<p> This dissertation describes the recent advancements in micromechanical testing that inform how deformation mechanisms in austenitic stainless steels (SS) are affected by the presence of irradiation-induced defects. Austenitic SS is one of the most widely utilized structural alloys in nuclear energy systems, but the role of irradiation on its underlying mechanisms of mechanical deformation remains poorly understood. Now, recent advancement of microscale mechanical testing in a scanning electron microscope (SEM), coupled with site-specific transmission electron microscopy (TEM), enables us to precisely determine deformation mechanisms as a function of plastic strain and grain orientation.</p> <p> </p> <p>We focus on AISI 304L SSs irradiated in EBR-II to ~1-28 displacements per atom (dpa) at ~415 °C and contains ~0.2-8 atomic parts per million (appm) He amounting to ~0.2-2.8% swelling. A portion of the specimen is laser welded in a hot cell; the laser weld heat affected zone (HAZ) is studied and considered to have undergone post-irradiation annealing (PIA). An archival, virgin specimen is also studied as a control. We conduct nanoindentation, then prepare TEM lamellae from the indent plastic zone. In the 3 appm He condition, TEM investigation reveals nucleation of deformation-induced <i>α</i>’ martensite in the irradiated specimen, and metastable <i>ε</i> martensite in the PIA specimen. Meanwhile, the unirradiated control specimen exhibits evidence only of dislocation slip and twinning; this is unsurprising given that alternative deformation mechanisms such as twinning and martensitic transformation are typically observed only near cryogenic temperatures in austenitic SS. Surface area of irradiation-produced cavities contribute enough free energy to accommodate the martensitic transformation. The lower population of cavities in the PIA material enables metastable <i>ε</i> martensite formation, while the higher cavity number density in the irradiated material causes direct <i>α</i>’ martensite formation. In the 0.2 appm He condition, SEM-based micropillar compression tests confirm nanoindentation results. A deformation transition map with corresponding criteria has been proposed for tailoring the plasticity of irradiated steels. Irradiation damage could enable fundamental, mechanistic studies of deformation mechanisms that are typically only accessible at extremely low temperatures. </p>

O presente trabalho avaliou o efeito de tratamentos térmicos ou diferentes graus de deformação plástica na transformação da austenita do microconstituinte AM de uma chapa de aço alta resistência baixa liga (ARBL) classe API 5L X80 usada para gasodutos. A chapa tem espessura de 19 mm e passaria pelo processo de conformação UOE, mas a deformação foi realizada por laminação a frio, a temperatura ambiente, com reduções de 5 a 20%. O propósito foi compreender melhor o microconstituinte AM, explorar a transformação martensítica induzida por deformação (SIMT) e a decomposição austenítica por tratamento térmico, com ênfase em seu comportamento magnético. A transformação da austenita foi acompanhada através de medidas de polarização magnética, comparada com a densidade de massa e difração de raios X. A deformação plástica e os tratamentos térmicos alteraram a polarização magnética de saturação e a densidade de massa da amostra de aço de forma compatível com a eliminação da austenita retida metaestável. O método de densidade hidrostática foi considerado sensível para mensurar transformações de fase. Os dados obtidos revelam expansão volumétrica de aproximadamente 0,13%, correspondendo a 3,2% a quantidade de austenita retida original do material, enquanto os valores obtidos por polarização magnética de saturação são 2,8% pelo histeresígrafo e 2,1% por MAV. A difração de raios X nas amostras sob deformação ou tratamentos térmicos resultaram em queda nos primeiros picos da austenita quando comparadas com a amostra como recebida. / This study evaluated the effect of different degrees of plastic deformation or heat treatment on the transformation of austenite into martensite of an HSLA steel plate API 5L X80 for pipelines. A 19 mm thickness plate would be submitted to UOE forming process, but the cold work instead occurred by cold rolling at room temperature, with reductions of 5 up to 20%. The purpose was to better understand the MA constituent, explore the strain-induced martensitic transformation (SIMT) and austenitic decomposition by heat treatment with emphasis on its magnetic behavior. The transformation was accompanied by saturation magnetization measurements, compared with the mass density and X-ray diffraction. The plastic deformation or the heat treatment altered the saturation magnetization and the mass density in a manner consistent with the elimination of metastable retained austenite. The density method is sensible to measure phase transformations induced by strain. The data obtained shows a volumetric expansion of about 0.13%, corresponding to an amount of retained austenite of the original material of 3.2%, while the values obtained by magnetization saturation are 2.8% by hysteresigraph and 2.1% by VSM. By X-ray diffraction there is a clear drop in first peaks of austenite of the samples under deformation or heat treatment compared with the sample as-received.

O aumento no consumo energético mundial e a perspectiva de esgotamento das reservas de combustíveis fósseis têm estimulado o desenvolvimento de tecnologias e materiais para aplicações nos futuros reatores de fusão nuclear e reatores de fissão a nêutrons rápidos. O foco deste trabalho é avaliar a estabilidade microestrutural de um material tecnologicamente promissor por meio de diferentes técnicas de caracterização. O material estudado, o aço ODS-EUROFER, é um aço ferrítico-martensítico de atividade reduzida de composição 9%Cr-1%W (em massa) endurecido pela dispersão de 0,3% (em massa) de óxido de ítrio. Amostras foram laminadas até 80% de redução e submetidas a tratamentos isotérmicos em 800 °C por até 6 meses (4320 h) de duração para se investigar a ocorrência de fenômenos tais como recuperação, recristalização, crescimento de grão, precipitação e engrossamento de Ostwald. Outro conjunto de amostras foi recozido por 1 hora em temperaturas entre 900 e 1300 °C para se estudar a transformação martensítica neste material. Diversas técnicas de caracterização microestrutural complementares entre si (MEV, MET, DRX, EBSD, APT, ensaios de microdureza Vickers, dilatometria, DTA e magnetização) foram empregadas. Os resultados obtidos indicam que a dispersão de partículas nanométricas de Y2O3 confere uma grande resistência à recristalização primária, favorecendo a recuperação estática como principal mecanismo de amolecimento durante o recozimento prolongado deste aço. De modo similar, o crescimento de grão foi suprimido no campo austenítico em temperaturas tão altas quanto 1200 °C. / The rise in the world energy consumption and the possibility of depletion of the fossil fuel reserves have stimulated the development of new technologies and new materials for applications in the future nuclear fusion reactors and in the fast breeder fission reactors. The aim of this study is to evaluate the microstructural stability of a technologically promising material by using different characterization techniques. The investigated material, the ODS-EUROFER steel, is 9Cr-1W (%wt) reduced-activation ferritic-martensitic steel reinforced with a dispersion of 0.3%wt of yttrium oxide nanoparticles. Samples were cold rolled to 80% thickness reduction and subjected to isothermal annealing at 800 °C for up to 6 months (4,320 h) to investigate the occurrence of phenomena such as recovery, recrystallization, grain growth, precipitation, and Ostwald ripening. Another set of samples was annealed for 1 hour at temperatures between 900 and 1300 °C to study the martensitic transformation in this steel. Several complementary microstructural characterization techniques were employed (SEM, TEM, XRD, EBSD, APT, Vickers hardness, dilatometry, DTA and magnectic measurements). The results suggest that the dispersion of nanoscaled particles of Y2O3 provides a high resistance to discontinous recrystallization and favors static recovery as the main softening mechanism during long-term annealing in this steel. Similarly, grain growth was suppressed even in temperatures as high as 1200 °C in the austenitic field.

O aumento no consumo energético mundial e a perspectiva de esgotamento das reservas de combustíveis fósseis têm estimulado o desenvolvimento de tecnologias e materiais para aplicações nos futuros reatores de fusão nuclear e reatores de fissão a nêutrons rápidos. O foco deste trabalho é avaliar a estabilidade microestrutural de um material tecnologicamente promissor por meio de diferentes técnicas de caracterização. O material estudado, o aço ODS-EUROFER, é um aço ferrítico-martensítico de atividade reduzida de composição 9%Cr-1%W (em massa) endurecido pela dispersão de 0,3% (em massa) de óxido de ítrio. Amostras foram laminadas até 80% de redução e submetidas a tratamentos isotérmicos em 800 °C por até 6 meses (4320 h) de duração para se investigar a ocorrência de fenômenos tais como recuperação, recristalização, crescimento de grão, precipitação e engrossamento de Ostwald. Outro conjunto de amostras foi recozido por 1 hora em temperaturas entre 900 e 1300 °C para se estudar a transformação martensítica neste material. Diversas técnicas de caracterização microestrutural complementares entre si (MEV, MET, DRX, EBSD, APT, ensaios de microdureza Vickers, dilatometria, DTA e magnetização) foram empregadas. Os resultados obtidos indicam que a dispersão de partículas nanométricas de Y2O3 confere uma grande resistência à recristalização primária, favorecendo a recuperação estática como principal mecanismo de amolecimento durante o recozimento prolongado deste aço. De modo similar, o crescimento de grão foi suprimido no campo austenítico em temperaturas tão altas quanto 1200 °C. / The rise in the world energy consumption and the possibility of depletion of the fossil fuel reserves have stimulated the development of new technologies and new materials for applications in the future nuclear fusion reactors and in the fast breeder fission reactors. The aim of this study is to evaluate the microstructural stability of a technologically promising material by using different characterization techniques. The investigated material, the ODS-EUROFER steel, is 9Cr-1W (%wt) reduced-activation ferritic-martensitic steel reinforced with a dispersion of 0.3%wt of yttrium oxide nanoparticles. Samples were cold rolled to 80% thickness reduction and subjected to isothermal annealing at 800 °C for up to 6 months (4,320 h) to investigate the occurrence of phenomena such as recovery, recrystallization, grain growth, precipitation, and Ostwald ripening. Another set of samples was annealed for 1 hour at temperatures between 900 and 1300 °C to study the martensitic transformation in this steel. Several complementary microstructural characterization techniques were employed (SEM, TEM, XRD, EBSD, APT, Vickers hardness, dilatometry, DTA and magnectic measurements). The results suggest that the dispersion of nanoscaled particles of Y2O3 provides a high resistance to discontinous recrystallization and favors static recovery as the main softening mechanism during long-term annealing in this steel. Similarly, grain growth was suppressed even in temperatures as high as 1200 °C in the austenitic field.

No description available.

No description available.

La surface des pièces mécaniques est une zone sensible soumise à des conditions de sollicitations particulières, tant mécaniquement (frottement, contrainte maximale) que chimiquement (atmosphère ambiante, corrosion). Ainsi, la ruine des pièces de service est généralement initiée en surface ; les grands secteurs industriels sont donc à la recherche de solutions technologiques permettant une amélioration des propriétés mécaniques globales par une modification des propriétés de surface. De nombreuses techniques ont été développées dans ce but, notamment les traitements de surface mécaniques. Parmi ceux-ci, le grenaillage ultrasonique permet de déformer sévèrement et superficiellement les pièces par de nombreux impacts de billes ayant des trajectoires aléatoires au sein de la chambre de traitement. Le propos de cette étude repose sur l'analyse et la compréhension des microstructures de déformation induites par un traitement de grenaillage ultrasonique, particulièrement sous conditions cryogéniques ; sujet très peu exploré à ce jour voir nouveau concernant i) des métaux susceptibles de subir une transformation martensitique et ii) l'influence d'un tel traitement sur la tenue en fatigue cyclique. Pour ce faire, plusieurs nuances d'aciers inoxydables austénitiques présentant des stabilités différentes vis-à-vis de la transformation de phase ont été traitées à très basses températures et les propriétés obtenues ont été comparées à celles mesurées sur les échantillons traités à température ambiante. Les premières observations ont montré que, suite à un traitement sous condition cryogénique (-130 °C), une baisse de dureté intervient en sous-couche de l'alliage 310S stable, associée à une hausse des propriétés mécaniques sous basse température rendant le matériau plus difficile à écrouir. Ce phénomène est complètement supprimé au sein de l'alliage métastable 304L par une transformation martensitique facilitée, intervenant plus profondément qu'à température ambiante et entrainant une augmentation de la dureté de sous-couche. Deux alliages métastables (304L et 316L) ont donc été sélectionnés afin de détailler l'influence des paramètres de traitement sur le durcissement de sous-couche par une étude paramétrique comprenant l'amplitude de vibration (40 et 60 µm), la durée (3 et 20 min) ainsi que la température de traitement (ambiante, -80 et -130 °C). Il en ressort qu'augmenter l'énergie de traitent par une hausse de l'amplitude et/ou de la durée de grenaillage entraine une augmentation des duretés de surface et de sous-couche, accompagnée par la production de couches durcies plus épaisses. L'utilisation de températures cryogéniques permet une augmentation du potentiel de durcissement, et ce principalement en sous-couche. En associant les gradients de dureté aux distributions de martensite le long des épaisseurs affectées, il a été montré que la fraction de martensite était directement liée au potentielle de durcissement en profondeur. La fraction de martensite produite étant dépendante de la température de déformation et, afin de prendre en compte la stabilité initiale de l'alliage comme paramètre additionnel, des mesures complémentaires ont été faites sur l'alliage 316L plus stable. Les résultats ont alors montré qu'il est primordial d'adapter la température de traitement à la stabilité de l'échantillon afin d'optimiser l'efficacité du durcissement de sous-couche et éviter ainsi une baisse de la dureté en profondeur. Finalement, les structures de déformation obtenues sous condition cryogénique ont été reliées à la tenue mécanique sous sollicitations cycliques en flexion rotative. Comparé à un traitement réalisé à température ambiante, un grenaillage cryogénique permet une baisse la rugosité de surface et la production de contraintes résiduelles de compression plus élevées par la présence de martensite. Cependant, une plus grande relaxation de ces dernières associée à une réduction de l'épaisseur [...] / The surface of mechanical components is a sensitive zone subjected to particular mechanical (friction, maximum stress) and chemical (ambient atmosphere, corrosion) interactions. Hence, the rupture is generally initiated on the surface. In order to increase the global integrity of the working parts, the industrial groups are still seeking technological solutions allowing the modifications of the surface properties. Nodaway, plenty of surface modification techniques have been developed like the mechanical surface treatments. Among them, the ultrasonic shot peening (or surface mechanical attrition treatment) focus on superficially deform the mechanical parts through numerous collisions of peening medias having random trajectories inside a confined chamber. The purpose of this study is based on the analysis and the comprehension of the deformed microstructures induced by the ultrasonic shot peening treatment, especially under cryogenic temperatures. To do so, several austenitic stainless steel grades having different stabilities regarding the martensitic transformation have been treated under cryogenic conditions and compared to the properties obtained under room temperature. The first observations have shown that, after a cryogenic peening, a decrease of the subsurface hardness takes place in the stable 310S alloy which was attributed to an increase of the mechanical properties under cryogenic temperature. This phenomenon is suppressed in the metastable 304L by triggering a martensitic phase transformation promoted under low temperature and happening deeper compared to room temperature, increasing substantially the subsurface hardness. Two metastable alloys (304L and 316L) were then selected to conduct an ultrasonic shot peening parametric study including the vibration amplitude (40 and 60 µm), the treatment duration (3 and 20 min) and temperature (room temperature, -80 and -130 °C). It has been shown that increasing the treatment energy by raising the vibration amplitude and/or the duration leads to an increase of the surface and subsurface hardnesses as well as the affected layer thickness. The use of cryogenic temperatures allows an additional increase of the hardness, especially in subsurface. By comparing the different hardness gradients with the martensite distributions along the hardened layers, a direct correlation with the hardening rate and the martensite fraction was observed. The initial stability of the treated material was also taken in account by carried out additional observations on the 316L having a higher stability. The results have indicated that the deformation temperature needs to be wisely chosen regarding the stability of the processed material in order to avoid a decrease of the subsurface hardness. Finally, the deformed microstructures generated under cryogenic ultrasonic shot peening were associated to the mechanical behaviors of cylindrical specimens using rotating bending fatigue tests. Compared to a room temperature treatment, a cryogenic peening allows a decrease of the surface roughness and the generation of higher surface compressive residual stresses by the formation of martensite. However, compared to a room temperature treatment, the fatigue behavior was not increased after a cryogenic peening because of a more pronounced surface residual stress relaxation and a reduction of the affected layer. However, the potential increase of the fatigue life after a cryogenic surface deformation was depicted by the study of the rupture surfaces. It was observed that, if the involvement of the surface defects introduced by the high surface roughness can be lowered, a single subsurface crack initiation can be produced increasing considerably the fatigue behavior of the processed material

Les alliages NiMnSb, matériaux multifonctionnels nouveaux, ont attiré une attention en raison de leurs multiples propriétés, telles que l'effet de mémoire de forme, magnétocalorique, de biais d'échange, de magnétorésistance. Jusqu'à présent, de nombreux aspects des NiMnSb, tels que structure cristalline, microstructure, propriétés magnétiques et mécaniques ont été étudiés. Cependant, de nombreuses questions fondamentales de ces matériaux n'ont pas été entièrement révélées, ce qui limite leur développement. Une étude a été menée sur les alliages ternaires NiMnSb en termes de structures cristallines de l'austénite et de la martensite; Caractéristiques microstructurales et cristallographiques de la martensite; La relation d'orientation (OR) de transformation martensitique et sa corrélation avec l'organisation des variantes; Les caractéristiques de déformation de la transformation et l'autoaccommodation de la déformation de transformation. Le travail a confirmé que l'austénite possède une structure cristalline L21 cubique, groupe spatial Fm3m (No. 225). La martensite a une structure orthorhombique modulée (4O) à quatre couches, groupe spatial Pmma (No. 051). Les constantes de réseau de martensite de Ni50Mn37Sb13 et Ni50Mn38Sb12 sont aM = 8.5830 Å, bM = 5.6533 Å et cM = 4.3501 Å, et aM = 8.5788 Å, bM = 5.6443 Å et cM = 4.3479 Å. La microstructure de la martensite 4O NiMnSb modulée possède une caractéristique d'organisation hiérarchique. Les lamelles fines de martensite sont d'abord organisées en larges plaques. Chaque plaque possède 4 variantes apparentées aux jumeaux A, B, C et D formant des jumeaux de type I (A et C, B et D), de type II (A et B, C et D) et des macles composées (A et D; B et C). Les interfaces des variantes sont définies par les plans de maclage correspondants. Les éléments de maclage sont entièrement déterminés pour chaque relation de maclage. Les plaques sont ensuite organisées en sous-colonies et les sous-colonies en colonies de plaques. Les plaques voisines d'une sous-colonie et d'une colonie de plaques partagent une interface de plaque commune. Des colonies de plaques avec différentes interfaces de plaques ayant différentes orientations occupent finalement l'ensemble du grain d'austénite original. La OR de Pitsch, spécifiée comme {011}A // {221}M et <011>A // <122>M, est l'OR effective entre l'austénite cubique et la martensite 4O modulée. Sous cette OR, un maximum de 24 variantes distinctes peut être produit. Les 24 variantes sont organisées en 6 colonies de variantes distinctes, 12 sous-colonies distinctes et enfin 6 colonies de plaques distinctes. Le plan de maclage de type I et les interfaces intra-plaques correspondent tous à la même famille de plans {011}A de austénite. La formation des colonies de variantes martensitiques peut être à la fois intragranulaire et intergranulaire pendant la transformation de phase La colonie de variantes structurée en sandwich est l'unité micro-structurale de base de la martensite. Cette structure est composée de variantes de relation macles et possède des interfaces de variantes internes totalement compatibles et les plans d'habitat invariants. Les caractéristiques de déformation des variants en relation de macles conduisent à la fraction de volume élevée de macles de type II et affecte la morphologie des colonies en sandwich. La structure en forme de coin est composée de deux sandwichs compatibles et reliés par un plan de nervure médiane avec une petite incompatibilité atomique. Tous ces résultats indiquent que la transformation martensitique est autoaccommodée et la microstructure est déterminée par l'auto-accommodation des constituants microstructuraux. Ce travail vise à fournir des informations cristallographiques et micro-structurales fondamentales des alliages NiMnSb pour l'interprétation de leurs caractéristiques magnétiques et mécaniques associées à la transformation martensitique et des recherches complémentaires sur l'optimisation des propriétés / NiMnSb based Heusler type alloys, as a novel multi-functional material has attracted considerable attention due to their multiple properties, such as magnetic shape memory effect, magnetocaloric effect, exchange bias effect, magnetoresistance effect. To date, many aspects of the NiMnSb alloys, such as crystal structure, microstructure, magnetic properties and mechanical properties etc., have been widely investigated. However, many fundamental issues of this family of materials have not been fully revealed, which largely restricts the development of this new kind of multi-functional materials. In the present work, a thorough investigation has been conducted on ternary NiMnSb alloys in terms of crystal structures of austenite and martensite; microstructural and crystallographic features of martensite; martensitic transformation orientation relationship (OR) and its correlation with variant organization; transformation deformation characteristics and self-accommodation of transformation strain. The work confirmed that the austenite of NiMnSb alloys possesses a cubic L21 crystal structure belonging to the space group Fm3m (No. 225). The martensite has a four-layered orthorhombic (4O) structure with space group Pmma (No. 051). The lattice constants of the Ni50Mn37Sb13 and Ni50Mn38Sb12 martensite are aM = 8.5830 Å, bM = 5.6533 Å and cM = 4.3501Å, and aM = 8.5788 Å, bM = 5.6443 Å and cM = 4.3479 Å, respectively. The microstructure of the 4O NiMnSb modulated martensite possesses a hierarchical organization feature. Martensite fine lamellae are first organized into broad plates. Each plate possesses 4 distinct twin related variants A, B, C and D forming type I twins (A and C; B and D), type II twins (A and B; C and D) and compound twins (A and D; B and C). The variant interfaces are defined by the corresponding twinning planes. The complete twinning elements for each twin relation are fully determined. The plates are further organized into sub-colonies and sub-colonies into plate colonies. The neighboring plates in one sub-colony and plate colony share one common plate interface orientation. Plate colonies with different oriented plate interfaces finally take the whole original austenite grain. The Pitsch OR, specified as {011}A // {221}M and <011>A // <122>M, is the effective OR between the cubic austenite and the 4O modulated martensite. Under this OR, a maximum of 24 distinct variants can be produced. The 24 variants are organized into 6 distinct variant colonies, 12 distinct sub-colonies and finally 6 distinct plate colonies. The twinning plane of type I twin and the intra-plate plate interfaces all correspond to the same family of {011}A planes of austenite. The formation of martensite variant colonies can be both form intragranular and intergranular during the phase transformation. The sandwich structured variant colony is the basic microstructural unit of the martensite. This structure is composed of twin related variants and possesses the full compatible inner variants interfaces and invariant habit planes. The deformation manner of the twin related variants result in the high occurrence frequency of the type II twins and affects the morphology of the sandwich colonies. The wedge-shaped structure is composed of two compatible sandwiches and conjoined by a midrib plane with a small atomic misfit. All these results indicate that the martensitic transformation is self-accommodated and the microstructure is determined by the self-accommodation of the microstructural constituents. The aim of this work is to provide fundamental crystallographic and microstructural information of NiMnSb alloys for interpreting their magnetic and mechanical characteristics associated with the martensitic transformation and further investigations on property optimization

En tant que nouveau matériau magnétique à mémoire de forme, les alliages basés sur le système Ni-Mn-Sn possèdent de multiples propriétés physiques telles que l'effet de mémoire de forme des alliages polycristallins, l'effet magnétocalorique géant, l'effet de magnétorésistance et l'effet de polarisation d'échange. Jusqu'à présent, la plupart des études ont été axées sur l'amélioration des multifonctionnalités de ces alliages, mais l'information fondamentale qui est fortement associée à ces propriétés n'est toujours pas claire. Ainsi, une étude approfondie sur les structures cristallines de la martensite et de l'austénite, les caractéristiques microstructurales et cristallographiques de la transformation martensitique a été menée dans le cadre du présent travail de doctorat. Il a été confirmé que l'austénite de Ni50Mn37.5Sn12.5 possède une structure cubique L21 (Fm3 ̅m, No.225). Le paramètre de réseau de l'austénite dans Ni50Mn37.5Sn12.5 est aA = 5.9813 Å. La martensite possède une structure orthorhombique (4O) à quatre couches (Pmma, No.51). Les paramètres de réseau de la martensite dans Ni50Mn38Sn12 et Ni50Mn37.5Sn12.5 sont a4O = 8.6068 Å; b4O = 5.6226 Å and c4O = 4.3728 Å, and a4O = 8.6063 Å, b4O = 5.6425 Å, and c4O = 4.3672Å, respectivement. La martensite 4O Ni-Mn-Sn présente une microstructure hiérarchiquement maclée. La martensite est organisée en larges plaques dans le grain d'austénite d'origine. Les plaques contiennent des colonies à forme irrégulière avec deux modèles caractéristiques de microstructures : le motif lamellaire classique et le motif en arête de poisson. Dans chaque colonie, il existe quatre variantes d'orientation (A, B, C et D) et elles forment trois types de macles (Type I, Type II et macles composées). Les interfaces entre les variantes correspondantes sont en coincidence avec leur plan de maclage K1. Les plans d'interface des paires de macles composées A-D et B-C peuvent avoir une ou deux orientations différentes, ce qui conduit aux deux modèles microstructuraux. Les variantes correspondantes dans les colonies voisines dans une même large plaque (colonies intra-plaques) possèdent des orientations proches et le joint de colonie est courbé, tandis que la limite de colonie inter-plaques est relativement droite. La relation d’orientation de Pitsch (Orientation Relation OR), spécifiée comme {1 0 1} A//{22 ̅1}4O and <1 0 1 ̅> A//<1 ̅2 2>4O, a été exclusivement déterminée à être une OR effective entre l'austénite cubique et la martensite modulée 4O. Sous cette OR, 24 variantes peuvent être générées dans un grain d'austénite. Ces 24 variantes sont organisées en 6 groupes et chaque groupe correspond à une colonie de martensite. La structure de martensite finement maclée (microstructure sandwich) est le composant microstructural de base produit par la transformation martensitique. Une telle structure assure une interface de phase invariante (plan d'habitat) pour la transformation. Au cours de la transformation, les variantes de la martensite sont organisées en clusters en forme de diamant composés de colonies de variantes et avec des structures en forme de coin au front de transformation. Chaque coin est composé de deux structures sandwich séparées par un plan de nervure médiane {1 0 1}A. Les paires de variantes dans chaque coin devraient avoir le même type de macles avec une relation de Type I ou de Type II pour garantir de bonnes compatibilités géométriques des variantes à l'interface de phase et au plan de la nervure centrale. Dans les diamants, les colonies sont séparées par des frontières présentant des marches à faible énergie interfaciale qui évoluent vers les joints des colonies intra-plaques et par des joints droits qui deviennent les joints entre les plaques. Les diamants s'allongent le long de la direction presque parallèle aux plans de la nervure centrale des coins et la forme de la plaque de la martensite est finalement formée. [...] / Being a novel magnetic shape memory material, Ni-Mn-Sn based alloy systems possess multiple physical properties, such as shape memory effect of polycrystalline alloys, giant magnetocaloric effect, large magnetoresistance effect and exchange bias effect. So far, most studies have been focused on the improvement of the multifunctionalities of these alloys, but the fundamental information which is highly associated with these properties is still unclear. Thus, a thorough study on the crystal structures of martensite and austenite, microstructural and crystallographic features of martensitic transformation has been conducted in the present PhD work. The austenite of Ni50Mn37.5Sn12.5 was confirmed to possess a L21 cubic structure (Fm"3" ̅m, No.225). The lattice parameter of austenite in Ni50Mn37.5Sn12.5 is aA=5.9813 Å. The martensite possesses a four-layered orthorhombic (4O) structure (Pmma, No.51). The lattice parameters of martensite in Ni50Mn38Sn12 and Ni50Mn37.5Sn12.5 are a4O = 8.6068 Å; b4O = 5.6226 Å and c4O = 4.3728 Å, and a4O = 8.6063 Å, b4O = 5.6425 Å, and c4O = 4.3672Å, respectively. The 4O Ni-Mn-Sn martensite exhibits a hierarchically twinned microstructure. The martensite is organized into broad plates in the original austenite grain. The plates contain irregularly shaped colonies with two characteristic microstructural patterns: classical lamellar pattern and herring-bone pattern. In each colony, there are four orientation variants (A, B, C and D) and they form three types of twins (Type I, Type II and compound twin). The interfaces between the corresponding variants are in coincidence with their twinning plane K1. The interface planes of the compound twin pairs A-D and B-C can have one or two different orientations, which leads to the two microstructural patterns. The corresponding variants in the neighboring colonies within one broad plate (intra plate colonies) possess close orientations and colony boundary is curved, whereas the inter plate colony boundary is relatively straight. The Pitsch OR, specified as "{1 0 1}" A//"{2 " "2" ̅" " "1" ̅"}" 4O and "<1 0 " "1" ̅">" A//"<" "1" ̅" " "2" ̅" 2>" 4O, was uniquely determined to be an effective OR between the cubic austenite and 4O modulated martensite. Under this OR, 24 variants can be generated within one austenite grain. Such 24 variants are organized into 6 groups and each group corresponds to a martensite colony. The finely twinned martensite structure (sandwich microstructure) is the basic microstructural constitute produced by martensitic transformation. Such a structure ensures an invariant phase interface (habit plane) for the transformation. During the transformation, martensite variants are organized into diamond shaped clusters composed of variant colonies and with wedge shaped structures at the transformation front. Each wedge is composed of two sandwich structures separating by a midrib plane {1 0 1}A. The variant pairs in each wedge should have the same twin type with either Type I or Type II relation to ensure good geometrical compatibilities of the variants at phase interface and at the midrib plane. Within the diamonds, colonies are separated by step-like boundaries with low interfacial energy that evolve into the intra plate colony boundaries and by straight boundaries that become the inter plate colony boundaries. The diamonds elongates along the direction nearly paralleled to the midrib planes of the wedges and plate shape of martensite is finally formed. Such features of the diamond structure in Ni-Mn-Sn alloys are realized by self-accommodation of transformation strains for energy minimization. The present work provides comprehensive microstructural and crystallographic information on martensite and on martensitic transforamtion of Ni-Mn-Sn alloys and it is useful for understanding their multi functionalities associated with martensitic transformation and helpful on property optimization

O presente trabalho avaliou o efeito de tratamentos térmicos ou diferentes graus de deformação plástica na transformação da austenita do microconstituinte AM de uma chapa de aço alta resistência baixa liga (ARBL) classe API 5L X80 usada para gasodutos. A chapa tem espessura de 19 mm e passaria pelo processo de conformação UOE, mas a deformação foi realizada por laminação a frio, a temperatura ambiente, com reduções de 5 a 20%. O propósito foi compreender melhor o microconstituinte AM, explorar a transformação martensítica induzida por deformação (SIMT) e a decomposição austenítica por tratamento térmico, com ênfase em seu comportamento magnético. A transformação da austenita foi acompanhada através de medidas de polarização magnética, comparada com a densidade de massa e difração de raios X. A deformação plástica e os tratamentos térmicos alteraram a polarização magnética de saturação e a densidade de massa da amostra de aço de forma compatível com a eliminação da austenita retida metaestável. O método de densidade hidrostática foi considerado sensível para mensurar transformações de fase. Os dados obtidos revelam expansão volumétrica de aproximadamente 0,13%, correspondendo a 3,2% a quantidade de austenita retida original do material, enquanto os valores obtidos por polarização magnética de saturação são 2,8% pelo histeresígrafo e 2,1% por MAV. A difração de raios X nas amostras sob deformação ou tratamentos térmicos resultaram em queda nos primeiros picos da austenita quando comparadas com a amostra como recebida. / This study evaluated the effect of different degrees of plastic deformation or heat treatment on the transformation of austenite into martensite of an HSLA steel plate API 5L X80 for pipelines. A 19 mm thickness plate would be submitted to UOE forming process, but the cold work instead occurred by cold rolling at room temperature, with reductions of 5 up to 20%. The purpose was to better understand the MA constituent, explore the strain-induced martensitic transformation (SIMT) and austenitic decomposition by heat treatment with emphasis on its magnetic behavior. The transformation was accompanied by saturation magnetization measurements, compared with the mass density and X-ray diffraction. The plastic deformation or the heat treatment altered the saturation magnetization and the mass density in a manner consistent with the elimination of metastable retained austenite. The density method is sensible to measure phase transformations induced by strain. The data obtained shows a volumetric expansion of about 0.13%, corresponding to an amount of retained austenite of the original material of 3.2%, while the values obtained by magnetization saturation are 2.8% by hysteresigraph and 2.1% by VSM. By X-ray diffraction there is a clear drop in first peaks of austenite of the samples under deformation or heat treatment compared with the sample as-received.