Les alliages ODS (Oxides Dispersion Strengthened), sont principalement étudiés pour leur capacité à répondre favorablement au cahier des charges de la fonction de gainage combustible pour les réacteurs nucléaire de type RNR-Na (Réacteur à Neutrons Rapides à caloporteur sodium). Elaborés par métallurgie des poudres, mécanosynthèse puis extrusion, ils affichent des propriétés mécaniques, et notamment en fluage, extrêmement intéressantes. Néanmoins, la voie élaboration utilisée induit une forte anisotropie microstructurale. Cette anisotropie se retrouve au niveau de leurs propriétés mécaniques et conduit à une fragilité dans le sens de sollicitation transverse. Le but de cette thèse est d'étudier l'évolution microstructurale de ces matériaux. Les aciers ODS présentent des microstructures ultra fines en termes de grains, de précipités, et de formation d'amas qui conduisent à de grandes difficultés pour en obtenir la recristallisation. De plus, les microstructures obtenues présentent souvent une recristallisation avec croissance anormale. De telles évolutions demandent des investigations à très fine échelle et ont été relativement peu examinées dans le domaine des alliages ODS. Il faut en effet être capable d'une étude structurale la plus quantitative possible de la microstructure des nanograins, ainsi que de la précipitation afin d'étudier les mécanismes d'interaction précipitation / joints de grain. Ceci n'est possible que par un couplage de différentes méthodes : la microscopie électronique en transmission (en particulier avec l'utilisation des outils récemment développés pour l'étude de la nanotexturation, i.e. ACOM-TEM); la diffusion centrale des neutrons ou des rayons X; et enfin la sonde atomique tomographique, à la fois pour apporter les informations sur la morphologie et la chimie des amas et nanoprécipités mais surtout sur la composition chimique aux joints de grains. A partir de l'identification des mécanismes contrôlant la croissance anormale, une modélisation permettant de prédire son apparition dans la microstructure est confrontée à cette caractérisation microstructurale poussée. Cette modélisation prête une attention particulière à la migration des joints de grains couplée à la diffusion et effets d'ancrage préférentiel des joints triples par les précipités ainsi qu'à l'énergie motrice stockée sous forme de densité de dislocation. / Oxide Dispersion Steels (ODS) alloys are mainly studied for their ability to fulfil the technical specifications required for Sodium Fast Reactor (SFR) fuel cladding application. Their processing involves powder metallurgy, mechanical alloying and extrusion. Therefore, despite their interesting mechanical creep properties, the extrusion processing involves a high microstructural anisotropy. These particular feature leads to poor mechanical properties in the transverse direction which are worsen by the occurrence of abnormal grain growth. Unfortunately, since internal pressure increases in the tube with the accumulation of gas fission products, the major stress component is precisely applied in the transverse direction. As a result, the material faces a critical risk of failure and control of the microstructure is a key issue. The aim of this thesis is to study the microstructural evolution of ODS ferritic steels. ODS ferritic steels show ultrafine microstructures in terms both grains and precipitates which made the recrystallization very difficult and allow for abnormal grain growth. To observe such evolutions, fine scale microstructure characterization are necessary. This is only possible by coupling different characterization methods: transmission electronic microscopy (in particular with the new developed tools for nanotexturation studies, i.e. ACOM-TEM); neutron and X-ray small angle scattering; and atomic probe tomography. Based on the mechanisms that lead to and control the abnormal grain growth, a model to predict the occurrence of abnormal grain growth is confronted to the experimental results. This model that takes a particular attention to the dislocation stored energy effect to adequately reproduce the observed characterization results.

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Orientador: Peter Christian Hackspacher / Banca: Fernando Flecha Alckmim / Banca: Marcos Egydio Silva / Banca: Ticiano Saraiva / Banca: Hans Dirk Hebert / Resumo: A grande variedade de microestruturas e texturas encontradas nos minérios de ferro do Quadrilátero Ferrífero no Brasil gera uma ampla diversidade de propriedades físicas com grandes implicações para o seu beneficiamento. O vínculo entre reologia, mecanismos de deformação que atuaram na formação de várias microestruturas e texturas ou orientações cristalográficas preferenciais (OCP), fornecem resultados que podem ser aplicados para uma explotação estratégica dos diferentes tipos de minérios, implicando na melhoria de áreas alvos. Este estudo foi focado na avaliação da correlação de microestruturas/texturas com parâmetros de flotação, visando otimizar o processo de flotação para aumentar a recuperação dos minérios "pobres" (ricos em sílica), que comumente contêm menos de 64% de Fe. Uma série de técnicas, incluindo difração por nêutrons, raios-X e elétrons retroespalhados (elétron backscattering difraction), bem como análises granulométricas e de imagens dos concentrados de flotação foram aplicados neste trabalho. Os resultados obtidos por meio das análises microestruturais e texturais, permitiram enquadrar os diferentes minérios no seu contexto tectônico, dentro do Quadrilátero Ferrífero. Adicionalmente, a diversidade reológica, obtida por várias técnicas resultou na definição de parâmetros de correlação com a flotação, que podem ser aplicados na indústria de beneficiamento, contribuindo para aumentar a recuperação do minério de ferro. / Abstract: The wide range of minerals, microstructures and textures encountered in iron ores of the Quadrilátero Ferrífero region in Brazil, generates a diversity of physical properties with implications to its processing. The linking between rheology and deformation mechanisms which acted in microstructure and texture or crystallographic preferred orientations (CPO), formation provide results witch can be applied in strategic exploitation of different ore types, leading to the improvement of the selected targets. This study was focused in the evaluation and correlation of textures, microstructures with flotation parameters, aiming to optimize the flotation processing to increase the recovery of low-grade iron ores, which commonly contain less than 64% Fe. A series of techniques, including neutron diffraction, X-ray diffraction, electron backscattering diffraction as well as granulometric and imaging analysis of flotation concentrates were applied in this study. The results obtained through the textural and microstructural studies allow fitting different ores in your tectonic setting, into Quadrilátero Ferrífero. Additionally, the diversity of rheologic features defined by the different techniques led to define new correlation parameters with selectivity indices of flotation that can be applied to the iron ore processing industry, contributing to increase iron ore recovery. / Doutor

Orientador: Peter Christian Hackspacher / Banca: Luiz Sergio Amarante Simões / Banca: Nelson Angeli / Banca: Carlos José Archanjo / Banca: Marcos Egydio da Silva / Resumo: A zona de cisalhamento Itapetim (ZCI) desenvolveu foliação e lineação nos diferentes tipos de rochas, milonitos a ultramilonitos. Muitos dos tipos de microestruturas observadas na ZCI preservam evidências de condições metamórficas de alto grau e baixo grau de temperatura. O padrão das orientações preferenciais dos eixos [c] de quartzo, obtida a partir de agregados policristalinos deformados, mostra dois diferentes tipos de simetrias, guirlandas do tipo I e simples. A análise da textura sugere partição da deformação com cisalhamento coaxial e não coaxial na ZCI. Um veio de quartzo mineralizado em ouro encaixado em rocha ultramilonítica, constitui a zona de precipitação hidrotermal. O veio é bandado por segmentos de turmalina, o qual inclui agregados de grãos de quartzo maciço entre as bandas. Os grãos de quartzo mostram contatos poligonais e restritos limites intumescentes. O último sugere recristalização dinâmica por migração de limite de grão e os grãos poligonais (microestrutra em espuma) são melhor explicados por annealing. Os padrões de eixos [c] de quartzo obtido no veio aurífero é idêntico ao observado nos ultramilonitos da ZCI. Este padrão é interpretado como uma textura preservada formada durante o cisalhamento não coaxial. A estrutura bandada é interpretada como o resultado de variações da pressão de fluidos e a formação microfraturas, associadas a eventos de crack-seal. Mecanismos de crack-seal foram ativos antes ou durante a deformação da ZCI. As feições microestruturais suportam evidências para a última possibilidade. / Abstract: The Itapetim shear zone(ISZ) developed both foliation and lineation in the different rock types, from mylonites to ultramylonites. Most of the microstructure types observed in the ISZ preserve evidence of high temperature metamorphic conditions. The quartz [c]-axis, of deformed polycrystalline aggregates, show two distinct symmetries, type I crossed girdles and single girdles. The geometrical analysis of texture, suggest non-coaxial shear for deformation in ISZ. A gold mineralized quartz vein hosted in ultramylonitic rocks, constitutes the hydrothermal precipitation zone. The vein is banded by tourmiline segments, which include massive quartz grains aggregates between the bands. The quartz grains show polygonal contacts and minor intumescent limits. These latter suggest grain boundary migration recrystallization and the polygonal grains seem to be best explained by the annealing after stopping the shear deformation. The quartz [c]-axis obtained in the auriferous vein shows the same single girdle pattern observed in the ultramylonites of the ISZ. This pattern is interpreted as a preserved texture formed during the shear deformation. The banded structure is interpreted as the result of variations of the fluid pressure and the formation of microfractures, associated the crack-seal events. Crack-seal mechanisms can have been active previous or during the deformation of the IZS. The microstructurals features supports evidences for the last possibility. / Doutor

Les objectifs de cette thèse sont d’établir les corrélations entre l’histoire thermomécanique, la microstructure et la perméabilité aux ultrasons de l’Udimet 720.La première approche est expérimentale et concerne l’étude de l’influence des paramètres thermomécaniques de mise en forme (température, vitesse de déformation et taux de déformation) sur l’évolution microstructurale, et l’identification des mécanismes de recristallisation associés. En parallèle, une modélisation mésoscopique du forgeage a été développée en couplant un modèle cristallin de déformation de type éléments finis et un modèle de recristallisation basé sur la méthode des automates cellulaires, afin de prévoir l’évolution microstructurale en fonction de la microstructure initiale et des conditions thermomécaniques.Une dernière partie traite de l’identification des paramètres microstructuraux néfastes à la perméabilité aux ultrasons, et de la modélisation de la propagation des ultrasons dans un matériau polycristallin pour quantifier l’influence des désorientations et de la taille des grains. / This works deals with the correlations between the thermomechanical process, the microstructure and the permeability to ultrasonic waves of the Udimet 720 superalloy. The first approach is experimental and concerns the influence of the thermomechanical parameters (temperature, strain rate and deformation ratio) on the microstructure evolution. In particular, this study focuses on the identification of recrystallization mechanisms. In parallel, a mesoscopic crystalline modelling of deformation implemented in a finite element code coupled to a recrystallization Cellular Automaton code has been developed and applied to forging processes. The model predicts the evolution of different experimental microstructures as a function of thermomechanical parameters.The last part deals with the identification of unfavorable parameters of the microstructure on the ultrasonic permeation. Moreover a modeling of the ultrasounds propagation in a polycrystalline material is proposed to quantify the effects of the average grain size and the grain misorientation distribution.