Abstract This thesis has been made within the European Industrial Doctorate (EID) project called Mathematics and Materials Science for Steel Production and Manufacturing, abbreviated as MIMESIS, which has five partners: EFD Induction in Norway; SSAB, Outokumpu, and the University of Oulu in Finland; and Weierstrass Institute for Applied Analysis and Stochastics (WIAS) in Germany. The main aim of this work was to develop a steel composition and processing route suitable for making a slurry transportation pipeline with the aid of induction hardening, and to characterize the phase transformations and microstructures involved in the various stages of the processing route. A novel steel chemistry was designed based on metallurgical principles assisted by computational thermodynamics and kinetics. The designed composition is a medium-carbon, low-alloy steel microalloyed with niobium, in wt.% 0.40 C, 0.20 Si, 0.25 Mn, 0.50 Mo, 0.90 Cr, and 0.012 Nb. This was subsequently cast, thermomechanically rolled on a laboratory rolling mill to two bainitic microstructures, and finally subjected to the thermal cycles predicted to be encountered with the internal induction hardening of a typical pipe geometry. The phase transformations and microstructures found at various stages of the simulated production process have been characterized and algorithms developed to enable the optimization of microstructure and hardness through the pipe wall thickness. / Tiivistelmä Tämä väitöskirja on tehty osana Euroopan teollisuustohtori (European Industrial Doctorate, EID) -ohjelmaa projektissa eli Matematiikka ja materiaalitiede teräksen valmistuksessa ja käytössä (Mathematics and Materials Science for Steel Production and Manufacturing, MIMESIS). Ohjelmassa on viisi partneria: EFD Induction Norjasta; SSAB, Outokumpu ja Oulun yliopisto Suomesta; ja Weierstrass Institute for Applied Analysis and Stochastics (WIAS) Saksasta. Työn päätavoitteina oli kehittää teräksen koostumusta ja prosessointireittiä, jotka soveltuvat lietteen kuljetusputken valmistukseen induktiokarkaisun avulla, sekä karakterisoida prosessin eri vaiheiden aikana tapahtuvat faasimuutokset ja mikrorakenteet. Uusi teräskoostumus suunniteltiin metallurgisten periaatteiden pohjalta hyödyntämällä laskennallista termodynamiikkaa ja kinetiikkaa. Suunniteltu teräs on niobilla mikroseostettu, matalaseosteinen ja keskihiilinen, eli painoprosentteina 0,40 C, 0,20 Si, 0,25 Mn, 0,50 Mo, 0,90 Cr ja 0,012 Nb. Teräs valettiin, valssattiin ja jäähdytettiin termomekaanisesti laboratoriovalssaimella kahdeksi bainiittiseksi mikrorakenteeksi ja lopulta altistettiin lämpösykleille, joiden ennustettiin olevan tyypillisiä sisäisesti induktiokarkaistulle teräsputkelle. Simuloidun tuotantoprosessin eri vaiheissa havaitut faasimuutokset ja mikrorakenteet on karakterisoitu. Sen lisäksi on kehitetty algoritmit, jotka mahdollistavat mikrorakenteen ja kovuuden optimoinnin putken seinämän paksuuden läpi.

Ce travail de thèse vise à comprendre et à modéliser les mécanismes de transformation de phase d'austénite en bainite dans un acier bas carbone faiblement allié et en particulier d'étudier une éventuelle sélection de variants à l'échelle locale. Une campagne d'essais de torsion a permis de déterminer des lois de comportement des phases austénitique et bainitique à haute température afin d'améliorer un modèle existant de sélection de variants et d'obtenir des échantillons présentant différentes microstructures de l'austénite avant transformation. Puis des essais de transformation bainitique isotherme ont été réalisés afin de pouvoir étudier l'influence de la température de transformation et de la taille de grain austénitique sur la sélection de variants. L'étude des microtextures a été réalisée grâce à la technique EBSD qui nous a permis de confirmer la présence d'une répartition non aléatoire des variants voisins au sein d'un ancien grain austénitique. Le modèle micromécanique de sélection de variants porte sur un critère d'auto-accommodation de la déformation de transformation entre certains variants afin de réduire l'énergie globale du système composé de l'austénite et de plusieurs variants de bainite. Les déformations de transformation sont déterminées à l'aide de la PTMC, puis les interactions entre les différents variants sont obtenues en résolvant un problème d'inclusions d'Eshelby. La confrontation des résultats expérimentaux avec ceux du modèle induit une meilleure compréhension des microstructures de martensite et de bainite formées à basse température par le critère d'auto-accommodation des déformations de transformation que celles formées à haute température.

During this study, the correlation between the evolution of the prior austenitic grain size and of the precipitation state during thermal treatment performed on steels is presented. To do this, the precipitation state has been finely characterized. Precipitate volume fractions were measured by plasma spectroscopy. Transmission Electron Microscopy (TEM) was used to determine the precipitate size distributions (HAADF images) and the precipitate chemical composition (EDX, EELS for carbon and nitrogen). In order to treat ELLS spectra obtained on complex carbonitrides (V,Nb,Ti)(C,N), a routine based on the Least Mean square Fitting have been developed. Results obtained with this method are in gopd agreement with those obtained by EDX analysis for metallic elements (Nb, V, Ti, ...). Then, grain size distributions were determined using a special etching called "Bechet-Beaujard", which reveals the prior austenite grain boundaries. Two alloys have been characterized in this study. (i) A model alloy, the FeVNbCN, which presents two precipitate types, NbC and VCN. This alloy was chosen to study the role of nitrogen on the precipitation state during reversion treatments. A model predicting the precipitation kinetics, coupled with a model for grain growth, give a good agreement with experimental results on grain sizes, precipitate sizes and on precipitate volume fraction. (ii) An industrial steel, the 16MnCr5+Nb was also studied. This alloy exhibits the presence of AlN and NbC precipitates. The correlation obtained between the Prior Austenite Grain Size and the evolution of the precipitation state shows that a large volume fraction of small precipitates allows a great pinning of grain boundaries. Finally, during thermo-mechanical treatments performed in the industry, some large grains may grow faster than smaller grains, leading to the so-called abnormal grain growth. This kind of growth can lead to undesirable mechanical instabilities. We have developed a criterium for abnormal grain growth which predicts the risk of such growth for a given precipitation state. This model presents a good agreement with all experimental results for both studied alloys.

<p>The goal of this work has been to evaluate the different experimental techniques used for quantitative analysis of multi-phase materials systems. </p><p>Powder based specimens containing two-phases, austenite and ferrite , were fabricated and quantified. The volume fraction of ferrite varied from 2 Vol% to 50 Vol%. </p><p>X ray powder diffraction (XRD) measurements were based on two peak analysis. Computer based software Topas was used for quantitative analysis, which is believed to be the most advanced in this field. XRD results were found within the absolute limit of +/- 4% of given ferrite volume fraction. Volume fraction as low as 2 Vol% was successfully detected and quantified using XRD. However, high statistical error was observed in case of low volume fraction, such as 2 Vol% and 5 Vol% ferrite volume fraction. </p><p>Magnetic balance (MB) measurements were performed to determine the volume fraction of magnetic phase, ferrite. MB results were found in good agreement with given volume fractions. As low as 2 Vol% volume fraction was detected and quantified with MB. MB results were within the absolute limit of +/- 4% of given ferrite volume fraction. </p><p>Image analysis (IA) was performed after proper sample preparation as required by electron backscatter diffraction (EBSD) mode of Scanning electron microscopy (SEM). IM results were found within the absolute limit of +/- 2 % of given ferrite volume fraction. However, high statistical error was observed in case of 2 Vol% volume fraction.</p>

L'augmentation constante de la circulation automobile a travers le monde fait des effluents gazeux un des problèmes majeurs de toutes les sociétés modernes. Tant d'un point de vue économique et écologique, chacun s'accorde sur le fait que la consommation de carburants fossiles utilisés dans le transport doit baisser, principalement en réduisant le poids des véhicules. Le développement de matériaux à hautes performances et à bas prix est donc indispensable. Pour atteindre cet objectif, cette étude visait à élucider les interactions entre la déformation et les transformations de phase dans les aciers a hautes performances qui pourraient remplir les conditions de réduction de poids. En effet, une large gamme de travaux a montrer que les transformations de phase induites mécaniquement (effet TRIP) de l'austénite peuvent être à l'origine d'une amélioration des propriétés mécaniques dans de nombreuses nuances d'acier. Les transformations de phase induites par la déformation dépendent de deux paramètres : la stabilité relative et l'énergie de fautes d'empilement de l'austénite, qui sont affectes par différents facteurs. Les interactions entre les transformations de phase et les propriétés mécaniques de différentes nuances Cr-Ni et Mn-Si-Al furent examinées sous plusieurs conditions de taille de grain, de température et d'état de chargement. Des relations particulières furent établies entre les phénomènes qui se produisent a l'échelle des grains individuels et a l'échelle macroscopique. Les mécanismes cristallographiques des transformations de phase successives (austénite - martensite e - martensite a') ont été mis en évidence. Finalement, différentes techniques de raffinage de la taille de grain furent utilisées pour produire des aciers inoxydables comportant des tailles de grain variées, et l'efficacité de ces techniques a été comparée. Pour cela, les cinétiques de retransformation, recrystallisation et croissance des grains ont été étudiées. La réduction de taille des grains par cycles de transformations de phase fut établie comme plus efficace de la méthode classique par déformation - recristallisation. / The continuously increasing use of automobiles all over the world, is making of gas effluents one of the major concerns for all modern societies. From economical and ecological points of view, everyone agrees on the fact that the consumption of fossil fuels for transport must decrease, particularly by vehicle weight reduction. Development of high performance materials at low cost is therefore needed. In order to achieve this requirement, the present work aimed at investigating the interactions between straining and phase transformations in high performance steels that could meet the weight saving requirements. Indeed, a wide range of studies has shown that mechanically-induced phase transformations (TRIP effect) of the austenite may bring about improved mechanical properties in different steel grades. Strain-induced phase transformations depend on two parameters : the relative stability and the stacking fault energy of the austenite, which are affected by different factors. The interactions between the phase transformations and the mechanical properties of different Ni-Cr and Mn-Si-Al grades were examined under various conditions of grain size, temperature or stress state. Particular relationships were clearly established between the phenomena taking place at the scale of the individual grains and at the macroscopic scale. The crystallographic mechanisms of the successive strain-induced phase transformations (austenite - e-martensite - a'-martensite) has been clarified. Finally, different techniques of grain refinement were used to process stainless steels with various grain sizes, assessing the efficiency of these techniques. Therefore, the kinetics of retransformation, recrystallisation and grain growth were studied. Grain refinement by cycles of phase transformations was found more effective than the classical deformation - recrystallisation method.

For ecological reasons, the current main challenge of the automotive industry is to reduce the fuel consumption of vehicles and then emissions of greenhouse gas. In this context, steelmakers and automotive manufacturers decided for some years now to join their efforts to promote the development and use of advanced high strength steels such as TRIP steels. A combination of high strength and large elongation is obtained thanks to the TRansformation Induced Plasticity (TRIP) effect. However, improvement of the mechanical properties is still possible, especially by the refinement of the matrix. In this work, two main ways were followed in order to reach improved properties. The classical way consisting of the annealing of cold-rolled samples and an innovative way consisting of obtaining the desired microstructure by direct hot rolling of the samples. In the classical way, this refinement can be obtained by acting on the chemical composition (with such alloying elements like Cu and Nb). It was observed that complete recrystallisation of the ferrite matrix is quite impossible in presence of Cu precipitates. In addition, if the ferrite recrystallisation is not completed before reaching the eutectoid temperature, the recrystallisation will be slowed down by a large way. An innovative heat treatment consisting in keeping the copper in solid solution in the high-Cu steel was developed. Therefore, ferrite recrystallises quite easily and very fine ferrite grains (~1µm) were obtained. In the innovative way, the effects of hot-rolling conditions on TRIP-assisted multiphase steels are of major importance for industrial practice and could open new dimensions for the TRIP steels (i.e. thanks to precipitation mechanisms leading to additive strengthening). Impressive mechanical properties (true stress at maximum load of 1500 MPa and true strain at uniform elongation of 0.22) were obtained with a relatively easy thermomechanical process, the role played by Nb being essential.

This thesis contains the development of a physically-based model describing the microstructural evolution during hot deformation of microalloyed steels. The work is mainly focused on the recrystallization kinetics. During hot rolling, the repeated deformation and recrystallization provides progressively refined recrystallized grains. Also, recrystallization enables the material to be deformed more easily and knowledge of the recrystallization kinetics is important in order to predict the required roll forces. Hot strip rolling is generally conducted in a reversing roughing mill followed by a continuous finishing mill. During rolling in the roughing mill the temperature is high and complete recrystallization should occur between passes. In the finishing mill the temperature is lower which means slower recrystallization kinetics and partial or no recrystallization often occurs. If microalloying elements such as Nb, Ti or V are present, the recrystallization can be further retarded by either solute drag or particle pinning. When recrystallization is completely retarded and strain is accumulated between passes, the austenite grains will be severely deformed, i.e. pancaking occurs. Pancaking of the grains provides larger amount of nucleation sites for ferrite grains upon transformation and hence a finer ferrite grain size is achieved. In this work a physically-based model has been used to describe the microstructural evolution of austenite. The model is built-up by several sub-models describing dislocation density evolution, recrystallization, grain growth and precipitation. It is based on dislocation density theory where the generated dislocations during deformation provide the driving force for recrystallization. In the model, subgrains act as nuclei for recrystallization and the condition for recrystallization to start is that the subgrains reach a critical size and configuration. The retarding effect due to elements in solution and as precipitated particles is accounted for in the model. To verify and validate the model axisymmetric compression tests combined with relaxation were modeled and the results were compared with experimental data. The precipitation sub-model was verified by the use of literature data. In addition, rolling in the hot strip mill was modeled using process data from the hot strip mill at SSAB Strip Products Division. The materials investigated were plain C-Mn steels and Nb microalloyed steels. The results from the model show good agreement with measured data. / QC 20100706

The goal of this work has been to evaluate the different experimental techniques used for quantitative analysis of multi-phase materials systems. Powder based specimens containing two-phases, austenite and ferrite , were fabricated and quantified. The volume fraction of ferrite varied from 2 Vol% to 50 Vol%. X ray powder diffraction (XRD) measurements were based on two peak analysis. Computer based software Topas was used for quantitative analysis, which is believed to be the most advanced in this field. XRD results were found within the absolute limit of +/- 4% of given ferrite volume fraction. Volume fraction as low as 2 Vol% was successfully detected and quantified using XRD. However, high statistical error was observed in case of low volume fraction, such as 2 Vol% and 5 Vol% ferrite volume fraction. Magnetic balance (MB) measurements were performed to determine the volume fraction of magnetic phase, ferrite. MB results were found in good agreement with given volume fractions. As low as 2 Vol% volume fraction was detected and quantified with MB. MB results were within the absolute limit of +/- 4% of given ferrite volume fraction. Image analysis (IA) was performed after proper sample preparation as required by electron backscatter diffraction (EBSD) mode of Scanning electron microscopy (SEM). IM results were found within the absolute limit of +/- 2 % of given ferrite volume fraction. However, high statistical error was observed in case of 2 Vol% volume fraction.

<p>Recrystallization kinetics, during and after hot deformation, has been investigated for decades. From these investigations several equations have been derived for describing it. The equations are often empirical or semi-empirical, i.e. they are derived for certain steel grades and are consequently only applicable to steel grades similar to these. To be able to describe the recrystallization kinetics for a variety of steel grades, more physically based models are necessary.</p><p>During rolling in hot strip mills, recrystallization enables the material to be deformed more easily and knowledge of the recrystallization kinetics is important in order to predict the required roll forces. SSAB Tunnplåt in Borlänge is a producer of low-carbon steel strips. In SSAB’s hot strip mill, rolling is conducted in a reversing roughing mill followed by a continuous finishing mill. In the reversing roughing mill the temperature is high and the inter-pass times are long. This allows for full recrystallization to occur during the inter-pass times. Due to the high temperature, the rather low strain rates and the large strains there is also a possibility for dynamic recrystallization to occur during deformation, which in turn leads to metadynamic recrystallization after deformation. In the finishing mill the temperature is lower and the inter-pass times are shorter. The lower temperature means slower recrystallization kinetics and the shorter inter-pass times could mean that there is not enough time for full recrystallization to occur. Hence, partial or no recrystallization occurs in the finishing mill, but the accumulated strain from pass to pass could lead to dynamic recrystallization and subsequently to metadynamic recrystallization.</p><p>In this work a newly developed physically based model has been used to describe the microstructural evolution of austenite. The model is based on dislocation theory where the generated dislocations during deformation provide the driving force for recrystallization. The model is built up by several submodels where the recrystallization model is one of them. The recrystallization model is based on the unified theory of continuous and discontinuous recovery, recrystallization and grain growth by Humphreys.</p><p>To verify and validate the model, rolling in the hot strip mill was modeled using process data from SSAB’s hot strip mill. In addition axisymmetric compression tests combined with relaxation was modeled using experimental results from tests conducted on a Gleeble 1500 thermomechanical simulator at Oulu University, Finland. The results show good agreement with measured data.</p>

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