Cette thèse porte sur l'analyse d'un phénomène particulièrement important dérivant des conséquences mécaniques des transformations de phases solide-solide dans les aciers : la plasticité de transformation ou TRIP (Transformation Induced Plasticity) et son interaction avec la plasticité classique. Ce sujet est abordé à la fois par des investigations expérimentales et par une approche de modélisation numérique, pour les transformations martensitiques.

This thesis aims to examine the possibility of using Magnetic Barkhausen Noise technique in characterizing the ferritic-martensitic microstructure of hypoeutectoid steels quenched from the intercritical temperature range. For this purpose, rectangular specimens were prepared from SAE 1020, 1040 and 1060 steels. The specimens were heated at different temperatures within the intercritical temperature range and then quenched into water. Microstructures of the specimens were characterized by metallographic examinations and hardness measurements. The measurements of the Magnetic Barkhausen Noise (MBN) were performed by using both Rollscan and &amp / #956 / SCAN sensor connectors. It was seen that, for specimens having identical carbon content, Barkhausen emission decreased as the heating temperature increased. Moreover, in specimens heated at the same temperature, Barkhausen emission decreased as the carbon content of the specimen increased. In both cases, the decrease in Barkhausen emission is associated with the increase in martensite content. The results indicate that MBN is inversely proportional to hardness and that MBN is very sensitive to the microstructural condition of the material. It has been shown that using MBN is a powerful tool for evaluating the microstructure of hypoeutectoid steels quenched from the intercritical temperature range and that the use of this technique could be extended to characterize industrial dual phase steels.

Ni-Mn-Ga alloys close to the stoichiometric composition Ni2MnGa belong to the quite new family of ferromagnetic shape memory alloys. These alloys are characterized by the magnetic field induced strain (MFIS) based on the comparably easy motion of twin boundaries under a magnetic field. They are mostly chosen as a potential candidate for practical application especially promising for actuators and sensors because they are showing the largest MFIS so far. Depending on the chemical composition and heat treatment, at least three martensitic structures can be distinguished in the Ni-Mn-Ga system. However, the effect mentioned above only exists in two modulated structures. Since for the intended application of MFIS in technology polycrystalline materials seem to be more appropriate in contrast to single crystals, the specific polycrystalline aspects are considered. Factors important for decreasing the twinning stress and increasing the twinning strain of polycrystalline Ni-Mn-Ga alloys are texturing, adjusting the structure by annealing and training by thermomechanical treatments. To achieve pronounced MFIS in polycrystals, fabrication processes are needed to produce specific strong textures. The material texturing has been obtained by directional solidification and plastic deformation by hot rolling and hot extrusion as well as high pressure torsion (HPT). To examine the texture of coarse-grained Ni-Mn-Ga alloys (due to a solidification process or dynamic recrystallization), diffraction of synchrotron radiation and neutrons was applied. The texture results show that the texture of Ni-Mn-Ga subjected to directional solidification, hot rolling and hot extrusion is a fibre or weak biaxial texture. However, local synchrotron measurements reveal that the global fibre texture of the hot extruded sample is a ”cyclic” fibre texture, i.e. it is composed of components related to the radial direction rotating around the extrusion axis. This allows finding regions with a strong texture component. The texture after HPT is characterized by a strong cube with the cube favourably oriented. The initial microstructure of the Ni-Mn-Ga alloys is a typical self-accommodated microstructure of martensite. High resolution EBSD mappings show macro, micro twins and two types of microstructure. The twin plane is determined to be {110). In a typical martensitic transformation the high-temperature phase has a higher crystallographic symmetry than the low-temperature phase. Consequently, austenite may transform to several martensitic variants, the number of which depends on the change of symmetry during transformation. Generally, in a cubic-to-tetragonal transformation (5M case) three variants can form with the c-axis oriented close to the three main cubic axes of austenite. However, close examination of the high resolution EBSD mapping reveals that more than just three orientations, as expected from the Bain model, exist in Ni50Mn29Ga21. Each of three Bain variants may be split in some twin relations in different regions of the sample which differ from each other by about few degrees creating a much higher number of variants. The training process, as the last step in the preparation procedure of Ni-Mn-Ga alloys, consists of multi-axis compression finally leading to a single-variant state. Compression of polycrystalline samples leads to motion of those twin boundaries changing the volume fraction of particular martensitic variants in such a way that the shortest axis (c-axis) becomes preferentially aligned parallel to the compression axis. It allows reducing the twinning stress and maximizing the twinning strain. To understand the training process in more detail, the interaction of the twin variants with the neighbourhood of parent austenite grains was investigated.

This thesis concerns the mathematical modelling of phase transformations with a special emphasis on martensitic phase transformations and their application to the modelling of steels. In Chapter 1, we develop a framework that determines the optimal transformation strain between any two Bravais lattices and use it to give a rigorous proof of a conjecture by E.C. Bain in 1924 on the optimality of the so-called Bain strain. In Chapter 2, we review the Ball-James model and related concepts. We present some simplification of existing results. In Chapter 3, we pose a conjecture for the explicit form of the quasiconvex hull of the three tetragonal wells, known as the three-well problem. We present a new approach to finding inner and outer bounds. In Chapter 4, we focus on highly compatible, so called self-accommodating, martensitic structures and present new results on their fine properties such as estimates on their minimum complexity and bounds on the relative proportion of each martensitic variant in them. In Chapter 5, we investigate the contrary situation when self-accommodating microstructures do not exist. We determine, whether in this situation, it is still energetically favourable to nucleate martensite within austenite. By constructing different types of inclusions, we find that the optimal shape of an inclusion is flat and thin which is in agreement with experimental observation. In Chapter 6, we introduce a mechanism that identifies transformation strains with orientation relationships. This mechanism allows us to develop a simpler, strain-based approach to phase transformation models in steels. One novelty of this approach is the derivation of an explicit dependence of the orientation relationships on the ratio of tetragonality of the product phase. In Chapter 7, we establish a correspondence between common phenomenological models for steels and the Ball-James model. This correspondence is then used to develop a new theory for the (5 5 7) lath transformation in low-carbon steels. Compared to existing theories, this new approach requires a significantly smaller number of input parameters. Furthermore, it predicts a microstructure morphology which differs from what is conventionally believed.

Orietadores: Paulo Roberto Mei, Sadamu Koshimizu / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecanica / Made available in DSpace on 2018-07-22T11:12:58Z (GMT). No. of bitstreams: 1 Otubo_Jorge_D.pdf: 18862199 bytes, checksum: 741b9894b9a5962f8f8467424dd40055 (MD5) Previous issue date: 1996 / Resumo: É apresentado neste trabalho, pioneiro no Brasil, o desenvolvimento de ligas inoxidáveis com Efeito de Memória de Forma (EMF) assistido por transformação martensítica não termoelástica. Mostrou-se que a fusão por indução à vácuo é uma técnica adequada e que tanto o trabalho a quente como o trabalbo a frio são perfeitamente possíveis nas ligas em questão à medida que os parâmetros operacionais como temperatura de aquecimento, redução por passe, etc., sejam controlados. A eficiênciada técnica de treinamento na melhora do Efeito de Memória de Forma foi comprovada com a recuperação de forma em torno de 95 % da liga CrNi e de 89 % da liga CrNiCo após 5 ciclos com pré-deformação de 4% e aquecimento a 600 °e. Estes resultados são bastante promissores e comparáveis aos melhores resultados encontrados na literatura. O caráter inoxidável e a recuperação de forma de praticamente 4% das ligas desenvolvidas promovem-nas para aplicações práticas como conexões de tubo sem solda e mecanismo para liberação de painéis solares de satélite. Considerações sobre processamento, propriedades mecânicas e microestruturais são também analisadas / Abstract: It is presented in this work, pioneer in Brazil, the development of stainless alloys with shape memory effect assisted by non thermoelastic martensitic transformation. It was shown that Vacuum Induction Melting (VIM) is a suitable technique for melting these alloys and that hot working or cold working are perfectly possible as long as the heating temperature, reduction per pass, etc. are controlled. The efficiency of training technique in improving the Shape Memory Effect was shown by the 95 % shape recovery of the CrNi alloy and by 89 % of shape recovery of the CrNiCo alloy after five training cyc1es of 4 % pre-strain and annealing at 600°C. These results are very promising and comparable to the best ones published in the literature. The stainless character and the shape recovery of almost 4% promote these alloys for practical applications such as for pipe fitting and for satellite solar panel release mechanism.The alloys' processing, mechanicaland microstructural properties are also analyzed. / Doutorado / Materiais e Processos de Fabricação / Doutor em Engenharia Mecânica

CoordenaÃÃo de AperfeiÃoamento de Pessoal de NÃvel Superior / O presente trabalho visou estudar o efeito da deformaÃÃo plÃstica prÃvia por laminaÃÃo e o efeito da deformaÃÃo por traÃÃo no processo de seleÃÃo de variantes durante a transformaÃÃo martensÃtica no aÃo inoxidÃvel austenÃtico AISI 301L. Foram comparadas amostras previamente laminadas e deformadas em ensaio de traÃÃo com amostras apenas deformadas plasticamente em traÃÃo. Aspectos relativos a macrotextura obtidos pela tÃcnica de difraÃÃo de Raios-x e microtextura obtidos por difraÃÃo de elÃtrons retro-espalhados (EBSD) foram estudados. A macrotextura analisou a evoluÃÃo das principais componentes de textura da fase martensÃtica a partir do cÃlculo das funÃÃes de distribuiÃÃo de orientaÃÃo cristalogrÃfica (FDOC). As figuras de pÃlos obtidas por EBSD para grÃos selecionados foram comparadas com figuras de pÃlos calculadas utilizando a teoria fenomenolÃgica da cristalografia da transformaÃÃo martensÃtica cuja sigla em inglÃs à (PMTC). O modelo de Patel-Cohen para simular a influÃncia da tensÃo aplicada durante o processo de transformaÃÃo martensÃtica foi utilizado. Os resultados mostraram que a textura da martensita induzida por deformaÃÃo à tÃpica de uma microestrutura cÃbica de corpo centrado (CCC). Mostraram tambÃm que as amostras apenas tracionadas seguiram o modelo de Patel-Cohen para a seleÃÃo de variantes. Jà as amostras prÃ-deformadas por laminaÃÃo apresentaram uma maior dispersÃo em relaÃÃo ao modelo principalmente as que tiveram posteriormente pouca deformaÃÃo plÃstica por traÃÃo. / The present work aimed to study the effect of the plastic prior strain for rolling and the effect of the strain for tensile test in the process of variants selection during the martensitic transformation in the austenitic stainless steel AISI 301L. There were compared samples previously rolled and deformed in tensile test with samples only plastically deformed in tensile test. Relative aspects to macrotexture obtained by the technique of diffraction of X-rays and microtexture obtained by Electron backscattered diffraction (EBSD) were studied. The macrotexture analysed the evolution of the principal texture components of the martensitic phase from the calculation of the orientation distribution function (ODF). The pole figures obtained by EBSD for selected grains were compared with pole figures calculated using the phenomenological theory of martensite crystallography whose acronym in English is (PMTC). The model of Patel-Cohen to simulate the influence of the tension applied during the process of martensitic transformation was used. The results showed that the texture of the deformation induced martensite is typical of a body-centered cubic microstructure. They showed also that the only tensile samples followed the model of Patel-Cohen for the variants selection. The prior deformed samples by rolling presented a bigger dispersal regarding model principally those who subsequently had little plastic deformation for traction.

Diversos componentes mecânicos como engrenagens, rolamentos, cilindros de laminação, trilhos e rodas de trem sofrem uma determinada solicitação conhecida por fadiga de contato, que consiste em uma solicitação causada pela tensão gerada entre o contato de dois corpos sob a ação de uma carga cíclica. Este trabalho teve como objetivo avaliar a resistência a esta solicitação para um aço ferramenta com microestruturas martensíticas e bainíticas. Para isto, foi utilizado um equipamento na configuração esfera contra plano, onde as esferas foram confeccionadas em material comercial ABNT 52100 e os discos em aço ferramenta tratados termicamente para obtenção de microestruturas martensíticas e bainíticas. Os ensaios foram realizados com a aplicação de uma pressão máxima de contato de 4,8 GPa até que ocorresse a falha por microlascamento da superfície do disco. Os resultados de vida em fadiga destes materiais foram apresentados por uma distribuição de Weibull que demonstraram uma maior resistência do material bainítico. Os resultados apresentados para ambas as microestruturas demonstraram que as falhas se iniciaram predominantemente na sub-superfície, atendendo as premissas iniciais do trabalho que buscava uma baixa ocorrência de falhas superficiais prematuras ocasionadas por possíveis inclusões, defeitos ou poros superficiais que agiriam como um concentrador de tensões, levando a uma falha antes que efetivamente as características físicas e metalúrgicas das microestruturas sejam testadas. / Several mechanical components such as gears, bearings, rolling mill rolls, rails and train wheels suffer a particular request known to contact fatigue, which consists of a request caused by the tension generated between the contact of two bodies subjected to a cyclic loading. This study aimed to evaluate the resistance to this request for tool steel with bainitic and martensitic microstructures. For this, was used a machine in the configuration ball against flat washer, where balls were made of commercial material ABNT 52100 and flat washer in tool steel heat-treated to obtain martensitic and bainitic microstructures. The tests were performed by applying a maximum contact pressure of 4.8 GPa until the failure by micro-spalling on the disk surface or subsurface. The results of the fatigue life of those materials were presented by a Weibull distribution that showed a better resistance to the bainitic material to this request. The results presented for both microstructures showed that the failures were initiated predominantly sub-surface, given the initial goals of the work, as evidenced by the low occurrence of premature superficial failures possibly caused by inclusions, pores or surface defects that would act as a stress concentrator leading to a premature failure before the physical and metallurgical microstructures characteristics were really tested.

Orientador: Rubens Caram Junior / Tese de Doutorado - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica / Made available in DSpace on 2018-08-22T19:13:03Z (GMT). No. of bitstreams: 1 Contieri_RodrigoJose_D.pdf: 5581364 bytes, checksum: b95f94b00d984d338e4134cd12621962 (MD5) Previous issue date: 2013 / Resumo: Ligas do sistema Ti-Cu com composições próximas à eutetóide exibem potencial para aplicações estruturais, pois apresentam interessantes propriedades mecânicas, baixa densidade e alta resistência à corrosão. O comportamento mecânico dessas ligas depende diretamente das condições de processamento e tratamentos térmicos aplicados. Em condições de equilíbrio, a microestrutura dessas ligas é formada pela fase ? e pelo composto intermetálico Ti2Cu. Dependendo das condições de processamento, estruturas metaestáveis podem ser formadas. O objetivo deste trabalho foi avaliar o efeito de diferentes tratamentos térmicos na microestrutura e nas propriedades mecânicas de ligas Ti-Cu. Inicialmente, amostras com composições hipoeutetóide, eutetóide e hipereutetóide foram resfriadas a partir de altas temperaturas em um dispositivo de ensaio Jominy modificado e por ensaios de "splat colling". Na sequência, ensaios de envelhecimento aplicados a amostras com microestruturas metaestáveis também foram realizados. A caracterização das amostras envolveu microscopia óptica, eletrônica de varredura e de transmissão, difração de raios-X, tomografia atômica tridimensional e ensaios mecânicos. Os resultados obtidos indicam que altas taxas de resfriamento resultam na formação de microestruturas formadas por martensita ? ' e pelo composto Ti2Cu com composições diferentes das de equilíbrio. O módulo de elasticidade não apresentou variação com a taxa de resfriamento. Resultados de envelhecimento sugerem que o máximo valor de dureza Vickers e de resistência mecânica correspondem à perda de coerência entre os precipitados do composto intermetálico Ti2Cu e a matriz de fase ? / Abstract: Alloys in the Ti-Cu system with compositions close to the eutectoid exhibit potential for structural applications because they present interesting mechanical properties, low density and high corrosion resistance. The mechanical behavior of these alloys depends directly on the processing conditions and heat treatments applied. Under equilibrium conditions, the microstructure of these alloys is formed by the ? phase and the Ti2Cu intermetallic compound. Depending on the processing conditions imposed, metastable structures may be formed. The aim of this study was to evaluate the effect of different heat treatments on the microstructure and mechanical properties of Ti-Cu alloys. Initially, sample of hypoeutectoid, eutectoid and hypereutetoid compositions were cooled from high temperatures by in a modified Jominy test setup and by the "splat cooling technique". Following, aging heat treatments were applied to the samples with metastable microstructures. The sample's characterization included optical microscopy, scanning and transmission electron microscopy, X-ray diffraction, 3-dimensional atomic tomography and mechanical testing. The results suggests that high cooling rates result in the formation of microstructures formed by martensite ? ' and the Ti2Cu compound with compositions different from the equilibrium composition. The elastic modulus does not vary with the cooling rate. Aging results suggest that the maximum values of Vickers hardness and mechanical strength correspond to the loss of coherence between the Ti2Cu intermetallic compound precipitates and the ? phase matrix / Doutorado / Materiais e Processos de Fabricação / Doutor em Engenharia Mecânica

Mainly two different morphologies of martensite can be obtained in steels depending on the amount of alloying elements. The first morphology, referred to as lath martensite, forms in low alloy, low carbon steels. It is, by far, the most extensively studied form of martensite due to its industrial applications. The second morphology of martensite, referred to as plate martensite, forms in highly alloyed and in high carbon steels and in particular in Fe-High Ni alloys. In this case, the transformation product is disc shaped and internally twinned. This morphology is the only form of martensite that has the potential to exhibit shape memory properties. It is therefore of great interest to understand the mechanisms of its formation. This is investigated in the present dissertation through the study of the martensitic transformation occurring in a Fe-30.5%Ni-0.155%C alloy. More precisely, the influence of stress and grain size on the crystallography of plate martensite is discussed in the general framework of the phenomenological theory of martensite crystallography. This theory allows associating a unique shape deformation to each orientational variant. In this way, the experimental observations carried out at different length scales by means of optical microscopy, EBSD and TEM can be used to infer the transformation path followed under different conditions. Firstly, the burst configurations of variants observed in coarse-grained austenite under stress free conditions are rationalized by considering the mechanical couplings between the variants. It is shown that self-accommodating and autocatalytic couplings are responsible for the formation of hierarchical configurations of variants. More precisely, the transformation is shown to occur through the alternate formation of perpendicular plate groups of variants. Self-accommodation is the dominant coupling between variants of the same plate group while autocatalytic couplings are responsible for the transfer of the transformation from one generation to the next. It is suggested that the plastic accommodation of the shape deformation plays a dominant role in propagating the transformation to a lower length scales. Secondly, the influence of a uniaxial stress state on the transformation is studied. It is seen experimentally that only the most favoured variants are systematically formed in coarse Cube grains while coarse non-Cube grains generally transform into plate groups of variants that are only moderately favoured by the stress. These observations are well explained by considering the interaction energy between the applied stress and the shape deformation associated with the transformation. Thirdly, the influence of the austenitic grain size on the transformation is also studied. A decrease in grain size is seen to decrease the martensite start temperature. For a grain size below about 10µm, the thermal transformation in liquid nitrogen is indeed suppressed in the present alloy. This observation is related to the increasing yield strength of austenite as the grain size is reduced. A noticeable change in the morphology of martensite also accompanies the decrease in grain size. Indeed, martensite forming in coarse-grained austenite is mostly lens shaped and partially twinned while it appears plate shaped and fully twinned in smaller grains. Furthermore, martensite forming in fine-grained austenite develops self-accommodating configurations suggesting that most of the transformation deformations are elastically accommodated in this case. This is believed to be related to the observance of a shape memory effect in the present alloy in its fine-grained condition. / Doctorat en Sciences de l'ingénieur et technologie / info:eu-repo/semantics/nonPublished

Abstract Whenever a foreign material is implanted into a human body an implant–tissue interface area forms between them. In this microenvironment, interactions take place between the implant and the surrounding tissue. The implantation of a biomaterial into tissue results in injury and initiation of the inflammatory response. This host response to biomaterials is an unavoidable series of events that occur when tissue homeostasis is disturbed by the implantation process. In bone tissue, biocompatible implants must initially be capable of strong bone implant contact and subsequently, allow the normal bone remodeling cycle around the implant. NiTi is a metal alloy composed of approximately a 50:50 ratio of nickel and titanium. It possesses shape memory and superelasticity properties, which make it an interesting biomaterial. NiTi has two phases: austenite and martensite. A decrease in temperature or applied stress induce the austenite-to-martensite transformation. Heating or removing the stress restores the parent austenite phase. The alloy in its martensite structure can be reshaped and strained several times more than a conventional metal alloy without irreversible deformation of the material. The alloy returns to its original shape as it changes from martensite-to-austenite. This transformation is seen as the macroscopic shape memory effect. This study further investigated the biocompatibility of NiTi, especially the bone cell response to both austenite and martensite. Different surface treatments were investigated in order to improve and possibly even control NiTi's bioactivity as a bone implant material. Osteoclasts grew and attached well on the austenite NiTi phase, but the results indicated that the biocompatibility of martensite NiTi was compromised. Oxidation of the NiTi surface improved osteoblast attachment and viability. This was due to the formation of a TiO2 surface layer of moderate thickness. Coating the NiTi surface with the extracellular matrix protein fibronectin was shown to enhance osteoblast proliferation and increase the number of cells in the G1 cell cycle stage. Austenite was more prone to show these effects than martensite. A sol-gel derived titania-silica surface treatment was observed to increase the bone implant contact of functional NiTi intramedullary nails. The surface treatment was most effective with the constant bending load provided by the NiTi nail.