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. 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. 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. 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. / QC 20101118

This study focuses on the laser powder bed fusion processing of NiTi alloys and the feasibility of fabricating very thin stent structures for biomedical applications. A comprehensive correlation between the process and the material’s-structure and properties is established to facilitate the fabrication of NiTi alloys with tailored properties. In the first step, the impact of LPBF processing parameters and post-treatments on evolving the microstructure, texture, superelasticity, and asymmetry is examined. Subsequently, the feasibility of manufacturing very thin mesh structured stents is scrutinized followed by in-depth investigations into differently designed stents considering properties such as surface characteristics, mechanical properties, superelasticity, and recoverability. The obtained results and the represented discussions offer imperative insights, helping to better understand the complexity of the LPBF process and the present challenging aspects. Moreover, detailed contributions are made with the goal of paving the road ahead for the production of patient-specific NiTi stents with enhanced properties. / Thesis / Doctor of Philosophy (PhD)

L'Inconel 718 est un superalliage base-nickel très utilisé pour la fabrication de pièces aéronautiques soumises à de fortes contraintes et de hautes températures. La maîtrise de la microstructure finale issue de la mise en forme à chaud est un des éléments clés pour le contrôle des propriétés mécaniques et pour répondre aux exigences strictes du secteur. Dans cette étude, l'évolution de la microstructure de l'Inconel 718 est étudiée au moyen d'essais de torsion suivis d'une trempe à l'eau (pour examiner les évolutions dynamiques) ou d'un maintien à la température de déformation puis d'une trempe à l'eau (pour examiner les évolutions post-dynamiques). Ces essais sont réalisés dans les domaines de température δ-supersolvus et δ-subsolvus et pour des vitesses de déformation de 10-2 à 0.1 s-1. Des analyses microstructurales par microscopie électronique à balayage et cartographie des orientations cristallographiques par EBSD sont réalisées pour suivre l'évolution de la fraction recristallisée, de la taille de grains recristallisés ainsi que de l'état de précipitation lors de la déformation et des maintiens pré- et post-déformation. Sur base de ces observations expérimentales, les principaux mécanismes métallurgiques actifs sont identifiés, puis modélisés : écrouissage, germination de nouveaux grains, migration de joints de grains, et interaction avec les particules de seconde-phases. Un modèle d'évolution microstructurale en champ moyen a été enrichi pour prendre en compte l'ensemble de ces mécanismes élémentaires et leur dépendance aux conditions thermomécaniques. Ce modèle permet de décrire, pour les domaines δ-subsolvus et δ-supersolvus, les cinétiques de recristallisation dynamique et post-dynamique de l'Inconel 718, les cinétiques de précipitation et dissolution de la phase δ, ainsi que l'évolution de la taille de grains. Il prédit également les courbes contrainte-déformation dans le domaine de température δ-supersolvus. / Inconel 718 is nickel-based Superalloy widely used in the aeronautic industry to manufacture aircraft parts subjected to extreme in-service conditions of high stresses at elevated temperatures. Controlling the microstructure after hot forming is a key element to control the mechanical properties of the final products and meet the tight specifications imposed by the aeronautic industry.In this work, the microstructure evolution of Inconel 718 was investigated via isothermal and iso-strain rate torsion tests followed by water quenching (to investigate dynamic evolution) or by annealing at deformation temperature then water quenching (to investigate post-dynamic evolution). These tests were conducted in both δ-Supersolvus and δ-Subsolvus temperature domains and for strain rates of 0.01 to 0.1 s-1.Scanning electron microscopy (SEM) and Electron Back Scattered Diffraction (EBSD) were used to characterize the microstructure and follow the evolution of the recrystallized fraction, the recrystallized grain size and the δ-phase precipitation after deformation and during pre-deformation and post-deformation annealing. Based on these experimental observations, the main metallurgical mechanisms have been identified and modelled: hardening, nucleation of new grains, grain boundaries migration and the δ-phase- recrystallization interaction.A two-site mean field approach having a low computational cost was chosen to model the microstructural evolution at different thermomechanical conditions. This model describes the main mechanisms taking place during hot forming of Inconel 718 in both δ-Supersolvus and δ-Subsolvus domains and predicts the recrystallization kinetics in both dynamic and post-dynamic regimes , the δ-phase precipitation and dissolution kinetics and the grain size evolution. The model predicts also the strain-stress curves at high temperatures in the absence of δ-phase particles.

La présente thèse s’inscrit dans un contexte d’optimisation des procédés de forgeage et de traitements thermiques des alliages de titane pour les pièces de moteurs Snecma.Les sociétés TIMET, élaborateur, et SNECMA, motoriste, ont identifié des enjeux très analogues concernant le forgeage des billettes en alliage de titane destinées à la fabrication de disques moteurs. Il est nécessaire d'acquérir une maîtrise complète de la gamme de transformation, de la coulée au produit final. Ce traitement thermomécanique comporte une alternance d’étapes de forgeage dans les domaines bêta, à haute température, et alpha + bêta, à basse température.L’objectif est de déterminer expérimentalement et de modéliser le comportement mécanique ainsi que les évolutions de microstructure de l’alliage Ti17 au cours d'une déformation dans le domaine alpha + bêta suivie d’un maintien en bêta.En amont, ces travaux mènent à une meilleure compréhension des facteurs qui influencent la taille de grain dans le domaine bêta : la taille de grain bêta initiale, les orientations des aiguilles alpha dans le grain, la déformation et la désorientation subies lors du forgeage en alpha + bêta, etc.En ce qui concerne les applications, ils s’intègrent à un post-processeur métallurgique dédié au forgeage des alliages de titane, qui utilise les histoires thermomécaniques issues d’un calcul par éléments finis. / The thesis is part of a broader optimization program related to the forging and the heat treatments of SNECMA-engine components in titanium alloys.TIMET (producer) and SNECMA (engine manufacturer) companies have identified very similar issues concerning the forging of billets in titanium alloy for manufacturing engine discs. They need thus to gain complete control over the transformation range, from the casting to the final product. This thermomechanical treatment involves alternating forging steps in the beta domain, at high temperature, and in the alpha + beta field, at lower temperatures.The aim is to simulate the forging step in the two-phase, alpha + beta, range followed by recrystallization in the beta field during which microstructure evolves. This simulation involves the following phenomena: grain deformation, recrystallization and grain growth of the beta matrix and disorientation/fragmentation of the alpha-Widmanstätten platelets. More specifically, the effects of deformation in the alpha + beta field on the subsequent beta-grain growth during the heat treatment at higher temperatures have been analyzed in the case of Ti17 titanium alloy.Upstream, the work leads to a better understanding of the factors that influence grain size in the beta domain: the initial beta-grain size, the orientation of alpha needles in the grains, the distortion and disorientation experienced during the alpha + beta forging, etc. With regard to the applications, the above results will be implemented into a metallurgical post-processor dedicated to the forging process of titanium alloys, using the thermomechanical history resulting from a finite-element calculation.

L'élaboration des aciers ODS fait appel à une étape de consolidation par filage à chaud. Les propriétés très anisotropes de ces matériaux à l'état filé, notamment les nuances purement ferritiques (>12% Cr), nécessitent une meilleure compréhension des effets du procédé de filage sur la microstructure. Ainsi, ce travail de thèse a pour objectif principal d'étudier les évolutions de la microstructure lors de la transformation à chaud des aciers inoxydables ODS ferritiques, et plus globalement de comprendre le comportement de ces matériaux sous sollicitation mécanique à haute température. Pour cela, des essais de filage interrompus et des essais thermomécaniques de torsion et de compression à chaud (1000-1200°C) ont été réalisés sur plusieurs aciers ferritiques à 14% de Cr présentant différents taux de renfort en titane et en yttrium. Les microstructures obtenues après déformation ont été caractérisées par EBSD.L'ensemble des analyses microstructurales effectuées montre que la mise en forme à chaud des aciers ferritiques par filage s'accompagne d'une recristallisation dynamique de type continue. Après formation des sous-joints par restauration, leurs désorientations continuent à croître, et ceux-ci se transforment graduellement en joints de grains au cours de la déformation. La cinétique de ce mécanisme semble néanmoins fortement influencée par les caractéristiques de la précipitation présente dans le matériau ; la recristallisation devenant moins complète lorsque les précipités sont plus fins et plus nombreux. En plus du taux de renfort, l'étude de la déformation de ces nuances en torsion et en compression dans des conditions proches de celles observées en filage révèle également une forte influence de la température sur leur comportement. Les microstructures de déformation présentent une évolution d'autant plus importante que la température et/ou le taux de renfort sont limités. À 1000°C, les évolutions observées indiquent la présence de la recristallisation dynamique continue. En revanche, lorsque l'on augmente la température et/ou le taux de renfort, la déformation s'accompagne d'une évolution limitée de la microstructure, notamment en torsion où un endommagement sévère aux niveaux des joints de grains est observé. Dans ce cas, les résultats sont interprétés par un mécanisme d'accommodation de la déformation au voisinage des joints de grains. Les paramètres rhéologiques calculés à partir de ces essais mécaniques confirment la tendance à une faible activité plastique au sein des grains dans les nuances renforcées. / The production of ODS steels involves a powder consolidation step usually using the hot extrusion (HE) process. The anisotropic properties of extruded materials, especially in the ODS ferritic grades (>wt%12Cr), need a better understanding of the metallurgical phenomena which may occur during HE and lead to the observed microstructure. The hot working behavior of these materials is of particular interest. The methodology of this work includes the microstructure analysis after interrupted hot extrusion, hot torsion and hot compression (1000-1200°C) tests of ferritic steels with 14%Cr and different amounts in Ti and Y2O3.The microstructure evolution during hot extrusion process is associated with continuous dynamic recrystallization (CDRX). It leads to the creation of new grains by the formation of low angle boundaries, and then the increase of their misorientation under plastic deformation. The investigations highlight also the role of precipitation on the kinetics of this mechanism; it remains incomplete in the presence of fine and dense nanoprecipitates. After hot deformation in torsion and compression, it is noticed that both precipitates and temperature deformation have a significant impact on the deformation mechanisms and microstructure evolution. Indeed, the CDRX is dominant when temperature and amount of reinforcement are limited. However, when they are increased, limited microstructure evolution is observed. In this case, the results are interpreted through a mechanism of strain accommodation at grain boundaries, with low dislocation activity in the bulk of the grains.

Les raccords et connexions de caténaires ont un rôle important dans l’intégrité électrique et mécanique des caténaires. Ces pièces sont pour la plupart constituées d’un alliage de cuivre Cu-Ni-Si mis en forme par forgeage à chaud. Dans un contexte de fiabilisation du réseau ferroviaire, l’amélioration de leurs performances et de leurs procédés de fabrication est recherchée. Ces travaux se concentrent sur l’étape de mise en forme de ces pièces, et ont pour objectif de mieux comprendre les couplages matériaux-procédés des alliages Cu-Ni-Si.Une campagne expérimentale de compression est menée. Elle permet de développer un modèle rhéologique à base physique décrivant le comportement d’un alliage Cu-Ni-Si dans les gammes de température 800 - 950 °C et de vitesse de déformation 0.1 - 10 s−1. Il tient compte des phénomènes d’adoucissement par restauration et recristallisation dynamiques. Le modèle ainsi créé est ensuite implémenté dans un logiciel éléments finis.Un nouvel essai de formabilité est proposé. Il permet de reproduire les sollicitations mécaniques rencontrées lors d’un procédé de forgeage et vise à déterminer les conditions limites de formabilité d’un matériau. La mise en forme d’une pièce de référence est étudiée par le biais de cet essai. Sa caractérisation précise en matière de champ de déformations et de contraintes permet d’identifier les paramètres expérimentaux. Les résultats identifient une température limite de forgeage en-deçà de laquelle des fissures sont prédites dans la pièce. / Contact wire splices play a leading role in the electric and mechanical integrity of the catenary systems. Most of these parts are made of Cu-Ni-Si alloys and manufactured by a hot forging process. With the aim of increasing the reliability of the railway network, the improvement of their performances and their manufacturing processes is sought. This work is focused on the forming stage of these parts and aims to give a better understanding of the materials-processes couplings for the Cu-Ni-Si alloys.An experimental campaign including compression tests is conducted. It allows the development of a physically-based model to describe the rheological behavior of a Cu-Ni-Si alloy deformed in the temperature range between 800 °C and 950 °C, at strain rates in the range of 0.1 - 10 s−1. It takes into account the work-softening implied by dynamic recovery and dynamic recrystallization. The model thus created is then implemented in a finite element software.A new workability test is proposed. Its purpose is to reproduce the mechanical conditions encountered in a forming process and to determine the critical conditions of workability related to a material. The forging process of a reference part is studied by means of this test. An accurate characterization of the process in terms of strain magnitude and stress field allows the identification of the experimental parameters. The results lead to the identification of a limit temperature of workability below which fractures are predicted in the part.

京都大学 / 0048 / 新制・課程博士 / 博士(工学) / 甲第20703号 / 工博第4400号 / 新制||工||1684(附属図書館) / 京都大学大学院工学研究科材料工学専攻 / (主査)教授 辻 伸泰, 教授 乾 晴行, 教授 安田 秀幸 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DFAM

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In this study polycrystalline NiAl has been subjected to torsion deformation. Torsion has been used because of its characteristics. By this deformation mode high shear strains (gamma = 18 in this study) can be imposed on the sample. The deformation conditions are well-defined because of the local deformation mode, which is simple shear. Due to the monoclinic sample symmetry one half of the pole figure is needed in order to obtain the complete texture information, which is more than is needed e.g. by extrusion or rolling. Therefore, texture analysis might be more sensitive with respect to texture components. Furthermore, torsion deformation is characterized by being inhomogeneous in terms of the amount of shear strain and shear strain rate along the sample radius. The shear strain gradient makes the analysis of different stages of deformation on the same sample (i.e. under the same deformation conditions) possible. Another characteristic being special for torsion is that samples change their length, although no axial stress is applied. This effect is known as Swift effect and will be analyzed in detail. The deformation, microstructure and texture development subject to the shear strain are studied by different techniques (Electron Back-Scatter and High Energy Synchrotron Radiation). Beside the development of microstructure and texture with shear strain, the effect of an initial texture as well as the deformation temperature on the development of texture and microstructure constitute an important part of this study. Therefore, samples with three different initial textures were deformed in the temperature range T = 700K – 1300K. The development of the microstructure is characterized by two different regimes depending on the deformation temperature T. For T up to 1000K, continuous dynamic recrystallization (CDRX) takes place. This mechanism leads to the deformation-induced dislocations forming low angle grain boundaries (LAGBs) or being incorporated into them and the successive transformation of these boundaries into high angle grain boundaries (HAGBs) by a further increase of their misorientation. The predictions of this model were compared with the experimental results. The shear stress – shear strain curves are characterized by a peak at low strains, which is followed by softening and a steady state at high strains. This condition is fulfilled for a number of samples, but especially <111> oriented samples do not show a softening stage at low temperatures. Grain refinement takes place for all samples and the average grain size decreases with temperature. The predicted LAGB decrease is in best agreement with the experiments at the lowest temperatures (T = 700K and 800K). Deviations from the model can be explained by the temperature dependence of the grain boundary mobility. For temperatures T > 1000K, discontinuous dynamic recrystallization (DDRX) occurs, by which new grains form by nucleation and subsequent growth. The texture is characterized by two components, {100}<100> (cube, C) and {110}<100> (Goss, G). The intensity of G increases with temperature, while that of C decreases independent of the initial orientation. Both components have their maximum deviated about the 1 axis. The deviation is larger for grains containing the C component and decreases with temperature. Grains containing the G component have the smaller deviation, which decreases with temperature and strain. Texture simulations based on the full constraint Taylor model under the assumption of {110}<100> and {110}<110> slip were done with the experimental <110> and <111> fibres as well as a theoretical <100> fibre and a {100}<100> single orientation (ideal as well as rotated about the torsion axis). The G component is predicted by the simulations and is therefore a deformation texture. However the C component does not appear in the simulation. It therefore must originate by different mechanisms. For the non-<100> oriented samples, possibly nucleation is responsible for the formation of C oriented nuclei. Simulations with single orientations lead to the conclusion, that the ideal C orientation rotates about the 1 axis, while other C orientations, which are rotated about the torsion axis, increasingly converge towards the G component with strain. A single G orientation on the other hand is stable against such a rotation and is therefore the most likely steady state texture. Based on these results it is proposed, that ideally C oriented nuclei rotate until an orientation is reached into which they grow. These new grains are further rotated up to a critical angle, at which a part of them disappears either by adjacent grains or new C oriented nuclei. The recrystallization texture for T > 1000K is most likely the C component as well. Torsional creep of NiAl is characterized by a stress exponent, which depends on temperature and an activation energy, which is stress dependent. A model incorporating both dependencies is proposed and applied to the creep data. It is shown that these equations are able to describe the experimental findings. Thus creep of NiAl based on this model is dominated by non-diffusional processes such as cross slip of <100> screw dislocations for T  1000K. For T > 1000K the stress exponent and the activation energy are in a region, which according to previous reports is rather dominated by dislocation-climb controlled creep. The Swift effect, due to which samples change their axial dimension during torsion without applied axial stress, is observed for NiAl. It is strongly related to the texture development and in the case of NiAl the C component is identified as being responsible for shortening, whereas the G component leads to lengthening as long as it is not aligned with the shear system. Both tendencies can be explained based on the active slip systems. Simulations fail to predict the experimental observation, because the C component is not present. HESR and EBSD were compared with respect to local texture measurements. It was concluded depending on the average grain size HESR has an advantage in terms of grain statistics. For DDRX samples however, both methods are limited. Local texture inhomogeneities can be better detected using EBSD, whereas for an overall local texture information HESR is better suited.