels. This reverse response is oset from the positive direction to create a hysteresis loop for the material. The

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positive oset of the magnetization at zero applied eld is the property which allows the creation of permanent magnets.

Figure 2.14 Magnetic hysteresis curve for an austenitic stainless steel after undergoing 55% reduction in thickness to produce 75 vol.% martensite [8] The curve in Figure 2.14 can be modeled as two distinct parts, the linear loweld response, and the approach to saturation [33]. According to Berkowitz [36], the approach to saturation will follow the equation: M = Ms 1 a b c 2 3 ... . H H H (2.9)

where M is the magnetic response, Ms is the magnetic saturation, H is the applied eld and a, b and c are material constants.

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The magnetic saturation is a material property that varies with temperature, crystal structure and material chemistry [37], and as such, can be used to dierentiate the volume fraction of crystal structures within a material. This is a well established technique and is commonly applied to materials which contain several phases of known magnetic saturations by stepping the sample through temperature ranges and measuring the total magnetic saturation of that sample. Since each crystal structure has a magnetic saturation that varies with temperature, the magnetic contribution of each phase, and therefore its volume percent, can be calculated [37]. In the case of TRIP steels this process can be simplied by assuming that the material only consists of two phases, ferrite and austenite. Given that the austenite is non-magnetizing (para-magnetic) the magnetic response is entirely due to the response of the ferrite. The presence of martensite and cementite in the structure does create a source of uncertainty; however, the volume fraction of these phases is low, and their magnetic saturation is close to that of ferrite, so their aect on the retained austenite measurements should be minimal [33]. If the magnetic saturation of pure ferrite is known for the TRIP steel chemistry, then the volume percent retained austenite can be directly determined from the ratio of the measured magnetic saturation to that of pure ferrite. The magnetic saturation of a given sample can be calculated by tting Equation 2.9 to the measured hysteresis curve and then solving for Ms [33].

2.4

Literature Summary

TRIP steels have great potential for use in high-strength forming operations. Their formation and the basis of their excellent mechanical properties are, however, very complex. To this point low alloy TRIP steels have been formed and tested with a variety of chemistries and microstructures. Alloying elements will greatly aect

Literature Review

35

the formation and retention of austenite in the steels and the resulting mechanical properties [10, 14], especially in the case of carbon, silicon and manganese. Through the use of the bainite transformation these steels can be produced with a carbon enriched and meta-stabilized austenite phase [12]. The volume fraction of this metastable phase is one of the most important factors aecting the formability of the steel [10] and can be characterized through optical, X-ray and magnetic methods [33, 34, 38]. The formability of TRIP steels is aected by the transformation characteristics of the retained austenite phase, which is in turn aected by the austenite chemistry, steel morphology and the stress/strain state applied to the material [26]. It has been found that TRIP steels with lamellar morphologies have austenite with a greater resistance to transformation. This extra resistance could be most benecial to the steel in strain paths, such as plane-strain, which show a transformation of retained austenite at lower strain level [17].

Chapter 3

Experimental Methods
3.1
3.1.1

Heat Treatments
The As-Received Condition

The material for this study was produced at CANMET-MTL. As received, the steel contains roughly 0.17 wt.% carbon, 1.5 wt.% manganese and 1.5 wt.% silicon. The full chemistry of the steel is shown in Table 3.1. The steel was received in a hot rolled condition. It was rolled in two stages, from 127 mm to 50.8 mm, and then from 50.8 mm to 5 mm with a reheat in between. The steel was rolled rst through eight passes from 127 mm to 50.8 mm and from 1220 C to 920 C. The steel was then reheated to 1200 C and rolled through seven passes to a thickness of 5 mm and a nal temperature of 825 C. The nal sheet, excluding the rounded tails, measured aproximately 600 mm by 180 mm. Sections of approximately 10 cm by 9 cm were then cut from the uniformly rolled area of the sheet. The mill scale of these smaller pieces was removed from the surface of the material using a rotary grinder. The samples were then cold-rolled in the same direction as the hot-rolling, to a nominal thickness of 1 mm, by approximately twenty passes through the experimental rolling mill at Queens University. The resulting sheet was used to make heat treatment coupons, tensile samples, and in-plane plane-strain samples.

36

Experimental Methods Table 3.1 Chemistry of the TRIP steel, as received in weight percent, balance is iron
C 0.17 Si 1.53 Mn 1.50 Al 0.03 Ti 0.021 P 0.007 S 0.005 O 0.002 N 0.0048

37

3.1.2

TRIP Steel Heat Treatments

In this study, two heat treatment schedules were used to make two distinct TRIP steel morphologies: one with equiaxed grains of retained austenite and one with lamellar grains of retained austenite. These two microstructures shall be referred to as equiaxed and lamellar, respectively. In both of these treatments the steel is heated to the inter-critical region to form a mixture of austenite and inter-critical ferrite, and is then cooled to the bainite temperature range where it is held, allowing some of the austenite to transform into bainite. This transformation enriches the remaining austenite with carbon, stabilizing it to room temperature. The steel is then quenched in water. The resulting microstructure consists of inter-critical ferrite, bainitic ferrite and retained austenite. If the austenite is not suciently stabilized some high-carbon martensite may also be present in the microstructure. Cementite will also form at the edges of the bainite sheaves if the bainite hold time is sucient to allow for the diusion of silicon through the carbon-rich austenite away from the bainite interfaces. The dierence between the equiaxed and the lamellar microstructures stems from the starting condition of the material. To form the equiaxed microstructure, the steel undergoes the above treatment from the as-cold-rolled condition, while for the lamellar microstructure the cold-rolled steel is rst heated to the fully-austenitic range and then quenched in water to form martensite before undergoing the intercritical and bainite holds.

Experimental Methods

38

For all heat treatments the steel was heated to the inter-critical or fully-austenitic range using an electrical resistance air furnace. The bainite holds were performed in a 101.6 mm salt pot containing molten NaCl. All quenching was performed by immersing the sample in still, room-temperature water. Initial heat treatments were performed to investigate the optimal conditions for the bainite hold for the equiaxed microstructure. Heat-treatment coupons, measuring 25.4 by 50.8 mm were cut out of the cold-rolled sheet using a hydraulic shear. These coupons were heated to an inter-critical temperature of 750 C and held for 5 minutes. The coupons were then held in the bainite region at either 350, 400 or 450 C, for times varying from 30 to 1800 seconds and then quenched to room temperature. A schematic graph of this process is shown in Figure 3.1. The heat-treated coupons were analyzed optically, magnetically and using X-ray diraction to determine the volume fraction of retained austenite in the steel, and the morphology of the various phases. From these heat treatments it was found that holding the steel at 450 C produced the largest volume percent (14.6 vol.%) of retained austenite in the equiaxed microstructure. This temperature was then adopted for the bainite holds in all further heat treatments. In order to create tensile samples with an equiaxed structure and varying levels of retained austenite, heat-treatment blanks measuring 100 by 16 mm were cut from cold-rolled sheet. These blanks were then held in the inter-critical region at 750 C for ve minutes. This was followed by a bainite hold at 450 C for times of 30, 60, 100, 300 and 1800 seconds and a nal quench in water. The blanks were then cut into sub-sized tensile specimens and magnetic testing specimens using a water-jet cutter as shown in Figure 3.2. The magnetic test revealed that the peak level of retained austenite, 14.1 vol.%, was created through a bainite hold of 100 seconds. Blanks measuring roughly 50 by 90 mm were cut from the cold-rolled sheet and used to

Experimental Methods

39

Figure 3.1 Schematic graph of the two-stage heat treatment used to produce the equiaxed microstructure.

create in-plane plane-strain samples. These samples were heated to the inter-critical range as above, and then held at 450 C for 30, 60 and 100 seconds. The blanks were then cut into in-plane plane-strain samples, and magnetic testing samples as shown in Figure 3.3. The level of retained austenite in these samples increased to a peak of 11.4 vol.% at the 100 second hold. To create samples with lamellar microstructures the steel was rst cold-rolled to a thickness of one millimeter. The cold-rolled sheet was then cut into tensile and in-plane plane-strain blanks measuring 100 by 16 mm and 50 by 90 mm, respectively. Each blank was placed in a circulating air furnace at 950 C for 1000 seconds, and then quenched in water. Following this treatment, the tensile blanks were heated to 750 C and held in the inter-critical region for ve minutes. The samples were subsequently moved to the salt pot for bainite holds at 450 C lasting 60, 100, 300 and 1800 seconds

Experimental Methods

40

Figure 3.2 Coupon dimensions for tensile sample heat treatments showing position of tensile bar and magnetic testing discs, all dimensions in mm.

Experimental Methods

41

Figure 3.3 Coupon dimensions for IPPS sample heat treatments showing position of IPPS sample and magnetic testing discs, all dimensions in mm.

Experimental Methods

42

and then quenched in water. A schematic graph of this process is shown in Figure 3.4. Sub-sized tensile samples and magnetic testing samples were cut out of the blanks using a water-jet cutter as shown in Figure 3.2. The samples were characterized magnetically and optically, and mechanically tested under uniaxial tension. From characterization of the magnetic samples it was found that the maximum volume fraction of retained austenite of 9.53 vol.% was produced with a bainite hold of 100 seconds.

Figure 3.4 Schematic graph of the three-stage heat treatment used to produce the lamellar microstructure. The in-plane plane-strain blanks were taken from the as-quenched condition and placed in a circulating air furnace at 750 C for ve minutes, and then moved to a salt pot for a bainite hold of 100 seconds at 450 C followed by a quench in water. In-plane plane-strain and magnetic testing samples were cut out of the blanks using a water-jet cutter as shown in Figure 3.3.

Experimental Methods

43

3.2
3.2.1

Magnetic Saturation Measurements

Magnetic Theory

Measuring the magnetic properties of a material provides a wealth of information about its structure, chemistry and composition. If the phases present in a material have dierent magnetic properties it is possible to calculate the volume fraction of each phase present by measuring the magnetic response. In steels, the ferrite crystal structure is very strongly ferro-magnetic (an increasing eld will produce an increasing magnetic response) whereas austenite is paramagnetic and does not respond to magnetic elds. For a ferromagnetic material, such as ferrite, when the applied magnetic eld becomes large enough to change all of the magnetic orientation of the domains, the material will approach a magnetic saturation point, where an increase in the applied eld does not increase the magnetic response. This saturation point is reliant only on the temperature, crystal structure, chemistry and volume of the material. Assuming that the sample contains only ferrite and austenite, the volume fraction of ferrite in a sample can be directly related to the magnetic saturation that the steel achieves as a fraction of the magnetic saturation of pure ferrite. Magnetic saturation measurements were made using a vibrating sample magnetometer (VSM). This machine creates a large, variable and uniform magnetic eld, and the sample being tested is vibrated perpendicular to the applied eld. The applied magnetic eld and the resulting magnetic moment created by the magnetized sample are measured. The magnetic response of the material under a high magnetic eld is used to determine the magnetic saturation.

3.2.2

Magnetic Sample Preparation

The samples tested with the VSM were discs with a ve millimeter diameter, cut out of one millimeter thick heat-treated sheet samples. The discs were machined

Experimental Methods

44

using a water-jet cutter and were left in place in the heat-treated samples with tabs attaching the disc to the surrounding material. The discs were then broken out of the samples and the tabs ground down using sandpaper. The top and bottom surfaces of the material were also ground down to remove any oxide incurred during the heat treatment. This grinding was done so that the exact mass of the magnetizing steel could be determined. The samples were weighed using a mass balance with an uncertainty of 0.05 mg.

3.2.3

Magnetic Testing Conditions

For all magnetic testing, a VSM facility at the Royal Military College of Canada (RMC) was used. The system consists of ve pieces of equipment including the VSM itself. The VSM uses two large, water-cooled electromagnets to produce a constant magnetic eld between +6500 and -6500 Oer. A Hall probe placed between the magnets at the height of the sample measures the applied magnetic eld, while four pick-up coils measure the magnetic moment produced by the sample. The sample is placed on the end of a long, non-magnetizing rod which is oriented perpendicular to the magnetic eld. The rod is vibrated along its length, moving the sample perpendicular to the magnetic eld. The end of the rod can be raised, lowered and angled so that the sample vibrates exactly in the centre of the pick-up coils. A schematic of the VSM is shown in Figure 3.5. The VSM is powered by a large transformer which converts AC electricity into a high-current DC output, and is capable of producing 26 A. A current control box determines the level of current supplied to the magnets controller displays the measurements made by the pick-up coils and the Hall probe. This controller can also be used to step the applied magnetic eld up and down to determine the hysteresis properties of the sample. The measurement conditions can also be set using the VSM controller. A computer interface allows the user to change

and can either be controlled manually or through the VSM controller. The VSM

Experimental Methods

45

the settings of the VSM controller and record the data produced through the testing. For the testing performed with the TRIP steel samples a hysteresis loop was produced for elds varying from -6500 to +6500 Oer. The magnetic eld was stepped through 1000 discrete points over the course of 1000 seconds to produce this hysteresis loop. The time constant of these measurements was 0.1 seconds and the sensitivity of the controller was xed at 100 emu.

Figure 3.5 VSM showing the dierent parts of the machine, the sample is vibrated vertically through the magnetic eld. Before beginning each set of VSM tests, the VSM controller was calibrated using a known mass of pure, annealed nickel. This nickel sample weighed 0.09 grams, and had a known saturation magnetization of 55 emu/g. The current supplied to the magnets was manually adjusted to its maximum positive and negative values. The resulting eld is large enough to fully magnetically saturate the nickel. The magnetic moment produced by the nickel sample under this eld was measured. The span of the magnetic moment from the positive to negative saturation was set equal to twice the known magnetic saturation of the nickel sample. The VSM always produced a slightly positive oset for these hysteresis curves, but since it was calibrated using

Experimental Methods

46

the full span of the positive and negative saturation of the nickel sample this oset did not aect the calibration. Before each sample was magnetically tested, both for the nickel calibration and for the TRIP steels, the sample had to be centered within the pick-up coils. To accomplish this task a constant current was applied to the magnets and the sample was adjusted in three orthogonal directions. The sample was calibrated rst in the vertical direction, along the axis of the vibrating rod, to center the sample vertically between the pick-up coils. The center position corresponded to a maximum in the measured magnetic moment of the sample. Similarly, a minimum moment was found in the horizontal direction in the plane of the pick-up coils at the location of the sample center. Lastly, a maximum magnetic moment was found in the direction perpendicular to the plane of the pick-up coils, placing the center of the sample in the center of the pick-up coils in this direction. It is important to adjust the sample in the vertical direction rst so that there will be only one minima or maxima in the horizontal directions. Spatial calibration is important as it aects the measured magnetic moment. In addition to testing samples from the heat-treated TRIP steel, it was necessary to produce a sample with the same chemistry which contained known volume fractions of ferrite and cementite. To this end, a piece of cold-rolled TRIP steel was heated to the fully austenitic range at 1000 C, held for half an hour, and equilibrium cooled to room temperature in a closed furnace. From the carbon content of the TRIP steel, the equilibrium concentration of ferrite and cementite can be estimated to be 97.3 vol.% ferrite and 2.7 vol.% cementite from the iron-carbon phase diagram. This sample was tested in the VSM to produce a hysteresis loop, and the magnetic saturations of the sample was calculated through a curve-tting procedure. By using the known ratio between the magnetic saturation of ferrite and cementite of 1.73, from Zhao [33], it was possible to predict the magnetic saturation of a pure ferrite sample which had the

Experimental Methods

47

same chemistry as the ferrite of a TRIP steel. As the sample contained 97.5 vol.% ferrite and 2.4 vol.% cementite, and the ratio between the magnetic saturation of ferrite and cementite is 1.73, the magnetic saturation of pure ferrite can be estimated to be 1.01 times the measured magnetic saturation of the equilibrium cooled sample. This value was used as a comparator to determine the fractional dierence between the magnetic saturation of the TRIP steel samples and the calculated magnetic saturation of a pure ferrite sample. In this way, it was possible to determine the volume fraction of the retained austenite in the heat-treated TRIP steel samples. Magnetic hysteresis loops for two TRIP steel samples are shown in Figure 3.6.

Figure 3.6 Magnetic hysteresis loops for pure ferrite (calculated) and sample TE100-1 with 13.1 vol.% retained austenite.

Experimental Methods

48

The level of magnetic saturation achieved in the VSM is not sucient to fully saturate the steel samples. While these samples were brought very close to the fully saturated condition, curve tting the data with the known equation for magnetic saturation, Equation 2.9 in Section 2.3.2, provided a reasonable estimate of the full magnetic saturation of the samples. This curve-tting is especially important as the samples with lower levels of magnetic saturation also approach saturation at a lower rate, and so if the maximum magnetization of these samples is taken as the saturation magnetization the calculated level of retained austenite will be higher than what actually exists in the sample. The magnetic hysteresis loop of the material has two distinct parts. In low magnetic elds the magnetic moment produced by the sample varies linearly with the applied eld. In higher magnetic elds the material exhibits a non-linear response, known as the approach to saturation, which exhibits a continually decreasing slope. Only the sections of the hysteresis loop which are formed under decreasing positive eld or increasing negative eld were used for this curve tting, as they show a greater amount of data for the approach to saturation. In this current study, the curve tting was performed using a least-squares criterion. The linear and non-linear sections of the hysteresis curve are determined by taking the rst derivative of the magnetic respsonse and nding the inection point where the slope changes over from a susceptibility-dominated behavior to the approach to saturation. A plot of this rst derivative is shown in Figure 3.7, and the resulting curve-t is shown in Figure 3.8. One result of tting to only the non-linear data for the approach to saturation is that the samples with high magnetic saturations (low volume percents of retained austenite) will have fewer data points available for curve-tting and the quality of the curve-tting is not as high. The magnetic saturation constant was found from curve-tting the positive and negative approaches to saturation. An average was taken of these two constants,

Experimental Methods

49

Figure 3.7 Second derivative of the magnetic hysteresis loop of the equilibrium-cooled sample showing peak values at the inection point of the rst derivative.

Experimental Methods

50

Figure 3.8 Curve-tting results for sample TE100-1 showing the negative approach to saturation.

Experimental Methods

51

which produced a better estimate of the magnetic saturation and also eliminates the slightly positive oset of the VSM. This magnetic saturation constant was compared to the magnetic saturation constant calculated for pure ferrite from the equilibriumcooled sample. The magnetic method outlined above carries with it several assumptions about the composition and magnetic behaviour of the TRIP steel. First, given that the volume fraction of transformed martensite is not known, the magnetic saturation of martensite is assumed to be the same as that of ferrite. Martensite has a slightly lower magnetic saturation than ferrite [36]. This assumption will introduce a very small error in the calculated volume fraction of retained austenite, especially for those samples with longer bainite hold times, as these samples will contain almost no martensite after quenching. It is also assumed that no cementite has formed in the samples. This is a good assumption for all but the longest hold times. As with martensite, cementite has a lower magnetic saturation level than ferrite [36], so in a sample containing cementite the volume fraction of retained austenite would be slightly over-predicted. The use of an equilibrium cooled sample assumes that the alloying elements are distributed in the ferrite in the same way as in the heat treated TRIP samples. While not necessarily true, the equilibrium cooled sample will be as close to the heat-treated ferrite chemistry as possible for a given composition. Overall, these assumptions will create a very slight over-prediction in the volume fraction of retained austenite, and this over-prediction will be reduced in the samples with higher volume percents of retained austenite as these samples approach a binary mixture of austenite and ferrite.

Experimental Methods

52

3.3
3.3.1

X-Ray Diraction Measurements

X-Ray Diraction Theory

X-ray diraction was used as a second method for determining the volume fraction of retained austenite in the heat-treated TRIP steel samples. This method was also used to validate the measurements made by magnetic saturation. X-ray diraction is a standard method for determining the volume fractions of crystal phases in metal alloys. As the lattice spacing of ferrite, martensite, austenite and cementite are all dierent the diraction angles of the phases will dier. To perform X-ray diraction with a given TRIP steel sample, the surface of the sample was ground and polished, and then exposed to a monochromatic copper X-ray source. The angle that the Xrays hit the sample at was varied from 2 = 42 to 101 , and the resulting intensity of the diracted X-ray beam was measured. The volume fraction of the phases in the steel can be determined by integrating under the intensity prole of the characteristic peaks for each phase and then applying ratios of the theoretical maximum intensites to average out any texture eects in the steel. The austenite and martensite/ferrite peaks that were measured are shown below in Table 3.2 along with the expected diraction angle of each peak. An intensity prole produced by this method is shown for sample AH60 containing 6.4 vol.% retained austenite (as measured by XRD) in Figure 3.9, and sample AM200 with 11.2 vol.% retained austenite in Figure 3.10. It was found that the copper radiation used in the X-ray diraction analysis actually contained two separate wavelengths, Cu K1 and Cu K2 . In order to properly t an intensity prole to these double curves a Pearson VII t was used with the procedure from Gupta [35] outlined in Section 2.3.1. The resulting tted prole for the ferrite/martensite (200) peak is shown in Figure 3.11.

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53

Table 3.2 The measured ferrite and austenite peaks with their corresponding expected diraction angles
Measured Ferrite Peaks (110) (200) (211) (220) Measured Austenite Peaks (111) (200) (220) (311) (222) Diraction Angle (degrees) 44.6 65.0 82.2 98.9 Diraction Angle (degrees) 43.6 50.8 74.6 90.6 96.0

Figure 3.9 Full XRD prole for sample AH60 with 6.4 vol.% R.A.

Experimental Methods

54

Figure 3.10 Full XRD prole for sample AM200 with 11.2 vol.% R.A.

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55

Figure 3.11 Deconvolution of the double copper ferrite (200) peak for sample AL200. The original data is shown with the two Pearson VII curves, background radiation level, the total curve t and the residuals (dotted)

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56

Once the peaks were t to a Pearson VII distribution, the area under these curves was numerically integrated, subtracting out the background radiation and adding together the intensity of the K1 and K2 peaks.

3.3.2

X-Ray Diraction Sample Preparation

In order to get a true representation of the bulk characteristics of the TRIP steel, the heat-treated coupons were cut into strips longitudinally and then stacked and mounted in bakelite so that the cross section of the material faced the outside of the mould. In this way, the X-rays are sampled through the thickness of the material at several locations across the width of the coupon. While the X-rays only penetrate a very shallow distance into the steel, this sectioning allows for a good estimate of the material bulk. After the material strips were mounted, the surface of the steel was ground using silicon carbide grit paper progressing from 220 to 600 grit. The samples were then rinsed thoroughly and polished using a rotary wheel with a cotton cloth and 4 m diamond particles. The samples were thoroughly rinsed again and further polished using 0.05 m alumina particles on an Alpha-lap synthetic cloth and then a colloidal suspension of 0.04 m silica particles on a Raynal synthetic cloth, rinsing after each step. After mechanical polishing the samples were electro-polished using an A2 electropolishing solution combined with an applied voltage of 45 V. Samples were electro-polished for 12 seconds. During this electro-polishing, the polishing solution and the back of the samples were cooled using dry-ice in order to prevent pitting of the sample surface.

3.4

Optical Microscopy

Optical analysis was performed on each heat treatment condition for both the lamellar and equiaxed microstructures. Samples were cut in cross-section, mounted, polished

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57

and etched to reveal the ferrite and austenite grain size and composition. The samples were then studied using a reection light microscope.

3.4.1

Optical Sample Preparation

For each heat treatment condition, samples were cut out of the heat-treated TRIP steel in the longitudinal and transverse directions. They were mounted in bakelite to reveal the through-thickness of both sections. The samples were ground using silicon carbide grit paper progressing from 220 to 600 grit. The samples were then washed thoroughly and polished on a rotary wheel using a cotton cloth and 4 m diamond particles. The sample was again washed and then polished using 0.05 m particles of alumina, followed by a colloidal suspension of 0.04 m silica, rinsing thoroughly after each step. After the samples had been polished, they were etched using a mixture of picric acid and sodium metabisulte as described by Girault et al. [39]. This etch must be prepared from fresh chemicals just before use. The picric acid solution was prepared from 4 grams of dry picric and 100 ml of ethanol. The sodium metabisulte solution was prepared from 1 gram of sodium metabisulte and 100 ml of distilled water. These two solutions were mixed together directly before immersing the samples. The polished TRIP steel samples were immersed vertically into the etchant for 25 seconds. The samples were then removed and rinsed thoroughly with cold water and dried using ethanol and compressed air. This etchant colours the ferrite and bainite brown or blue, while the austenite and martensite remain white. The etch is designed to allow for dierentiation between the bainite and inter-critical ferrite; however, a clear dierence was not seen in this study so the etch was simply used to determine the size and morphology of the martensite/austenite grains and the grain size of all phases. The samples were examined under a reection light microscope at various magnications to determine the amounts and the morphologies of the phases in the TRIP steel. Digital images were acquired using a CCD camera

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58

attached to the microscope. These pictures were used for qualitative descriptions of the sample microstructure and also for point counting to determine the volume fraction of retained austenite and martensite in the sample. This point counting was performed using ImagePro, an image analysis software package. Images of the etched TRIP steel microstructures were automatically cropped and randomly rotated to eliminate selection bias. A grid of 100 points was overlaid on the sample image and then the presence of martensite/austenite or ferrite/bainite was visually conrmed and recorded for each grid. This process was carried out at ve locations across the longitudinal and transverse sections of the sample. An average was then taken of each point count and a volume fraction was determined for the martensite/austenite.

3.5

Uniaxial Tensile Testing

Uniaxial tensile tests were performed for several heat treatments of the lamellar and equiaxed microstructures. These tests helped determine the macroscopic mechanical properties of the material and allowed for a rough determination of the sheet formability. From this test, the yield strength, ultimate tensile strength (UTS) and strain at UTS were determined for each sample.

3.5.1

Sample Preparation and Dimensions

Sub-sized tensile samples were machined from the tensile heat-treated blanks using a water jet cutter. The dimensions of these samples are shown in Figure 3.12. The gauge length was 31.8 mm, and the samples had a nominal thickness of 1 mm. As the water jet cutter leaves roughened edges on the tensile samples, these were ground using silicon carbide paper until smooth. The thickness and width of the samples were measured at three points along the gauge length. An average of these measurements

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was used to determine the gauge cross sectional area, with an average error in the cross sectional area of 0.027 mm2 .

Figure 3.12 Sub-sized tensile sample geometry, sheet thickness of 1 mm, all dimensions in mm.

3.5.2

Testing Equipment and Conditions

The samples were pulled in uniaxial tension using a hydraulic Instron machine. The cross-head speed was set at 0.625 mm/minute, which produced a nominal initial strain rate over the gauge length of 0.025 min1 . The Instron was equipped with a 100 kN load cell. The strain in the gauge length of the samples was measured using a contact extensometer with a gauge length of 25 mm. The output of the load cell and extensometer were recorded using a computer interface.

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3.5.3

Data Analysis

The output of the load cell was used to determine the force applied to the sample. This force, along with the original cross-sectional area of the sample, was used to determine the applied engineering stress, as dened by the equation: S =
Fapp , Ao

where

Fapp is the applied force and Ao is the original cross-sectional area of the gauge region. The The displacement output from the extensometer was used to determine the engineering strain in the sample, dened by the equation: e =
l , lo

where l is

the change in the gauge length and lo is the original gauge length. The true strain of the samples was calculated using the equation = ln llo where l is the measured

gauge length of the sample. True stress was calculated using the engineering stress and strain so that = S (1 + e). This equation assumes constant volume and so is only valid up to the point of necking. The engineering stress and strain were used to create stress-strain curves for the tensile samples. The engineering strain at the point of maximum stress in the sample was used as a rough estimate of the formability of the steel. The true stress and strain were used in calculations of the instantaneous n values of the samples.

3.6

In-Plane Plane-Strain Testing

In order to better measure the relative formabilities of the dierent TRIP heattreatments and microstructures, samples were tested under in-plane plane-strain (IPPS). This forming path characteristically produces the earliest possible instance of local necking at the lowest major strain. The geometry of an IPPS sample is such that the center of the sample is almost entirely constrained in the minor strain direction while strain is applied in the major direction and the sample is free to deform through its thickness. As one of the criteria for local necking, that there be a direction of zero strain across the sheet, is satised by the constraints of the sample and the

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loading conditions, the sample will neck at lower strains than for any other forming path. To dynamically measure the local strain in the sample throughout the test, a grid of dots were painted onto the sample surface as shown in Figure 3.13, and a digital camera was used to take successive images throughout the test. A photograph of the experimental setup is shown in Figure 3.14. The strain was then calculated for each individual four-dot grid on the sample. The strain in the sample where the neck formed was compared to the strain immediatly above and below the neck, as shown in Figure 3.15, in order to develop a criterion for the onset of local necking. The major strain at local necking could be compared between samples.

Figure 3.13 Position of the grid dots on the surface of the IPPS samples, dots were centered in the major and minor directions

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Figure 3.14 Experimental setup for IPPS testing, showing digital camera, Instron with wide grips and digital clock [40]

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Figure 3.15 Post-processed image of deformed grids showing necked and un-necked rows [40]

3.6.1

Sample Preparation and Geometry

The IPPS samples were cut out of heat-treatment blanks measuring 50 by 90 mm using a water jet cutter. The samples were cut so that the rolling direction of the material matched the major strain direction of the test. The dimensions used for the IPPS samples are shown in Figure 3.16. As the water jet cutting leaves rough edges on the samples, the edges of the gauge region were ground using silicon carbide paper until smooth. The surface of the material was covered in an oxide layer from the heat-treatments which did not facilitate good contrast for the digital image-based measurement of strain. Furthermore, the oxide would ake o during testing and take with it the strain grid markers. Hence, the oxide layer was removed using an ultra sonic cleaner lled with 10 % solution of phosphoric acid and silicon carbide paper to abrade the surface. As well as helping to lift the oxide layer from the surface, the phosphoric acid forms a phosphate coating which has a light matte nish and improved adhesion of the paint. After preparing the surface, a regular pattern of dots were painted onto the sample surface using an automated microscope stage and a oil-paint pen. A grid of eight by eight points was applied, centered in the middle

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of the sample and oriented along the major and minor axis. The grid spacing was 3.175 mm between points, as shown in Figure 3.13. The grid was made using either blue or green paint as these colours could be easily pulled out of the RGB signal of the digital images. Red was not used as the surrounding grips and background were dominated by red shades which made point identication more dicult.

Figure 3.16 Geometry of IPPS samples, all dimensions in mm, sheet thickness is 1 mm

3.6.2

Testing Equipment and Conditions

The IPPS samples were tested using a hydraulic Instron machine. The samples were placed in wide grips and carefully aligned so that the grips pulled the samples straight in the major direction. The tests were conducted using a constant cross-head speed of 2.5 mm/min. As the samples were pulled, successive pictures were taken using

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an automatically controlled digital SLR camera. The time at which the images were taken was determined by placing a digital timer in the eld of view. These time signatures allowed the strain data from each test to be curve-t with respect to time. Pictures were also taken of the sample before it was loaded to provide a reference spacing for the grid points for the determination of grid strains in each deformed image.

3.6.3

Data Analysis

Using the successive digital images of the gridded surface of the sample it was possible to determine the local strain in the IPPS sample as it deformed. The dots of the grid were extracted from the background of the image using ImagePro image analysis software. The centroid of each dot was found automatically and its position in the image was recorded. The time at which the image was taken was then manually determined from the in-view clock. The dot-positions were then analyzed using strain analysis software so that the spacing of each grid was compared to the zerotime spacing to calculate a strain value. The major and minor strains were calculated for the center of every four dots. The local strain was therefore calculated for 49 locations on the sample in a seven by seven grid, for each time step of the test. In order to dene the necking behaviour of the material, the local strain must be found inside and outside the local neck as it develops. The points with the maximum major strain in the nal time step were determined to be those points inside the local neck. These were also the points along the line of fracture of the sample. Samples which fractured through a line of grid points (ie. where the strains were not being measured) were not considered for subsequent analysis. In order to better dene the necking behavior, the strain was then averaged for every three adjacent strain points along the necked region (in the minor direction) and along the grid spacings immediately above and below the necking row. An average was then found for each grid spacing

Experimental Methods

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along the minor direction of the strains above and below the neck. Average strains were therefore calculated for ve locations across the width of the sample, within, and just outside the local neck. The rate of change within these strain points was found by determining the slope between each point of major strain with respect to time. The dierence in the strain rate between the points within the local neck and those just outside was also calculated. This dierence was used to determine the necking behavior of the material; that is, as the neck forms the strain rate will localize in the necked region and the dierence between the strain rate inside and outside the neck will increase. A criterion for the onset of local necking was dened as a dierence in strain rate of 0.001 /s, and the local major strain that is achieved by the sample before reaching this criterion is considered a measure of its sheet formability. It is important to note that this criterion is strictly a comparative value, and while it will not match industrial forming limits exactly, it can be used to compare the formability of the dierent heat-treatments and microstructures produced in this study.

Chapter 4

Results
4.1 Characterization and Validation of the Magnetic Determination of Retained Austenite
4.1.1 Vibrating Sample Magnetometer Setup and Results

The rst step in using the VSM to determine levels of retained austenite in the TRIP steel was to test the equilibrium cooled sample of steel. The preparation of this sample and the theory surrounding this method was presented in Section 3.2. The magnetic saturation of this sample was measured to be 208 +/-1.28 emu/g. The cementite to ferrite ratio in the sample is assumed to be 0.0242 from the Fe-C phase diagram [41]. As the steel also contains several other alloying elements, this ratio is not exact but is assumed to be very close to the actual ratio. This ratio, combined with the ratio between the magnetic saturation of these two phases, 1.73 [33], was used to calculate that the ferrite has a magnetic saturation of 210 emu/g. Employing the same settings of the VSM, the magnetic saturation was determined for all of the other heat treatments.

4.1.2

X-Ray Diraction Results

The preliminary heat treatments were used to compare the measurement of retained austenite based on magnetic, X-ray diraction and optical measurements. For samples AH60, AH200, AM200, AL200 and AL1800 it was found that the volume percent of 67

Results Table 4.1 Volume percent retained austenite as measured by VSM and XRD
Sample AH60 AH200 AM200 AL200 AL1800 Retained Austenite by VSM (vol.%) 5.62 11.73 13.26 7.17 8.42 by XRD (vol.%) 6.43 6.22 11.18 6.86 6.43

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retained austenite varied from 6.6 vol.% to 14.1 vol.% using the magnetic saturation method. For these same samples tested under X-ray diraction it was found that the volume percent varied from 6.2 vol.% to 11.2 vol.%. These results are summarized in Table 4.1 which shows the volume percent of retained austenite measured for each sample by both methods. As is shown in Table 4.1 the values measured by X-ray diraction are consistently lower than those for the VSM method, except for sample AH60. Furthermore, the variation between the samples as measured by XRD also does not follow the same trend as the magnetic measurement. This discrepancy is thought to be a result of problems due to the sample preparation for the XRD samples. In preparing the samples they are both mechanically ground and exposed to very cold temperatures through dry ice application during electro-polishing. Given that the X-ray diraction method is a very surface specic measurement, if the mechanical deformation imparted through the polishing and the cold temperatures transform the surface austenite into martensite this measurement could underrepresent the levels of retained austenite present in the bulk of the material. In order to determine whether or not the surface preparation of the X-ray diraction samples aects the volume percent measured, a sample (AM200) was measured in the VSM and then placed on a piece of dry-ice for 30 seconds in order to simulate the temperatures achieved in the surface

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preparation for the XRD. The sample was then tested again in the VSM to determine the change in measured volume percent of retained austenite. The original measured volume percent was 13.4 vol.%. This dropped to 5.9 vol.% after treating with dry-ice, which matches closely with some of the dierences in the volume percent measured using the XRD technique. While the initial correlation between the VSM and XRD measurements of volume percent of retained austenite is very poor, the result of the dry-ice test indicates that the dierence may be partly, or entirely due to the transformation of retained austenite into martensite when the sample is cooled for electro-polishing. This transformation is certainly possible, as the RA in the TRIP steel is thermo-mechanically unstable, and could be triggered by the application of dry-ice.

4.1.3

Optical Analysis

The preliminary heat treated samples were also characterized optically, both to gain an understanding of the microstructure of the material and to provide a second method for verifying the retained austenite measurements obtained through the magnetic saturation method. Optical metallography was performed on the same samples analyzed by X-ray diraction, both in the transverse and longitudinal directions. No large dierences were seen from one sample to the next in terms of the morphology of the phases or in terms of the size of individual grains. For the optical samples it was possible to dierentiate between the ferrite/bainite and the martensite/retained austenite. Sample AH300 showed the highest volume percent of retained austenite, so this sample was used to validate the magnetic measurement of the same sample. This validation was performed by using a point count of the volume percent of the light martensite/austenite phase from optical micrographs of the sample, as described in Section 3.4.1. It was important to perform this comparison using the sample with the

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maximum volume percent of retained austenite as it is not possible to dierentiate between austenite and martensite optically; hence, the martensite content must be minimal in order to allow a proper correlation between the two methods. From the point counting of 5 micrographs along the length and width of the sample was found to contain 16 vol.% of retained austenite, in close agreement with the 15.5 vol.% measured through magnetic testing. This result is within the error of the magnetic testing method, and provides further evidence to the validity of the magnetic testing method.

4.2
4.2.1

Heat Treatments
Equiaxed and Lamellar Microstructures

In order to produce a TRIP microstructure with equiaxed grains of retained austenite, a two-stage heat treatment was employed. For the heat treatment of the initial coupons, a 750 C inter-critical hold for 5 minutes was followed by bainite holds of 350, 400 and 450 C for between 30 and 1800 seconds and then a water quench to room temperature. The bainite hold temperatures were selected to span the bainite formation region in order to dene the optimal bainite hold temperature. The resulting microstructures consisted of small islands of martensite/austenite surrounded by a matrix of larger bainite/ferrite grains as shown in Figure 4.1. There was little dierence seen between the transverse and longitudinal sections of the steel. All optical analysis of the equiaxed microstructure was performed on the A-series heat treatment coupons. It was assumed that the microstructure that resulted from the heat treatment of the tensile and IPPS samples would be very similar to those seen in the coupons. As the bainite hold temperature of 450 C showed the largest and most easily varied volume percents of retained austenite, this temperature was used for the bainite holds of all further heat treatments.

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Figure 4.1 a) Longitudinal and b) transverse section of sample AM200. Etched with picric/sodium metabisulte, martensite/austenite is light, ferrite/bainite dark.

The lamellar microstructure was produced through a three stage heat treatment. The samples were rst heated to the fully austenitic region at 950 C and held for 1000 seconds. The samples were then water quenched and heated to the inter-critical range at 750 C for ve minutes. The samples were then cooled to the bainite region and held at 450 C for 60, 100, 300 and 1800 seconds. These dierent hold times were used to dene the transformation to bainite and stabilization of austenite during the bainite hold. The bainite hold temperature was chosen as the best of those tested for the equiaxed microstructure as it was assumed that the thermodynamics of the transformation would not dier with the morphology. The resulting microstructure from this treatment consists of small elongated grains of martensite/austenite in a matrix of larger grains of ferrite/bainite, and is shown in Figure 4.2. From these micrographs it can be seen that the grains of martensite/austenite appear elongated in both the transverse and longitudinal sections. This is because the grains of both martensite/austenite and ferrite are shaped in thin plates like the martensite from which the austenite is grown. The martensite/austenite is found in small grains which are approximately 5 m long and 1 m thick. The plates of

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Figure 4.2 Micrographs of sample TL300-2 in a) longitudinal and b) transverse directions. Etched with picric/sodium metabisulte, martensite/austenite is light, ferrite/bainite is dark.

martensite/austenite are much smaller than those of the ferrite/bainite which are both longer and thicker, and having a width of approximately 20 m and a thickness of 5 um. The phases of all the plates are oriented in the same direction over short ranges through the sample. It is also dicult to distinguish between dierent grains of ferrite/bainite, but it is assumed that the martensite/austenite grains are located at the boundaries of grains or sub-grains. Some of the grains of martensite/austenite and ferrite/bainite seem to be much thicker while still having roughly the same length. This is thought to be due to the angle at which the plates intersect the surface, as opposed to representing an actual large variation in the sizes of the grains.

4.2.2

Investigation of the Bainite Hold

The rst set of heat treatments performed in this study were those to dene the optimal conditions of the bainite hold for the material using the equiaxed heat treatment. Thirteen coupons were produced, all of which were held in the inter-critical region for 5 minutes at 750 C and then cooled to 350, 400 or 450 C and held in the bainite region for 30 to 1800 seconds. Samples in this rst series of heat treatments were

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labeled as AX###-# for A(temperature of bainite hold - Low, Middle, High)(time of bainite hold in seconds)-(sample number). The magnetic saturation of each heat treatment of the initial series was compared to the magnetic saturation of pure ferrite in order to calculate the volume percent of retained austenite. The percent of retained austenite calculated for each heat treatment is shown in Table 4.2 and illustrated in Figure 4.3. In order to calculate the condence interval of the magnetic retained austenite measurements, as shown by the error bars shown in Figure 4.3, repeated tests were performed on a non-austenite containing TRIP sample. The sample was tested in the VSM 23 times, and its magnetic saturation was calculated for each trial. This set of data was used to calculate the repeatability of the magnetic testing using a student t-test and a 95 % condence interval. The condence interval was found to be 2.90emu/g It was then assumed that the condence interval of all other tests scaled linearly with the measured magnetic saturation. The calculated condence interval of the austenite-free sample and the assumed condence interval of the measured sample were used to perform a partial derivative error propogation through the calculation of the retained austenite volume fraction to nd the condence interval of the retained austenite measurements. This process was used for all austenite measurements and the condence interval is shown as the error bars on each plot of retained austenite. As can be seen from Figure 4.3, the volume percent of retained austenite increases to a maximum with increasing bainite hold times for each bainite hold temperature. With longer bainite hold times the level of retained austenite slowly decreases. The maximum level of retained austenite is seen for samples held at 450 C for 300 seconds. These samples also show a very clear development of retained austenite levels from 30 seconds to 300 seconds, making 450 C the best of those tested for the purpose of varying the level of retained austenite in the samples.

Results Table 4.2 A-series heat treatment conditions and volume percent retained austenite, as measured by magnetic saturation
Sample AL60 AL200 AL300 AL1800 AM60 AM200-1 AM200-2 AM300 AM1800 AH30 AH60 AH200 AH300 AH1800 Bainite Hold Temperature ( C) 350 350 350 350 400 400 400 400 400 450 450 450 450 450 Bainite Hold Time (s) 60 200 300 1800 60 200 200 300 1800 30 60 200 300 1800 Retained Austenite (vol.%) 1.95 7.17 14.03 8.42 7.48 13.26 12.55 11.02 10.06 0.85 5.62 11.73 14.63 9.22

74

Figure 4.3 The volume percent of RA produced at bainite hold temperatures of 350, 400 and 450 C, as a function of bainite hold time

Results Table 4.3 Bainite hold times and measured volume percent retained austenite for equiaxed tensile samples.
Sample TE30-1 TE60-1 TE60-2 TE100-1 TE100-2 TE100-3 TE100-4 TE100-5 TE100-6 TE200-1 TE200-2 TE300-2 TE300-3 TE1800-1 TE1800-2 Bainite Hold Time (s) 30 60 60 100 100 100 100 100 100 200 200 300 300 1800 1800 Retained Austenite (vol.%) 3.18 8.43 3.74 15.15 14.11 13.51 12.30 14.00 13.21 11.98 12.60 11.13 9.14 9.54 10.87

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4.2.3

Equiaxed Tensile Samples

The heat treatment of the uniaxial tensile samples was based on the treatments used in the testing coupons. The purpose of this set of heat treatments was to produce a large and varied volume percent of retained austenite in an equiaxed state. The same inter-critical hold condition of 750 C for 5 minutes was used. This was followed by a bainite hold at 450 C for 30, 60, 100, 200, 300 and 1800 seconds. Samples in this series are referred to as TE###-# for Tensile samples, Equiaxed microstructure followed by the bainite hold time in seconds and the sample number for each particular heat treatment. The volume percent of the samples was then determined using the magnetic method. The results are shown in Table 4.3 and illustrated in Figure 4.4. The volume percents of retained austenite measured from the TE samples are very close to those found for the A-series coupons held at 450

C (see Figure 4.3).

The same characteristic curve is exhibited by the volume percent of retained austenite

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Figure 4.4 Volume percent of RA as a function of bainite hold time for TE series heat treatments, employing a bainite hold temperature of 450 C

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in the tensile samples, but the peak hold time occurs at 100 seconds in the TE100 samples. A steep increase is seen in the volume percent of retained austenite from 30 to 100 seconds, with a slower decrease for longer bainite hold times. The large dierences observed in volume percent of retained austenite spanning from the TE30 to the TE100 samples were used to design the hold times used in creating in-plane plane-strain samples with varying levels of retained austenite.

4.2.4

Equiaxed IPPS

Three of the six heat treatments used in the TE series were subsequently chosen to produce samples for in-plane plane-strain testing. As before, the samples were held at the inter-critical temperature of 750 C for 5 minutes, followed by a bainite hold at 450 C for 30, 60 and 100 seconds, and then a water quench to room temperature. This treatment produced a good variation in volume percent of retained austenite to a maximum at 100 seconds. These samples are referred to as IE###-# for IPPS sample, Equiaxed microstructure followed by the bainite hold time in seconds and the sample number. These samples were then tested for their volume percent of retained austenite using the magnetic testing method. The measured volume percents are summarized in Table 4.4, and Figure 4.5. Figure 4.5 illustrates that the volume percent of retained austenite increases with holding times from 30 to 60 to 100 seconds, as was seen with the TE samples. In the case of the IPPS samples, this increase is more gradual, and the maximum volume percent of retained austenite obtained is smaller than the maximum obtained for the TE samples.

4.2.5

Lamellar Tensile

Tensile samples were formed with a lamellar microstructure using the three-stage heat treatment described in Section 4.2.1. Samples in this series of heat treatments are

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Table 4.4 Bainite hold times and average volume percent of retained austenite measured magnetically for equiaxed tensile samples. The A and B samples were taken from either side of the IPPS sample as shown in Figure 3.3.
Sample IE30-1 IE30-2 IE30-3 IE30-4 IE30-5 IE60-1 IE60-2 IE60-3 IE60-4 IE60-5 IE100-1 IE100-2 IE100-3 IE100-4 IE100-5 IE100-6 Bainite Hold Time (s) 30 30 30 30 30 60 60 60 60 60 100 100 100 100 100 100 Side A (vol.%) 5.20 7.08 5.67 3.56 5.21 5.98 6.05 9.30 5.45 6.76 9.62 11.96 11.65 9.27 9.78 8.23 Retained Austenite Side B (vol.%) 3.14 5.70 2.85 3.96 6.80 8.35 8.37 7.75 8.15 9.26 13.20 9.30 7.25 10.98 11.55 8.78 Average (vol.%) 4.17 6.39 4.26 3.76 6.00 7.16 7.21 8.53 6.80 8.01 11.41 10.63 9.45 10.12 10.67 8.51

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Figure 4.5 Volume percent of RA as a function of bainite hold time for IE series heat treatments, employing a bainite hold temperature of 450 C

Results Table 4.5 Bainite hold times and volume percent of retained austenite measured magnetically for lamellar tensile samples.
Sample TL60-1 TL60-2 TL100-1 TL100-2 TL300-1 TL300-2 TL1800-1 Bainite Hold Time (s) 60 60 100 100 300 300 1800 Retained Austenite (vol.%) 8.82 9.24 9.53 9.52 9.41 8.42 4.55

80

referred to as TL###-# for Tensile sample, Lamellar microstructure followed by the bainite hold time in seconds and the sample number. These samples were analyzed optically to determine the morphology of the dierent phases, and magnetically to measure the volume percent of retained austenite contained in each sample. The variation of volume percent of retained austenite with bainite hold time is presented in Table 4.5, and illustrated in Figure 4.6. The maximum average volume percent of retained austenite again occurred at the bainite hold time of 100 seconds; however, the maximum is lower than that of the equiaxed microstructure. For the TL samples the maximum volume percent also presents a less dened peak, with the bainite hold times of 60 and 300 seconds being very close to this maximum value. As with the equiaxed microstructure, a large decrease in retained austenite content is seen with very long hold times. In order to conrm the presence of the peak at 30 to 300 seconds an additional sample was prepared by quenching directly from the inter-critical hold, corresponding to a bainite hold time of zero seconds. This sample was expected to have no retained austenite. Magnetic testing revealed a volume percent of retained austenite of -1.89 vol.%. This negative result is slightly troubling, but most likely represents a very low volume percent of retained austenite, and is simply negative due to the larger errors

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Figure 4.6 Volume percent of RA as a factor of bainite hold time for TL series heat treatments, employing a bainite hold temperature of 450 C

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expected with samples which have high magnetic saturations. This very low value indicates that this sample had a higher magnetic saturation than that calculated for pure ferrite. This conrms that the retained austenite volume percent continues to decrease with hold times shorter than 100 seconds.

4.2.6

Lamellar IPPS

The heat treatment used for the lamellar in-plane plane-strain samples was based on the TL100 treatments which produced a maximum volume percent of retained austenite. In order to compare the performance of the lamellar to the equiaxed microstructure under in-plane plane-strain, similar volume percents of retained austenite were required. It was expected that the IPPS samples would show a decrease in maximum volume percent RA from the tensile samples as was seen with the equiaxed samples. On testing the samples it was found that the volume percent of RA in the samples ranged from 7.9 to 11.3 vol.%, while most samples were ranged between 10 and 11 volume percent, with the average of 10.13 +/-0.94 vol.%. The lamellar IPPS samples tested from this series showed a very uniform volume percent of RA. The average volume percent was comparable to that measured in the smaller tensile coupons (TL series). This high volume percent of RA in the lamellar IPPS samples is at odds with the equiaxed samples which showed a denite drop in maximum RA from the tensile to the IPPS samples. The samples in this series of heat treatments are referred to as IL###-# for IPPS sample, Lamellar microstructure followed by the bainite hold time in seconds and the sample number. The volume percent of retained austenite calculated for each sample using magnetic saturation is shown in Table 4.6.

Results Table 4.6 Lamellar IPPS samples with volume percent of retained austenite measured magnetically on either side of the IPPS sample as shown in Figure 3.3, bainite hold time is 100 seconds.
Sample Side A (vol.%) IL100-1 IL100-2 IL100-3 IL100-4 IL100-5 IL100-6 9.87 10.16 7.92 9.79 10.46 10.00 Retained Austenite Side B (vol.%) 11.34 10.83 10.01 10.01 10.03 10.06 Average (vol.%) 10.60 10.49 8.97 10.19 10.25 10.30

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4.3

Tensile Results

Tensile tests were performed on sub-sized tensile samples of the equiaxed and lamellar TRIP microstructures, for several heat treatment conditions and levels of retained austenite. Stress-strain curves and calculations of instantaneous n values were obtained for each heat treatment. The yield and UTS were noted for each sample. The major strain at the UTS point was also used as a simple preliminary measure of the sample formability. The calculated instantaneous n value was plotted versus the true strain for each sample in order to get an appreciation of the strain hardening behavior of the sample, and to look for sustained hardening which is useful for sheet formability and one of the main advantages of TRIP steels over conventional steels. The strain at UTS and the instantaneous n values were compared to the volume percent of retained austenite in samples and to the phase morphology of the sample.

4.3.1

Equiaxed Stress Strain Analysis

The equiaxed samples of the TE series were tested under uniaxial tension. The load and the gauge strain were measured to produce data for the engineering strain and

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engineering stress of each sample as it deforms. This data was used to produce the stress-strain curves shown in Figure 4.7. This gure shows a representative sample for each heat treatment. The yield strength, ultimate tensile strength (UTS) and strain at UTS are shown in Table 4.7. The yield strength was dened by a 0.2% strain oset from the elastic portion of the stress-strain curve.

Figure 4.7 Typical engineering stress-strain curves for TE series samples From the stress-strain curves it is evident that the bainite hold time has a large eect on the tensile properties of the equiaxed samples. The TE30 samples, with a very short bainite hold and low volume percent of retained austenite exhibit a high yield strength and the highest UTS of all the samples. However, these samples were much less ductile than the others, having a low strain at UTS. As the bainite hold time increases to 60 seconds in the TE60 series the samples yielded at a lower stress

Results Table 4.7 Tensile properties of TE samples

Sample TE30-1 TE60-1 TE60-2 TE100-1 TE100-2 TE100-3 TE100-4 TE100-5 TE100-6 TE200-1 TE200-2 TE300-2 TE300-3 TE1800-1 TE1800-2 Yield Strength (MPa) 402 370 386 328 333 348 356 358 362 329 315 310 340 377 357 UTS (MPa) 863 806 813 783 820 838 861 835 849 811 800 781 811 746 724 Eng. Strain at UTS 0.129 0.135 0.122 0.179 0.157 0.180 0.173 0.187 0.184 0.145 0.165 0.129 0.133 0.162 0.142

85

True Strain at UTS 0.121 0.127 0.115 0.165 0.146 0.166 0.160 0.171 0.169 0.135 0.153 0.121 0.125 0.150 0.133

and reached a lower UTS than the TE30 samples, but the UTS occurred at a higher strain. The TE100 samples, with the maximum volume percent of retained austenite, exhibited both a higher UTS and a higher strain at UTS in comparison to the TE60 samples. The TE100 series obtained the highest strain at UTS, and the highest UTS of all the samples except for the TE30 series. With longer bainite hold times, where the volume percent of retained austenite decreases, so do the tensile properties, with the TE200, TE300 and TE1800, each having progressively lower UTS and lower strains at UTS. The strain at UTS was used as a preliminary predictor of formability. In Figure 4.8 this property is plotted against the bainite hold times of the samples and compared to the volume percent of retained austenite. From Figure 4.8 it is clear that the strain at UTS both varies with bainite hold time and is related to the volume percent of RA in the samples. The strain at UTS

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Figure 4.8 Strain at UTS and volume percent RA as a function of bainite hold time for TE series heat treatments, employing a bainite hold temp of 450 C

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shows the same peak at a bainite hold of 100 seconds that is seen in the retained austenite curve. The strain at UTS for the 30 and 60 second holds, however, are almost identical, while the retained austenite increases. Also, between the 300 and 1800 second holds the strain at UTS actually increases while the volume percent decreases. For very short hold times, as seen in the TE30 stress-strain curve, the tensile behaviour of the TRIP steel is very similar to that of a dual-phase steel with no discernible yield point, with failure occurring shortly after the point of UTS. Curves with longer hold times show a more dened yield seen as a noticeable change in the slope of the stress-strain curve. The yield is most dened in the TE1800 sample where the sample show prolonged discontinous yielding creating a plateau in the stress-strain curve.

4.3.2

Lamellar Stress Strain Analysis

As for the equiaxed microstructure, the lamellar microstructure was tested under uniaxial tension to produce stress-strain data for varying levels of retained austenite. The engineering stress is plotted against the engineering strain for each lamellar heat treatment, and the resulting curves are shown in Figure 4.9. The stress-strain curve of the TE100 series is included for comparison. The yield strength, UTS and strain at UTS are summarized in Table 4.8. The dierences between the stress-strain curves for the lamellar samples are not as great as those observed for the equiaxed samples. All of the curves have very similar ultimate tensile stresses, however the strain at UTS appears to vary with the bainite hold time just as it did in equiaxed series of samples. The bainite hold time of 100 seconds, which produced the largest volume percent of retained austenite, has clearly the largest strain at UTS of all the samples. The samples with shorter and longer bainite hold times show decreasing strains at UTS with the TL1800 samples

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Figure 4.9 Typical engineering stress-strain curves for TL series heat treatments

Table 4.8 Tensile properties of lamellar tensile samples

Sample TL40-1 TL60-1 TL60-2 TL100-1 TL100-2 TL300-1 TL300-2 TL1800-1 Yield Strength (MPa) 463 435 446 466 482 489 497 447 UTS (MPa) 733 728 745 726 743 727 750 727 Eng. Strain at UTS 0.183 0.169 0.201 0.191 0.219 0.156 0.170 0.156 True Strain at UTS 0.168 0.156 0.183 0.175 0.198 0.145 0.157 0.145

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being the lowest. Comparing the lamellar stress-strain curves to those of the equiaxed samples shows that all of the lamellar samples have a much higher yield strength than the equiaxed, and the strain at UTS is greater for these samples. The samples also show lower hardening rates and a lower UTS than the equiaxed samples. Unlike the equiaxed microstructure, all of the tensile samples with lamellar microstructures show a dened yield point. For all samples there is an obvious change in slope of the stress-strain curve at the point of yielding. This change in slope is very similar for all bainite hold times. None of the samples show a discontinuous yielding as pronounced as that seen for sample TE1800 in Figure 4.7. The strain at UTS was used as a preliminary predictor of formability for the tensile samples. This property is plotted against the bainite hold times of the samples and compared to the volume percent of retained austenite. This comparison is shown for the lamellar series of samples in Figure 4.10.

Figure 4.10 Strain at UTS and volume percent RA for TL series heat treatments

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From the comparison of TL series volume percent RA, bainite hold time and strain at UTS it can be seen that both the volume percent RA and the strain at UTS of the samples increase to a maximum at the 100 second hold time, and both decline with longer hold times. This peak is much more dened in the case of the strain at UTS, while there is little dierence observed between the volume percent of retained austenite from the TL60 to the TL300 samples.

4.3.3

Instantaneous n Values

Instantaneous n values were calculated from the true stress/true strain data of both the TE and TL series using Equation 2.2. High n values that are sustained up to large strains indicate superior formability of sheet materials. Figures 4.11 and 4.12 plot the instantaneous n values as a function of true strain for three samples of both the equiaxed and lamellar tensile series: one sample with a short bainite hold time, one with the highest volume fraction of retained austenite (intermediate bainite hold time), and one with a long bainite hold time. In Figure 4.11 it can be seen that the instantaneous n values of the equiaxed samples reach a sharp maximum at small strains and then quickly decay at higher strains. The most sustained hardening is observed in sample TE100-3, which reaches a peak instantaneous n of roughly 0.4 and then decays steadily to zero at a true strain around 20 %. This sample is from the tensile series with the highest volume percent of retained austenite. The shortest bainite hold time, (TE30) exhibits a distinctly lower maximum instantaneous n (0.325) which decays to zero at a true strain of roughly 14 %. For heat treatments longer than 100 seconds, where the volume percent of retained austenite decreases, the instantaneous n curves also showed lower sustained hardening than for the TE100 samples, as is seen in the curve for TE1800-2, shown in Figure 4.11.

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Figure 4.11 Instantaneous n as it changes with strain for three TE series heat treatments. TE30-1 - Green, TE100-3 - Blue, TE1800-1 - Red

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Figure 4.12 Instantaneous n as it changes with strain for three TL series heat treatments. TL60-1 - Green, TL100-2 - Blue, TL1800-1 - Red

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The lamellar samples, shown in Figure 4.12, demonstrate markedly dierent instantaneous n curves from the equiaxed samples. The lamellar samples produced much lower peak n values, with the largest being 0.3 for the TL1800 sample. As with the equiaxed samples, the samples with the most sustained instantaneous n values are from the TL100 series, corresponding to the largest volume fraction of retained austenite. The curves for this series have a peak instantaneous n of around 0.27, which slowly decays to zero at a true strain of 25%. The samples with shorter and longer hold times have slightly larger peak instantaneous n values than the TE100 series but these values decay more quickly. The shape of the instantaneous n curves for the lamellar structure are very dierent from the equiaxed samples. Namely, the lamellar samples have lower peak instantaneous n values, but the instantaneous n values are sustained to much greater levels of strain.

4.4

In-Plane Plane-Strain Testing

Samples of both the equiaxed and lamellar heat treatments were tested under in-plane plane-strain (IPPS). Three heat treatments with varying bainite hold times were used for the equiaxed samples in order to study the eect of retained austenite level on the IPPS behavior. A single heat treatment was used for the lamellar microstructure, (IL100) to reveal any dierences in the IPPS behavior that might arise from diering phase morphologies. The local deformation of the samples were measured during these tests following the strain measurement and forming limit procedures described in Section 3.6.3. The criterion used to dene the onset of local necking was a dierence in the local strain rate between the neck and surrounding regions of 0.01 /s. The major strain that each sample reached locally before meeting this criterion is used to compare the formabilities of the samples with varying microstructures and volume percents of retained austenite.

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For the IPPS testing, six samples were made of each unique heat treatment applied to both the equiaxed and lamellar microstructures. Due to problems during testing, including equipment failures, non-uniform deformation of the samples due to misalignment and the formation of necks through instead of between grid points (instead of between them). Only one sample from the IE30 and IE100 series, and only two samples from the IE60 and IL100 series were successfully analyzed.

4.4.1

Strain in Cells

The rst step in analyzing the IPPS test was to determine the development of local strains in each sample. Strains were found to be initially uniform across the samples, but towards the end of the test the strain localizes into a neck, which is evident in Figure 4.13, which plots the strain behavior of sample IE100-3. The three dimensional plots show the x and y grid numbers of the samples. The vertical axis of each plot shows the major strain at the centre of each grid point. Each layer of the plot shows a step in time, increasing upwards.

Figure 4.13 Strain proles for the a) beginning, b) middle and c) end of the IPPS testing of sample IE100-3 For the sample IE100-3 the strain clearly localizes near the end of the test into the centre grid row of the sample. The strain is also larger on one side of the sample than

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the other showing that, while the applied strain is fairly constant across the width of the sample the strain will undoubtably localize rst on one side of the sample center.

4.4.2

Comparative Forming Limits

The local strain rates within each sample were then analyzed and the dierence between the strain rate within and outside the necked row was determined for each of ve positions across the width of the sample. The development of this strain rate dierence, i.e. necked versus un-necked rows, is shown for sample IE100-3 in Figure 4.14. In this gure each curve represents the strain rate dierence for each of ve positions across the width of the sample. The dierence in strain rate between the neck and the surrounding material is initially very low, and remains low until near the end of the test. The strain rate dierence then sharply increases as the strain localizes within the neck of the sample. The comparison criterion used in this study, a strain rate dierence of 0.01 is indicated by the horizontal line in Figure 4.14. When the strain rate dierence at each horizontal position reaches this limit it is considered to have locally necked. The major local strain at that time was then calculated to produce a comparative forming limit for each sample in the heat treatment. Only the centre three positions were averaged in this analysis as it was assumed that these areas experienced truly IPPS loading. The comparative forming limit for equiaxed and lamellar samples is presented in Table 4.9 and is plotted in Figure 4.15 against the volume percent of retained austenite in each sample. The horizontal error bars shown in Figure 4.15 represent the 95 % condence interval of the retained austenite measurements as described in Section 4.2.2. The vertical error bars represent the 95 % condence interval of the strain-at-neckingcriterion for each sample. This condence interval was calculated directly from the

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Figure 4.14 Curves of the dierence in strain rate for sample IE100-3 between necked and un-necked rows at ve locations across the sample width

Results Table 4.9 Retained austenite and strain at the local necking condition for equiaxed and lamellar IPPS samples
Sample IE30-5 IE60-1 IE60-3 IE100-3 IL100-2 IL100-6 Retained Austenite (vol.%) 6.00 7.16 8.52 9.44 10.49 10.3 Strain at Local Necking Condition 0.111 0.140 0.135 0.145 0.186 0.168

97

samples by performing a student t-test on three strain measurements across the necked region of each sample. From Figure 4.15 a strong relationship is evident between volume percent of retained austenite in the samples and the local strain at onset of local necking for an IPPS test. This relationship is similar to that seen from the uniaxial tensile test data. Within the equiaxed series, the comparative forming limit steadily increases with bainite hold time and volume percent of retained austenite. In the lamellar series the two samples with the same bainite hold time have similar comparative forming limits. While these forming limits are substantially higher than those found in the equiaxed samples, the lamellar samples also have a higher volume percent of retained austenite and so it is not clear whether this increase is due to the dierent phase morphology of the microstructure or is simply a continuation of the trend seen for increasing volume percent of retained austenite.

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Figure 4.15 Strain at relative necking limit for IE and IL series samples plotted against the volume percent of RA in each sample

Chapter 5

Discussion
5.1
5.1.1

Characterization of TRIP steels

Use of Magnetic Saturation for the Measurement of Volume Percent of Retained Austenite

The use of magnetic saturation for the determination of volume percentage of retained austenite is not a new method, [37], but it is still not as widely used as other techniques, with X-ray diraction being the most prominent. The use of magnetic measurements for the current study was born out of the ease of sample preparation, and the speed of testing which allowed many bulk samples to be measured quickly and with good precision. Much of the work using the vibrating sample magnetometer (VSM) was done in order to verify the accuracy of the measurements of retained austenite and to assess the reliability of these measurements. The retained austenite levels measured in the TRIP steel samples generally made physical sense and corresponded with what is already known about TRIP steels. The presence of a clear peak volume fraction of retained austenite with increasing bainite hold times ts well with theory, as is discussed in Section 2.1. Such a peak in retained austenite was observed for all bainite hold temperatures, sample geometries and inital microstructures. The maximum volume percent retained austenite measured in this thesis, 14.6 vol.% in sample AH300, is below the theoretical maximum of approximately 21 vol.%, calculated from the Iron-Carbon phase diagram and the To curve 99

Discussion

100

for bainite transformations (shown in Figure 2.7), assuming that all austenite has a nal carbon content of 1 wt.% and is stabilized to room temperature. The lowest volume fraction of retained austenite measured was -1.89 vol.% for the lamellar sample quenched directly from the inter-critical hold. It is expected that this sample will have no retained austenite, and so this measurement, while below zero, ts well with expectations. The average 95% condence interval of all the samples was found to be 0.94 vol.%

from repeated measures of a single VSM sample. From the current set of results it appears that the level of condence depends on the magnetic saturation of the sample.

Samples with lower magnetic saturations (i.e. higher volume percent RA) that were tested multiple times seem to show much lower errors than are predicted by the equilibrium cooled sample. It is thought that the curve tting performed to calculate the magnetic saturation of a sample is closer to the actual saturation for lower-saturation samples. This is most likely due to the fact that only the non-linear portion of the magnetic hysteresis loop could be used for the curve-tting, and as samples with higher magnetic saturations only become non-linear at higher elds there are many fewer data points available for this curve tting. This means that the actual uncertainty for samples with higher volume percentages of retained austenite are probably lower than those reported, while samples with very low levels of RA seem to have a much higher error. There are several ways in which the magnetic measurements could be improved. The rst and most obvious is to have used a magnetometer with a much larger magnetic eld. The VSM at RMC applies a maximum eld of 6500 Oer (0.52 MA/m),

which brings the TRIP steel very close, but not entirely, to full magentic saturation. This deciency raises the necessity for curve-tting the magnetic measurements and introducing a new realm of systematic errors. If the VSM produced a larger eld it would be possible to use the maximum magnetization of the sample to determine the

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magnetic saturation, or to t the magnetic saturation curve with much greater certainty. A eld of about twice that provided by the VSM at RMC would be sucient. In the work of Zhao et al. [33] a SQUID magnetometer was used to create elds over seven times larger than those employed in this study, and to produce very accurate measurements of TRIP steel magnetic saturations. The underlying assumptions used in the calculation of the pure ferrite saturation magnetization could also be improved. If the composition and volume fraction of the ferrite in the equilibrium cooled sample were measured directly, instead of assumed from phase diagrams, it would lend a greater degree of condence to the calculated magnetic saturation. Also, if the chemical composition of the ferrite in the RA-containing TRIP steels was measured the magnetic saturation could be directly calculated from the chemical composition based on the procedure outlined by Bozorth [37]. This approach would eliminate the need for an equilibrium-cooled reference sample entirely.

5.1.2

X-Ray Diraction Measurements of Volume Percent of Retained Austenite

X-ray diraction (XRD) is a standard method for determining the volume fraction and composition of the retained austenite phase in TRIP steels. There are several serious drawbacks to the X-ray diraction method with relation to TRIP steels, some of which were observed in this study. XRD analysis was performed initially to validate the measurements of retained austenite made by the magnetic saturation method. Results of the two methods did not agree with each other, and it is thought that this discrepancy is due to limitations in the XRD measurements rather than problems with the magnetic testing method. The XRD measurements not only did not match the magnetic measurements, but they also did not follow the expected trends of increasing and decreasing volume fraction of retained austenite with bainite hold time, trends

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evident in the magnetic test data. Samples AM200 and AH200, which had the largest volume fractions as measured by magnetic saturation, showed much lower volume fractions when measured by XRD. Initially it was thought that the magnetic method was over-predicting the volume fraction of retained austenite, but further testing with the VSM produced results very close to what is predicted by theory, and closely matched the volume percentages found in similar works [6, 16]. The preparation of the XRD samples involved both mechanical grinding and polishing of the surface as well as electropolishing at low temperatures. Given that the retained austenite in the samples is mechanically and thermally unstable it is possible that either (or both) of these processes transformed the austenite at the surface of the sample, where it is measured by XRD, resulting in a lower measured volume percentage. When the samples were electropolished, the polishing solution and the back of the samples were cooled with dry-ice to prevent the surface from pitting. To reproduce this cooling condition, and determine whether a possible martensite transformation could be captured through magnetic measurements, a sample was heat treated with identical condition as sample AM200. It was then measured magnetically before and after treating with dry ice as described in Section 4.1.2 of the methods. The sample showed a decrease of 7.5 vol.% in measured retained austenite. This drop is larger than the dierence observed between any of the XRD and magnetic results, and so it is possible that this transformation accounts for all of the dierences seen in the two methods. The small dierences seen for samples with lower volume percents of retained austenite could be explained by the generally greater stability of the austenite which would resist transforming with mechanical and thermal changes. Another outcome of this dry-ice test is that it could be used as a measure of the stability of the retained austenite, by performing measurements before and after the application of dry ice. One of the drawbacks of the magnetic testing is that it does not provide any information about the retained austenite other than its volume

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percentage. In contrast, the XRD method can reveal information about the carbon content of the austenite through peak shifts, and microscopy methods can reveal the morphology and grain size of the retained austenite.

5.1.3

Microscopy and the Determination of TRIP Steel Microstructures

The optical metallography performed in this study was very good for determining the microstructure of the TRIP steels in terms of the grain sizes and morphologies of the austenite/martensite and ferrite/bainite phases. Where this method could be improved is in the dierentiation of each of the four phases. The etch used, as described by Girault et al. [39], should allow the ferrite and bainite phases to be dierentiated, with bainite appearing brown and ferrite as blue. Some colouration of this type was observed, such as in Figure 4.1, but the colouration was never consistent or clear enough to allow for condent identication of the two phases, even after careful mixing and preparation of the etch to bring out these colours. In the case of the micrographs for the lamellar samples in Figure 4.2 no attempt was made to adjust the mixing ratios to bring out these colours as the dierentiation between austenite/martensite and bainite/ferrite was adequate to dene the phase morphologies and grain sizes. It may be possible to re-create the results of Giraults etches using the TRIP steel, but this would require more careful experimentation with dierent etch mixtures, and possibly fresher chemicals and a cleaner working environment than that used in this study. It is also possible to dierentiate the separate phases through electron microscopy. Martensite can be dierentiated from austenite by heating the steel to 200 C and allowing the martensite to temper, and then etching with a simple Nital solution and examining under an SEM [17]. Bainite and inter-critical ferrite can be dierentiated by their diering morphologies under SEM. In cases where the bainite sub-grains are

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too small to to be viewed under SEM, TEM can be used to dierentiate it from the inter-critical austenite. In the case of Marks Ph.D. work on lamellar TRIP steels, the position and morphology of the bainite was not clearly identied, even under TEM [5]. Conclusively showing where, and in what shape, the bainite grows in a TRIP steel is important to understanding how the microstructure develops during the bainite hold. Understanding this transformation will in turn assist in the design of processing conditions that promote the growth of bainite and the subsequent partitioning of the stabilizing carbon to the austenite.

5.2
5.2.1

Microstructural Evolution
Initial Microstructures

The formation of the two microstructures investigated in this work (ie. the equiaxed and lamellar) relied on the creation of the necessary starting microstructures. In the case of the equiaxed structure the initial steps involved cold-rolling the steel from 5 mm down to 1 mm and then heating to the inter-critical region. The cold-rolling was mainly performed to create the proper sheet thickness, but also served to deform the initial hot-rolled microstructure of the steel. This additional stored energy allows the steel to recrystallize more quickly at the inter-critical temperature, and also helps to reduce the grain size of the steel. The steel was held at the inter-critical temperature for 5 minutes. After this time, it is assumed that the steel consisted of only equilibrium austenite and ferrite. This structure was never analyzed given that the steel produced the expected microstructures after bainite holding, but quenching the steel directly from the inter-critical hold and performing metalloraphy could conclusively show the desired combination of martensite and ferrite. The preparation of the lamellar microstructure again started by cold-rolling the received slab from 5 mm down to 1 mm. The sample was then re-heated to the fully

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austenitic region and quenched to produce a structure of ne martensite. The sample was then heated to the inter-critcal region as with the equiaxed structure. The resulting structure again contained a large amount of stored energy, in this case from the grain boundaries and deformation caused by the martensitic transformation, and this energy undoubtedly helped to develop the inter-critical microstructure. Although no direct observations were made of the microstructure after these intermediate stages, such experiments could be performed to conrm the proposed microstructural evolution.

5.2.2

The Inter-critical Hold

The temperature of the inter-critical hold employed in this work (450 C) is towards the lower end of the inter-critical region. The lowest end of the inter-critical range was chosen because it produces the largest possible volume fraction of equilibrium austenite. The formation and chemistry of equilibrium austenite are well understood, and follow a predictable process and so it was thought that if more carbon is partitioned through this process (than through the more complex growth of bainite), then the nal structures would be more predictable and would vary more regularly with changes in the bainite hold time. The hold time of ve minutes seemed to be long enough for both the equiaxed and lamellar samples to produce the desired microstructures, without any evidence of prior cold-rolled or martensite grains in the nal microstructure. In the case of the equiaxed microstructure the slow cooled and cold rolled structure recrystallized producing a new structure of smaller, undeformed ferrite and austenite grains. At this temperature, the newly formed austenite grains would contain approximately 0.8 wt.% carbon. The lamellar structure develops in a similar way, but instead of starting from the as-cold-rolled condition, it begins the inter-critical hold comprised completely of

Discussion

106

martensite grains. During the inter-critical hold these grains of martensite were partitioned into higher carbon austenite and ferrite. As the thin plates of martensite decompose into ferrite and austenite they do so over short ranges to produce a structure of alternating plates of ferrite and austenite oriented in the same direction as the initial martensite plates.

5.2.3

The Bainite Hold Curve

The formation of bainite is the most essential step in creating low-alloy TRIP steels, as the bainite transformation partitions carbon to the austenite, raising its level above the 1 wt.% required to stabilize the structure at room temperature [9]. By varying the bainite hold temperatures and times, TRIP steels were produced with large differences in their volume percent of retained austenite. For the equiaxed structure, temperatures of 350, 400 and 450 C were used for the bainite hold of the A-series samples. Surprisingly, little dierence was observed from one temperature to another in either the maximum volume percent retained austenite or in the time it took the steel to reach this maximum. It was thought that because of the temperature and chemistry relation of the bainite transformation the samples at higher temperatures would exhibit higher volume percentages of less stable retained austenite while lower temperatures would produce lower volume percentages of retained austenite that was more stable. It is possible that this occurred, and that the 450 C samples did yield substantially more austenite, but more of it transformed upon cooling in comparison to the lower temperature samples. To determine if this truly happened, the volume fraction of martensite could be determined through careful SEM metallography to determine what fraction of the austenite transformed during each heat treatment. The temperature of 450 C was chosen as the optimal temperature for varying the volume percent of retained austenite through the bainite hold as it exhibited the strongest trend. This choice was somewhat arbitrary as both the 400 and 350 C

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samples exhibited similar curves; that is, the dierences between the three are not much greater than the level of measurement uncertainty for retained austenite. The bainite hold temperature of 450 C is higher than that used for most other TRIP steel research [12, 14], but these studies have carefully designed the heat treatments to obtain optimal mechanical properties such as percent elongation and formability. For all bainite hold temperatures, the retained austenite volume percentage increases to a peak at around 100 seconds and then decreases slowly with longer hold times. For short hold times, there is not enough time for the bainite to fully grow into the austenite and not enough carbon will partition into the austenite to stabilize it. As the bainite hold time increases, progressively more and more of the austenite will be stabilized by carbon partitioned from the growing bainite until the bainite transformation completes. At some point the volume percent of austenite retained at room temperature reaches a maximum. Beyond this critical point, longer bainite hold times cause the carbon-rich austenite to decompose into cementite and ferrite. This reaction usually accompanies the bainite transformation, but it is delayed in TRIP steels through the addition of silicon which is highly insoluble in cementite and must diuse away before the cementite can grow. The retained austenite curves seen for both the equiaxed and lamellar microstructures follow this expected pattern. The increase in austenite content with bainite hold time is much more rapid than the decrease at longer hold times. This dierence occurs because the formation of bainite is a very fast, short range reaction while the diusion of silicon and the formation of carbides are much slower processes. The lamellar samples achieved a much lower maximum volume percent retained austenite than the equiaxed samples. This may be due to the geometric constraints on the formation of bainite in the thin lamellar grains of austenite. The growth of bainite can be restricted by grain size, with smaller grains producing higher nucleation rates but slower growth rates and nal volume fractions [12].

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5.2.4

Temperature and Heating Rate Dependance of Microstructure

Not only does the temperature of the bainite hold aect the volume fraction of retained austenite, but the cooling rate in transferring the sample from the inter-critical hold to the bainite temperature can also have an impact. Faster cooling rates generally produce larger volume fractions of retained austenite as shown by Traint et al.[14]. Dierences were found in the peak volume percent of retained austenite produced in the equiaxed samples of dierent geometries. The smallest A-series heat treatment coupons showed the largest peak volume percent (14.6 vol.%), followed by the TE series tensile samples (14.0 vol.%) and the IE series IPPS samples (11.4 vol.%). These dierences could be due to the variation in the cooling rate between the sample groups. The 101.6 mm salt-pot used for the bainite hold time is small enough that the dierence in size between the A series and the IE series samples could cause a signicant dierence in the sample cooling rate. This dierence could be conrmed by measuring the cooling rate for an IPPS sample immersed in the salt-pot, and comparing this to the rate of measured for the tensile samples. The heat treatment of the lamellar samples did not show this same reduction in volume percent of retained austenite with increasing coupon size. The lamellar samples generally exhibit less sensitivity to bainite hold times, as seen in Figure 4.10, with the volume percent peak changing less sharply as a function of bainite hold time when compared to the equiaxed results in Figure 4.8 and Figure 4.3. Hence, the lamellar IPPS samples had a higher volume percent of retained austenite than the equiaxed samples, despite having lower volume percentages when comparing the tensile samples. This resulted in the IL series samples having a higher volume percent of retained austenite than any of the IE series samples, which prevented the IPPS results from being directly compared with each other.

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5.3
5.3.1

Role of Retained Austenite in Formability

Retained Austenite in Uniaxial Tension

The presence of retained austenite has a great positive inuence on the mechanical properties of the TRIP steels both for the equiaxed and lamellar structures. The strain at UTS increased with increasing levels of retained austenite, indicating that higher volume percentages of retained austenite delay the onset of diuse necking, and can improve the formability of the steels. For both the equiaxed and lamellar structures the samples with the maximum volume percentages of retained austenite showed the greatest strain at UTS of all the samples in the series. This result agrees with the general results in the eld, as summarized by DeCooman et al. [9] and Jacques et al. [12]. Improved mechanical properties of TRIP steels with increasing volume percent of retained austenite are explained by the increased, and sustained material hardening that accompanies the austenite-to-martensite transformation.

5.3.2

Eect of Retained Austenite on Material Hardening

It was seen from the instantaneous n curves that the steel samples with the highest volume percent retained austenite displayed the most sustained hardening behaviour. This was seen for both the equiaxed and the lamellar microstructures, despite the fact that these steels showed very dierent hardening behaviour. For both microstructures the samples with more retained austenite did not have the highest peak instantaneous n values, but they remained higher than the other samples at higher strains. It was expected that the presence of greater volume percents retained austenite in the microstructure of these steels would give them better sustained hardening properties. Steel samples with shorter or longer bainite hold times posses a lower volume percent retained austenite and it is assumed that this austenite is also less stable due to a lower carbon content, either from an incomplete bainite reaction with shorter

Discussion

110

bainite hold times or from the formation of carbides with longer hold times. The samples therefore not only have less retained austenite available to harden the material, but this austenite will probably transform at lower strains, reducing the sustained hardening behaviour of the material. The instantaneous n curves, especially for the equiaxed samples, did not match very well with other published curves such as those presented by Keeler [4] and Jacques et al. [42]. The instantaneous n values were higher initially, but did not show the almost-horizontal prole of a TRIP steel with good sustained hardening. This discrepancy is most likely due to the fact that the TRIP steels in this study have been designed to have large volume percents retained austenite, not optimized for their mechanical properties, and so do not display the exceptional properties seen in studies of more intensely developed steels. The largest dierence between the steels in this study and those produced elsewhere is the relatively high bainite hold temperature of this study. This temperature was chosen as it produces larger volume percents retained austenite, but this retained austenite has a lower carbon content and is therefore less stable. The high initial hardening rates seen in this study are likely due to the early transformation of much of the retained austenite. This would produce a large initial hardening rate, but would decay quickly, like those seen in this study. As this hardening mechanism is exhausted the resulting microstructure is close to that of a dual-phase steel, and would produced a similar hardening prole.

5.3.3

Retained Austenite in IPPS

The volume percent of retained austenite in the samples was also found to have a large eect on the local necking behavior of the sheet when deformed under in-plane plane-strain. As illustrated in Figure 4.15, samples with increasing levels of retained austenite also show an increase in their resistance to local necking, as measured by

Discussion

111

the local strain achieved before reaching the comparative forming limit. This result was expected as the increase in hardening rate and specic volume that accompany the TRIP transformation will improve the steels ability to resist the localization of incipient necks. While only one set of heat treatments were performed for the lamellar microstructure, it is assumed that the high comparative forming limits for these samples are partly due to the microstructure of the steel and partly due to the high level of retained austenite in the samples. It is expected that the comparative forming limits of the lamellar samples would vary directly with the volume fraction of retained austenite in the sample.

5.4

Aect of Phase Morphology on Performance of TRIP Steel

5.4.1

Dierences in Morphology

The purpose of the lamellar and equiaxed heat treatments was to produce two steel samples with substantially dierent morphologies of retained austenite, while leaving the surrounding matrix relatively unchanged. In many ways the heat treatments were a sucess; the austenite, while appearing in similar volume percentages, has an elongated lamellar structure as opposed to the small equiaxed grains found in the other series. The composition of the surrounding matrix is also believed to contain a similar mixture of inter-critical ferrite and bainite as the chemistries, inter-critical hold and bainite holds are identical for the two sample groups. These surrounding phases also dier in their morphology, which is an unfortunate result of the processing required to alter the retained austenite. The ferrite/bainite phases in the equiaxed samples are large, simple equiaxed grains, whereas in the lamellar samples they have a much more complex structure. The ferrite/bainite phase in the lamellar samples

Discussion

112

retains the shape of the initial martensite plates, but these plates are further broken into sub-grains as evidenced by the position of the austenite/martensite grains in the micrographs, and also shown by Mark [5] where a TEM analysis was performed on a similar lamellar structure. The higher yield stress of the lamellar structure may be due to the grain renement caused by the matrix being composed of thin grains of ferrite/bainite with a complex sub-grain structure. The morphology of the surrounding matrix can also impact how the austenite deforms, transforms and yields which, in turn, changes the mechanical and formability properties of the steel.

5.4.2

Dierences in Mechanical Properties

There are several major dierences seen in the mechanical properties of the lamellar and equiaxed microstructures as evident in their stress-strain curves. The lamellar structure has a signicantly higher yield strength than any of the equiaxed samples, which is probably due to the grain renement discussed in Section 5.4.1. The lamellar samples also exhibit higher strain at UTS than the equiaxed samples, albeit with lower UTS values. Similar results were reported by Sugimoto et al. [6] where TRIP steels with lamellar, equiaxed and bainitic structures were compared. The increased elongation at UTS found for the lamellar structure is attributed to the increased stability and sustained transformation of the retained austenite leading to a higher sustained hardening. The lower UTS of the lamellar structure is mentioned, in that the lamellar steels have a much higher ratio between the yield strength and the UTS, as observed in this study; however, no explanation is oered. The lower UTS in the lamellar samples is certainly due in part to their low rates of initial hardening. Although these samples have better sustained hardening they never achieve the same UTS as the equiaxed samples. This lower initial hardening rate can also be related to the greater stability of the retained austenite in the lamellar structure.

Discussion

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5.4.3

Dierences in Hardening Behavior

The equiaxed and lamellar microstructures showed very dierent hardening behaviours, as seen from the dierences in their instantaneous n curves. The equiaxed samples showed much greater initial hardening rates than the lamellar samples, but these decayed more quickly, leaving the steel with much less sustained hardening. It is thought that this dierence is tied to the stability of the retained austenite in the steel. The equiaxed samples show a behaviour that would be expected if the austenite transformed in the rst part of the tensile test, leaving less hardening available for higher strains. The lamellar sample on the other hand shows evidence of a much more constant hardening through the test with instantaneous n values which are sustained to much higher strains. The supposed dierence in the stability of the austenite could be due to several factors. Firstly the thin plates of austenite seen in the lamellar structure require higher stresses and strains in order to transform due to the geometric constraints placed on the grains as discussed by Sugimoto et al. [6] and Mark [5]. The austenite stability might also be higher due to higher chemical stability. As lower levels of retained austenite were found in the lamellar samples it is possible that this austenite contains more carbon than that of the equiaxed microstructure. A nal possiblity is that the matrix which surrounds the austenite is stronger in the lamellar structure and so is shielding the austenite from stress and making it seem to have a higher apparent stability as discussed in [42]. This may be due to the structure of the ferrite grains which was described by Mark [5] as being highly disordered and contain sub-grains which form through the annealing of the martensite.

5.4.4

Dierences in IPPS

In addition to the dierences in uniaxial tensile properties and hardening behaviour, the lamellar structure showed superior forming properties in testing under IPPS. The performance of the TRIP steels under this strain path is very important as it

Discussion

114

typically represents the strain path with the lowest resistance to necking. The lamellar samples tested in this study exhibited a much higher resistance to local necking, as measured by the comparative forming limits. These increases in forming limits are also accompanied by larger volume percents of retained austenite; however, it is not entirely clear if the superior formability is due to the dierent phase morphology, and not simply due to the higher volume percent of retained austenite. If the IPPS forming limit of the TRIP steel varies linearly with volume percent of retained austenite, then the lamellar samples lie clearly above this trend. Any possible improvement in the IPPS behaviour of the steel due to the phase morphology would be much easier to discern if the two sample groups contained comparable volume percentages of retained austenite. The IPPS strain path is especially important for TRIP steels as the transformation of retained austenite and its associated volume increase is aected by the applied strain. The IPPS strain path allows more freedom for the volume increase than the uniaxial tensile path and so the transformation of austenite to martensite may progress more rapidly [17]. Given that austenite is assumed to be much more stable in the lamellar microstructure, the improvements seen in the IPPS test results could be explained by the more gradual transformation of the austenite, which leads to better sustained hardening. The improved IPPS formability for the lamellar structure is consistant with the work of Sugimoto that investigated the formability of lamellar TRIP steels [6].

Chapter 6

Conclusions and Recommendations

6.1
6.1.1

Conclusions
Microstructure

In this study, two very dierent morphologies of retained austenite (equiaxed and lamellar) were produced from a common TRIP steel chemistry, surrounded by intercritical and bainitic ferrite. The surrounding matrix in both microstructures were similar in composition and volume percent, allowing the eects of the volume percent and morphology of the austenite phase to be examined. The lamellar microstructure was based on the work of Mark [5] and Sugimoto [6]. For both austenite morphologies the inuence of the bainite hold time and volume percent retained austenite were studied. The volume fraction retained austenite is a very important factor inuencing the mechanical properties of a TRIP steel. A simple process of varying volume fraction of retained austenite was used. By varying the bainite hold times of the samples the volume fraction retained austenite was seen to increase to a peak with short bainite hold times and then decay with longer hold times. The presence and position of this peak were very close to previous work in the eld and matched well with theory. The equiaxed structure showed the highest volume fraction of retained austenite, above 14 vol.%, but this high value drops o quickly with shorter or longer hold times. The lamellar structure had a lower peak measured volume fraction of retained austenite, but this peak was less sensitive

115

Conclusions and Recommendations

116

to variation in bainite hold time. The lamellar structure also seemed to be less sensitive to changes in cooling rates, as the tensile and IPPS geometries showed identical volume percents retained austenite, whereas large dierences were seen for the equiaxed microstructure.

6.1.2

Mechanical Properties

Both of the austenite morphologies produced in this study displayed good mechanical properties, with ultimate tensile strengths above 700 MPa and strains at UTS over 20 %. The two steels, however, behaved markedly dierent from one another. The lamellar structure showed a much higher yield strength, but did not reach the same high UTS as the equiaxed steel. The lamellar structure also showed slightly better strain at UTS values. The strain at UTS shown for both steel structures was tied very closely to the volume fraction of retained austenite in the steels. The instantaneous n values of the equiaxed samples reached very high initial values, but then decayed very quickly and did not show the sustained hardening expected for TRIP steels. The lamellar samples showed better sustained hardening, with lower peak hardening rates and a much more gradual decay in the instantaneous n values. For both the equiaxed and the lamellar microstructures the instantaneous n values were sustained to greater strains in the samples with higher volume percents of retained austenite. The IPPS testing of the two structures also showed a very strong relationship between the strain at the onset of local necking in the samples and the volume percent retained austenite. The samples in the lamellar series, while having higher volume fractions retained austenite seemed to perform better under IPPS than the equiaxed samples would at this level of RA. A direct comparison of these two microstructures at the exact same level of retained austenite would make this dierence clearer.

Conclusions and Recommendations

117

6.1.3

Characterization

X-ray diraction was used as a characterization technique in this study to both determine the volume percent and carbon content of the retained austenite phase. There were signicant problems found with the X-ray diraction method in terms of the measurement of volume fraction. It was found that the retained austenite was being transformed during the sample preparation, possibly through grinding, but more likely through cooling the samples for electro-polishing. This result, along with the relatively onerous sample preparation, led to the selection of the magnetic method as the main austenite characterization technique in this study.

6.2

Recommendations

While the ndings of this thesis provide further insight into the relationship between the retained austenite phase and the formability of these TRIP steel sheet, further research is needed. For example, this study demonstrated that the two morphologies of retained austenite, with similar volume percents, could exhibit very dierent mechanical properties. Hence, a followup study could be undertaken to optimize the lamellar microstructure for its forming properties. Much work has already been done to improve the mechanical properties of the more traditional equiaxed microstructure. Improvements in the lamellar structure may be accomplished by altering the chemistry and/or the processing times and temperatures of the processing; an investigation of lower bainite hold temperatures would be the best starting point. In order for TRIP steels to be used in automotive applications they must be suitable for galvanizing, so low silicon alternative chemistries should also be examined, such as those containing aluminum and phosphorus.

Conclusions and Recommendations

118

6.2.1

Microstructure

In this study the main objective in producing both the equiaxed and lamellar structures was to maximize the volume percent retained austenite in the structures. It is likely that better mechanical properties would have been observed if the steel contained smaller volume percents of more stable retained austenite, produced through lower bainite hold temperatures. It can be seen from the instantaneous n curves that there is very little sustained hardening. While it is still useful to compare the two structures with their high levels of retained austenite, it would have been more benecial to compare the two structures in their most formable state with more stable austenite.

6.2.2

Mechanical Properties

Further work is required to better understand the mechanical properties of the different forms of TRIP steels, and to get a better understanding of how dierent morphologies of retained austenite behave under dierent strain paths. In-situ neutron diraction could be employed for this purpose, as utilized in studies by Mark [5] and Jacques et al. [17]. This would provide a wealth of information not only about the transformation of the retained austenite during loading, but also the micro-mechanical stress state that each phase is subjected to. Such a study would allow the researcher to study the amount and type of retained austenite that transforms as the material is deformed along dierent applied strain paths such as uniaxial tension and IPPS.

6.2.3

Characterization

The magnetic testing performed in this study proved to be a very accurate bulk measure of retained austenite which is simple to prepare and perform. Some problems with the system remain in the measurement of low volume fractions of RA; however,

Conclusions and Recommendations

119

it is believed that this is a result of the curve-tting performed with the samples. If a larger magnetic eld were used, up to 4 KOer, it would eliminate the need for curve-tting, along with the errors associated with low volume percent measurements. Optical analysis of the samples was eective in revealing the size and morphology of the retained austenite and the surrounding phases. More extensive characterization of the size and shape of the phases could be performed through SEM or TEM. This would better dene the shape and position of each phase within the microstructure which would both better characterize the dierences in morphology and improve the microstructural development through the heat-treatment schedule. If X-ray diraction is used with TRIP steels care must be taken to preserve the meta-stable austenite through the surface preparation of the sample. Care should be taken grinding the samples and the samples should never be cooled below room temperature for any reason as this will cause at least some of the retained austenite to transform.

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