O Processamento e Análise Digital de Imagens é utilizado cada vez mais para agilizar processos, aumentar a precisão, segurança e confiabilidade de dados extraídos de imagens nas mais diversas áreas de pesquisa. No entanto, muitas vezes é necessário que o pesquisador faça, ele próprio, o pré-processamento das imagens, mesmo não sendo um especialista nesta área. Isto coloca em risco o próprio objetivo do uso do Processamento e Análise Digital de Imagens. Este trabalho analisa a relação dos dados extraídos de uma imagem (micrografia) através do software livre ImageJ com relação ao seu processamento final desejado, avaliando assim, a necessidade ou não, de uma ou mais sequencias de pré-processamento para adequar a imagem para o processamento final, indicando ainda quais fatores de influência apresentam informações irrelevantes ou incompletas para o processamento final utilizando ferramentas da Lógica Paraconsistente Anotada. Os resultados obtidos mostram que esta abordagem carece de informações diversificadas sobre a imagem original capturada que possam subsidiar a tomada de decisão quanto aos procedimentos necessários e, para o pré-processamento adequado ao objetivo desejado. / Processing and Analysis of Digital Images is increasingly used to streamline processes, improve accuracy, safety and reliability of data extracted from images in various research areas. However, it is often necessary for the researcher to make himself, the preprocessing of images, although not an expert in this area. This puts at risk the very purpose of using the Processing and Analysis of Digital Images. This paper analyzes the relationship of the data extracted from an image (micrograph) through the free software ImageJ, with respect to its desired final processing. Thus, evaluating the necessity or not, of one or more sequences of preprocessing to adjust the image to the final processing, further indicating which factors influence presents incomplete or irrelevant information for final processing using tools of Annotaded Paraconsistent Logic. The results show that this approach lacks diversified information about the original image captured that can support decision making about procedures for appropriate preprocessing to the desired goal.

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.

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.

Les aciers renforcés par dispersion d’oxydes (ODS) sont des matériaux candidats pourconstituer les gaines de combustibles des réacteurs nucléaires de IVème génération refroidis au sodium(RNR-Na). Le soudage par résistance en bout de ces gaines est étudié dans ce travail, avec pourobjectif la détermination et la compréhension des effets du procédé sur l’évolution de la microstructuredes aciers ODS à 9 % et 14 % de chrome à l’échelle des grains et des oxydes nanométriques. Uneapproche couplant caractérisations microstructurales sur soudures, simulation numérique et simulationphysique du procédé, à l’aide d’un simulateur thermomécanique Gleeble 3500, est adoptée. Le soudagepar résistance en bout impose localement des conditions de sollicitations sévères en termes dedéformation, vitesse de déformation et température. Ces sollicitations induisent un affinement de lamicrostructure dont l’origine peut être attribuée à un mécanisme de recristallisation dynamique (acier à14 % de chrome) ou à l’association de la recristallisation dynamique et des transformations de phase(acier à 9 % de chrome). Les conditions d’occurrence de la recristallisation dynamique sont étudiéessur ces matériaux. On montre notamment la possibilité d’une transition entre recristallisation dynamiquecontinue et discontinue sur l’acier à 14 % de chrome en fonction des conditions de sollicitation. Il estégalement observé que ces sollicitations thermomécaniques sévères induisent une augmentation de lataille des oxydes nanométriques associée à une diminution de leur fraction volumique. / Oxide dispersion strengthened (ODS) steels are considered as candidate materials for thedevelopment of fuel cladding for sodium-cooled fast reactors (SFR). Resistance upset welding of thecladding is studied in this work. The aim is to determine and to understand the process effects on themicrostructure of ODS steels with 9% and 14% of chromium at the scales of the grains and thenanometric oxides. An approach coupling microstructural characterization of welds, numericalsimulation and physical simulation of the process, using a thermomechanical simulator Gleeble 3500,is proposed. Resistance welding locally imposes severe thermomechanical conditions in terms of strain,strain rate and temperature. Refinement of the microstructure is noted and correspond to a dynamicrecrystallization mechanism (14 % Cr steel) or the combination of dynamic recrystallization and phasetransformations (9 % Cr steel). The conditions of occurrence of dynamic recrystallization are studied.The possibility of a transition between continuous and discontinuous dynamic recrystallization is shownfor the 14 % Cr steel according to the loading conditions. Such severe thermomechanical conditionsinduce an increase in the size of nanoscale oxides associated with a decrease of their volume fraction.

Les alliages aluminium-silicium (Al-Si) ont attiré une attention considérable en raison de leur importance pour les applications industrielles. Dans le présent travail, des alliages à haute pureté (Al-12.7 wt. % Si) avec et sans ajout de strontium (400 ppm), solidifiés lentement en creuset ou de façon dirigée (DS), ont été préparés et traités thermiquement. L'influence de l'ajout de strontium et des post-traitements thermiques sur les caractéristiques microstructuraux et cristallographiques des phases eutectiques a été étudiée de façon systématique. Les caractéristiques de croissance du silicium eutectique (Si) dans l'alliage non modifié ainsi que dans l'Al-12.7Si Sr-modifié ont été étudiés. Pour le cas du non-modifié, la formation répétée de variantes de macles mono-orientées permet une croissance rapide du silicium eutectique selon le mécanisme twin plane re-entrant (TPRE). Microscopiquement, les cristaux de silicium ont une forme de plaque allongée dans la direction <1 1 0> non conforme à la croissance selon <1 1 2> présumée par le modèle TPRE. L'élongation selon <1 1 0> est réalisée par des paires en zigzag <1 1 2> sur des plans de maclage parallèles, conduisant à une disparition alternative et à la création de macles rentrantes à 141°. Ce mécanisme de croissance permet aux cristaux de silicium de n'exposer que les plans {1 1 1} à faible consommation d'énergie à la consolidation. Pour les alliages modifiés au strontium, des changements importants de morphologie apparaissent dans le silicium eutectique, attribuable à la croissance de TPRE restreinte et au maclage induit par les impuretés (IIT). Ce dernier améliore la croissance latérale en formant de nouvelles macles avec des plans de macles parallèles, tandis que le second conduit à une croissance isotrope en formant des macles orientées différemment. Le traitement thermique provoque l'affinement des grains des deux phases eutectiques. L'affinement de l'α-Al se produit en même temps que la fragmentation et la sphéroïdisation du silicium et est principalement lié à la fracture des grains de silicium en raison de leur capacité limitée à accommoder la très grande dilatation thermique l'α-Al, ainsi qu'à la diffusion des atomes d'aluminium au cours du traitement thermique. La rupture du silicium génère une force de "capillarité" qui active la diffusion d'atomes d'aluminium dans la fissure. En raison du caractère de substitution de la diffusion de l'aluminium, la migration des lacunes vers l'intérieur de l'α-Al est induite lorsque l'aluminium se déplace dans les fissures, ainsi les vides de la fracture du silicium sont transférés à l'α-Al. De cette façon, les cristaux d'α-Al sont altérés et déformés. Les défauts cristallins produits, à leur tour, initient la restauration et même la recristallisation du α-Al, ce qui entraîne une diminution de taille de grain. La phase α-Al dans l'alliage de Al-12.7Si-0.04Sr solidifiée directionnellement, affiche une forte texture de fibre <1 0 0> parallèle à la direction de solidification. De très gros grains <1 0 0> α-Al sont principalement formés à la périphérie de l'échantillon cylindrique en raison des directions d'évacuation de chaleur favorables disponibles pour les trois directions [1 0 0]. Après traitement thermique, l'intensité de la texture de la phase α-Al diminue en raison de la restauration et de la recristallisation, mais le type de texture ne change pas. Pour la phase de silicium eutectique dans l'alliage de coulée, il y a deux fibres principales de texture, <1 0 0> et <1 1 0> parallèles à la direction de solidification, accompagnées de deux composantes faibles, <2 2 1> et <1 1 3> dans la même direction. Les fibres <1 0 0> et <1 1 0> correspondent à des grains de silicium situés sur la périphérie et dans le centre de l'échantillon. Les composantes <2 2 1> et <1 1 3> proviennent de plusieurs macles de grains orientés <1 1 0> et <1 0 0>. Les faibles intensités de ces deux composantes sont liées à leur fraction volumique mineure [...] / Al-Si alloys have attracted considerable attention due to their importance to industrial applications. In the present work, both crucible slowly solidified and slowly directionally solidified (DS) high-purity Al-12.7 wt. % Si alloys with and without 400 ppm Sr addition have been prepared and heat treated. The influence of Sr addition and post heat treatments on the microstructural and crystallographic features of the eutectic phases has been systematically studied. The growth characteristics of eutectic Si in the unmodified and the Sr-modified Al-12.7Si alloys were investigated. For the non-modification case, the formation of repeated single-orientation twin variants enables rapid growth of eutectic Si according to the twin plane re-entrant (TPRE) mechanism. Microscopically, Si crystals are plate-like elongated in one <1 1 0> direction that is not in accordance with the <1 1 2> growth assumed by the TPRE model. The <1 1 0> extension is realized by paired <1 1 2> zigzag growth on parallel twinning planes, leading to alternative disappearance and creation of 141° re-entrants. This growth manner ensures Si crystals to expose only their low-energy {1 1 1} planes to the melt. For the Sr-modification case, substantial changes appear in eutectic Si morphology, attributable to the restricted TPRE growth and the impurity induced twinning (IIT) growth. The first enhances lateral growth by forming new twins with parallel twinning planes, while the second leads to isotropic growth by forming differently oriented twins. Heat treatment brings about refinement of both eutectic phases. The refinement of the α-Al occurs concomitantly with the fragmentation and spheroidization of Si and is mainly related to the fracture of the Si crystals due to their limited capacity to accommodate the giant thermal expansion of the α-Al and the diffusion of Al atoms to the cracks during the heat treatment. The Si fracture generates “capillarity” force that activates the diffusion of Al atoms to the gap of the crack. Due to the substitutional feature of Al diffusion, the migration of vacancies toward the interior of the α-Al is induced when Al moves to the gaps, thus the voids of the Si fracture are transferred to the α-Al. In this way, the crystals of α-Al are distorted and defected. The produced crystal defects, in turn, initiate recovery and even recrystallization of the α-Al, resulting in grain refinement. The α-Al phase in the directionally solidified Al-12.7Si-0.04Sr alloy, displays a strong <1 0 0> fiber texture in the solidification direction. Giant <1 0 0> α-Al grains are mainly formed in the outer circle region of the cylindrical specimen due to the favorable heat evacuation directions available for the three <1 0 0> directions. After heat treatment, the texture intensity of the α-Al phase decreases due to the recovery and recrystallization, but the texture type does not change. For the eutectic Si phase in the as-cast alloy, there are two main fiber texture components, <1 0 0> and <1 1 0> in the DS direction, accompanied by two weak components, <2 2 1> and <1 1 3> in the same direction. The <1 0 0> and <1 1 0> components are from Si crystals located in the outer circle and center regions of the cylindrical specimen. The <2 2 1> and the <1 1 3> components are from multiple twins of the <1 1 0> and <1 0 0> oriented crystals. The weak intensities of these two components are related to their minor volume fraction. Once heat treated, the twinned parts with minor volume fractions enlarge at the expense of their twin related matrix, thus the <1 1 0> component is weakened and accompanied by the intensification of the components from the twins. The disappearance of the <1 1 3> component and the appearance of the <1 1 5> component are due to crystallographic rotation of Si crystals during their fragmentation

Les aciers bainitiques sont utilisés industriellement pour leur bon compromis entre résistance, ductilité et ténacité. Cependant, après obtention de sa microstructure d'emploi, l’acier peut subir des maintiens additionnels en température (soit en fin de fabrication et/ou lors de son utilisation), susceptibles de dégrader ses propriétés. Ces travaux de thèse cherchent à comprendre les origines microstructurales de cette dégradation. Pour ce faire, des traitements thermiques contrôlés ont été appliqués à des aciers de nuances modèles FeNiC et FeNiMnC. Une première série de traitements a permis de fabriquer des microstructures bainitiques supérieure, inférieure, martensitique et mixtes. Ces produits de transformation bruts ont été caractérisés et analysés en détail, en particulier par EBSD en résolution angulaire améliorée. Les données ont été exploitées pour reconstruire les ex-grains austénitiques et distinguer les différents produits de transformation par l'organisation spatiale de leurs variants cristallographiques. Une deuxième série de traitements a consisté à soumettre ces microstructures à des maintiens isothermes prolongés. Nous avons montré que ces microstructures bainitiques en lattes ne sont pas stables dans certaines conditions ultérieures de maintien isotherme. Dans les cas les plus sévères, nous avons observé un processus de « granularisation » de la microstructure en lattes avec disparition des variants fortement désorientés et une maturation des carbures. Ces phénomènes sont observés sur nos alliages modèles y compris sur des temps courts (<1h) à basses températures (300°C). Ces évolutions ainsi que leurs cinétiques ont été investiguées à différentes échelles en couplant des observations en MEB, EBSD, MET et aussi in situ par DRX Haute Energie sur grands instruments. La composition chimique et la microstructure initiale affectent sensiblement les cinétiques. Mais nous avons surtout pointé le rôle majeur de la présence (même résiduelle) de bainite dite supérieure dans la microstructure initiale pour amorcer le processus de granularisation, indépendamment de la température de dénaturation. L’ensemble des résultats permet de discuter les possibles mécanismes sous-jacents et leurs forces motrices et ouvre une discussion plus large sur la classification des bainites / Bainitic steels are widely used in industry thanks to their good combinations of strength, toughness and ductility. Meanwhile, after obtaining the targeted microstructure, the steel can undergo additional isothermal holdings (either during manufacturing and/or during usage) prone to degrade its properties. The thesis work aims at understanding the microstructural origins of this degradation. To achieve this, we applied controlled heat treatments on model FeNiC and FeNiMnC steel grades. A first set of heat treatments allowed us to obtain different microstructures; upper and lower bainites, martensite and mixed concepts. These transformation products were characterized and analyzed in detail, particularly by EBSD with improved angular resolution. Data was operated to reconstruct prior austenitic grains and to distinguish the different transformation products according to their crystallographic variant spatial organization. A second set of heat treatments consisted in aging these microstructures by extended isothermal holdings. We show that lath-like bainitic microstructures are not stable under certain isothermal conditions. In the most advanced cases, we observed a « granularization » process of the lath microstructure, associated with high misoriented variant disappearance and carbides ripening. These phenomena were observed for the studied model alloys, even within short holding times (<1h) and at low temperatures (300°C). These highlighted evolutions as well as their kinetics were investigated at different scales, coupling SEM observations, EBSD, TEM and in situ XRD High Energy on large instruments. The initial microstructure and the steel chemical composition affect significantly the « granularization » kinetics. But we have above all put the light on the major role of the presence of an upper bainite fraction (even a residual one) in the initial microstructure, to start the granularization phenomenon, independently of aging temperature. All of these results allow discussing possible mechanisms with their respective driving forces and opening larger discussion about bainite classification

O Processamento e Análise Digital de Imagens é utilizado cada vez mais para agilizar processos, aumentar a precisão, segurança e confiabilidade de dados extraídos de imagens nas mais diversas áreas de pesquisa. No entanto, muitas vezes é necessário que o pesquisador faça, ele próprio, o pré-processamento das imagens, mesmo não sendo um especialista nesta área. Isto coloca em risco o próprio objetivo do uso do Processamento e Análise Digital de Imagens. Este trabalho analisa a relação dos dados extraídos de uma imagem (micrografia) através do software livre ImageJ com relação ao seu processamento final desejado, avaliando assim, a necessidade ou não, de uma ou mais sequencias de pré-processamento para adequar a imagem para o processamento final, indicando ainda quais fatores de influência apresentam informações irrelevantes ou incompletas para o processamento final utilizando ferramentas da Lógica Paraconsistente Anotada. Os resultados obtidos mostram que esta abordagem carece de informações diversificadas sobre a imagem original capturada que possam subsidiar a tomada de decisão quanto aos procedimentos necessários e, para o pré-processamento adequado ao objetivo desejado. / Processing and Analysis of Digital Images is increasingly used to streamline processes, improve accuracy, safety and reliability of data extracted from images in various research areas. However, it is often necessary for the researcher to make himself, the preprocessing of images, although not an expert in this area. This puts at risk the very purpose of using the Processing and Analysis of Digital Images. This paper analyzes the relationship of the data extracted from an image (micrograph) through the free software ImageJ, with respect to its desired final processing. Thus, evaluating the necessity or not, of one or more sequences of preprocessing to adjust the image to the final processing, further indicating which factors influence presents incomplete or irrelevant information for final processing using tools of Annotaded Paraconsistent Logic. The results show that this approach lacks diversified information about the original image captured that can support decision making about procedures for appropriate preprocessing to the desired goal.

Objetivo principal desta dissertação foi verificar os efeitos da temperatura de laminação na formação de martensita induzida por deformação e na sua posterior reversão da martensita para austenita no aço inoxidável austenítico AISI 304L. O estudo foi predominantemente microestrutural e para análise e caracterização foram utilizadas as técnicas de microscopia óptica, microscopia eletrônica de varredura, difração de raios X, medidas de dureza Vickers e medidas de fases ferromagnéticas por ferritoscopia. As amostras foram inicialmente solubilizadas a 1100 ºC por uma hora, visando a dissolução de uma pequena quantidade residual de ferrita encontrada nas amostras na condição como recebida, depois laminadas em diferentes temperaturas, determinando-se curvas de endurecimento por deformação e de formação de martensita induzida por deformação em função do grau de deformação. Em seguida, foram realizados pré-recozimentos a 600 ºC, favorecendo apenas a reversão da martensita para austenita, de maneira que não ocorresse a recristalização. A quantidade e a temperatura de deformação apresentaram forte influência na quantidade de martensita formada, no endurecimento por deformação e na cinética de amolecimento durante o recozimento. Os pré-tratamentos realizados a 600 ºC causaram acentuada reversão da martensita, algum amolecimento e pequeno efeito no tamanho de grão recristalizado durante o posterior recozimento a 600 ºC. / The main objective of the present dissertation was to verify the effects of the rolling temperature on the formation of strain induced martensite and in its subsequent martensite reversion to austenite in a AISI 304L stainless steel. The study was predominantly microstructural and, for the analysis and characterization, several techniques have been used, namely optical microscopy, scanning electron microscopy, X-ray diffraction, Vickers hardness measurements and magnetic phase measurements, using the ferritoscope. The samples were initially solution annealed at 1100 ºC for one hour, aiming at the dissolution of a small quantity of the residual -ferrite found in the samples in the as-received condition; then rolling was performed at different temperatures, evaluating strain hardening and the strain induced martensite as a function of strain. Following, pre-annealing treatments at 600 ºC have been performed, favoring only the martensite to austenite reversion, in a way that no recrystallization would occur. Strain and temperature had a strong influence on the amount of formed martensite, on the strain hardening and on the softening kinetics during annealing. The pre-annealing treatments at 600 ºC caused an accentuated effect on the martensite reversion, some softening and a small effect on the recrystallized grain size during the subsequent annealing at 600 ºC.

Made available in DSpace on 2016-08-18T18:19:27Z (GMT). No. of bitstreams: 1 LUCIENE ARAUJO NASCIMENTO.pdf: 1402629 bytes, checksum: b9ce204098b2c4fe0362b6792a692744 (MD5) Previous issue date: 2010-02-25 / FUNDAÇÃO DE AMPARO À PESQUISA E AO DESENVOLVIMENTO CIENTIFICO E TECNOLÓGICO DO MARANHÃO / Austenitic stainless steels have low economic value compared to titanium and its alloys, considered the most resistant to corrosion in biological environment, and for over fifty years are widely used in the manufacture of orthopedic implants, particularly in public health service. Currently the ISO 5832-1 steel (ASTM F 138) is the most used in the manufacture of orthopedic prosthesis, especially the temporary ones. However, because it is susceptible to localized corrosion when in contact with human tissue, it is being gradually replaced by austenitic stainless steel of low carbon and high nitrogen called ISO 5832-9. The same is already used extensively in Europe and the United States, while in Brazil it's use is more recent and smaller scale. This work investigates the behavior of dynamic recrystallization in an ISO 5832-9 steel through hot torsion tests and optical microscopy, for different conditions of temperature, strain and strain rate. It was found through the plastic flow curves of the studied material crystallizes dynamically and that the high value of its apparent activation energy for deformation can be attributed to the presence of a large amount of precipitated particles and nitrogen dissolved in the matrix. Micrographs confirmed that tests carried out at low temperatures reveal a strong retardation of dynamic recrystallization. Moreover, the presence of serrated grain boundaries and nucleation of new grains in the old deformed grain boundaries, are strong indications that the recrystallization occurred by a necklace mechanism. The behavior of the average recrystallized grain size, DDRX, with temperature resembles the behavior of the austenitic grain growth in microalloyed steels. The presence of a minimum in the behavior of DDRX with the strain rate can be attributed to a minimum strain rate required to cause the greatest amount of dynamics precipitation. / Os aços inoxidáveis austeníticos possuem um baixo valor econômico quando comparados ao titânio e suas ligas, considerados os mais resistentes à corrosão em meio biológico, e há mais de cinquenta anos são amplamente utilizados na confecção de implantes ortopédicos, em especial no serviço de saúde pública. Atualmente o aço ISO 5832-1 (ASTM F 138) é o mais utilizado na confecção de próteses ortopédicas, principalmente as temporárias. Entretanto, devido o mesmo ser suscetível à corrosão localizada quando em contato com tecido humano, ele está sendo gradativamente substituído pelo aço inoxidável austenítico de baixo teor de carbono e alto teor de nitrogênio denominado de ISO 5832-9. O mesmo já é utilizado em larga escala na Europa e nos Estados Unidos, enquanto no Brasil a sua utilização é mais recente e em menor escala. Este trabalho investiga o comportamento da recristalização dinâmica em um aço ISO 5832-9, através de ensaios de torção a quente e microscopia ótica, para diferentes condições de temperatura, deformação e taxa de deformação. Foi constatado através das curvas de escoamento plástico que o material estudado recristaliza dinamicamente e, que o alto valor da sua energia de ativação aparente para a deformação pode ser atribuído à presença de uma grande quantidade de partículas de precipitados e ao nitrogênio em solução na matriz. Micrografias confirmam que ensaios realizados a baixas temperaturas revelam um forte retardamento da recristalização dinâmica. Além disso, a presença de contornos de grão serrilhados e nucleação de novos grãos nos antigos contornos de grãos deformados, são fortes indícios de que a recristalização ocorreu por mecanismo colar. O comportamento do tamanho de grão médio recristalizado, DDRX, com a temperatura, se assemelha ao comportamento do crescimento de grão austeníticos de aços microligados. A presença de um mínimo no comportamento do DDRX com a taxa de deformação pode ser atribuído a uma taxa de deformação mínima necessária para que ocorra a maior quantidade de precipitação dinâmica.

La thèse s'inscrit dans le cadre du projet GENOME « Gestion Optimisée de l'Energie » dont l'enjeu majeur est la conception d'un avion plus électrique. L'augmentation de l'efficacité énergétique et de la compacité des systèmes électriques de ces avions entraîne de fortes sollicitations en température. Ces sollicitations sont liées à la compacité des systèmes (réduction de masse et de volume) ainsi qu'à leur localisation par rapport aux sources chaudes (réacteur d'avion par exemple). De ce fait, les matériaux magnétiques des nouveaux convertisseurs électriques doivent pouvoir fonctionner sous des conditions de hautes températures, supérieures à 200°C. Il s'agit du polycristallin FeCoV dédié à la fabrication des tôles du stator et du rotor des génératrices rapides (situées à proximité des réacteurs) et le nanocristallin FeCuNuSiB dédié à la conception des inductances et transformateurs des convertisseurs statiques. Ce manuscrit s'intéresse à l'étude du vieillissement thermique de ces deux familles de matériaux magnétiques. Ces matériaux, fournis par la société APERAM, se déclinent sous plusieurs nuances et finitions. L'étude du vieillissement consiste en l'application de plusieurs essais de vieillissement continus sous différentes températures (jusqu'à 300 °C pour les FeCoV et 240 °C pour les nanocristallins). Plusieurs grandeurs macroscopiques magnétiques, électriques et mécaniques (pour les FeCoV) sont mesurées à chaque intervalle de vieillissement. Grâce à ces mesures macroscopiques et à des mesures complémentaires effectuées à l'échelle microscopique, des analyses sont faites et des hypothèses sont proposées afin d'expliquer les mécanismes de vieillissement de ces deux familles de matériaux et dans le but de proposer des modèles phénoménologiques fiables / The thesis takes part of the project GENOME “Gestion Optimisée de l’Energie” whose major issue is the design of the more electrical aircraft. The increase in the energy efficiency and the compactness of the electrical systems of these aircrafts lead to high temperature stresses. These thermal stresses are related to the compactness of the systems (reduction of mass and volume) as well as their location with respect to the hot sources (aircraft engine for example). Thus, the magnetic materials of the new electrical converters must be able to operate under conditions of high temperatures, above 200 °C. Typically, the FeCoV polycrystalline materials are dedicated to the fabrication of the stator and rotor sheets of the fast generators (located near the aircraft engine) and the FeCuNbSiB nanocrystalline materials are dedicated to the design of inductors and transformers of the static converters.This manuscript concerns the thermal ageing study of these two magnetic material families. These materials, supplied by the company APERAM, are available in several shades. The ageing study consists on applying several continuous ageing treatments at different temperatures (up to 300 °C for FeCoV and 240 °C for FeCuNbSiB). At each ageing step, several macroscopic properties namely: magnetic, electrical and mechanical (for the FeCoV materials) properties are measured. Using these macroscopic properties and complementary measurements carried out on a microscopic scale, analyses are made and hypotheses are proposed in order to explain the ageing mechanisms of these magnetic material families. The understanding of the magnetic ageing mechanisms is necessary towards establishing of phenomenological ageing models