O crescente interesse em novos métodos para a geração de energia limpa e sustentável contribui para o desenvolvimento de materiais avançados destinados a aplicações estruturais em reatores de fusão nuclear. Os principais resultados obtidos quanto à caracterização microestrutural de dois aços endurecidos por dispersão de óxidos, candidatos potenciais a este tipo de aplicação, são apresentados. Um dos aços contém 9%Cr e o outro 13%Cr (% em massa). Os aços foram laminados até 80% de redução e recozidos até temperaturas próximas a 0,9 Tf, onde Tf é o ponto de fusão. A cinética de amolecimento foi acompanhada por meio de medidas de dureza Vickers em função da temperatura de recozimento e do tempo. Amostras representativas foram caracterizadas via microscopia eletrônica de transmissão e de varredura e por difração de elétrons retroespalhados. As temperaturas das transformações de fases foram determinadas por técnicas como dilatometria e análise térmica diferencial. Curvas de magnetização em função do campo magnético aplicado até 15 kOe foram obtidas para o aço com 9%Cr. Medidas de difração de raios X para determinar a densidade de discordâncias também foram realizadas em amostras representativas do aço com 9%Cr. Os resultados até o momento mostram que o engrossamento microestrutural destes aços só se torna significativo quando o recozimento é feito em temperaturas acima de 0,8 Tf. Em temperaturas mais baixas, ainda no campo ferrítico, a recuperação prevalece e a fração recristalizada é baixa. A resistência destes materiais à recristalização se deve à presença das partículas de óxido de ítrio dispersas na matriz que dificultam a movimentação e o rearranjo das discordâncias e contornos durante sua migração. Por outro lado, partículas grosseiras como as dos carbonetos M23C6 estimulam a recristalização atuando como sítios preferenciais para a nucleação. O recozimento em temperaturas elevadas no campo austenítico resultou no aumento considerável na dureza Vickers e na densidade de discordâncias para o aço com 9%Cr devido à transformação martensítica. No aço com 13%Cr os resultados também sugerem a ocorrência da transformação martensítica. / There is an increasing interest in the development of new, sustainable, clean and safe sources of energy. In view of these requirements, the development of advanced materials for future nuclear fusion reactors becomes essential. This work investigates the annealing behavior and the microstructural stability of two oxide dispersion strengthened steels with 9%Cr and 13%Cr ODS steels. These materials are potential candidates for structural applications in future fusion reactors. The two ODS steels were cold rolled to 80% thickness reduction. Samples were annealed in vacuum at temperatures of about 0.9 Tm, where Tm is the melting point. The microstructural characterization was performed by Vickers hardness testing, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) performed by a highresolution SEM. Important temperatures related to the phase transformations were determined with aid of dilatometry and differential thermal analysis (DTA). Magnetization curves as a function of applied magnetic fields up to 15 kOe were obtained for 9%Cr ODSEurofer. X-ray diffraction experiments were also performed on 9%Cr steel to evaluate the dislocation density in several metallurgical conditions. Results show that microstructural coarsening becomes significant when annealing is performed above 0.8 Tm. Below 800°C, static recovery is the main softening mechanism of these steels and the volume fraction of recrystallized grains is quite low. The resistance of these steels to recrystallization can be explained by the strong interaction between boundaries and mobile dislocations with fine particles of Y-based oxides. Contrastingly, coarse M23C6 particles act as preferential nucleation sites through the well-known particle stimulated nucleation (PSN) mechanism. Samples annealed above 800oC (austenitic phase field) display larger dislocation densities in the 9%Cr ODS steel. Results concerning to 13%Cr steel suggest the occurrence of martensitic transformation.

Amostras de nióbio de alta pureza na forma de monocristais, bicristais e policristais foram retiradas de seções longitudinais de lingotes fundidos por feixe eletrônico. As amostras foram deformadas via extrusão em canal angular (ECAE - Equal Channel Angular Extrusion) em temperatura ambiente até 8 passes, utilizando a rota Bc numa matriz com ângulo de intersecção entre os canais de  = 90º. As amostras foram caracterizadas em termos da evolução microestrutural e da textura de deformação. A caracterização microestrutural foi realizada com o auxílio de microscopias ótica, eletrônica de varredura e eletrônica de transmissão, além de medidas de difração de elétrons retroespalhados (EBSD) para determinação da microtextura e da mesotextura. Medidas de microdureza Vickers foram realizadas para acompanhar o encruamento e o amolecimento das amostras. Um outro monocristal de nióbio foi deformado em 1 passe via ensaio interrompido, utilizando uma matriz com ângulo  = 120º, a fim de estudar a evolução da textura durante a passagem pelo canal de ECAE. A textura foi determinada por meio de difração de raios X e comparada com os dados da literatura para materiais deformados via ECAE com estrutura CCC e também com as texturas simuladas pelo modelo VPSC (visco-plastic self-consistent). No estudo comparativo numa escala maior (monocristal e policristal), verificou-se que houve um refinamento microestrutural significativo após 8 passes. O espaçamento médio entre os contornos de alto ângulo medido perpendicular à direção de extrusão foi próximo nos dois casos (500 nm), maior que o observado para o monocristal deformado numa escala menor (440 nm). Os resultados mostram ainda que os grãos do policristal deformado são mais equiaxiais que os do monocristal. Amostras foram recozidas isotermicamente para avaliar o comportamento frente ao engrossamento microestrutural. Os resultados mostram que o engrossamento torna-se apreciável, em geral, a partir de 500oC com a ocorrência de recristalização descontínua. Acima de 700oC, o crescimento normal de grão passa a ser o principal mecanismo de engrossamento microestrutural. Efeitos de orientação importantes foram observados no bicristal nos estados encruado e recozido. / High-purity niobium single crystals, bicrystals and polycrystals were cut out from longitudinal sections of ingots processed by electron beam melting. Samples were deformed by Equal Angular Channel Extrusion (ECAE) at room temperature up to 8 passes, using the route Bc with a die angle  = 90o. Samples were characterized in terms of their microstructural evolution and deformation textures. Microstructural characterization was performed using optical, scanning electron, and transmission electron microscopies, as well as electron-backscatter diffraction measurements (EBSD) to determine both microtexture and mesotexture. Vickers microhardness testing was performed to follow hardening and softening behaviors in the samples. Another single crystal was deformed by 1 pass in an interrupted ECAE experiment using a die angle  = 120o to follow the changes in texture through the extrusion channel. Texture was determined by X ray diffraction and compared with those reported in the literature for deformed bcc materials and also with those predicted using the viscoplastic self-consistent model (VPSC). A comparative study in a larger scale (single and polycrystals) was also performed. It was observed that there is a significant refinement of the microstructure after 8 passes. The average spacing between high angle boundaries perpendicular to extrusion direction was close in the two cases (500 nm), larger than observed in the single crystal deformed in a smaller scale (440 nm). Results also show that ultrafine grains of the deformed polycrystal are more equiaxial compared to those found in the deformed single crystal. Samples were annealed to evaluate their behavior regarding microstructural coarsening. Results show that coarsening becomes noticeable at temperatures higher than 500oC by means of discontinuous recrystallization. Above 700oC, normal grain growth becomes the main microstructure coarsening mechanism. Important orientation effects were observed in the bicrystal in both deformed and annealed states.

As ligas de magnésio atraíram a atenção novamente nos últimos anos por causa de suas propriedades de baixa densidade, resistência à tração e rigidez específica. Por outro lado, a maior limitação para o uso de ligas trabalhadas é a baixa conformabilidade em temperatura ambiente devido à estrutura hexagonal compacta (HCP) das ligas. O presente trabalho de pesquisa teve como objetivo estudar o encruamento, recristalização e crescimento de grãos durante a laminação de liga magnésio AZ31B em alta e baixa temperatura, analisando a evolução da microestrutura, da textura e a variação das propriedades sensíveis à microestrutura. A liga AZ31B é sensível à taxa de deformação em alta temperatura, entretanto, a anisotropia é negativamente afetada na laminação a frio, portanto, apresenta uma melhor laminação na faixa de temperaturas de 200 a 300ºC, devido ao refinamento de grãos, causado pela recuperação e recristalização dinâmica. O estudo foi realizado em amostras de uma chapa de liga de magnésio AZ31B recristalizada (2 mm de espessura). Amostras foram deformadas por laminação em temperaturas diferentes (25, 100, 200, 250 e 300ºC) e com diferentes taxas de deformação. A caracterização microestrutural foi realizada com auxílio de várias técnicas complementares de análise microestrutural, tais como microscopia óptica, microscopia eletrônica de varredura, análise de raios-X por dispersão de energia, difração de raios X e microdureza Vickers. A deformabilidade e a ocorrência de recristalização dinâmica e crescimento de grãos mostraram forte dependência com as condições de laminação. Na laminação a frio, o refinamento de grão foi mais efetivo com baixas taxas de deformação (1,6 s-1) do que na laminação a quente. Entretanto, a intensa textura basal foi enfraquecida em temperaturas próximas a 300ºC e com taxas de deformação próximas a 3,5 s-1. A ductilidade das ligas pode ser melhorada em altas temperaturas de deformação, pelo refinamento dos grãos que produz a diminuição da fração volumétrica das regiões macladas e pelo aumento do número de sistemas de deslizamento, além do enfraquecimento da intensa textura basal, característica das ligas de magnésio. / Magnesium alloys have attracted the attention again in recent years because of their low density, their specific tensile strength and rigidity. However, the greatest limitation for the usage of wrought magnesium alloys is their poor formability at room temperature due to the hexagonal closed packed (HCP) crystal structure. The present research focused on study the work-hardening, recrystallization and grain growth during rolling of AZ31B magnesium alloy at low and high rolling temperature. It was made through the analysis of microstructure and texture evolution and variations of microstructure-sensitive properties. The AZ31 magnesium alloy is sensitive to strain rate at high temperature, meanwhile, the anisotropy is adversely impacted in cold rolling sheets. Thus, AZ31B magnesium alloy exhibits better workability in 200-300°C temperature range due to the grain refinement caused by dynamic recovery and dynamic recrystallization. This research was carried out on samples of recrystallized sheet (2 mm in thickness). Samples were deformed by rolling at different temperatures (25, 100, 200, 250 and 300°C), using different strain rates. Microstructural characterization was done by using several complementary techniques of microstructural analysis, such as optical microscopy, scanning electron microscopy, X-ray analysis by energy dispersive, X-ray diffraction and Vickers microhardness tests. A competition between dynamic recrystallization and grain growth depends on rolling conditions. Low strain rate (1,6 s-1) at cold rolling improved more effective in refining grains than warm rolling. Meanwhile, the intense basal texture was weakened at 300°C with a high strain rate of 3,5 s-1. The ductility of magnesium alloys can be greatly improved at high temperature, with a fine grain structure that causes the reduced volume fraction of twins, and an increase the number of slip systems, weakening the intense basal texture, rather characteristic for magnesium alloys.

Chapas laminadas a quente com 6 mm de espessura dos aços AISI 304L e 316L apresentaram na condição inicial uma microestrutura composta por grãos recristalizados equiaxiais de austenita e ilhas de ferrita δ, em maior quantidade no centro da chapa. A austenita apresentou textura cristalográfica fraca, com um gradiente de textura ao longo da espessura. Os tratamentos térmicos de solubilização causaram a eliminação da ferrita, mas não causaram modificação substancial na textura. Os fenômenos de encruamento, recuperação e recristalização foram então estudados após solubilização, seguida de deformação por laminação em diferentes temperaturas e posterior recozimento das amostras deformadas. O endurecimento por deformação e a porcentagem de martensita α’ formada mostraram forte dependência com a composição química da austenita e com a temperatura de deformação. A textura de deformação encontrada nos aços inoxidáveis austeníticos 304L e 316L é característica dos materiais CFC com baixa e média energia de empilhamento laminados a frio. A temperatura de reversão da martensita α’ foi próxima de 550°C, praticamente não depende da quantidade presente e é praticamente idêntica nos dois aços. O aço 316L apresentou maior resistência à recristalização, pois tem maior EDE e apresenta menor endurecimento por deformação em relação ao 304L. A temperatura de recristalização situouse aproximadamente 150°C acima da temperatura de reversão da martensita α’. A temperatura de laminação não influenciou significativamente a temperatura de recristalização. A textura de recristalização nos dois aços continuou sendo semelhante à textura de deformação. As propriedades mecânicas de tração dos dois aços mostraram-se muito sensíveis à temperatura do ensaio. Tratamentos mecânicos e térmicos adequados produziram combinações interessantes de propriedades mecânicas nos dois aços, tais como limite de escoamento por volta de 1000 MPa com alongamento da ordem de 10%. Os resultados do presente trabalho sugerem que para se obter nos aços inoxidáveis austeníticos combinações atrativas de alta resistência mecânica com ductilidade razoável, por meio de tratamentos mecanotérmicos ou termomecânicos, duas diretrizes devem ser observadas: i) durante a deformação grandes quantidades de martensita devem ser produzidas e as principais variáveis neste aspecto são a EDE do aço e a quantidade e a temperatura de deformação; ii) durante o recozimento do material encruado deve ocorrer reversão da martensita, mas a recristalização completa deve ser evitada, por meio do controle rigoroso da temperatura e do tempo de recozimento, obtendo-se uma microestrutura muito fina de grãos e sub-grãos. A possibilidade de tratamentos sucessivos de deformação/recozimento é promissora e deve ser explorada em trabalhos futuros. A caracterização microestrutural foi realizada com auxílio de várias técnicas complementares de análise microestrutural, tais como microscopia óptica, microscopia eletrônica de varredura (MEV), microscopia eletrônica de transmissão (MET), medidas magnéticas, difração de raios X (análise de fases e determinação de textura) e microdureza Vickers. A caracterização mecânica envolveu a realização de ensaio de tração em várias temperaturas, com a determinação de limite de escoamento, limite de resistência, alongamento total e coeficiente de encruamento n. / Hot rolled AISI 304L and 316L austenitic stainless steel sheets, 6mm thick, presented recrystallized equiaxial grains with austenite and islands of delta ferrite, in larger quantities mainly in the center of both steel sheets. The austenite had a weak texture, with a gradient through the thickness. The solution annealing eliminated delta ferrite, however it did not change the texture. Phenomena such as work hardening and strain induced α’ martensite formation showed strong dependency on the chemistry composition and rolling temperature. The rolling texture observed in AISI 304L and 316L austenitic stainless steels is characteristic of FCC materials with low and medium stacking fault energy (SFE), after cold rolling. The α’ reversion temperature was around 550°C for both steels and was independent of the volume fraction of α’ martensite. The AISI 316L showed a strong recrystallization resistance as it has higher SFE and smaller work hardening than the AISI 304L. The recrystallization start temperature is approximately 150°C higher than the α’ reversion temperature. The rolling temperature did not influence the recrystallization temperature. Recrystallization texture for both steels remained similar to the rolling texture. Proper thermal and mechanical treatments provided interesting combinations of mechanical properties for both steels, such as yield strength around 1000 MPa with 10% elongation. These results suggest that the obtained austenitic stainless steels provide attractive combinations not only with high mechanical resistance but also with reasonable toughness and ductility. Through thermo-mechanical treatments, two point must be stressed: i) during the deformation great quantities of α’ martensite are being produced due to the SFE of the steel and the degree and the temperature of deformation; ii) during the annealing treatment of the work hardened material the α’martensite reverts to austenite, but complete recrystallization must be avoided, thus strict control of temperature and annealing time must be ensured to obtain a refined microstructure (of grains and subgrains). The possibilities of employing successive deformation / annealing treatments is promising and should be explored in future research. Several microstructural characterization techniques have been employed: optical microscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), magnetic measurements, X-ray diffraction to analyze phases and textures, and Vickers microhardness tests. Mechanical characterization involved tensile testing at different temperatures, with determination of yield strength, tensile strength, total elongation and strain hardening coefficient n.

Du fait de leurs très bonnes propriétés mécaniques jusqu’à des températures approchant les 700°C, les superalliages base nickel polycristallins sont utilisés pour la fabrication de disques de turbine (ou compresseur) de moteur d’avion. La voie conventionnelle pour l’élaboration et la mise en forme de ces alliages est la voie dite «coulé-forgé». Ainsi, une première série de forgeages, appelée conversion, est appliquée au lingot coulé afin d’homogénéiser et de raffiner la microstructure. Elle aboutit à un demi-produit appelé billette qui est ensuite forgée/matricée à son tour pour obtenir l’ébauche de la pièce finale. Pour les superalliages γ-γʹ avec de hautes teneurs en éléments d’alliage, il est courant que l’étape de conversion ne soit pas suffisamment efficace pour complètement homogénéiser la microstructure. C’est le cas pour l’alliage AD730TM récemment mis au point par la société Aubert&Duval, dont les billettes présentent des zones de grains équiaxes recristallisés et des plages restaurées caractéristiques. L’objectif de cette thèse est de comprendre comment les hétérogénéités de microstructure peuvent se résorber pendant les dernières étapes de forgeage menant à la microstructure finale. Après avoir caractérisé les hétérogénéités de microstructure présentes dans les billettes d’alliage AD730TM, des essais thermomécaniques simulant un procédé de forgeage ont été appliqués à la billette afin de suivre l’évolution des différentes microstructures locales. Les mécanismes d’évolutions statiques (pendant les traitements thermiques) et dynamiques (pendant la déformation) des zones équiaxes et des plages restaurées ont été caractérisés par microscopie électronique à balayage, EBSD et EDS. Une attention toute particulière est portée à l’influence des précipités γʹ sur ces évolutions. Notamment, une interaction front de recristallisation-précipités jusque-là très peu reportée dans la littérature et générant des précipités γʹ en quasi relation de macle ou de quasi même orientation que la matrice a été étudiée en détail. / Due to their excellent mechanical properties at temperatures up to 700°C, polycrystalline nickel-based superalloys are widely used in aero-engine turbine (or compressor) disk manufacturing. These alloys are usually processed following the conventional “cast-and-wrought” route. During this route, the cast ingot goes through a first series of forging operations which is named “conversion”. The goals of the conversion are to homogenize and refine the microstructure. It leads to a semi-finished product called billet. Then, the billet is forged again to obtain a draft of the final part. Yet, for the γ-γʹ nickel-based superalloys with high contents in alloying elements, it is common that the conversion process does not succeed in fully homogenizing the microstructure. Such is the case of the alloy AD730TM which has been recently developed by the Aubert&Duval Company. Indeed, AD730TM billets show both recrystallized equiaxed areas and characteristic recovered areas. The objective of the current PhD thesis is to understand how such microstructural heterogeneities can disappear during the last forging operations which lead to the final microstructure. First, the microstructural heterogeneities found in AD730TM billets have been characterized. Then, thermomechanical tests which aimed at simulating a forging process have been performed on billet samples in order to follow the evolutions of each local microstructure. The static (during thermal treatments) and dynamic (during deformation) evolutions of both equiaxed and recovered areas have been characterized using scanning electron microscopy, EBSD and EDS. A special attention has been paid to the influence of the γʹ precipitates on those evolutions. In particular, a specific interaction between a recrystallization front and γʹ precipitates have been studied in detail. This interaction, which has been weakly reported in literature so far, produces γʹ precipitates with either an imperfect twin orientation relationship to the matrix or an imperfect cube-cube orientation relationship to the matrix.

O crescente interesse em novos métodos para a geração de energia limpa e sustentável contribui para o desenvolvimento de materiais avançados destinados a aplicações estruturais em reatores de fusão nuclear. Os principais resultados obtidos quanto à caracterização microestrutural de dois aços endurecidos por dispersão de óxidos, candidatos potenciais a este tipo de aplicação, são apresentados. Um dos aços contém 9%Cr e o outro 13%Cr (% em massa). Os aços foram laminados até 80% de redução e recozidos até temperaturas próximas a 0,9 Tf, onde Tf é o ponto de fusão. A cinética de amolecimento foi acompanhada por meio de medidas de dureza Vickers em função da temperatura de recozimento e do tempo. Amostras representativas foram caracterizadas via microscopia eletrônica de transmissão e de varredura e por difração de elétrons retroespalhados. As temperaturas das transformações de fases foram determinadas por técnicas como dilatometria e análise térmica diferencial. Curvas de magnetização em função do campo magnético aplicado até 15 kOe foram obtidas para o aço com 9%Cr. Medidas de difração de raios X para determinar a densidade de discordâncias também foram realizadas em amostras representativas do aço com 9%Cr. Os resultados até o momento mostram que o engrossamento microestrutural destes aços só se torna significativo quando o recozimento é feito em temperaturas acima de 0,8 Tf. Em temperaturas mais baixas, ainda no campo ferrítico, a recuperação prevalece e a fração recristalizada é baixa. A resistência destes materiais à recristalização se deve à presença das partículas de óxido de ítrio dispersas na matriz que dificultam a movimentação e o rearranjo das discordâncias e contornos durante sua migração. Por outro lado, partículas grosseiras como as dos carbonetos M23C6 estimulam a recristalização atuando como sítios preferenciais para a nucleação. O recozimento em temperaturas elevadas no campo austenítico resultou no aumento considerável na dureza Vickers e na densidade de discordâncias para o aço com 9%Cr devido à transformação martensítica. No aço com 13%Cr os resultados também sugerem a ocorrência da transformação martensítica. / There is an increasing interest in the development of new, sustainable, clean and safe sources of energy. In view of these requirements, the development of advanced materials for future nuclear fusion reactors becomes essential. This work investigates the annealing behavior and the microstructural stability of two oxide dispersion strengthened steels with 9%Cr and 13%Cr ODS steels. These materials are potential candidates for structural applications in future fusion reactors. The two ODS steels were cold rolled to 80% thickness reduction. Samples were annealed in vacuum at temperatures of about 0.9 Tm, where Tm is the melting point. The microstructural characterization was performed by Vickers hardness testing, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) performed by a highresolution SEM. Important temperatures related to the phase transformations were determined with aid of dilatometry and differential thermal analysis (DTA). Magnetization curves as a function of applied magnetic fields up to 15 kOe were obtained for 9%Cr ODSEurofer. X-ray diffraction experiments were also performed on 9%Cr steel to evaluate the dislocation density in several metallurgical conditions. Results show that microstructural coarsening becomes significant when annealing is performed above 0.8 Tm. Below 800°C, static recovery is the main softening mechanism of these steels and the volume fraction of recrystallized grains is quite low. The resistance of these steels to recrystallization can be explained by the strong interaction between boundaries and mobile dislocations with fine particles of Y-based oxides. Contrastingly, coarse M23C6 particles act as preferential nucleation sites through the well-known particle stimulated nucleation (PSN) mechanism. Samples annealed above 800oC (austenitic phase field) display larger dislocation densities in the 9%Cr ODS steel. Results concerning to 13%Cr steel suggest the occurrence of martensitic transformation.

O objetivo deste trabalho é realizar um estudo comparativo da recristalização de dois aços rápidos, AISI M2 (Werkstoffnummer 1.3343) e ABC III (Werkstoffnummer 1.3333), após o encruamento resultante do processo de laminação a frio de chapas planas utilizadas para a confecção de serras fitas. Estudar a recristalização estática nesta classe de aços é relevante, pois eles freqüentemente são laminados a frio e recozidos na etapa final de processamento, antes da confecção da peça ou componente. Inicialmente, foi realizada a caracterização das amostras no estado como recebido, ou seja \'\'laminado a quente\'\'. A caracterização envolveu análise química, ensaios mecânicos, microscopia óptica, microscopia eletrônica de varredura, medidas de dureza e dilatometria. Em seguida, as amostras sofreram deformação a frio da ordem de até 50% de redução em espessura para determinação das curvas de endurecimento por deformação. Amostras com 25% de redução foram recozidas entre 100ºC e 750ºC, durante 1 hora e os resultados de dureza foram utilizadas para determinar as curvas isócronas de amolecimento. Amostras com 25% redução foram recozidas entre 600ºC e 750ºC, entre 15 e 480 minutos para cada uma das temperaturas, para determinação curvas isotérmicas de amolecimento. Resultados da análise microestrutural mostraram que o aço rápido AISI M2 apresenta uma distribuição mais homogênea de carbonetos. Esses carbonetos são mais finos em relação aos do aço ABC III, que apresenta uma distribuição mais heterogênea. Os dois aços apresentaram curvas muito similares de endurecimento por deformação. Após recozimento das amostras encruadas, foi verificado que o aço AISI M2 apresenta recuperação e recristalização levemente mais rápidas quando comparado com o ABC III. Ainda na etapa de recuperação e antes da recristalização, notou-se nos dois aços um pequeno aumento de dureza, principalmente entre 30 e 60 minutos de recozimento, na faixa de 650 ºC e 700ºC. Utilizando-se análises por difração de elétrons retroespalhados (microtextura e mesotextura) observou-se que o aço ABC III apresenta maior resistência para a recristalização se completar que o aço AISI M2. / This work aims at the comparative study of the recrystallization of two high-speed steels, namely AISI M2 (Werkstoffnummer 1.3343) and ABC III (Werkstoffnummer 1.3333), hardened by cold rolling of sheets employed in the production of band saws. Studying static recrystallization in this class of steels is relevant, since frequently they are cold rolled and annealed in their final processing stage, prior to the actual work piece manufacturing. Initially, samples have been characterized in the as-received condition, i.e. hot rolled. Characterization involved chemical analysis, tensile testing, optical metallography, scanning electron microscopy, hardness measurements and dilatometry. Following, samples have been cold worked with a 50% thickness reduction in order to evaluate the cold work hardening curves. Samples with 25% reduction have been annealed at temperatures in the 100oC to 750oC range, for one hour and hardness results have been used to determine the isochronous softening curves. Samples with 25% reduction have been annealed between 600 oC and 750oC for 15 to 480 minutes, for each one of the temperatures, to determine the isothermal softening curves. The microstructural analysis has shown that the AISI M2 steel presents a homogeneous carbide distribution. These carbides were fine when compared to those of the ABCIII steel that presented a heterogeneous distribution. Both steels presented similar work-hardening curves. After annealing the cold worked samples, it has been observed that the AISI M2 steel presented a slightly faster recovery and recrystallization than the ABCIII steel. Still in the recovery stage, prior to recrystallization, both steels showed a small hardness increase, mainly on annealing during 30 to 60 minutes in the 650oC to 700oC temperature range. Using electron backscattered diffraction analysis (microtexture and mesotexture) it has been observed that the ABCIII steel presented higher resistance to complete recrystallization than the AISI M2 steel.

Les revêtements GalvAnnealed (GA), constitués de phases Fe-Zn, sont utilisés pour protéger les aciers contre la corrosion. Ces revêtements sont réalisés en trois étapes principales: le recuit de recristallisation, l'immersion dans un bain de zinc contennant de 0,11 à 0,13% poids d'aluminium et le traitement thermique du revêtement de zinc. Lors de la première étape, l'oxydation sélective des éléments d'alliage se produit à la surface de l'acier. Dans le cas des aciers chargés en éléments d'alliage (TRansformation Induced-Plasticity), les oxydes sélectifs sont connus pour créer des problèmes de réactivité entre l'acier et le zinc liquide. L'état d'oxydation sélective dépend du point de rosée (PR) de l'atmosphère de recuit. La formation du revêtement Fe-Zn implique des réactions complexes: la formation de la couche d'inhibition, sa rupture, la consommation du zinc et l'enrichissement en fer. Dans ce travail, l'effet du PR de l'atmosphère de recuit sur l'oxydation sélective et la formation du revêtement sur un acier TRIP MnAl a été étudié. Il a été montré que l'atmosphère de recuit influe principalement sur la morphologie (films ou nodules) et la localisation des oxydes par rapport à la surface de l'acier (externe / interne). Les résultats expérimentaux sont en accord avec les calculs thermodynamiques. Indépendamment du PR, la couche d'inhibition est constituée de deux phases, δ (FeZn7) et Fe2Al5Znx. Les oxydes externes formés lors du recuit sont incrustés dans ces phases. La couche d'inhibition ne bloque les réactions Fe-Zn que temporairement. Lors du traitement galvannealing, la rupture de la couche d'inhibition se produit par deux mécanismes réactionnels qui dépendent de l'état d'oxydation sélective. Globalement, les films d'oxyde (bas PR) incrustés dans la couche d'inhibition ont un effet retardateur sur les réactions Fe-Zn par rapport aux oxydes nodulaires (haut DP). / GalvAnnealed (GA) coatings, composed of Fe-Zn phases, are used to protect steels against corrosion. These coatings are produced in three main steps, namely recrystallization annealing, immersion in a zinc bath with 0.11 to 0.13 wt.% aluminum and heat treatment of the zinc coating. In the first step, the selective oxidation of the alloying elements occurs at the steel surface. In the case of high alloyed steels (e.g. TRansformation-Induced Plasticity), the selective oxides are known to be detrimental for the reactions between the steel substrate and liquid zinc. The selective oxidation state depends on the dew point (DP) of the annealing atmosphere. The coating formation involves complex reactions: the inhibition layer formation, its breakdown, the liquid zinc consumption and the iron enrichment. In this work, the effect of the DPof the annealing atmosphere on the selective oxidation and the coating formation on a TRIP MnAl steel was investigated. It was shown that the annealing atmosphere mainly affects the morphology (films or nodules) and the location of the selective oxides with respect to the steel surface (external / internal). The experimental results are in line with the thermodynamic calculations. The inhibition layer is composed of two phases, δ (FeZn7) and Fe2Al5Znx, irrespective of the DP. In addition, it contains the external oxides formed during the first step. The inhibition layer hinders the Fe-Zn reactions only temporarily. Depending on the selective oxidation state, during galvannealing treatment the inhibition layer rupture occurs by two different reaction mechanisms. Globally, the oxide films (low DP) embedded in the inhibition layer, delay the Fe-Zn reactions compared to nodular oxides (high DP).

La glace est un matériau de structure cristallographique hexagonale ayant une anisotropie plastique très importante. La déformation est principalement accommodée par le glissement des dislocations dans le plan basal. Cette forte anisotropie du monocristal de glace conduit lors de la déformation d’un polycristal, à de fortes hétérogénéités de déformation et de contrainte. Lors de la déformation à haute température, les mécanismes de recristallisation dynamique permettent, par le développement d’une nouvelle microstructure et d’une nouvelle texture, d’augmenter la ductilité du matériau. L’objet de cette étude est de mieux caractériser les mécanismes de recristallisation et leurs liens avec les hétérogénéités de déformation afin de mieux comprendre le développement des nouvelles microstrutures et textures ainsi que leurs impacts sur le comportement du matériaux.Ce travail est basé sur des essais de type fluage dans les conditions où la recristallisation dynamique est importante (T > 0.95T f et 0.5 < σ < 1 M P a). Deux types de polycristaux sont étudiés : la glace granulaire, considérée comme un volume élémentaire représentatif, qui permet d’appréhender d’un point de vue statistique l’impact de la recristallisation sur le développement des microstructures et des textures ; et la glace colonnaire, qui permet d’étudier les différents mécanismes de germination et leurs liens avec les hétérogénéités de déformation à l’échelle inter et intra-granulaire. Les outils de caractérisation utilisés sont la mesure in situ de l’évolution du champ de déformation par corrélation d’images numériques et la caractérisation des microstructures et des textures pré- et post- déformation par mesure optique et Electron BackScatter Diffraction (EBSD).Étant donné les fortes hétérogénéités de déformation, les mécanismes de recristallisation dynamique continue et discontinue sont actifs au cours de la déformation. La formation de sous-joints de grains, la germination par gonflement (bulging), où la migration de joints de grains ont été mises en évidence. Des germes fortement désorientés par rapport aux grains parents ont également été observés. Ces observations impliquent un mécanisme de germi- nation différent de ceux mentionnés ci-dessus. De plus, les dislocations géométriquement nécessaires composants les sous-joints de grains ont été caractérisées à l’aide du tenseur de Nye extrait des mesures EBSD. Cela a permis d’observer des sous-structures de dislocations composées de dislocations c. Ces dislocations c étaient jusqu’alors très rarement observées et seulement dans des conditions très spécifiques.Une forte corrélation entre les hétérogénéités de déformation et les mécanismes de recristallisation a été mise en évidence grâce aux mesures de champs de déformation. Les mécanismes de recristallisation se concentrent dans les zones où la déformation est importante et ont tendance à réduire les hétérogénéités de déformation. De plus, ces bandes de déformation, où la recristallisation est active, sont orientées à environ ±45° et ont une dimension supérieure à la taille moyenne des grains, ce qui montre une organisation des hétérogénéités de déformation et de contrainte à grande distance.Un modèle théorique pouvant contraindre l’orientation des germes crées par la germination spontanée est proposé. Ce modèle, basé sur la relaxation de l’énergie élastique, du fait de l’anisotropie élastique du mono-cristal de glace, permettrait de favoriser les cristaux dont l’axe c est aligné avec la direction de la contrainte principale locale. Cette étude a été complétée par des expériences numériques, basées sur un modèle à champ complet et une loi de plasticité cristalline élasto-viscoplastique qui permet de reproduire les hétérogénéités de déformation et de contrainte. Ces expériences numériques ont montré que ce mécanisme de germination orienté pourrait permettre d’expliquer le développement des textures de recristallisation. / Ice is an hexagonal material in which deformation mainly occurs by dislocation glide along the basal plane conferring a strong viscoplastic anisotropy to the single crystal. Hence, during polycrystalline ice deformation the incompatibility between grains lead to highly heterogeneous strain. During ice creep at high temperature, dynamic recrystallisation occurs, leading to the development of a new microstructure and strong recrystallisation textures.These new microstructure and texture increase the ductility of the material. The aims of this study is to investigate dynamic recrystallisation mechanisms and their links with strain heterogeneities to better understand the development of these microstructure and texture.Creep experiments are carried out in conditions where dynamic recrystallisation is important (T > 0.95T f and 0.5 < σ < 1 M P a). Two kinds of polycrystalline samples are used: granular ice, which can be considered as a representative elementary volume and enable to understand the global impact of dynamic recrystallisation mechanisms on texture and microstructure; and columnar ice which enable to better constrain the dynamic recrystallisation mechanism such as nucleation and their link with the strain heterogeneities down to the intra and inter-granular scales. Strain field evolution is measured in situ using digital images correlation and pre- and post- deformation microstructures and textures are measured using optical imaging and Electron BackScatter Diffraction (EBSD).Due to the strong strain heterogeneities, both continuous and discontinuous recrystallisation mechanisms occured. Sub-grain boundary formation, nucleation by bulging and grain boundary migration are mechanisms very active during dynamic recrystallisation in ice. On top of that, we also observed new grains with orientations highly disoriented compared to the neighbouring grains. This observation implies a nucleation mechanism different compare to the one mentioned above. Using Nye theory on EBSD measurements constrains the geometrically necessary dislocations of the sub-grain boundaries. Tilt sub-grain boundaries made of non-basal c dislocations have been observed. Only few observations of c dislocations existed so far, all of them made in very specific conditions.A strong correlation between recrystallisation mechanisms and strain field heterogeneities have been observed. Recrystallisation mechanisms lead to a decrease and spread of strain heterogeneities. The strain localise into bands of deformation oriented at around ±45° from the compression axis and with a typical length higher than the mean grain size. These bands of high deformation localise most of the dynamic recrystallisation mechanisms. This observation shows that the long range interaction of the strain and stress heterogeneities.We propose a new model which could be able to constrain the nucleus orientation for spontaneous nucleation. This model, based on the elastic energy relaxation during nucleation tanks to the elastic anisotropy of ice single crystal, should constrain the c axis to be aligned with the locale principal stress direction. To investigate the impact of such oriented nucleation mechanism on the texture development, a numerical experiment has been proposed using full field simulation with an elasto-viscoplastic law able to simulate the strain and stress fields heterogeneities. These numerical experiments show that the oriented nucleation mechanism might be able to explain the development of recrystallisation texture.

Elektron 43 (WE43C) is a modern magnesium rare earth alloy (Mg-RE) with potential light-weighting applications in wrought civil aerospace components. Rare earth elements are known to improve mechanical properties and weaken texture of wrought Mg-RE alloys, but for Elektron 43 the parameters of thermomechanical processing (TMP) that produce optimum microstructure development are not well understood. A large data-set of Elektron 43 flow stress data was collected in an extensive range of hot compression tests at typical TMP temperatures (350-500°C) and strain rates (0.001-100\s). Friction parameters were determined in a ring compression study. Material data was corrected for friction, strain rate and temperature variations. Parameters were fit for a sinh constitutive equation. The corrected material data and used to develop an initial finite element model in the commercial software package QForm. Further work to calibrate the heat transfer parameters is required. The effect of two extrusion parameters (temperature and ram speed) on microstructure and mechanical properties was explored. Extrusion of 60 mm diameter Elektron 43 billets to 20 mm diameter rods (ER=9.92) was conducted at three temperatures (380°C, 420°C and 460°C) and a range of ram speeds (~0.1-15 mm/s). An approximate extrusion limit diagram was formed from empirical relations for extrusion load and hot cracking. Extruded microstructures were bi-modal consisting of dynamically recrystallised (DRX) grains and elongated deformed grains. The typical `prismatic' deformation texture (extrusion direction ED||) was weakened by increasing DRX fraction, concomitant of increased ram speed and temperature. Small DRX grains at low temperature/ram speed had very weak preferences for the 'RE component' with ED||. Increase in ram speed/temperature resulted in a rarely reported 'c-axis' RX texture (ED||) becoming increasingly prominent. This texture dominated at high temperatures and speeds. C-axis grains were larger than those of the RE and prismatic orientations, with the relative difference increasing with DRX fraction. Thus a growth advantage of c-axis grains has been demonstrated: it is postulated these grain boundaries have higher boundary mobility (considering the 90° misoreintation with the deformation texture) and driving pressure (as they are not well oriented for basal slip). Suppression of all RE texture modification followed extrusion at 460°C, 0.16 mm/s. The RX texture was typical of non-RE Mg alloys: ED||. It is argued that at this condition solute segregation is suppressed. Extrusions showed low ambient yield asymmetry. The highest measured yield stresses were correlated with partial RX. These two observations can be explained by a balance of texture, Hall-Petch strengthening and work hardening. One unexplained observation of note is that the maximum observed yields generally correspond to a reversed yield asymmetry.