6. 10. ie Te 3g42-S Stellingen behorende bij het proefschrift “{ntercritical deformation of low-alloy steels” Andre Bodin De voorspellende waarde van simpele mengregels voor het constitutief gedrag van een tweefasenstructuur neemt af met een toenemend verschil in constitutief gedrag tussen beide fasen. Het gebruik van het Speich-Fisher model voor de beschti verdient de voorkeur boven het gangbare Avrami model fing van de reksistallisatic van staal De EBSD-technick in combinatie met OIM is bij miccostructauronderzock onmisbaar geworden. : In die gevallen waarin begrip van de onderliggende processen belangrijker is dan een 20 Klein mogelijke fout in de voorspelling, verdient een fysisch-metaalkundig model de voorkcur boven zuiver empirische of statistische modellen. Het belang van nauwkeurige en representatieve data uit de industriéle praktijk voor de modelvorming van het productieproces wordt gewoonlik onderschat, net als de grootte van de inspanning die men zich moet getroosten om dergelike data te verksijgen. Rekgeinduceerde precipitatie van NbC in warmgedeformeerd austeniet wordt veroorzaakt door koolstofsegregatie bij de celwanden als gevolg van dynamische veroudeting en niet, zoals recentelijk is gesuggereerd door Liu, door de diffusie van Nb-vacature complexen, Het koolstofsegregatiemechanisme geeft echter geen uitsluitsel over de vraag of de precipitatie oorzaak of gevolg is van de rckristallisatievertraging van warmgedeformeerd austeniet. (WJ. Lin, Mater'Trans.A, 264 (1995), 1641) Een technologische vinding kan op verschillende manieren openbaar worden gemaakt, bijvoorbeeld in een wetenschappelijke publicatic of in een octrooi. De inhoud van deze publicaties is in principe gelijk, in tegenstelling tot de vorm; over de leesbaarheid verschillen de meningen. Het falende Franse militaire leiderschap in 1870 heeft in belangrijke mate bijgedragen aan het creéren van de voorwaarden waaronder de eerste wereldoorlog, mopelik is geworden, en heeft daarmec het verloop van de Europese geschiedenis ingsijpend beinvloed. Het overlevingsinstinct van de mens, met name de drang tot voortplanting en het vergaren van bevit, zal uiteindelifk bijdragen aan de ondergang van de huidige menselijke beschaving, Willem Mengelberg heeft veel betekend voor de ontwikkeling van de uitvoeringspraktijk van klassieke muziek in Nederland cn Europa aan het begin van de twintigste eeuw. Door uitvoering van de muriek van Matthijs Vermeulen te weigeren heeft hij daarentegen de Nederlandse muziekwereld geen dienst bewezen. Het ontstaan van een applaus is cen kiemvorming-en-groeiproces. Dit is het best waar te nemen na afloop van een voor de tochoorders onbekend modern muzickstuk. Bij bekendc muziekstukken is de drijvende kracht 20 hoog dat de incubatietijd vrijwel nul is.10. MW Propositions accompanying the th “Tnterctitical deformation of low-alloy steels” Andre Bodin The predictive value of simple rules of mixtures for the constitutive behaviour of a two-phase structure decreases with an increasing difference in constitutive behaviour between both phases. ‘The use of the Speich-Fisher model for the recrystallisation of steel is preferable over the commonly used Avrami-model. The EBSD-technique in combination with OIM has become essential to microstructural research. In those cases where understanding of the underlying process is more important than minimising the error in the prediction, a physical-metallurgical model should be preferred over a purely empirical or statistical model. ‘The importance of accurate and representative data from industrial practice for modelling of the production process is usually underestimated, as well as the effort required to obtain these data. Strain-induced precipitation of NbC in hot-deformed austenite is caused by segregation of carbon to the cell walls due to dynamic ageing and not, as recently suggested by Liu, by diffusion of Nb-vacancy complexes. The carbon segregation mechanism does not answer the question whether the precipitation causes the retardation of recrystallisation of hot-deformed austenite ot whether it is a consequence thereof. (WJ. Liu, Mater-Trans.A, 26A (1995), 1641) A technological discovery can be made public in several ways, for example in a scientific paper or in a patent. While the content of these publications is essentially similar, and the form is not, opinions about their readability differ. The failing French military command in 1870 has contributed significantly to the creation of the conditions in which the First World War became possible. This way it influenced the course of European history radically. The human survival instinct, particularly the urge for reproduction and accumulation of property, will ultimately contribute to the downfall of the current human civilisation. Willem Mengelberg has played an important tole in the development of the performance practice of classical music in the Netherlands and Europe in the first decades of the twentieth century. However, by refusing to perform the music of Matthijs Vermeulen, he did the Dutch musical scene a strong disservice, The formation of applause is a nucteation-and-growth process. ‘This can best be observed after a performance of an unknown modern composition. The driving force after a well-known composition is so high that the incubation time is virtually zero.Bb Tr gue Intercritical deformation of low-alloy steelsTitle: Author: ISBN: Copyright: Printed by: Corus by Night: Intercritical deformation of low-alloy steels Proefschrift, Technische Universiteit Delft, Nederland A. Bodin 90-805661-2-8 Corus Technology BV Grafisch Bedeijf Ponsen & Looijen BV Fotostudio Fix, Beverwijk. All sights reserved. No past of the material protected by this copyright notice may be reproduced in any form of by any means without written permission from the author.Intercritical deformation of low-alloy steels Proefschrift ter verkrijging van de graad van doctor aan de ‘Technische Universiteit Delfi, op gezag van de Rector Magnificus prof.dr:ir. JT. Fokkema, voorzitter van het College voor Promoties, in het openbaar te verdedigen op dinsdag 5 november 2002 om 13.30 uur door Andre Bodin materiaalkundig ingenieur geboren te GroedeDit proefichrift is goedgekeurd door de promotor: Profdrir. S. van der Zwaag ‘Toegevoegd promotor: Dri. J. Sietsma Samenstelling promotiecommissie: Rector Magnificus, voorzitter Profidriir. S. van der Zwaag, Technische Universiteit Delft, promotor Dr.ir. J. Sietsma, Technische Universiteit Delft, toegevoegd promotor Profdr. J. H. Beynon, University of Sheffield (United Kingdom) Prof.dr.ir. L. Kestens, Rijksuniversiteit Gent (Belgié) Prof.dr. LM. Richardson, Technische Universiteit Delft Prof.dr. R. Boom, Technische Universiteit Delft Dr. E, Aeby-Gautier, [icole des Mines de Nancy (France) ‘The research in this thesis was sponsored by Corus Research, Development & Technology. ISBN 90-805661-2-8 Printed in the NetherlandsNum achte wobl, und lass mich seh'n bist du ein Tor und rein, welch Wissen dir auch mag beschieden sein, Richard Wagner Voor OpoeCONTENTS INTRODUCTION ut 12 13 14 SCOPE OF THE THESIS DEVELOPMENTS IN THE STFEI. INDUSTRY: FACILITIES 1.2.1 Conventional production facilities 1.22. Thin-slab casting and disect roling INTERCRITICAL ROLLING OUTLINE ‘THEORETICAL BACKGROUND 24 22 23 28 INTRODUCTION WORK-HARDENING .AND SOFTENING DURING HOT-ROLLING WORK-HARDENING FOR SINGLP-PHASE SYSTEMS 23.1 Work hypothesis 23.2 Ludwik-Hollomon model 23.3 Bergstrém model SOFTENING 24.1 Introduction 24.2 Dynamic recrystallisation 243° Static recovery 244 Static recrystallisation BACKGROUNDS OF METHODS TO QUANTIFY SOFTENING Introduction, Double-hit uni-axial compression experiments Conventional methods to determine fractional softening Dislocation balance method Discussion Stress-relaxation experiments OSTRUCTURE 26-1 Austenite-ferrite two-phase region in iron-carbon alloys 2.6.2 Chatacterisation of two-phase systems 2.63 Mixture rules CRYSTALLOGRAPHIC TEXTURE, 27.1 General 27.2 Representation of texture 3 Texture development in austenite 274 ‘Transformation texrure 2.7.5 Texture development during intercrtieal rolling 2.7.6 Texture development by seceystallisation of ferrite ‘THE RESEARCH QUESTION EXPERIMENTAL 3a 32 33 34 INTRODUCTION MATERIALS 1 Chemical composition 3.22 Sample preparation 3.2.3. \ustenite fraction PILOT-MILL ROLLING EXPERIMENTS 33.1 Rolling schedule 33.2 Determination of mean flow stecss DILATOMETRY AND UNI-AXTAT. COMPRESSION 34.1 Dilatometry 34.2 Unicaxial compression experiments 3.43. Double-hit compression experiments 3.44 Stress-rclaxation experiments PINITE ELEMENT SIMULATIONS PERIMENTS, i ul ul u 12 14 5 17 v 18 19 19 19 19 2B B 24 26 2 29 29 30. 31 33 34 35 36 36 37 38 42. 42 42 a 44 45 45 47 "7 Pe 7 48 48 9 49 Li 31 St 53 35 56 373.5.1 Finite element modelling versus model alloys 3.5.2. Simulation details 3.53. Contiguity and friction 36 ARTIFICIAL NEURAL NETWORK 3.6.1 Introduction 3.6.2 Modelling of intercritical deformation using artificial neural networks 3.7 MICROSTRUCTURAL CHARACTERISATION 3.7.1 Metallography 3.7.2 Scanning Blectron Microscopy 3.8 TEXTURE 3.81 Orientation distribution function 3.82 In-situ high-temperature X-ray diffraction experiments 3.83. Electron Back-Scattering Diffraction WORK-HARDENING 41 INTRODUCTION 42 FLOW STRESS 4.2.1. Deformation dilatometry 422. Pilot hot-rolling 43 MODELLING OF WORK-HARDENING, 43.1 Ludwik Hollomon model 43.2. Bergstrém model 43.3 Comparison of Ludwik-Follomon model to Bergstrém model 44 ARTIFICIAT NEURAL NETWORKS 44.1 Modelling the influence of strain rate 44.2 Modelling the influence of the chemical composition 45. HYBRID MODFLLING 45.1 Introductio 45.2 ANN for Qand ¥ 453 Discussion 46. FINITE ELEMENT SIMULATIONS 4.6.1 Work-hardening model for FE-simulations 4.6.2. Influence of contiguity 4.7 CONCLUSIONS SOFTENING 34 INTRODUCTION 5.2 MODEL SIMULATIONS OF SOFTENING VERSUS FRACTION RECRYSTALLISED, 5.2.1 Aim of the simulations 5.2.2 Results of simulations 53. DOUBLE-HIT COMPRESSION EXPERIMENTS 53.1 Results 53.2 Discussion of results 54 STRESS-RELAXATION EXPERIMENTS, 5.5 COMPARISON OF DOUBLE-HIT COMPRESSION TO STRESS. RELAXATION METHOD 5.6 CONCLUSIONS HIGH-TEMPERATURE X-RAY DIFFRACTION, 6.1 INTRODUCTION 6.2 SLOW COOLING 6.3 SLOW HRATING 64 CONCLUSIONS MICROSTRUCTURE AND CRYSTALLOGRAPHIC TEXTURE 7.1 INTRODUCTION 7.2 PILOT HOT-ROLLING: MICROSTRUCTURE 7.21 Optical Microscopy 722 Scanning Electron Microscopy of CMn-steel 7.23. EBSD-Orientation Image Mapping of CMa-steel 73. CRYSTALLOGRAPHIC TEXTURE: RESULTS 7.3.1 Initial texture of the semi-finished samples 37 58 59, ot 61 6 68 6 6 64 64 64 66 69 Co 9 69 B 9 1» 83 87 88 88 88 89 89 89 92 95, 07 98 98 98 101 101 105 107 Tt us 117 7 7 123 127 129 129 130 130 133, 134 138 1387.3.2 Diffect of thermal path prior to finish rolling (schedule R). 7.3.3. Texture after accelerated cooling after austenttic rolling (schedule AC), 734 KLC: schedules Q and C 735 Rested whedides Qand C 736 73.7 CMa-steel cao Qand ¢ 74 CRYSTALLOGRAPHIC TEXTURE: DISCUSSION 7.4.1 Schedule R: quenching prior 10 finish rolling 742 Schedule AC: accelerated cooling after austenitic rolling 743. Schedule Q: quenching after finish-rolling 744 Schedule C: coiling after Gnish rolling 7.3 GENERAL DISCUSSION 7.5.1 Carbon steels: austenitic deformation 75.2. Carbon steels: intercritical deformation 753. Carbon stecls:ferrtic deformation 754 TF-steel 755 1.C-siccls: cementite morphology 7.5.6 Microstructure: recrystalisation nucleation and grain growth of fertite 7.5.7 Influence of catbor on microstructure and texture 16 1 SUMMARY SAMENVATTING SOAMEVATTIENG IN‘T WEST ZJIWS-VLAOMS DANKWOORD LIST OF PUBLICATIONS CURRICULUM VITAE REFERENCES LIST OF FREQUENTLY USED SYMBOLS AND ABBREVIATIONS APPENDIX A: GENERAL PRINCIPLES OF GROWTH AND NUCLEATION MODELS APPENDIX B: FE-MESHES FOR THE COMPUTER GENERATED MICROSTRUCTURES 139 140 141 142 143, 143. 144 145 145 147 147 147 149 149 149 150 151 152 152 155 161 167 169 m 173 175 179 181 18510Derriére les ennuis et les vastes chagrin Qui chargent de leur poids existence brumeuse, Heurcux eclui qui peut d'une aile vigoureuse S’alancer vers les champs lumineux et sereins. Charles Baudelaire 1 Introduction 1.1 Scope of the thesis In conventional low-alloy steel production, steel is hot-rolled entifely in the austenitic stare. Shifting the rolling-temperature to values in the intercritical region could open new possibilities for process and product development. In order to benefit fully from the possible advantages of intercritical rolling, a number of metallurgical issues need to be understood. It is the purpose of this thesis to contribute to the understanding of the development of microstructure and crystallographic texture during and after deformation in the intercritical region of low-carbon steels, Because of the limited availability of relevant information in the literature, a broad approach was considered appropriate. strip casting soaking & reheating @ 5 2 thin slab casting z 2 > conventional § 3 i dS 3 3 le 2 Bo . as ° so 100150200 annual capacity [Mv] casting thickness [mm Fig. 1-3. Capital cost of casting and rolling Fig. 1-4. Energy consumption per ton as a facilties per ton of capacity (normalised 10 function of casting thickness. the costs of 5 Mv). than a typical hot-strip mill despite the 310 m long soaking furnace. ‘The advantages of a thin-slab caster (TSC), as far as capital costs are concerned, are obvious. Fig, 1.3 compares the capital costs per ton of produced steel in strip casting and thin slab casting to that of an integrated production facility of 5 Mt/a [1]. However, the i stallations have a relatively low ptoduction capacity in comparison to conventional hot-strip mills. In thin-slab casting and direct rolling, the reheating furnace is omitted from the production process resulting in significantly lower energy consumption (see Fig. 1-4). Thin-slab casting and direct rolling results in the lowest energy consumption. Because of the highcr surface area, the energy losses in thin. slab casting or strip-casting increase with decreasing thickness of the cast slab or strip. Another significant cost reduction results from the reduction in staff required for operating a thin-slab casting and direct rolling facility as compared to a thick-slab caster and hot-rolling mill. This implies that the productivity per capita increases. From Fig, 1-3 and Fig, 1-4 it appears thar thin-slab casting and direct rolling is an interesting alternative to the conventional process, both from a perspective of capital costs and operational costs. The capital costs of strip-casting facilities are even lower, but at present these facilities are unable to produce high-quality low-alloy steels. The concept of strip-casting is not easy to scale up and combine economically with conventional steel plants. It appears that strip-casting is currently more suited for niche markets with relatively small amounts of highly alloyed steels (c.g. G%silicon steels or stainless steels). Kor production of large quantities of high quality conventional low-carbon steel grades a thin-slab caster would be more appropriate. ‘The good temperature homogeneity of the slab after the homogenisation furnace makes it jon between austenite to ferrite, the intercritical region. Although intercritical rolling is a well-known suitable for the production of steels where temperature control is vital: the trans production method in plate rolling, where it is a consequence of the production process rather than the objective, it is the temperature homogeneity of the TSC that opens a window to intercritical rolling s a means to obtain interesting mechanical properties {2],13]. However, in osder to be able to benefit fully from these new potential process routes, a number of issues in the physical metallurgy of intercritical deformation have to be addressed. Production aspects like 13work-hardening during deformation, G ee and softening during and after Y Ze deformation have to be addressed as Ho Ay HFeC well as product aspects like ‘i 727 |a WY A, eon microstructure, crystallographic P $ texture and mechanical properties. os 1.3 Intercritical rolling FR ree After leaving the — slab-reheating Q $$$ furnace, the slab starts to cool down. 008 08 8 In the conventional _hot-rolling wt.% Carbon Process, the strip has to be finish fg 4.5. ron-Carbon binary phaso diagram. rolled while still in the austenitic state, ive. the temperature of the strip may not decrease below Ar, If the final strip thickness is small, the surface of the strip is large and hence the heat loss duting the finish-rolling process increases. ‘The reheating temperature cannot be increased without limit because of the formation of low melting point compounds at high rcheating temperatures. As a result, the trend to produce thinner hot strip on conventional hot-strip mills necessitates leaving the concept of full austenitic finishing and adopting the concept of fetritic or intercritical rolling. Ferritic rolling is defined as hot-rolling of a ferritic steel. Strictly speaking, this means that for steels with carbon contents below 0.02% the minimum finishing temperature depends on the carbon content and above 0.02% is given by A, (see Fig. 1-5). However, finish rolling in ‘the lower part’ of the (++Y)-region is usually also referred to as ferritic rolling. For reasons of clarity, in this thesis the term fertitic rolling or deformation will be used for full-fertitic deformation, austenitic deformation for full austenitic deformation, and intercritical deformation for all intermediate deformation conditions. During fettitic ot intercritical rolling, the phase transformation from austenite to ferrite starts between casting of the thin-slab or reheating of the thick-slab and finish rolling of the strip. This implies that, at least during some part of the process, the deformation of the sttip is performed concurrently with the transformation of austenite to ferrite. The transformation is known to influence the deformation resistance of the steel [1]. The thickness performance of industrial hot rolling largely depends on the ability to predict the deformation resistance [4]. It is also known that uncontrolled rolling in the intercritical region leads to undesirable product properties 2}, [5]. In plate mills, rolling in the intercritical region is used for production of high-strength stecls, mainly high-strength, low-alloy (FISLA) stecls. This results in high-strength and weldable steels with good toughness values. Interctitical rolling of high-strength steels is not a common practice in hot-strip mills. To apply this technique in the strip mill, several aspects of production and product have to be clarified. In a conventional hot strip mill (ie. without a coil-box) the temperature distribution over the strip length is considered too variable for controlled intercritical rolling. However, in a TSC with its long soaking furnace (see Fig. 1-2) the temperature is homogenised over the length and width of the strip prior to rolling. The homogeneous temperature distribution should prevent 1414 13 12 14 normalised Fy, 10 09, to 100 0.1 02 03 04 05 08 07 08 09 10 1.50 1.28 1.00 075 oso normalised property 025 0.00 0 04 02 03 04 05 06 07 08 09 10 % 25 °). -o- normalised property a 10 00 0.1 02 03 04 08 06 O7 08 08 1.0 My Fig. 1-6. Effect of thermal path after intercritical rolling - (a). normalised tensile strength (Rn) of IF- and LC-steel; (b) fraction recrystallised and normalised tensile strength; (c). normalised tensile strength and yield strength (F,), all as function of normalised strip length (6) 7] differences in fraction transformed over the width of the strip from occurring. One could therefore assume that it is more likely that intercritical rolling, could be applied in a TSC rather than in a conventional hot-strip mill. One of the practical problems in applying intercritical rolling is the yield of hot-rolled coils. Because of inhomogeneous cooling of a coil, the thermal path of a given part of the strip depends on its location in the coil. Head and tail ends as well as edges of the strip cool more rapidly than the centre of the coil. In a series of full-scale production tials, the sensitivity of the mechanical properties to the thermal path has been assessed [6],{7]. When using a constant coiling temperature, the difference in behaviour between the IF- and LC-steel is clearly visible. From Fig. 1-6a it appears that about 10% of the tail and head end of the IF-steel show a considerable strength (R,) as compared to the middle of the strip. The LC strip shows a similar behaviour but the difference between head and body is much smaller (less than 10% increase in R,) as compared to the IF steel (up to 40% increase at head end and 20% at tail end). From Fig. 1-6b the correlation between R,, and the fraction recrystallised ferrite is obvious deviation in tensile Therefore, controlling the softening, behaviour means controlling the mechanical properties. It should be noted that the effect on yield strength (R,) is even larger (see Fig, 1-6c) indicating that there is an additional contribution to the inhomogeneity of R, of the different thermal paths during coil cooling, possibly as a result of precipitation of interstitial elements. 1.4 Outline In chapter 2 the metallurgical backgrounds of deformation in the intercritical region and subsequent softening are discussed. Particular attention is paid to the development of microstructure and crystallographic texture as both have a significant influence on the final mechanical properties of the material. ‘The microstructure, and particularly the distribution ofphascs, also influences the properties of the steel during processing. The concept of contiguit introduced to explain the behaviour of two-phase materials during deformation. Chapter 3 concentrates on the experimental part of the study and introduces the main assumptions as well as the general aspects of the experimental techniques. In order to study the deformation behaviour in more detail and under equilibrium conditions, single-hit compression experiments were performed in a deformation-dilatometer. Chapter 4 shows the results of fitting the deformation data to Bergstrém’s work-hardening model. This model serves as a virtual model alloy and is used in finite element calculations. In a multi-pass industrial rolling process, work- hardening and softening processes occur simultaneously. The predictive capability of the Bergstrém model is compared to that of Artificial Neural Networks (ANN) and to that of a so- called hybrid model, which is @ combination of a physically based metallurgical model and a neural network. Softening may occur either duting deformation (dynamic softening) ot after deformation (static softening). Quantitative information on static softening is considered crucial in rolling models to predict rolling forces, and in mictostructure models. Chapter 5 presents the tesults of double-hit uni-axial compression experiments and stress-rclaxation experiments to determine the static softening behaviour along with the results of model simulations. ‘The texture development during the phase transformation ftom austenite to ferrite was studied using the in-situ high-temperature X-ray diffraction technique (in-situ HT-XRD). Chapter 6 discusses the results of this study. Hot- rolling experiments wete performed on the pilot-mill of Corus Research, Development and Technology (CRD&') and these experiments yicld the majotity of the microstructure and texture data. Additional information regarding the microstructural and texture development was obtained by scanning electron microscopy (SEM) and Electron Back-Scattering Diffraction (EBSD) measurements. Chapter 7 discusses these experiments and results. 16Questo desiderio di semplificazione é piustficato, la semplificazione non sempre lo é. Eun ipotesi di lavoro, utile in quanto sia riconosciuta come tale € non scambiata per l reali; la maggior parte dei fenomeni storie naturali non sono semplici, o non semplici della semplicita che piacesebbe a noi Primo Levi 2 O 2 Theoretical Background 2.1 Introduction This chapter discusses the different metallurgical phenomena in more detail, explains their relevance for intercritical deformation and gives the background of several experimental techniqnes that will be used in this study. In a multi-pass rolling process, work-hardening and softening processes occur simultaneously. Plastic deformation leads to the formation of dislocations. The dislocation density of annealed metals is reported to be between 10” and 10 m*, whereas deformed metals have a dislocation density of between 10” and 10" m* [8]. The distribution of the dislocations is not homogeneous [2]. ‘There are pile-ups against obstacles, tangles, and diffuse sub-grain boundaries. The intersection of moving dislocations in a slip plane with other mobile or immobile dislocations produces tangled dislocations, which act as a barrier to subsequent dislocation movement. Hence, an extra force is required to continue deformation. Multiple slip, with two or mote slip directio: results in the same effect. Dislocations may move to other slip planes to by-pass the barriers. This is called cross-slip. Work-hardening increases more slowly in materials that allow cross-slip Point defects like vacancies and interstitials are also present in the structure. After and during deformation the dislocation density is reduced by softening processes such as recovery and rectystallisation Since the flow stzess of a material is related to the dislocation density, modelling the flow stress during and after deformation requires modelling of the dislocation density. In the following sections the evolution of the dislocation density during work-hardening and dynamic softening and subsequent static softening is discussed. Kor a complete work-hardening and softening model, five sub-models are requiredwork-hardening (§ 2.3) dynamic recovery (§ 2.3); dynamic recystallisation (§ 2.4.2); static recovery (§ 2.4.3); static reerystallisation (§ 2.4.4) In § 2.5 the different methods to quantify softening are discussed, whereas § 2.6 introduces some typical aspects of the microstructure of a two-phase structure. This chapter concludes with a review of the development of the crystallographic texture during and after hot deformation. 2.2. Work-hardening and softening during hot-rolling In an industrial hot-rolling process, the low-alloy steel is heated into the austenite region (see Fig. 1-5). During the roughing process, the work-hardening is followed by complete softening after each rolling pass. When the material enters the next stand of the roughing mill, the material has undergone complete softening by recrystallisation and recovery. In the conventional process, the ‘material is austenitically deformed throughout the entire finishing process as well, although there may be a point where softening is no longer complete. This retardation of softening can be used to obtain a desirable combination of mechanical properties, particularly in the case of thermomechanical rolling of micro-alloyed stecls [5]. If the retardation of softening can be maintained until the accelerated cooling on the run-out table (see Fig. 1-1 for a schematic representation of a hot-strip mill), thermomechanical rolling will lead to smaller ferrite grain sizes compared to a rolling process where no retardation of softening occurs. The retardation of softening can be stimulated by rolling at low temperatures in the austenite region or by micro- alloying with (e.g) niobium. Depending on the chemistry, the temperature where no softening by austenite recrystallisation occurs (T,) can be as low as the transformation temperature of austenite to ferrite. In that case, no retardation of receystallisation occurs. a. b. c. d. Fig. 2-1. Schematic drawing showing the progress of transformation of austenite to fernte. - (a) Austenite microstructure; (b) Ferrite nuclei form at the comers and boundaries of the austenite grains; (c) The ferrite ‘nuclei grow, possibly with a higher growth rate along the grain boundaries to form a necklace of ferrite grains along the former austenite grain boundaries: (d) The ferrite grains grow. The resulting austenite in the interior of the former austenite grain will eventually transform to pearlte. When the rolling process cannot (cither intentionally or unintentionally) be finished in the single- phase austenite region, the austenite will have started to transform into ferrite before the last deformation. The ferrite will nucleate on the boundaries between the austenite grains and gradually form a network around the austenite grains (see Fig. 2-1) As the ferrite has a different work-hardening and softening behaviour from austenite, this will have a significant effect on the 18behaviour during and after rolling. The microstructure and crystallographic texture will also be affected strongly by the presence of the ferrite during deformation, In some cases, these effects are considered as negative (in the case of low temperature austenitic rolling where abnormal gruin growth occurs as a result of small ferritic deformations), in other cases the intercritical or ferritic deformation can be beneficial (in case of ferritic rolling of IF-steels |10). 2.3, Work-hardening for single-phase systems 2.3.1 Work hypothesis To describe the development of the microstructure of a deformed two-phase structure qualitatively and quantitatively it is important to assess whether or not models describing single- phase behaviour can be used to describe the behaviour of the two-phase structure. If both phases can be modelled independently and subsequently moulded together, the problem will be reduced to determining the distribution of deformation effects over both phases. 2.3.2 Ludwik-Hollomon model ‘The Ludwik-Hollomon model is perhaps the simplest of all deformation models and it is often used as a first approximation. The advantage of this model, its simplicity, is also its main disadvantage because its model parameters lack physical significance. The model describes the stress-strain curve by o(€)=0, +K-e" 2.1) where is the flow stress, 0; the stress at strain 0, € is the strain and K and are constants. Although it is possible to extend the model with terms for strain rate and grain size effects, in essence the model remains an empirical model. 2.3.3. Bergstrim model ‘The relation between the flow stress and the dislocation density can generally be described by O(6,8,T)= 09 + a-G(T)-bT) (p©éT)+o (eT) 22) where G, is a strain independent friction stress, ais a proportionality constant which depends on the strength of the dislocation /dislocation interaction, G is the shear modulus, & is the Burgers vector, is the total dislocation density, é is the strain rate and T'is the temperature [11},{12] The last term, 0, in eq. (2.2) represents the other contributions to the flow stress (c.g. thermally activated motion of mobile dislocations etc.). Work by Van Liempt shows that this term can be neglected under warm and hot-rolling conditions [13]. It appears from eq. (2.2) that the dislocation density is a critical parameter in the modelling of the flow stress. ‘The general dislocation evolution rate during deformation can be given as do _ 4) 2 de de de (2.3) work-handening rcrytalationBergstrém proposed a single-parameter model that describes the development of the dislocation density during deformation [12},{14]. It describes the change in dislocation density during work- oral “aa wT FT pee ae Pe) hardening and dynamic recovery (first and second terms on the right hand side of eq. (2.3)). ‘The model is based on the following Fig. 2-2. Schematic representation of the Borgstrém model assumptions: © the total population of dislocations consists of mobile dislocations with a density p,,and immobile dislocations with a density p, ; © the influence of the dislocation structure on the deformation behaviour is neglected; © Pp isin dynamic equilibrium at a value independent of strain and is much smaller than p,, In the Bergstrim model, four main processes can be distinguished (see Pig, 2-2): © creation of mobile dislocations (p,, increases); * immobilisation of mobile dislocations (p,, decreases; p, increases); © remobilisation of immobile dislocations (p,, increases; p, decreases); © annihilation of mobile or immobile dislocations (p,, decreases; p, decreases). In this model, the mobile dislocation density is determined by the rate at which dislocations are created and at which dislocations are remobilised. ‘The combined production rate of mobile dislocations, U(), is therefore given by @4) le where the index indicates the process concerned. The second equality follows from the assumption that the mobile dislocation density is constant. U(é) therefore represents the total rate at which mobile dislocations are either immobilised or annihilated. ‘The net rate at which the total dislocation density increases is equal to the increase rate of the immobile dislocation density, and can be written as the difference between the rates of creation of mobile dislocations and annihilation of mobile and immobile dislocations, according to 5) The rate at which immobile dislocations are remobilised is assumed proportional to p, by a factor 6. The annihilation of mobile dislocations can occur by any of the three following processes: through reaction with other mobile dislocations (probability proportional to ,,), through interaction with an immobile dislocation (probability proportional to p,.-p) and by annihilation at dislocation sinks such as gtain boundaries, inclusions, specimen surface etc. (probability proportional to p,,'N with N being the sink density). This results in Bl aa pita-p.- 0.48, N-p, 26) 20in which A,, A, and @, are strain-independent parameters. Combining eq. (2.5) and (2.6) results in (Note that p,, is assumed constant and much smaller than p, and that P,= p - 2.) a —=U(e)- A, -Q, D @=UE)-A-2-p en with 4,=(4,-4,) pi +@,-N-@)-p, and Q,=0,+4,-p, In eq. (2.7) A, represents the probability of annihilation of a mobile dislocation and Q, represents the probability of remobilisation, The probability of two mobile dislocations meeting and annihilating is much smaller than annihilation at a dislocation sink. Since p,, is assumed constant and Nis a strain independent density of annihilation sites [10], 4) is a constant as well and can be included in U(e). In that case eq. (2.7) can be simplified to: ie _ eure ae 28) where U(é) is a measure of the rate of dislocation immobilisation and annihilation and Q a measute of dislocation remobi tion only. In order to integrate eq. (2.8), the strain dependence of U(é) has to be determined. U is related to the lifetime of the dislocation. During deformation, the dislocation travels through the lattice cover a distance in which it encounters no obstacles: the mean free path, s. During the travel, the dislocation can be annihilated or immobilised. U is therefore directly related to the mean free path. The change of the dislocation density with time can be written as dp _¥'Pn dts) 29) In this equation, » represents the velocity of the mobile dislocations. The strain rate can be written as de dt (2.10) where 7% is an orientation factor equal to 2 and 3.1 in b.c.c. and Ecc. metals respectively. Combining eq, (2.9) and (2.10) yields dp_dp dt_ om Ven Te dy de bse) @.11) Because sis strain independent [12}, so is U. In isothermal experiments, eq. (2.8) can then be integrated to yield ee ple)= = (- "+p, @.12) Q where p, is the initial dislocation density and U/ represents the steady-state dislocation density for € > 0, For cases where the values of G, , and fare unknown, eq. (2.12) can be transformed using eq.(2.2) by taking YT) = (@G-5)*U and neglecting 0, and o* into : K aeen=| ¥(r) (ae 2@ p02 eee! » 19 2ET) For cold deformation, the remobilisation parameter {2 can be assumed independent of temperature [12]. However, in general, 2 contains an a-thermal contribution (@), and a thermal and strain rate dependent contribution, (Q)), according to Q= Q,+Q(8,T) 4) where (2) is a parameter depending on the chemical composition, but not on temperature of on strain rate. If remobilisation occurs primarily in the sub-grain boundaties and takes place by climb, the diffusion of vacancies plays an important role. Bergstrém derived an equation based on the assumption of Einstein-type vacancy diffusion (vacancy diffusion to the dislocation is the rate-controlling step) 26 T)=L-n JETP oof Ee \ew = ben af D% (2.15) J SRT in which & is the number of vacancies to mobilise or annihilate immobile dislocations, 1, is the density of vacancies, D, is the diffusion constant, Q,, is the activation energy for vacancy diffusion, and R is the gas constant. Yoshie [15] and Laastaoui & Jonas [16] included the grain size, d, of the mate land generalised eq. (2.15) into 2 c.gt gn ea = nage QQ +C-d-é “emf a ot Q=Q,+C-d"-Z 2.16) or, in general Q=2,+ f@)2" (2.17) where Z's the Zener-Hollomon parameter and # and 7 are model parameters. For warm and hot-rolling of a recrystallised steel, ) and gj, can be neglected. For a given temperature and strain rate, eq. (2.13) can be simplified into (2.18) y % o(e)= [- - ey which implies limo =, It is important to note that Gi,, represents a saturation stress. This saturation stress will be relevant in the dynamic recrystallisation model. In eq. (2.2) the shear modulus, G, and the Burgers vector, 4, are temperature dependent. Equations for the shear modulus were fitted to data presented by Nadai [17] yielding Spy 5 7 2 pe G,(T) = 1.45-10° -137-T +3.48-107 +7 2.19) = 207-10" G(T) =2.07 10" + (2.20) 22where G(7) is the shear modulus in MPa and the temperature is given in Kelvin. ‘The Burgers vector as a function of temperature can be calculated from the lattice parameters of austenite and ferrite. Onink has determined equations for the lattice parameters (in nm) as a function of temperature from neutron diffraction experiments [18}. The Burgers vectot (in nm) as a function of temperature can be calculated using these lattice parameters by taking the geometry of the fic.c. and b.c.c. unit cells into account using the following equations b,(T) = 4N2- (0.36320: (1+ 2473-10" - fr - 1000))) 21) b4(T) = 43 -(0.28863-(1+17.55-10~ -[T -800])) 222) where the temperature is given in Kelvin. So, to recapitulate, eq. (2:18) gives the work-hardening behaviour in which Y and Q are the variable model parameters for a given temperature and strain rate, and is the main equation in this thesis. Eq. (2.13) is the general work-hardening equation. Eq. (2.17) represents the general equation between Qand temperature, 2.4 Softening 2.4.1 Introduction Usually two types of softening are distinguished: recrystallisation and recovery. The term recovery is used to indicate restoration processes that do not result in the replacement of the deformed grains by new grains, but nevertheless lead to structural changes within the existing grains. During the process of recovery, considerable rearrangements occur with the result that, since the defects disappear, energy is released in the form of heat. The driving force for recovery is the seduction in strain energy achieved by the removal of excess point and line defects. The recovery Process often involves cross-slip of the dislocations in order to be able to annihilate. Cross-slip is facilitated by high stacking fault energies. ‘The higher the stacking fault energy, the smaller the separation between the partial dislocations and the lower the shear stress required to associate the partial dislocations. Metals with high stacking fault energy like ferrite and aluminium generally tend to recover readily whereas metals with a low stacking fault energy like austenite, copper and nickel do not tend to recover easily. Obviously, if climb is assumed the dominant mechanism, recovery is a thermally activated process (diffusion of vacancies) and there is no incubation time. Unlike recovery, recrystallisation enables the reeystalision mechanical and physical propertics of the reieate of stor0d oneay deformed metal to return completely to those of the annealed (or initial) state, Recrystallisation is : tinea tne —— a nucleation and growth process since unstrained _ Fig. 2-3, Effect of overlapping recovery nuclei begin to grow in the deformed metal ang recrystalisaton on release of stored when the temperature is high enough and energy [8]gradually absorb the entire deformed matrix. ‘The driving force for recrystallisation is the reduction in dislocation density. Therefore, important variables in the recrystallisation process are strain, strain rate, temperature (because these influence the initial dislocation density) and the annealing time and temperature after deformation. Since the process of nucleation is thermally activated, a longer annealing time dynamic recovery static recrystallisation 4 higher temperature increase Fig. 2-4. Schematic representation of hot-rolling and the probability of producing a softening processes: Dynamic recovery, static recovery and ' static recrystallisation. In case of a material with low nucleus, and correspondingly stacking fault energy (e.g. austenite, lead) dynamic reduce the threshold strain. The recrystallisation occurs instead of dynamic recovery. ae need for thermal activation also accounts for the period often observed before recrystallisation becomes detectable (incubation time). Since the dislocation density is the driving force for recrystallisation, there is a competition between both softening processes. Extensive recovery may reduce the stored energy to a value below a certain critical value for recrystallisation, cither by annihilation of dislocations or by formation of a stable substructure. The concurrent occurrence of recovery and recrystallisation is schematically illustrated in Fig. 2-3. Fig, 2-4 shows the different softening mechanisms in relation to hot rolling. Dynamic recovery is modelled implicitly in the Bergstrim model by the remobilisation parameter @ (§ 2.3.3). In the order of occurrence during hot rolling, dynamic recrystallisation, static recovery, and static recrystallisation will be discussed. 2.4.2. Dynamic recrystallisation ‘The second term on the right hand side of eq. (2.3) represents the dectease in dislocation density due to dynamic recrystallisation. It has been demonstrated empirically that the critical strain &,, for the onset of dynamic recrystallisation (see Fig. 2-5) can be written as (19},[20] Ey, = 08-8, 223) in which 6, is the strain at which the flow stress reaches its maximum (6, will be referred to as peak strain in the remainder of this thesis). Once the material is deformed beyond the critical strain, some of it will recrystallise dynamically ue. whilst being deformed). It will depend on the strain sate whether a steady state level is attained or whether cyclic behaviour occurs. If the strain rate is low, repeated cycles of work hardening and dynamic recrystallisation result in an undulating stress (see Fig. 2-6a). If the strain 24dynamic recovery. Work hardening oynamic al | recrystalisation gq °, ‘grain growth ‘no recrystalisation ‘strain Fig. 2-5. Work-hardening and softening processes - (a) Work-hardening and dynamic softening processes; (b) post-dynamic and static softening processes (including grain growth). rate is high, the repeated cycles result in a constant steady-state stress level (see Fig, 2-6b). In hot rolling trials and compression tests, the strain rate is usually high cnough to attain the steady-state level. The undulating stress behaviour is usually observed at strain rates obtained in tensile tests. ‘The decrease from the maximum flow stress or peak stsess, d,, to the steady-state stress, J, can be modelled by any sigmoid function (usually the well-known Avrami equation). If no dynamic recrystallisation had occurred, the material would have softened by dynamic recovery only. The stress level would then have reached a level that can be described by eq. (2.18) and the maximum dislocation density is given by ¥ lim(ole))= 5 (224) After the onset of dynamic recrystallisation, the stress level can be approximated by 98% recystalised stress strain Fig. 2-6. Dynamic recrystalisation - (a) Low strain rate; (b) High strain rate (8F = Gig — Cm — Fy) X, (2.25) ‘The fraction dynamic recrystallisation, X,,,, as a function of time is given by a sigmoid equation, eg, the wellknown Avrami equation Yy x()ei-eg{-00n ( } | (2.26) Cabrera reported a number of values for ranging from 1.4 to 2 for CMn-steel [20]. The time to 50% recrystallisation (f,,) can be calculated from [20] ty a2 Se) 27 In analogy to the stress evolution, the evolution of dislocation density can be calculated as well This enables calculation of the dislocation density at the end of the deformation. This dislocation density is the initial dislocation density for the static softening processes that may take place after deformation, ie. either static recovery or static recrystallisation. 2.4.3. Static recovery The recovery of dislocations in a deformed structure involves annihilation in the sub-grain and in the (sub-)grain boundaries, and transfer of dislocations between the interior and the boundaries of the sub-grain. The development of the dislocation density as a function of time, under the assumption of a homogeneous distribution of dislocations, is given by [21] 4p dt -2:M-t-p? (0.28) in which M is the mobility of the dislocation and 7 is the average energy per unit length of dislocation [21]. This relation assumes equal densities of dislocations with positive and negative sign. Sandstzém proposed to correct for a possible inequality by rewriting eq. (2.28) as Paap) iS in which p, sepresents the difference in density between dislocations of opposite sign. Eq. (2.29) shows that the final dislocation density after full recovery is not necessarily equal to zero. Sandstrém also estimated the magnitude of the other contributions and the essential conclusion is that the initial stages of recovery are governed by eq. (2.28) or (2.29) and that in a later stage absorption of dislocations at the boundaries becomes more significant. However, the latter process is a significantly slower process and hence, for the sake of this study, eq, (2.28) is adopted as the main equation for static recovery Integrating eq. (2.28) gives SS PO pe =0) 1 =2-M-t-r ot 00" ayaa (2.30) 26with M= ag M=M, oa | (231) which can be approximated by assuming that the mobility of « dislocation can be directly related to self-diffusion. Therefore, M can be assumed proportional to the bulk diffusion coefficient and Qin eq, (2.31) is the activation energy for self-diffusion. 2.4.4 Static recrystallisation Unlike recovery, recrystallisation causes the mechanical and physical properties of the deformed metal to return completely to those of the annealed state. During recovery, properties change gradually. During recrystallisation, these properties alter drastically over a very small temperature and time range. Recrystallisation is a nucleation and growth process. Unsteained nuclei begin to grow in the deformed metal when the temperature is high enough, and gradually absorb the entire deformed matrix. Nucleation usually takes place on grain boundaries, phase interfaces, twins, deformation or shear bands, and the surface of the metal [8]. ‘These sites can be characterised cither as regions of heavy distortion or high dislocation density, or as sites with a marked change in orientation. Recrystallis tion may occur either during deformation, in which case it is referred to as dynamic recrystallisation (see § 2.4.2) or after deformation, in which case it will be referred to as static recrystallisation (this section). Metals with a low stacking fault energy (like austenite) do not undergo a latge dislocation rearrangement during recovery, whereas metals of high stacking fault energy (like ferrite) readily form sharply defined sub-structures which compete with recrystallisation in reducing the stored energy of the deformed metal [8]. Téa microstructure has recrystallised partially, the total dislocation density of the material can be calculated from P=(l-X)-py+X-p, (2.32) where p is the mean dislocation density, X is the recrystallised volume fraction, p, is the dislocation density of the deformed grains and p, is the dislocation density in the recrystallised grains. The driving force for nucleation is the difference in dislocation density between the recrystallised grains and the strained grains. According to Sandstrom and Lagneborg [22],[23] the relationship between the velocity » of a migrating grain boundary and the difference in dislocation density between a recrystallised grain and the unrecrystallised matrix can be written as He (D~P.) 233) pe where the temperature dependence of M,, is as given in eq. (2.31). During recrystallisation, the grain boundary, which has an area § per unit of volume, moves a distance dr into the matrix within a time interval dé ‘The volume that recrystallises duc to this movement of the grain boundary is Sidr. The dislocation density in the volume S-dr decreases from p, to p. The change in the mean dislocation density of the matrix with volume V’, is given by Vy-dp =-(p- p,)'S-dr=(p—p,)'S-v-dt (2.34)With the definition of v in eq, (2.33), eq. (2.34) can be rewritten as dp _ SM teat Cp) 4 2.35) Integrating the left-hand side of eq. (2.35) yields dos Pa-P (2.36) wn P=) (P~P APP) whete it was assumed that p’= p, at /= 0. After substitution of eqs. (2.32) and (2.36), the general solution of eq. (2.35) becomes S(t)de i 5 i“ MyT (Ps P.):J (Pi-P.)J5Od eX, 1+ Mg (0,-P): J Eq, (2.37) was derived by taking the migrating grain boundary area of only one recrystallised grain into account. However, by assuming that 5() represents the total migrating surface atea of all recrystallised grains, eq. (2.37) can be considered to be a general description of static recrystallisation. ‘The nucleation of recrystallisation occurs preferentially at grain boundaries and triple-points. This means that an assumption of random nucleation, as originally proposed by Avrami, is probably not cottect. Instead, it is preferable to consider clustered nucleation along edges and grain boundaries. In comparison to the homogeneous site saturation nucleation mechanism as proposed by Avrami (Fig, 2-72), Backofen-English (Fig, 2-7b) and Speich-Fisher (Fig, 2-7c), explored two other possibilities of clusteted nucleation followed by growth of the auclei. Cylindrical shaped grains have a constant radius 7) and constant axial growth rate (Fig. 2-7b). If site-saturated nucleation is assumed, the nucleation rate is zero for > 0 and thus the total surface area will remain constant. Eq, (2.38) becomes the English-Backofen equation (see Appendix A) by assuming a constant migrating surface area S(d) = 5(0). If on the other hand a configuration of nuclei is assumed as given in Fig, 2-7e where cylindrically shaped grains have a constant length /, and constant radial growth rate, the surface area of a single grain in this configuration will increase with time in a linear fashion. If site-saturation is assumed, then J() « ¢ If a non-zero but constant nucleation QO xy | a= 3.9 ,,| =| SEE Fig. 2-7. Three configurations for clustered nucleation and growth ~ (a) Homogeneous nucleation; (b) English-Backofen configuration; (c). Speich-Fisher configuration. 28rate is assumed, the total surface area S() « 7. By assuming S(/) % F, eq. (2.37) becomes the Speich-Fisher equation (see Appendix A). This discussion shows that the migrating surface area as a function of time depends on the shape of the grains, the dimension in which they grow and the time dependence of the growth and nucleation rates. Since the migsating surface area is an unknown function of time, a power law was proposed because it can be argued that all models predict that the migrating surface area is a power function of time. Therefore, a generalized Speich- By a By (2.38) The factor B accounts for the driving force and kinetics of the recrystallisation process, whereas 7 isher model can be written as accounts for the type of nucleation or the shape of the recrystallised grains. The result is similar for the Speich-Hisher (denoted by SF) and English-Backofen (denoted by EB) equation, the only difference being the value of n ‘The principal difference between the Avrami-model and the generalised SF/EB-model is the assumption of random nucleation as opposed to clustered nucleation. Initially the growth rate of the nuclei is similar, leading to similar evolution of the fraction recrystallised. However, the clustered nuclei will impinge sooner because two neighbouring nuclei are closer together than in the random sample. ‘The consequence of this impingement is that the recrystallisation rate in case of clustered aucleation is less than in case of random nucleation. In this thesis, the results of the experiments will be fitted to the generalised SF-model. The generalised Avrami model (eq, (2.39)) will only be used for comparison in the form of the equation’ -exp- GB, +1) 239) Appendix A shows the derivation of the EB/SF equation on the basis of the nucleation and x growth mechanism. Both the nucleation and growth mechanism and the dislocation density based approach lead to the equations for the Avrami model, the Speich-Fisher model and the English-Backofen model as given in this section 2.5 Backgrounds of methods to quantify softening 2.5.1 Introduction Quantitative information on static softening is crucial in hot-strip rolling models to predict rolling forces or in microstructure models. Several experimental techniques are available to obtain that information. The double-hit compression test is usually considered appropriate because it allows study of the softening process under similar conditions to multi-pass rolling processes (e.g, [16]) Other techniques such as stress relaxation tests (eg. [24)), creep tests (eg. [25)), direct metallographic observation (e.g. [26]) and in-situ observations using XRD-measurements can also be used [27]. As the aim of this study is to explore the intercritical region from an industrial point Bg, 2.26) is a special case of the generalised Avrami equation.of view (ic. during cooling from the austenite region), direct metallographic observation is not a feasible technique because as a consequence of the low alloy contents in the steels, the austenite fraction will not transform to martensite. This makes it impossible to distinguish between ferrite formed by transformation and ferrite formed by recrystallisation of deformed ferrite. In-situ observation using XRD-measurements can be used to determine the softening behaviour during annealing after cold rolling [27]. However, at present the equipment available for this study is not equipped with a deformation stage. In this study, we will therefore concentrate on double-hit claxation tests, compression experiments and stre 2.5.2 Double-hit uni-axial compression experiments The aim of the double-hit compression test is to determine the fractional softening during the inter-pass holding period after a deformation step (loading curve). During deformation of austenite, four critical strains can be distinguished [28]. The first is the strain where plastic deformation starts, characterised by the yield point (indicated by o,, see Fig, 2-5). Dynamic recovery starts as soon as the material is deformed beyond the yield point. The second relevant strain is the point before which no recrystallisation will occur, not even after very long holding times, the ctitical strain (€,,.). The third point is the strain after which dynamic recrystallisation starts (€,,). Loading the material between €, and €, induces a sufficiently large number of dislocations to induce static recrystallisation but the strain is insufficient to cause dynamic recrystallisation. The last point defines the strain beyond which a steady-state situation is reached when dynamic recrystallisation, dynamic recovery, and work hardening are in balance (€,) ‘These critical strains are relevant for the use of double-hit compression experiments because when the strain during loading exceeds the point where dynamic recrystallisation starts occuring, the kinetics of static recrystallisation will differ considerably from the situation where no dynamic recrystallisation has occurred. It is therefore important to know the values of these critical strains when designing double-hit compression experiments. It is also relevant to note that, although both softening processes are thermally activated processes, recovery processes do not show an incubation petiod whereas rectystallisation processes usually do. Fig. 2-Sb shows the influence of post-dynamic recrystallisation, static recrystallisation, static recovery, and grain growth on the reloading curve. Post-dynamic recrystallisation (sometimes confusingly called meta-dynamic recrystallisation) can be considered as the continuation of dynamic recrystallisation after unloading, In this case the nucleation of the recrystallisation has occurred during deformation, and the driving force for the growth of these nuclei is formed by the high dislocation density of the deformed structure. Fig, 2-5 indicates that deformation just beyond €,, induces static recrystallisation. Because of the small deformation, the number of nuclei is very small, resulting in a very large grain size and low yield strength after recrystallisation. Despite the fact that the double-hit method is a relatively straightforward experimental tecbnique, it appears that the analysis of the experiments can be rather complicated. Literature reveals no consensus on a best practice for the determination of fractional softening, § 5.2 and § 5.5 will come back to this issue in detail. Although it falls outside the scope of the present study, it may be of interest to note that the double-hit technique can also be used to determine hardening because of (e.g,) precipitation or grain refinement [29]. 30In this study, simulated work-hardening and softening curves will be used to evaluate several ways to determine fractional softening, 2.5.3 Conventional methods to determine fractional softening The fractional softening can be determined from the results of a double-hit deformation experiment by several methods. The three most commonly used methods are the offset method, the back-extrapolation method and the average flow-stress method using the respective equations 6. (2.40) (2.41) = Oo Arun = Az Gen Fron Anas A Co In eq. (2.40) Op, stresses at a certain strain, the offset strain, during the first and second deformation respectively. .. is the maximum stress during the first deformation, and 6; and 0, are the flow Usually 6; is determined on the loading curve, but it can be argued that it is better to determine @, from the second hit provided the material has completely recrystallised [24]. By back- extrapolating the loading curve, Oj, in eq. (2.41) can be determined and 0, and G, have the same meaning as in the offset method. ‘The average flow stress in eq. (2.42) in the first and second hit must be determined over a defined and equal strain range, Obviously, the average stress can also be expressed in terms of area below the stress-strain curve. A fourth method was proposed by Schindler and relates softening to a residual strain [30]. ‘Ihe softening parameter can then be expressed as given in eq. (2.43). ‘This method, less commonly used, uses the strain values rather than the stress, and the softened fraction is given by sind } (2.43) To determine the retained strain, the second stress-strain curve will have to be ‘back-extrapolated” (as in the back-extrapolation method). The initial stress-strain curve can be the loading curve (as, in the back-extrapolation method) or a model curve. Mier reloading the specimen immediately after unloading, no softening has occurred. The specimen has retained the initial strain level €, &, Just before reloading after complete softening, the retained strain will be zero. After intermediate delay times, the retained strain will be between 0 and &, Xu et al. [31] applied the first three methods described above and reported similar results from a qualitative point of view for all three methods. On the basis of double-hit compression experiments on Nb-'Ii micro-alloyed steels Xu et al. conclude that the 0.2% offset method and the average stress method yicld the same results qualitatively, whereas the back-extrapolation method showed a much lower fraction of softening at any holding time. However, if one looks at these results carefully, one is tempted to conclude that the average stress method gives a better aTrepresentation of events than the offset method. The softening parameter in the experiments considered is lower for the offset method at short inter-pass times (0.1 vs. 0.25 at an inter-pass time of 1 second) and the final values for both methods are the same (around 0.60 for the inter- pass time of 100 3). ‘The shape of the curve suggests that the recrystallisation was not completed at this time. Furthermore, since they studied Nb-containing steels, the likelihood of 25% softening after 1 second is small, Therefore, one would expect low values of the softening parameter at short inter-pass times. Laasraoui and Jonas [32] also conclude that the average stress, method corresponds more closely to the recrystallised fraction than the offset method and the back-extrapolation method. On the other hand, Li et al [33] conchude that the 0.2% offset method is probably preferable to the average stress method because the offset_ method determines mainly the recrystallisation effects whereas the average stress method also includes recovery. It is difficult to see how this can be true, firstly because recovery influences the average strain as well, and secondly because the recovery effects will be strongest at low strain values during reloading. Li et al. finally conclude that the 2% offset method gives the best results. Unfortunately, this work is not backed by metallographical evidence. Fernandez et al [34] conclude that the average stress method, the 5% offset and the 2% offset yield the best results whereas the back-extrapolation method and the 0.2% offset method do not perform as well. Kwon and DeArdo [35] concluded that the static softening behaviour, determined by the arca under the flow curve (proportional to average stress), correlated better with the degeee of microstructural distortion than the softening fraction determined by the offset method. In conclusion, this literature outline reveals that there is no consensus as to which method is to be preferred. In performing double-hit compression experiments, it is important that the second hit is as small as possible. If the second hit is too large, not only the effect of softening will be measured, because the work-hardening of the second hit will influence these measurements significantly. Conteol of the strain rate is extremely important. The sooner a steady strain rate is reached, the smaller the second hit can be. If the strain rate overshoots its target value, the yield strength will consequently be overestimated. Furthermore, it appears to be very difficult to determine the flow stress of a material accurately after only a limited amount of plastic strain (e.g. 0.2%). It is much easier to achieve that at larger plastic strains (e.g, 5%). The measurement of the yield strength at high temperatures is further complicated by the possible use of lubricants, the possible presence of grooves to contain the lubricant (or edges in the Rastagaev-shape) and the sometimes poor quality of strain rate control, especially at higher strain rates. Shape changes of the sample (barrelling) or changes in lubrication conditions (squeezing out of lubricant after the first hit) alter the stress-strain behaviour irrespective of the softening behaviour. These changes in lubrication conditions and sample geometry are additional arguments for determining 6, from a second hit after full recrystallisation rather than on the loading curve. ‘The analysis of the softening behaviour is significantly more complicated when dynamic recrystallisation occurs. Kwon and DeArdo [35] found that the softening fraction underestimates the actual fraction recrystallised when the pre-strain exceeds the critical strain for dynamic recrystallisation and overestimates the actual fraction when the pre-strain is lower than the critical value, It should be noted that the equations (2.40) to (2.43) assume validity of 2 mixture rule faeObviously, the assumption of two distinct phases does not hold once = [ dynamic recrystallisation starts. In 20 that case, the microstructure £45 consists of several fractions with g ok varying degrees of softening. Grain & refinement as a result’ of the 5 reerystallisation or precipitation (a hardening during the holding 0.00 0.05 0.10 period can further influence the strain softening (see also Fig. 2-5). Fig. 2-8. Dislocation balance method. 2.5.4 Dislocation balance method Bergstrim’s work-hardening and dynamic recovery model describes the stress-strain relationship of compression experiments (see § 2.3.3). It can also be used to derive the recrystallised volume fraction from double-hit compression experiments. Prior to the first hit the sample has a dislocation density 2,, When the sample is deformed to €,,,, the dislocation density has increased tO Prue Under the assumption that only static recrystallisation occurs, Ppa, is also the dislocation density at the beginning of the recrystallisation process. After an inter-stand time /,, the dislocation density has decreased to p(/,,). When the second hit is applied, the dislocation density will increase again and will reach the value 9, at strain & $ 6... Fig. 2-8 shows the strains and stresses at which the dislocation densities mentioned are reached. The softened volume fraction X,,is now defined ast Pon ~ Plt ow) Prax = X, (2.44) Eq, (2.44) is comparable with eq, (2.32), where it is assumed that 2... = Py and p, = p, (note that the softening fractions cannot be directly compared to the softening fraction as determined by the offset method because of the proportionality of @ to Vp). According to Bergstrém (eq. (2.12)), the value for P,,,. in the first hit is calculated by eu Wop Pass =“ t Po~ BIE (2.45) When the variable 6= U/Q- p, is introduced, eq. (2.43) becomes Prax ~ Pp = 5 eM (e!*™ —1) 46) ‘After the second hit the material reaches a dislocation density P, at €= & (247) (248)Substitution of eq, (2.45) in eq. (2.48) results in 49) Subtraction of eq, (2.49) from eq (2.45) and writing it in terms of 5 Pas = Pty) + 56-21) (2.50) Substitution of eqs. (2.46) and (2.50) in eq, (2.44) gives Xe Sa es To apply this equation, the Bergstrém parameter {2 needs to be determined from the results of a double-hit compression experiment. In § 2.5.5 the conditions under which this method can be applied will be defined. 2.5.5 Discussion The offset method can be applied independently of the softening mechanisms that may have occurred during the inter-stand time. The actual value of the softening parameter depends on the choice of the strain at which 6; and ; are measured. Consequently, the method is not the most suitable method to study static recrystallisation, For instance, consider a double-hit experiment with an inter-stand time /,, = 0. The recrystallised volume fraction is zero by definition. Since fa, = 0, the stress at strain € = 0 in the second hit is ,,. At higher strains the measured value G; is ©, > Gy,, and hence X < 0. Although one would like to measure G; and 0, at € = 0, this proves to be a technical impossibility because of the time a compression experiment needs to attain stable deformation conditions in terms of strain rate. ‘The dislocation balance method assumes that the recrystallised volume fraction is best expressed. in terms of dislocation densities. In order to derive eq. (2.51) the Bergstrim model was used. The method has therefore a certain physical justification. Fig. (2.51) is valid when the stress-strain relationship of both hits can be described by the Bergstrém equation. In the derivation of eq. (2.51) it was implicitly assumed that the Bergstrm parameters U and Q are independent of the deformation history. According to Bergstrém the parameter U depends on the mean free path of the mobile dislocations before they are immobilized. The mean free path is related to the average grain size. The parameter U is the same during both hits if the grain size is constant during the hits. As a first approximation, it is assumed that static recrystallisation does not alter the average grain size. Furthermore, Bergstrom showed that 2 depends on the strain rate, grain size and temperature (eq. (2.16). It is therefore concluded that eq. (2.51) is applicable when the experiment is carried out isothetmally at a constant strain tate and that the mean grain size is not altered during the inter-stand time. This can be tested by checking whether the slope at & is equal to the slope at Ea? do, do, el (% - (2.52) 34In the remainder of this thesis, this will be referred to as slope equality. Obviously, there is a relation between eq, (2.52) and eq, (2.8). With cq. (2.2) eq. (2.8) can be written as Gs oe ae azar | (2.53) Consequently, if eq. (2.52) applies, it is very likely that Vand Qare equal in both hits. do uaa) Fig. 2-9 shows an example of a double-hit compression experiment and of a single- a singe Mt hit experiment performed on the IF-steel v0 = at 700°C with a strain rate of 1s". ‘Ihe stress-strain curve of the second hit of the stress [MPa] s | feat second it double-hit experiment is inserted at the ] j end of the first hit. The inter-stand time a | between the two hits was /,, = 2s. It is ‘0000510 018 02 0a 037 as cal oa assumed that no softening of significance strain occurred during this time. Hence, the Fig, 2-9. Double-hit versus single-hit compression stress-strain curves should be the same for ©xPertment. both experiments. Fig. 2-9 shows that the first hit corresponds to the beginning of the single-hit curve. It is observed that at the start of the second hit both the stress and the derivative do/de differ from the values at the same strain in the single-hit compression curve. At a strain of approximately € = 0.05 after the start of the second hit, these values become equal and remain equal during the remainder of the curves. From this it is concluded that the data from the second hit obtained close to the onset of a stress-strain curve are unreliable. Therefore, these data should be disregarded when a strc: strain relationship is analysed. When €, is measured to lie in the onset of a second hit, the result should be disregarded. In this thesis, both the 5%-offset method and the dislocation balance method will be used to evaluate the double-hit compression experiment. 2.5.6 Stress-relaxation experiments Sun et al. demonstrated that the stress relaxation method can be used to monitor the occurrence of precipitation in austenite, to determine the start and finishing times of the reaction [25]. The precipitation event leads to the appearance of a plateau in the relaxation stress versus time after a ptedeformation. Djahazi et al. also observed that recrystallisation caused an abrupt increase in the relaxation rate and that the relaxation was terminated by the onset of precipitation, but the method was not used to study recrystallisation [36]. A stress relaxation experiment is a creep test performed under a non-steady stress. When a specimen is deformed to a given strain, part of this strain is clastic in origin and part of it is plastic, Because of creep, the plastic strain increases with time. Since the total strain is held constant in the stress relaxation experiment, the clastic strain must decrease with time. The elastic strain can decrease only if the applied stress decreases. When recrystallisation occuts, the dislocation density of the material decreases rapidly. As a result, the flow stress of the material ooaa decreases and the plastic strain a tate increases. ‘Ihe clastic steain rate must therefore decrease and hence the total stress decreases. stress ‘This total stress is measured during a stress__ relaxation oor, log) experiment. The major difference between double-hit compression experim- ents and the stress-relaxation Toe rs Teg time . : Fig. 2-10. Stress relaxation experiment: two linear stages a and fast softening because of recrystallisation in between. kept under stress in the stress- relaxation experiments. ‘The sample is loaded to a cestain strain at a certain strain rate. Subsequently, the strain is kept constant and the stress is monitored as a function of time. Initially, the stress decreases linearly as function of log(?) until recrystallisation starts (see Fig. 2-10). The second stage of the stress- relaxation curve shows a rapid decrease of the stress. A second inflection of the stress-log() recrystallisation). The remainder of the time the curve decreases linearly again because of creep, grain growth or finally attains a steady-state value. In curve marks the end of rapid softening ( case of recrystallisation it is not likely that recovery plays a role just after recrystallisation. In case of a non-recrystallising material, the slope of the stress-log() curve remains constant. This means that a gradual transition from creep and recovery at short times to creep at long times occurs. In compatison to the double-hit compression experiments, stress-relaxation experiments are not as straightforward an experimental technique. Loading the sample and holding the sample at the required strain proves to be difficult experimentally. This usually results in considerable scatter in the initial stages of the stress-relaxation curve. ‘The major advantage of the stress-relaxation technique in comparison to the double-bit compression technique is that it requires only one test to determine the complete recrystallisation curve at a given temperature as a function of time. Under the assumption that partially recrystallised material consists of two phases and that the simple iso-strain mixture rule is obeyed, the softening parameter Xy, can be determined from the experimental data by ©, =a, log(*))-9 "" ©,-9,)-@ ~@, log) x, (2.54) In other words, the fraction recrystallised is determined from the stress-relaxation data with the lever rule. 2.6 Microstructure 2.6.1 Austenite-ferrite two-phase region in iron-carbon alloys ‘Transformation is a nucleation and growth process and the occurrence of a phase transformation is govemned by the stability of the various phases as function of the chemical composition, 36temperature, and pressure. With the appropriate thermodynamic energy functions, usually the Gibbs free energy, the configuration of the phases (faction and composition) leading to the minimal energy of the system at the selected pressure, temperature, and overall chemical composition can be calculated. These equilibrium values can be represented in a phase diagtam. The relevant part of the iron-carbon phase diagram is schematically drawn in Fig. 1-5. Upon the decomposition of austenite, the iron lattice transforms from a face-centted cubic (Ec.c) crystal structure (J, austenite) to a body centred cubic (b.c.c.) crystal structure (0, ferrite) by ejection of the carbon that was dissolved in the austenite. Above the A,-temperatute this leads to a carbon enrichment of the austenite and below the A,-temperature to the precipitation of globular cementite (8, l'e,C) particles in a fertite matrix or to the decomposition of the austenite into pearlite, a lamellar structure consisting of ferrite and cementite. This thesis is concerned with deformation in the (0+Y)-region, so the transformation itself is not particularly relevant until after the deformation. The starting point of every experiment is a well- defined single-phase or two-phase structure. Obviously, the kinetics of transformation after deformation in the intercritical region will be affected, but that falls outside the scope of this study. After the deformation, the remaining austenite will transform during cooling. This part of the transformation is relevant because it determines, at least partly, the final microstructure and crystallographic texture 2.6.2 Characterisation of two-phase systems ‘A two-phase structure can be characterised by the volume fractions of the phases (f, and f), size and morphology of the phases, the strength ratio of both phases () and finally the continuity of the phases. With regard to continuity, all binary mixtures can be divided into three classes: © single-phase fully miscible mixtures (e.g. carbon in austenite) © two-phase system with one continuous phase and one dispersed phase (e.g. austenite with a small fraction of ferrite, nucleated on the corners of the austenite); two-phase system with two continuous phases (e.g. a sponge); For the purpose of this study, the first two are relevant. If the (0++Y)-microstructure is produced the ferrite by cooling from the austenite region, which is usually the case in hot-rolling proces will nucleate on the austenite grain comers and boundaries (see also Fig, 2-1). In the initial stapes of the transformation, when the ferrite fraction is small, the austenite matrix will be continuous and the ferrite phase discontinuous. At the later stages of the transformation (or at lower intercritical annealing temperatures) the ferrite grains will have coalesced and a ferrite network will have formed around the austenite. The ferrite phase has become continuous and the austenite discontinuous. This transition fom continuous to discontinuous austenite or from discontinuous to continuous ferrite is a gradual process and in some stage of this process both phases may be continuous. A quantitative measure for the continuity is the contiguity (C) of phase in a two-phase structure. ‘This is defined by the total boundary area of the phase with particles of the same phase. 37ose" 258" + 50 2.55) sy »"O57r4 507 (2.56) where Ca and C; represent the contiguity of the o- or Y-phase, and Sy, Sy" or Sy is the grain boundary area between O-G.-, Y-Y- or O-Y-grains per unit volume. It has already been said that during = transformation of austenite to ferrite upon @ 120 cooling the fractions of austenite and ferrite : Hr change. However, because of the decreasing & temperature, the carbon content of the 3 140 remaining austenite also changes significantly. | 105 ‘This results in an increase in strength of the E remaining austenite, not only because of the oe temperature decrease, but also because of the 0.95 increase in carbon content. Medina et al. have 00 02 04 06 08 1.0 published equations enabling calculation of the IC}, {wt.%6] increase in strength as a function of the carbon content of the austenite [37]38}. Blankenau Fig. 2-11. Influence of carbon content on pane flow stress of austenite. reports that these equations indicate that the flow stress of austenite is insensitive to variations in carbon content and that the variation in carbon content does not need to be considered [39]. Using the equations proposed by Medina and assuming equilibrium conditions it can be seen (see Fig. 2-11) that the flow stress of austenite is not insensitive to the carbon content of the austenite as Blankenau claims, but that there is 2 modest but definite strength increase with decreasing temperature as a consequence of the increase in carbon content. The initial decrease at low carbon contents is probably the result of a mathematical inconsistency in the empirical model. ‘The strength of the ferrite can be extrapolated from the single-phase ferrite region. The strength of the ferrite will only be marginally influenced by the very small change in carbon in solution. It is obvious that the strength of the ferrite in the two-phase region will deviate from the single- phase ferrite because no cementite precipitates are present in the fertite in the former whereas they may be present in the single-phase ferrite. In the steels under consideration in this study, other precipitating elements like aluminium and nitrogen will be neglected. The error in determining the flow stress of ferrite by this method is considered small and acceptable. 2.6.3 Mixture rules As shown in § 2.6.2 all binary mixtures can be divided into three general classes: single phase systems in which the second phase is completely miscible in the matrix, two-phase systems with one continuous and one discontinuous phase, and two-phase system with two continuous phases. 38‘The propertics of these mixtures can be empirically estimated using a rule of mixtures. There are general mixture rules or equations for each of these classes of mixtures, and the proper type of equation must be selected for an accurate estimate of any given property. Apart from selecting the appropriate equation, additional information about the nature of the mixture is required, e.g. properties of the single-phase constituent, interaction between constituents, size and distribution of the second phase, and the contiguity of the phases. ‘The simplest mixture rule is given by ei) (257) The given property of the mixture is P; P, and P, are the corresponding properties of the components 1 and 2 of the mixture, The volume fractions (or concentrations of the phases) are and f, where fi + /=1 Another simple mixture rule is the inverse rule of mixtures LAs PPP, 2.58) Eq. (2.57) could be considered an upper bound of property P, whereas eq. (2.58) 220 constitutes a lower bound. If stress is the 200 property of interest, then in case of eq. (2.57) . the strain is equal in both phases (jso-strain rule of mixture). In case of eq. (2.58), the 1 stress is equal in both phases (jso-stress rule of 140 mixtures). Hig. 2-12 illustrates both extremes. 120 (eq(2.58)) If the property P is plotted as a function of the a fraction of either of the constituents, the iso- stress rule of mixtures gives a straight linc rete tyet between P, and P,, whereas the iso-strain rule i h Fig. 2-12. Schematic relation between P; and Pe in iso-strain and iso-stress situation. of mixtures gives a curved line between P, and P,, Fig mixture rules (note that the volume fractions 13a also illustrates examples of both for both cases are not equal). ‘Tamura ct al. [92] proposed an alternative to the two simple rules of mixture (eq. (2.57) and (2.58). They postulate that the strains as well as the stresses should he taken into account simultaneously according to: (2.59) 2.60) Fig, 2-13b shows a graphical representation of this postulation. The slope, 9, defines the distribution of strains and stresses over both phases. The value of g can be calculated from [91] be(2.61) The larger the absolute value of g, the more the iso-strain situation is approached. The value of g will vary with volume fraction, z, morphology and distribution, the work-hardening behaviour, and with increasing strains. ‘he latter means that with increasing deformation, the softer phase absorbs more strain, whereas the harder phase absorbs less. In many mixtures, these simple rules of mixture are not capable of accurately predicting the properties of a binary mixture. Additional information must be supplied. For one-phase systems containing two components (full miscibility) the following equation is proposed [90] P=R-f +P fitl (2.62) where Tis an interaction parameter. ‘Mixtures containing 2 continuous phase and a dispersed or discontinuous phase can be described using P_1+A-B-fy Ro I-B eg: (2.63) 2 where A is a constant depending on the shape and orientation of the dispersed particles and on the nature of the interface. The constant B depends on the value of the properties of the components and is given by (2.64) in which P, is the property of the matrix phase. The factor @ is a reduced concentration term which is a function of the maximum packing fraction. In case of a two-phase structure of ferrite and austenite, = 1. If A is infinite, eq. (2.63) reverts back to eq, (2.57). When A=0 eq, (2.63) results in the inverse rule of mixture (eq. (2.58). Eq, (2.63) and (2.64) can therefore cover the complete range from upper bound to lower bound depending on the values of A. If the soft phase is the dispersed phase, eq. (2.63) and eq, (2.64) are rewritten as B_ 1+ A By fs (265) (2.66) (2.67)F a iso-stress pa mixture — at a). b). Fig. 2-13. Schematic representation mixture rules - (a). Iso-strain and iso-stress situation (note that different fractions were used); (b). Imermediate situation. “There are several occasions on which a mixture rule cannot be expected to apply. The following examples (taken from (90) are examples of situations in which mixture rules may be invali ‘¢ the nature of the system changes in some manner as a function of composition, e.g. change in morphology from spherical to rod-like particles; © the nature of one or more of the constituents may be changed by the presence of the other, and this change is not taken into account, e.g, electrical conductivity of salt in water; © another property, which affects the measured property, simultaneously changes non-linearly with the measured property e.g, viscosity of a mixture of liquids in which the density changes in a non-linear manner as a function of the composition; * some properties of mixtures may depend less upon the corresponding property of the constituents than upon some other property or characteristic of the mixture. For example, the strength of a composite material may depend very strongly on the nature of the interface between the phases, and upon the shape and distribution of the particles ‘Tamura et al. {92] found that two-phase systems obey the simple rule of mixture if the ratio Z between the flow stress of the hard phase and the flow stress of the soft phase is less than three. If this ratio exceeds three, the flow stress of the system increases with the volume fraction of the harder phase, linearly at first in the same rate as for Y =3, and then starts deviating from linearity where the flow stress increases rapidly. ‘This acceleration begins at smaller volume fractions as ‘increases. ‘lamura et al. explain this behaviour by stating that the assumption of equal strain in both phases is increasingly untrue for systems with increasing values of 7. Unckel made the same observation as early as 1937 (59. ‘Tamura ct al fail to explain why this would happen at a value of X =3, nor do they give any physical explanation of the fact that there should be a threshold at all In polycrystalline materials each grain has a different orientation. This means that during deformation, each grain has a different yield stress as a result of the different Schmidt factor for each grain. A two-phase system can therefore not be treated as two distinct phases with distinct yield stresses 42.7 Crystallographic texture 2.71 General Plastic deformation of a polycrystalline material results in a predominance of a particular crystallographic direction or plane, in conjunction to the direction of deformation, in the majority of the individual crystals comprising the material. In a tensile test on a single crystal, the slip direction rotates until it approaches the axis of tension, and in compression, the slip direction rotates until it is in the plane of compression. Similarly, rotations occur in the individual grains of a polycrystalline material. In this case, the grains undergo more complicated stress modes even in simple processes such as tension or compression; this leads to the development of preferred orientations or texture. The degree and nature of this texture depend on the particular deformation process as well as on the crystal structure of the metal. Texture may also result from recrystallisation or phase transformation: in both cases new grains are formed which have specific orientations with respect to the parent grains. 2.7.2 Representation of texture ‘Textures are usually presented in the form of an Orientation Distribution Function (ODF). The ODF is calculated from individual incomplete pole figures for low-index planes. The orientation of an individual crystallite can be specified by considering its crystal co-ordinate system (x’,y’ ¢) with the axes being the axes of the cubic unit cell, with respect to a common sample co-ordinate system (x; y, 2). These co-ordinate systems are related to each other by the Euler angles g, @and 9, (sce Fig, 2-14). ‘The ODF-intensity for orientation g can then be defined as the density of crystallites with a cube axis directed in the otientation g. ‘The ODF can be represented either by a perspective drawing of the Euler space or by a two-dimensional representation of cross-sectional planes. The intensity of an orientation is expressed with respect to the intensity this orientation would have had in a sample with a completely random orientation distribution. Apart from allowing 2 quantitative description of textures, the use of the ODF allows the identification of texture fibres and quantitative plots of intensity along these fibres. ‘These intensity data provide detailed information. ‘The volume fractions of any texture component may XG Co-ordinate system X,Y,Z, Co-ordinate system X.V,Z, Co-ordinate systam XYZ" Fig. 2-14. Definition of Euler angles used for rolled sheet. 42also be readily calculated from the ODF data by determining the total intensity within (for example) 11° ict eee aa Boe HE (001}<1 10> of the ideal orientation. ese ELE: (I11}ct10> quantitative representations of the Pome data may be compared directly with G:(110}<001> theoretical predictions or may form EANZ C1 ‘plore (81 1/ND) Ts (654}cz05> part of the specification of an industrial product because, based Me hemi on the ODF, theoretical values can be calculated [10]. The part of the ODE as shown in Fig, 215 © (defined by g; =45°) contains most Fig. 2-15. Important orientations in the go=45° section of ; the ODF. {892,112 of the relevant texture components and fibres for a b.cc. metal. ‘The most important fibres are the OL-fibre and the ‘-fibre. The O-fibre is the collection of orientations with the <110>-direction parallel to the rolling direction and the ‘y-fibre is the collection of orientations with the {111}-plane parallel to the normal direction. In body-centred cubic metals, a dominant orientation is {001}<110> with cube planes in the rolling planes and the <110>- direction in the rolling direction (H in Fig. 2-15), but there are other important components such as {112}<110> (I), (111}<110> (B) and {111} <112> (F). 2.7.3. Texture development in austenite ‘The deformation of fc. metals such as austenite occurs by slip or by twinning, The preferred slip system is always the same: the close-packed plane {111} slips in the close-packed direction <110> and the twinning occurs at the {111}<112> system [8]. Austenite has a predominant {110}<112> component with a {110}-plane in the rolling plane and a <112>-direction in the rolling direction (usually seferred to as “brass texture”). A second important rolling texture component is the {112}<111> component (“copper texture”). The S-component, {123}<634>, is also reported to be an important texture component in the austenite deformation texture, as well as the Goss-component {110}<001>, albeit to a lesser extent [40]. Because of variant selection during the subsequent phase transformation, neither the S-component nor the Goss- component will play an important role in the further texture development of the material. Neither component will be considered further in the remainder of this thesis. When a metal is deformed at a high temperature, the deformed microstructure usually recovers or recrystallises, The influence of recovery on the texture development is indirect, because recovery leads to a rapid polygonisation of grains on the Y-fibre in contrast to O-fibre orientations. ‘This polygonisation yields stable nuclei for recrystallisation, These consume the grains on the O-fibre and thus the intensity of the 7-fibre components is enhanced because of recovery-stimulated nucleation of recrystallisation [41]. The recrystallised structure possesses a preferred texture, which in many cases is even stronger than in the texture of the deformed structure. This rccrystallisation texture results from primary recrystallisation of the deformed Bgrains or from growth of selected grains in the recrystallised material (secondary recrystallisation), ‘The main recrystallisation texture component in austenite is the cube-component {100}<001>. ‘The magnitude of the influence of this component in the final texture depends largely on the degree of recrystallisation in austenite and hence on the temperature at which the deformation takes place with respect to the non-recrystallisation temperature (T,,). At higher temperatures, the austenite will recrystallise and the cube texture will be formed. At deformation temperatures below T,, the austenite will not recrystallise and a sharper deformation texture may develop by subsequent deformation [42]. 2.7.4 Transformation texture IE the austenite possesses a crystallographic texture, the ferrite that forms from the austenite upon cooling will also acquire 2 texture which can be related to the texture of the austenite by means of an orientation relationship. In general, orientation relationships are expressed as: | bas) | etstsdotuom) | where the subscripts 1 and 2 refer to the parent and product structures of the phase transformation respectively. In the case of steels, three orientation relationships are usually distinguished: the Bain orientation relation, the Kurdjumov-Sachs orientation relation and the Nishiyama-Wasserman orientation relation [43]. Experimental evidence indicates that the Kurdjumov-Sachs (KS) orientation relationship can be used to describe the transformation from. ferrite to austenite [44],{45],[46]. ‘The rotation axis in this case is the <112>-direction and transformation is the result of a rotation of 90° around that axis. A {111}-plane in the austenite phase transforms into a {011}-plane in the ferrite, and a <011>-direction in the austenite into a <111>-direction in the ferrite. Because of crystallographic symmetry, several equivalent orientations are possible. It appears that the transformation of austenite to ferrite involves only a restricted set of the 24 possible KS-variants. This phenomenon is known as variant selection and its origins have been investigated by many authors (eg, [40],[44]). As a result of the phase transformation, the {110}<112>y rolling texture component will transform into the Table 2-1. intercritical or territic rolling of steels [44]. Texture ‘Trantormation components in Kurgjumov-Sochs ‘austenite Tis RATS Fae SaaS (deformation, S) > {392}<113>, oe {110}<110>,, GE OS ORI (recrystallisation) = — {110}<001>,, + {10 K, (v.00) Origin and evolution of some characteristic texture components during austenitic, (2.68) Rotation around RD or Orientation py, & a) Inerrtea deformation S20 F-218) (00 Fig 2-15) ED) 5 2IE, r 30, 60,45 > (01t}5 —_pfibre(F) 90, 55,45 28 (TD) (445}<110>,wsibre > 80°(TD)_{111}<110>, pore ) 0, 85, 45 "S08 above: Vedibre, E ~~ See above . Tfibre, | : - i a ng . Goss . L 44{332}<113> q component (I* in Fig. 2-15) and the {112}<111> y rolling texture component into the {113}<110> « component in the ferrite. The cube-texture from recrystallised austenite will result in a {100}<110> component, in a {110}<001>q Goss component or in the (110}<110>q rotated Goss component (1). These transformations are summarised in Table 2-1. 2.7.5 Texture development during intercritical rolling In ferrite, with its b.c.c.-structure, no close-packed planes exist. The close-packed direction is the <111> direction and the plane with the highest density is the {110}-plane. Apart from the {110}<111> slip system the {112)<111> and the {123}<111> slip system can also be activated [43]. In addition, the ‘pencil glide’-phenomenon allows slip over any plane in the <111> direction. Whether the ferrite inherits a texture from the austenite depends mainly on the strength of the rolling texture of the parent austenite. ‘The deformation and subsequent cooling of an austenite ferrite two-phase structure leads to ctystal rotation by further deformation of the remaining austenite phase; (possibly) recrystallisation of the austenite; crystal rotation by deformation of the ferrite phase to more stable texture components; (possibly) recrystallisation of the fertite; eee ee completion of the austenite to ferrite transformation, “The intercritical deformation of austenite will not result in new texture components, neither dusing recrystallisation of the austenite nor during transformation into ferrite. Compared to fully austenitic rolling, the texture components {112}<111> and {110}<112> will intensify because of deformation at a lower temperature. Deformation of the ferrite will result in texture modifications, The ferrite grains rotate as a result of the deformation and the {113}<110> texture component changes into the stable component {112}<110> (rotation of 10° around <110> parallel to the rolling direction) and the {332}<113> component changes into {111}<110> via the intermediate stages (554}<225> and {111}<112> (rotation of 4°, 14° and 44° around <110> parallel to the transverse direction), Deformation of the ferrite after transformation has no influence on the occurrence of certain texture-components because the textures formed by rolling in the lower intercritical region should already be near the stable end otientations of the ferrite rolling texture. However, it has considerable influence on the intensity of those components. Especially if the steel undergoes a recrystallisation annealing treatment, further deformation can sharpen the {111} otientations (y-fibre) at the expense of the {hkl}<110> orientations (a-fibre), On recrystallisation of this structure, higher intensities of the {111} orientations may develop, which leads to more favourable deep-drawing properties [48]. 2.7.6 Texture development by recrystallisation of ferrite As already stated before, the {332}<113> q component will be formed from the {110}<112> y rolling texture and the {113}<110>@ component from the {112}<111>, rolling texture. Hutchinson reported that in case of deformation of ferrite, the stored energy in the grains 45increases in the sequence {001}<110> < {112}<110> < {111}<110> < {110}<110> [48], The stored energy has a considerable influence on the annealing texture because it determines which of the nucleation mechanisms for recrystallisation will dominate. Strain induced boundary migration Strain Induced Boundary Migration (SIBM), is based on bulging of a pre-existing grain boundary into grains of high stored energy [47]. This implies nucleation inside grains with a low stored energy, ie. {001}<110> and {112}<110> grains. Strain Induced Boundary Migration therefore favours formation of textures with {001}<110> and {112}<110> orientations. These texture components are usually considered undesirable for good forming properties. Subgrain coalescence Nucleation by Sub-Grain Coalescence (SGC) within individual deformed grains is facilitated if the stored energy of the grains is large, and this favours formation of textures with {111}<110> and {110}<110> orientations [48]. Since the fraction of {111}<110> is much larger than the fraction of {110}<110> orientations, the fraction of {111}-grains will dominate the final texture ‘This {111}-texture is very favourable for deep-drawing applications and attention during production of cold-rolled sheet for these applications is tailored to obtain this favourable texture starting in the steelworks, through the hot-strip mill down to the final annealing and temper rolling treatment after cold-rolling. Since the texture of the hot-band forms the basis for further development of the texture downstream, obtaining a favourable starting texture after the hot- rolling process is extremely important. 2.8 The research question Important issues that ate not addressed adequately in the available literature include the relation between the crystallographic texture and the microstructure, the relation between microstructure (particularly austenite:ferrite fraction and phase distribution) and work-hardening. As indicated in § 1.1, an exploratory approach has been chosen to address these issues.“Oh! Piglet”, said Pook excitedly, “we're going on an Expotition, all of us, with things to eat. To discover something.” “To discover what2” said Piglet anxiously “Oh! Just something.” “Nothing fierce?” “Christopher Robin didn’t say anything about fierce. ‘He just said it had an ‘x AA. Milne 888 3 Experimental 3.1 Introduction ‘As stated in § 1.1, it is the purpose of this research to contribute to the understanding of the development of the microstructure dusing and after deformation in the intercritical region of a low carbon stecl, The nature of the problem and the limited information that is presently available from literature justifies the use of an exploratory approach. A selection of commonly produced unalloyed or low-alloy steel grades has been studied by various experimental techniques. In this chapter these techniques will be discussed in as much detail as is necessary for the correct a: ment of the methods and results involved. 3.2 Materials 3.2.1 Chemical composition ‘The steel was supplied by Corus’ Hot Strip Mill No. 2 in IJmuiden (NL) and was taken fom commercially produced slabs. The chemical composition of the steels (in weight percent) is given in ‘Table 3-1. The interstitial-free (IF) steel has a very low carbon content and no free nitrogen at room temperature because of the titanium addition. The extra-low carbon (ELC) and low-carbon (LC) steel have nearly identical chemical compositions apart from a higher carbon content. The differences in manganese content can be neglected. The carbon-manganese (CMn) steel contains twice the level of carbon and manganese in comparison to the LC-steel. The nitrogen content of the CMn-steel is higher than that of the other stecls. A carbon-manganese-silicon (CMaSi) steel with high carbon content was used for the in-situ high-temperature X-ray diffraction experiments only (see chapter 6) 47Table 3-1. Chemical composition of the steels (in m%) Code c Mn si Pp s Al Ti N IF 0.002 0.150 0.008 -—«0.009~—=«O.007—~—~0.083—~=«i044 SC ELC 0.019 0.187 0.008 0.009 0.010 0.044 : 25 LC 0.052 0.230 0.004 0.010 0.012 0.052. : 26 CMn 0.103 0.490 0.006 0.010 0.014 0.035 - 45 CMnSi_ 0.180 1.500 0.180 0.012 0.007 (0.035 : 35 3.2.2 Sample preparation AAfier reheating the slabs in the reheating furnace of the IJmuiden Hot Strip Mill, the slabs were rolled in the roughing section of the hot strip mill to a thickness of about 37 mm. After roughing, the semi-finished bars were pushed off the roller table and allowed to cool to ambient temperature. After cooling, pieces of 100x150x37 (w x /x 4) mm* were cut from the bars. ‘These samples were used for the rolling trials. For the uni-axial compres: on experiments and stress relaxation experiments some samples were subjected to a laboratory hot rolling treatment in order to reduce the thickness of the strip to 6 mm for the uni-axial compression. The hot rolling treatment consisted of reheating the samples in a reheating furnace to 1250 °C over 30 minutes and then rolling to its final thickness in four passes (37 (1050 °C) - 24 (1020 °C) - 15 (1000 °C) - 10 (975 °C) - 6 mm (950 °C)). The rolling entry temperatures are given in brackets behind each pass. After hot rolling the strips were allowed to cool in still ai. From these strips the specimens for the uni-axial compression experiments in the deformation dilatometer were machined. ‘The dimensions of the samples were 10 mm in length and 5 mm in diameter. The samples for the stress relaxation experiments were 12 mm in width and 18 mm in height. The stress relaxation samples were prepared directly from the semi-finished slab with their longitudinal axis in the thickness direction of the slab. 3.2.3 Austenite fraction Fig, 3-1 shows the equilibrium austenite fraction during the hot-rolling experiments as calculated using MTData®. Since redistribution of substitutional elements like manganese is assumed to be too slow, the para-equilibrium condition was considered and not the ortho-equilibrium. It should be noted that the finish rolling temperatures were actually measured at the surface of the strip using a pyrometer. Since thete is a difference between the temperature of the surface and the centre of the strip which is estimated to be lower than 10 °C assuming a parabolic temperature distribution over the thickness of the strip), there will also be a difference in austenite fraction over the ferrite fraction 09 700 725 750 775 800 825 650 875 900 925 950 TPC} Fig. 3-1. Calculated austenite fractions as function of temperature for - (a) IF: (6) ELC: cee dea (c) LC and (d) CMn. 48To enable a quantitative evaluation of the behaviour of intercritically deformed steels, the equilibrium fractions austenite and fetrite as a function of temperature and chemical composition were calculated using MTData”, If the pseudo-binary ‘He-C’-diagram at a given Mn-concentration %yq is considered, the molar fraction of carbon in austenite in the two-phase region can be given as [49] x2 = 0.9514-0.126- X44, = (1.536-10°K 7 $2.766-10 Ky kT +(6.188-107K? +1.419-107K>- X Ma )r? G1) in which x,/ is the molar fraction of element A in phase i (note that due to the para-equilibrium assumption Xiyq'= Xiq° = Xa) T is the temperature (in K). The molar fraction of carbon in ferrite (x.°) in the two-phase region can be given as [49] 532:10°* 3.13810 + xy —(4.651-10°°K 7 -5.340-10°K7 xy, 62) ‘The ferrite and austenite fractions, fa and fy respectively, can be calculated using 63) G4) in which >; is the overall carbon content of the alloy. [irom these equations, the equilibrium fractions of ferrite and austenite as a function of carbon and manganese content and temperature can be calculated. 3.3 Pilot-mill rolling experiments 3.3.1 Rolling schedule ‘The thermomechanical treatment consisted of reheating the samples at 1250 °C for 30 minutes The samples were rolled on a Hille 100 pilot rolling mill according to the rolling schedules given [ eurcome 30 : foe | «s] 08, Se | =) % 65 =| “oe & = es 7 we = 13 € 7 a aoe average cooling rate = oa a 2) Dae a a8 - tits} Fig. 3-2. Experimental rolling schedule, Fig. 3-3. Coiling simulation from 650 °C. 49Table 3-2. Experimental roling schedule (Schedule 4 1 Table 3-2, Schedule A was used was used for the finish rolling at 950 °C, and schedule B for the finishing temperature of was used for finish rolling between 900 and 650 °C) 950 °C only, and schedule B was foo fe ae foal used for all finishing temperatures Se . from 900 down to 650 °C. F 7 37.0238 3510801050 ae ne oe Ce a eileen eater echoes were 3 153 «98 «© 95-—=—«t000-«S«« 8a = applied (eee Fig. 3.2). After 4 98 = «6335875. 85D. Finishing, the material was allowed 56340 40850900650 ty cool to the coiling temperature in still air (schedule C). Table 3-3 shows the coiling temperatures that were based on the actual (austenitic) rolling practice for the production of hot rolled finished products. The coiling simulation was performed by using controlled cooling of the specimens in a computer-controlled furnace. ‘The average cooling rate during this coiling simulation was 20 °C/h (see Fig 3-3). To investigate the influence of accelerated cooling after austenitic finishing a trial was added during which the sample was cooled to the coiling temperature on the laboratory run-out table cooling (schedule AC). The cooling rate during water-cooling on the run-out table was 40 °C, Table 3-3. Finish rolling and coiling temperatures (see also Fig 3-1). Material FRT (°C) FRT (°C) FRT (°C) eT rC) schedule Q & R ‘Schedule AC Schedule R ‘Schedule C & AC F ‘950, 900, 875 .. 700, 650 ‘950 ‘950, 900 .. 700 750 ELC 950, 900, 875 .. 700, 650 950 950, 900 .. 700 680 tc 950, 900, 875 .. 700, 650 900 900, 850 .. 700 680 Mn 950, 900, 875 .. 700, 650 900 900, 850... 700 650 To study the deformed microstructure, the specimens were quenched in water immediately after finish rolling (schedule Q). To study the microstructure and the texture before the last pass, a limited number of experiments at temperature intervals of 50 °C. (see Table 3-3) were quenched just before introduction into the mill for the last pass (schedule R) ‘After rolling, specimens for tensile testing, hardness testing, texture measurement, and Texture, hardness Fig 3-4. Orientation of the specimens for hardness, tensile tests, microstructure and texture from hot- rolled samples. 50microstructure investigation were machined from the hot rolled strip as indicated schematically in Fig 3-4. The tensile specimens were taken ftom the strip in the longitudinal direction. The gauge length was 80 mm. The specimens for the texture measurements were 49x49 mm? and the microstructure was studied in the transverse direction, 3.3.2. Determination of mean flow stress During rolling the finishing temperature, rolling forces, rolling torque and the coiling temperature are sampled. These measurements allow calculation of the flow stress of the material during rolling, The method proposed by Maccagno et al. [50] was adopted, which is based on Sims” rolling theory. The method approximates the mean flow stress by assuming sticking friction between the metal and the work rolls. ‘This results in an overestimation of the mean flow stress with regard to the true flow stress. [lowever, the inherent inaccuracies in the rolling trials and the measurement of both rolling force and torque do not justify the use of more sophisticated and mote accurate methods of calculating flow stresses from rolling experiments. As the friction coefficient during rolling is unknown, the flow stresses calculated with more sophisticated models ae not likely to be more reliable for semi-quantitative purposes than the ones obtained with Sims? approach, 3.4. Dilatometry and uni-axial compression experiments 3.44 Dilatometry For this study a Bahr 805A/D type deformation dilatometer was used. In the deformation mode the sample is mounted horizontally between two quartz tools. Fig 3-5 shows the quartz tools (1), the sample (2) with two spot-welded 0.2 mm thermocouples (type $: Pt/Pt-Rh 10%), the heating coil (3) and a quartz push rod (4). The sample is placed inside the heating coil (in the figure the sample is outside the coil for demonstration purposes). ‘The chamber can be closed and evacuated. ‘The force is applied to the left-hand tool by a hydraulic deformation system. As a result, the left-hand tool moves to the tight; the right-hand (ool remains stationary. The applied force was measured using a Burster 8438 load cell. The displacement of the left-hand tool was measured using a Schacvitz 250 HPA linear variable differential transducer (VDT). This detector is connected to the moving tool by the push rod. From the measured displacement the true strain can be calculated and from the applied force the true stress can be determined The latter calculation is done under the assumption of homogeneous deformation. Fig 3-5. Measurement chamber of Bahr dilatometer,ol . —9 ° 0 0 cc Ato coo) Boo. ts) a ts] Fig 3-8. Temperature difference T1-T2 (top) and measured temperature T1 during uni-axial compression tests — (a) good test; (b) bad test ‘The two thermocouples are spot-welded onto the surface of the sample, one in the centre of the specimen (T1, control couple), one 2 mm from the edge of the specimen (12, reference couple). ‘This allows for a rapid assessment of the temperature differences over the length of the sample and gives an indication about the homogeneity of the temperature (see Fig 3-6). The specimens are heated at a low pressure of 5x10° Pa by inductive heating using a high frequency (HF) generator. The quartz tools are not heated by the inductive heating and therefore the temperature at the tools is always lower than in the middle of the specimen because of heat conduction to the cool quartz tools, This will result in a phase gradient towards the tool in the case of intercritical annealing. ‘The specimens can be deformed by uni-axial compression with a true strain rate between 0.0005 and 10 s". The total true strain depends on the flow stress of the material and the strength of the tools, but is practically limited to 1.2. To avoid excessive barrelling of the specimens the total true strain was limited to -0.8. The specimens can be gas-cooled or quenched a). at any stage of the thermo-mechanical treatment. The cooling rate depends on the amount of deformation (increase of sample radius), the steel grade (transformation heat), and the quenching gas, but is between 50 and 100 °C/s from 800 to 500 °C. ‘The transformation temperatures were determined by reheating a solid specimen at a heating rate : : § 7 ‘equilbrium deformation ge | ie i \ — : ooo Tre} t{s) Fig 3-7. Determination of Curie temperature Fig 3-8. Dilatation as a function of time from HF-values. during intercritical annealing. 52of 3 °C/s to 1100 °C, annealing for 5 minutes and cooling at the same rate to room temperature ‘The transformation temperatures (Ac, and Ac, upon rcheating and Ar, and Ar, upon cooling) can be determined by the usual tangential method [18]. The Curie-temperature (T,) can be measured during reheating by monitoring the HI-power that is required to heat the specimen (see ig 3-7) ‘The change in magnetic properties results in a different efficiency of the HF-ficld and therefore in a change in electrical power required to impose a certain heating rate. ‘The Curie-temperature also provides an independent check on the temperature reading, 3.4.2 Uni-axial compression experiments For the uni-axial compression experiments the samples were heated in vacuum with a heating rate of 3 °C/s to Ac,+50 °C and annealed for 5 minutes at that temperature. The samples were allowed to cool to the deformation temperature freely at a maximum cooling rate of 10 °C/s. The samples were held at the deformation temperature for 60 seconds to obtain the equilibrium phase bution. Fig 3-8 shows an example of the dilatation of a CMn-sample during cooling from the annealing temperature to the subsequent intercritical holding temperature. Equilibrium conditions were already reached after 20 seconds of intercritical annealing. a).43202 0).74 £02 Fig 3-9. Austenite grain size (average over 7 points) of the steels (in ASTM, surface area micrographs 230 x 180 ur’) = (a) IF; (b) ELC; (c) LC and (d) CMn. To determine the initial austenite grain size prior to cooling to the deformation temperature in the uni-axial compression experiments, the thermal etching technique was applied [69]. Fig 3-9 shows the austenite grains at the end of the reheating stage. ‘The austenite grain size of the steels during the pilot hot rolling experiments could not be determined because of insufficient hardenability of the steels. ‘The transformation temperatures of the four steels were measured according to the procedure described in § 3.4.1, Table 3-4 shows the measured and calculated transformation temperatures and the measured Curie temperatures, Table 3-4. Calculated and measured transformation temperatures in [°C] Calculated Measured ‘Measured Ar As Aer Acs Terie a 982 915 887 916 766 ELC 720 900 730 901 768 uc 720 885 729 875 766 Mn 720 850 727 847 765From Table 3-4 it appears that the measurement of the transformation shows a good cortelation with the predicted values. These results indicate that eq. (3.1) to eq. (3.4) can be used to approximate the equilibrium phase distribution in these steels. The theoretical Curie temperature of 768 °C corresponds well with the experimental value, which indicates that the temperature measurement in the dilatometer was correct. ‘After the intercritical annealing period, the samples were compressed to a true strain of 0.8 at a strain rate of 0.1, 1.0 or 10 s" at temperatures starting from 950 °C for the IF-, ELC- and LC- steels, or 900 °C for the CMn-steel down to 650 °C at 10 °C intervals. Since the Bergstrém deformation model does not include an expression for dynamic recrystallisation, only part of the deformation curves can be used if the curve shows a maximum value d,,. In that case only the data for € < 0.8°6, are used, with & the strain corresponding to g,, (see Fig. 2-5). According to Sellars, no dynamic recrystallisation occurs below this strain &,, [19]. The measured data was fitted to the work-hardening models using an in-house developed application for the statistical software program “The SAS system for Windows” (release 8.1). The results of these experiments will be presented and analysed in § 4.3. ‘The stress-strain curves were determined from the force-displacement data assuming a homogeneous deformation. However, it is not possible to maintain homogeneity of deformation during uni-axial compression because of the friction between the metal and the tools. As a result, the material at the centre of the sample flows more easily than that near the tools. This causes the cylindrical shape to become batrcl-shaped. ‘The degree of barrelling increases with increasing friction between tool and metal. At high strains the contact area between tool and metal not only increases as a result of the compression, but also by an inversion of the cylindrical surface, a part of which was flattened out to become the peripheral ring of the circular base. Since the metal adhering to the tool barely moves, the local plastic strain and work-hardening are low. Fig. 3-10a shows the general distribution of the strain after uni-axial compression. The two end zones show the lowest strain values (white). ‘The strain values increase from almost zero in the immediate vicinity of the contact surfaces through intermediate zones (light grey) to a maximum in the centre of the specimen (dark grey). This gradient in strain values not only influences the deformation forces required to deform the specimen, but also affects the development of the microstructure after the deformation. As an example, Fig. 3-10b shows the microstructure of an ELC-steel de- formed at 775 °C and held for 60 seconds before quench- ing (total height after deforma- tion is 4.5 mm). The local dif- ferences in Fig, 9-10. Zones of different strains during uni-axial compression = (a). schematic Stain values, representation; (b). ELC deformed at 775 °C at 1 s"'and held 60 s before quenching. (ie. dislocation 34density) are reflected in a different transformation and recrystallisation behaviour after deformation. Lubrication reduces the amount of batrelling, ‘The friction coefficient at the interface can be reduced by the use of a suitable lubricant or a smart choice of sample —_ geometry. Experiments with different geometry should be limited to the adaptation of height and diameter of o the sample, because changes to the Fig. 3-11. Temperature schedule of _double-hit cylindrical nature of the specimens Compression experiments, (for instance Rastagnev) prove to be experimentally difficult and as a result show significant scatter [51]. tool a The friction coefficient at the a interface is not known. From finite em | element (FE) calculations, the a2 | relation between barrelling and 0 | | friction coefficient can be derived. 7 Therefore, if the amount of oe sn Oe tee ee ee battelling is known, the friction oe coefficient can be calculated and the or 5 a strain and stress values in the sample et ee 4 can be calculated. The influence of § oop" ic ol inhomogencous deformation on the a an stress-strain curve can thus be a determined and the experimental 2h | data can be corrected for Sa ea 010 02s inhomogencous deformation. The sirin FE-analysis will be presented and . _ analysed in § 4.6. ale ; 3.4.3 Double-hit compression cl - experiments Bey The experiments consisted of ee, reheating the cylindrical samples (10 gh ed mm in length and 5 mm @) in vacuum to Ar3+50) °C in a strain Fig. 3-12. Examples of double-hit compression deformation dilatometer (Gee Fig. 3-2 saments ~ (a) double-it with no softening compared 11). The sample was annealed for 5 10 single-hit; (b) no softening; () full softening. etminutes in order to austenitise it, followed by cooling down to the deformation temperature T'yi5 which determines the ¥/0t ratio of the material. The sample remained at Ty; for 60 seconds in order to establish 2 uniform temperature and constant phase distribution throughout the sample volume. These samples were then compressed at the selected deformation temperature at a strain rate of 1 s' to a total true strain of 0.8. This constitutes the base curve (f,, = 0). Further tests were performed in which the samples were compressed to a strain of 0.2 with a strain rate of 1s” in their first hit. This first hit was then followed by different inter-pass times /,, ranging from 0 (Le. the base curve) to 3600 s, and a second hit. Immediately after the second hit the sample was quenched to room temperature using helium gas. The response of the sample to the second hit depends on /,, and is a measure for the static softening of the sample. The static softening was determined in the austenitic range, in the ferritic range and at temperatures in the intercritical region. Fig. 3-12 shows examples of results of double-hit compression experiments. Fig. 3-12a compares a continuous curve (base curve, /,, = 0) with two subsequent deformations. Fig. 3-12b shows the shape of the curves when no softening occurs in between the two hits and Fig. 3-12c shows the situation in case of full softening. 3.4.4 Stress-relaxation experiments ‘The stress-relaxation experiments were carried out on a Gleeble 1500 thermomechanical simulator. The cylindrical specimens were 18 mm in length and 12 mm in diameter and they were machined from the transfer bar thickness of 37 mm (see § 3.2) with the axis of the cylinder in the thickness direction of the slab. The flat surfaces of the specimens were grooved to contain the lubricant during the test. The specimens are uni-axially compressed between two flat tools of which one was moving and the other remained stationary. Graphite was used as a lubricant to prevent barrelling, and tantalum foil was used to prevent sticking to the tools. An argon atmosphere prevented oxidation of the specimens during testing. ‘The specimens were reheated using low frequency resistance heating (Joule heating). A linear variable transducer measures the diameter of the specimen during straining, ‘The true strain and true stress curves can be deduced from the force-displacement curves. The specimens were reheated to Ar,+50 °C at a heating rate of 16.6 °C/s, followed by annealing at that temperature for 5 minutes. After the +40 = annealing treatment, the samples were = 100 allowed to cool to the testing & (). recovery temperature, held at that temperature for = 8% =. 30 seconds to stabilise the temperature g 2 and then compressed to a true strain of rl 0.36 at a strain rate of 1.0 s", Since this el (b). recrystallisationsTecovery pre-strain should not exceed the critical ° strain to induce dynamic recrystallisation, 4 1 10 1001000 a single-hit deformation curve was t ‘s| measured at 950 °C for each material. at erie (ot eliees elaton aves = Based on these curves, the value of 0.36 (a) with recovery only; (b) with recovery and recrystallisation. was chosen as a maximum strain. 56Immediately after the samples were compressed, the stress was continuously measured at an appropriate sampling frequency. Vig. 3-13 shows an example of a measured stress relaxation curve under conditions where static recrystallisation occurs. Using eq. (2.54), the fraction recrystallised can be derived from these curves. The results of this analysis are given in § 5.4. Fig. 3-13 also shows a stress relaxation curve under conditions where no static re ‘stallisation occurs. 3.5 Finite element simulations 3.54 Finite element modelling versus model alloys Due to the complexity of the deformation of a two-phase structure, Finite Element (FE) modelling is a useful technique for modelling o(€)-behaviour during intercritical deformation The interactions between stress, strain, and temperature in both phases are too complex to solve analytically. Several studies have been published that deal with simulations of the deformation of two-phase structures (eg. [53] - [58)) Different approaches can be adopted. Firstly, the behaviour of cells, representative of the microstructure as a whole, can be used in the simulations. ‘This is based on the simulation of a meshed representative volume of the material, and for the translation to the materials behaviour as a whole, a certain periodicity is assumed. For some materials this assumption holds relatively well, eg, for Metal-Matrix-Composites [53]. Another approach consists of defining an KH-grid resembling the actual microstructure as closely as possible [54]. The problem with this approach is that it is quite difficult to vary the microstructure to study the influence of variations in phase fractions, size or contiguity of the phases as compared to the representative cell approach (although it should be acknowledged that it can also be very difficult to find a representative cell for a complicated two-phase structuse). In many cases, the simulations in literature concentrate on the description of a hard, non-ductile phase in a soft and ductile matrix such as ferrite-martensite dual phase steels (eg, [54), fertite- pearlite steels (eg, [55] and [56]) and Ti-Mn-alloys (eg. [57] and [58)). These studies indicate that the soft phase deforms before the hard phase does, and ultimately deforms more than the hard phase. Karlsson and Sundstrém [54] find that the deformation in a two-phase structure is distributed very inhomogeneously and that this depends largely on the ratio of the flow-stresses of the hard and soft phase, The work of Ankem and Margolin [57| illustrates the difficulty in applying the flow-curve data of the single-phase constituents to the multi-phase microstructure. Moreover, the real behaviour of the single phase is not necessarily cqual to the behaviour of the same phase in a multi-phase microstructure [57]. It is unlikely that the exact microstructural features like grain size and chemical composition of the single phase in be reproduced in the multi-phase material. This is even more obvious when the composition and phase fractions change as a function of temperature as in the case of the austenite-ferrite two-phase structure in low-carbon steels. The combination of physical-mathematical models for the materials behaviour and finite-element simulations in principle circumvents this problem because these models should be capable of describing the materials behaviour as a function of composition, temperature and thermo-mechanical history 37An ideal model for the study of a two-phase system should enable mixing different quantities of phases while keeping the mechanical properties constant and should also enable different levels of continuity between the phases. Numerous studies using model alloys have been published starting as early as 1937 in a famous study by Unckel [59]. Others have used Al-Mg alloys, brasses, duplex stainless steels, or dual-phase steels as model alloys but all these attempts showed the limitations in flexibility that is required. For this reason, in the present study the response of different morphologies of the austenite-fertite two-phase structure to mechanical loading will be simulated with finite clement simulations. The inaccuracies arising from using one of the aforementioned physical model systems is felt to be larger than the inaccuracies of using a virtual model system in finite element simulations. 3.5.2, Simulation details In this study, the uni-axial compression experiments were simulated by modelling a quarter of the surface and using axial-symmetric elements. Each element therefore constitutes a ring of material. A recent study on the behaviour of dual-phase steels under plane strain compression has revealed quantitative differences between a 2D-approach and a 31D-approach with the latter providing better quantitative results, but with little or no qualitative difference [60]. Therefore, since this FE-study is not primarily concerned with accurate quantitative prediction but rather with recognising and understanding trends in the deformation behaviour of a two-phase material, it was assumed that the 31D-uni-axial compression could be approximated with a 2D-FE. simulation using axial symmetric elements. In the case of equal element size over the entire mesh, not every element represents an equal volume fraction. ‘This has to be taken into account when setting up the calculations. For the calculations the general purpose non-linear finite element program MARC* (version 7.2) has been used in combination with the graphical user interface MENTAT® (vetsion 3.2). As the fractions of ferrite and austenite depend on the temperature, the materials model in the FE-code needs to be able to take the change of materials behaviour as a function of deformation temperature into account. As shown in § 2.3.3, the model parameters in the Bergstrém work hardening model can be made temperature and strain rate dependent. This model was implemented into MARC and the FE-code was subsequently used to simulate uni- axial compression experiments of the LC-steel in the intercritical region. Calculations were performed with this system and the predicted flow curves at different temperatures were compared to the measured curves. The results are presented in § 4.6. ‘The deformation model simulates uni-axial compression tests on material samples at different temperatures. Bec two-dimensional (quarter) section of the sample (see Fig. 3-14a). Dimensions are chosen according to the experimental settings, ic. 10 mm length and 5 mm diameter. The computation domain is divided into a grid of 50 elements in the axial direction and 25 clements in the radial direction. Consequently, a single element in the 50 x 25 grid has a length and width of 200 jim. Ferrite grain sizes of hot-rolled low-carbon steels are usually of the order of 5 to 10 [im. For a 1- to-1 modelling of the actual grain size, mesh sizes of 1000 x 500 would be required. Test runs using the same microstructure but divided into different grids show that the influence of the mesh on the calculated deformation behaviour is negligible if the grid dimensions exceed 30 x 15 of the rotational symmetry, the model is confined to the description of a 58a). b). Fig. 3-14, The computation domain in undeformed (left) and deformed state (right). cells (see Fig. 3-15). As shown in Fig. 3-15, the grid refinement beyond 50 x 25 would have affected the results neither qualitatively nor quantitatively. Deformation is brought about by the movement of a pointed stamp into the material. This stamp is included in the model as a rigid body, represented here by a line because of the rotational symmetry (see Fig. 3-14a for the 50 x 25 case). The angle between the pointed tool and the sample is 0.75°. Compression is pursued to a true strain of 0.5 at a strain rate of 0.1 s". As far as the temperature is concemed, the model assumes a homogeneous and isothermal behaviour of the material. The thermal flux into the stamps is neglected. 3.5.3 Contiguity and friction The contiguity of a two-phase material (see § 2.6.2) has an influence on the deformation behaviour of the aggregate. The directionality of both phases has a strong influence as well. The latter can be easily understood by compasing the iso-strain (both phases parallel) and the equi- stress (both phases in series) versions of the mixture rule (see § 2.6.3). In contrast to the mixture rule, which adds up the flow stresses or strains o 102 of the two separate 840° 10x5 . 100 x 100 phases weighed with _ a: - e = their fractions, finite’ ok ee & element models take into = 60} 6 Fo 3 —O- 1055 3 account local differences 8 4g | eee enae a8 3 6 in strain behaviour. The —O- 50x25 ; 20 S— 70x35 70x35 4 92 influence ofthe “ : ° 90 contiguity can be studied 00 01 02 03 04 05 045 046 i cee ee strain strain structures with a Fig, 3-15. Compression curves of a two-phase microstructure predicted different degree of by the mode! for diferent FE-meshes. linkage between the 59phases. However, in a practical model alloy, the influence of the contiguity cannot easily be separated from the possible change in inherent strength of the constituent phases. FE simulations do allow changing the contiguity and directionality without affecting the constitutive behaviour of the constituents. A number of calculations have been performed to assess the train curve and on the stress-strain magnitude of the influence of contiguity on the stre: behaviour of the phas ‘The uni-axial compression experiments were simulated by an inward movement of the faces perpendicular to the axis. Initially, this movement was taken to be frictionless and uniform Microstructures were constructed by randomly assigning material properties of either the ferrite of the austenite phase to individual elements, while the total volumes of both phases were in accordance with the imposed fractions. AAs a sequel, the contact between tool and sample and the resulting friction has been taken into account. Additionally the phase distribution at a given fraction was varied. This made it possible to investigate the influence of phase distribution on the flow curve in a more systematic way. In this case, no comparison with measured compression curves is possible, because these have not been determined for similar microstructures as constructed in the calculations. The friction coefficient that should be used in FE-calculations to describe the deformation dilatometer experiments under the chosen experimental conditions (see § 3.4.2) could be determined by comparing the barrelling found in actual experiments with the calculated barrelling, Furthermore as a result of the chosen approach, friction is implicitly incorporated in the Bergstrim model parameters. ‘The Bergstrom model parameters for the FE-simulations were determined based on the experiments with the LC-steel as described in § 3.4.2. The model parameters implicitly include the influence of friction. In this form the Bergstrém model can be used to simulate the flow curve of LC-steels (see § 4.6) under the assumption that the friction conditions remain unaffected. The model can also be used to study the qualitative effect of friction on the flow curve or the shape of the sample during compression. A friction coefficient can be determined by simulating the flow curve with different friction coefficients. However, it is not justified to simulate the flow curve using the Bergstrém model parameters and the optimum friction coefficient because the friction is already implicitly included in the model parameters. So imposing friction using these model parameters would not be justified. Friction is known to play an important role in the contact between tool and sample. It leads to an inhomogeneous dilatation of the material in the radial direction, and barrel shaped samples after deformation, In the simulations, this friction is described by a Coulomb model. ‘This model is characterised by a friction coefficient [71]. Fig. 3-16 displays the barrel shapes predicted for different values of this coefficient J1 at 720 °C (100% ferrite) and at 880 °C (100% austenite). Sample radii have been measured. ‘The average diameter in the middle of the sample is 3.75 mm and 3.33 mm at the edges for 720 °C, and 3.65 mm in the middle and 3.35 at the edges for 880 °C. By using a friction coefficient of {= 0.1 the best agreement between observed and predicted barrel shape is obtained. For comparison, compression curves are given in Fig. 3-17 for a calculation at 720°C using a flat tool without friction, a pointed tool without friction and a pointed tool with friction. It appears 60