Aluminium alloys have the possibility to be infinitely recycled. By only generating 5% of the emissions compared to primary aluminium, great CO2 savings can be made. One of the issues in manufacturing components entirely from post-consumer scrap is the presence of trace elements and impurities. Such elements can be Fe, Cu, Cr, P and Pb. In sheet metal manufacturing, these elements can also react with process agents such as Ti, B, Na and Sr and affect the recrystallization behavior and in turn mechanical properties.In this work, a derivative of the 3003 alloy made entirely from post-consumer scrap has been analysed. The alloy achieved insufficient formability due to lack of recrystallization and grain growth. With the use of scanning electron microscopy (SEM) equipped with energy dispersive spectroscopy (EDS) and electron backscatter diffraction (EBSD) together with focused ion beam (FIB) lamella preparation, the microstructure was characterized.The characterization shows both larger particles of α-Al15Si2M4 (M=Mn,Fe,Cr) from solidification and dispersoids from heat treatment, pinning the grain boundary movement together with Q-AlCuMgSi. With the use of high throughput computational thermodynamics, Thermo-Calc was used to effectively screen compositions lowering the amount of α-Al15Si2M4 and removing the Q-AlCuMgSi phase. The new alloy was cast using directional solidification at different cooling rates to study the particle morphology, which in turn plays a role in the particle break up and distribution during cold working as the interparticle spacing affects the grain growth.Varying cooling rates was seen to affect morphology and distribution. Hot compression was utilized to examine the particle redistribution before cold work. It was however shown that hot compression was not sufficient in redistributing the particles as would be the case in rolling.

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<p>    </p> <p>Electrical steels are one type of soft magnetic material. They are based on Fe-Si alloys and are widely used for magnetic cores in transformers and electric motors. It is well known that Fe- 6.5Si wt% is the most efficient composition; however, at such a high silicon concentration (6.5wt.% = 12.1 at.% Si in Fe), the poor workability of the alloy makes it unacceptable for industrial production via conventional sheet steel rolling processes. This problem was approached in two different ways. First, a machining-based approach that suppresses the mechanisms that lead to cracking during conventional rolling was implemented for processing of thin metal strips. Two related machining-based sheet production technologies called free machining (FM), and hybrid cutting extrusion (HCE) were used to produce strips of high resistivity electrical steel. The maximum strip width achieved was 50 mm, and it was produced with a combination of FM and light rolling with a surface roughness comparable to cold-rolled sheet surfaces. Second, a new experimental alloy Fe-4Si-4Cr wt% was developed with improved magnetic properties compared to ~ Fe-3.2Si wt% and outstanding workability. Results report that the new experimental alloy has an electrical resistivity of 85 ± 3 𝜇Ω ∙ 𝑐𝑚 which is higher than Fe-6.5%Si. Also, the results on the Fe-4Si-4Cr workability show that this new alloy can withstand 75% cold-rolled reduction. The magnetic properties characterization was done via standard stacked toroid testing, and results show that Fe-4Si-4Cr experimental alloy exhibits excellent magnetic performance with a reduction in core losses of 33% at 400 Hz compared to commercial alloys with ~ Fe-3.2Si wt%. Recrystallization kinetics and texture evolution in the experimental alloy were evaluated for traditionally rolled and machining-based samples. Results were used to construct annealing maps. These maps represent the stages of the annealing process for a range of temperature versus time conditions, i.e., the annealing maps are a graphical summary showing the different stages of the annealing process for the Fe-4Si-4Cr experimental alloy in the two conditions. Despite the significant differences in the deformation texture of the two conditions, the recrystallization kinetics were similar. Finally, the two conditions retained the as-deformed texture in the intermediate annealing but to a lesser degree after completing a full anneal. In the case of the rolled sample, it is possible to trace the original texture fibers (γ-fiber, the partial α-fiber, and the θ -fiber) in the fully annealed data, but the texture intensity is just 2.5 mrd. On the other hand, the texture of the fully annealed HCE sample changes as compared to the as-deformed condition, located close to (110)[112] with a surprisingly strong peak of ~ 25 mrd. </p>

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.

Les travaux portent sur deux nuances d’alliages Ni-Cr-W, l’une contenant des précipités de W (EM722) et l’autre non (EM721). Les matériaux forgés, fournis par Aubert & Duval, présentaient des microstructures hétérogènes avec de très gros grains. Dans un premier temps, une procédure thermomécanique a été développée afin d’obtenir un état de référence avec une microstructure homogène avec une faible taille de grains et une texture relativement peu accusée. A partir de cet état de référence, l’évolution de la texture, au cours du laminage à froid (différents taux de réduction), a été analysée par diffraction des neutrons et a montré un renforcement de la texture de type Laiton. Les mécanismes de déformation ont été étudiés en microscopie électronique en transmission et par EBSD (Electron BackScatter Diffraction) afin de comprendre la formation de ce type de texture. Les bandes de cisaillement sont supposées être un facteur important pour la formation de ce type de texture. A partir des états déformés, la cinétique de recristallisation a été déterminée pour deux températures (700°C et 900°C) à partir de mesures de microdureté et par EBSD. Les mécanismes de recristallisation ont été étudiés par MET. Le mécanisme de SIBM (Strain Induced grain Boundary Migration) est le mécanisme prépondérant pour la nuance EM721. Pour l’autre nuance, EM722, possédant des précipités de W, le mécanisme de SIBM est présent, mais en plus, un second mécanisme de PSN (Particle Stimulated Nucleation) a été mis en évidence. De plus, quel que soit le mécanisme de recristallisation, une fois que les germes sont formés, ils maclent très rapidement. Par conséquent, une étude complémentaire sur l’évolution des joints de macle pendant la recristallisation primaire a été réalisée, en employant l’EBSD et surtout le système ASTAR installé dans un MET. Il a alors été montré que cette évolution dépend à la fois de la taille des grains et de l’énergie stockée par les grains pendant la déformation. Enfin, une simulation de la recristallisation primaire de type Monte-Carlo a également été mise en œuvre. Son originalité réside notamment dans sa capacité à rendre compte de la formation des joints de macles cohérents et rectilignes. / This work focuses on two grades of Ni-Cr-W alloys, one containing W precipitates (EM722) and the other not (EM721). The forged materials, provided by Aubert & Duval, had heterogeneous microstructures with very large grains. At first, a thermo-mechanical procedure was developed to obtain a reference state with a homogeneous microstructure with a small grain size and a texture relatively weak. From this reference state, the texture evolution during cold rolling (different reduction rates), was analyzed from neutron diffraction measurements and showed the strengthening of the Brass-type texture. The deformation mechanisms were studied by TEM (transmission electron microscopy) and EBSD (Electron Backscatter Diffraction) to understand the formation of this type of texture. The formation of shear bands is assumed to be the most important factor for the formation of such a texture. From the deformed states, the recrystallization kinetics was determined for two temperatures (700°C and 900°C) from micro-hardness and EBSD measurements. The recrystallization mechanisms were investigated by TEM. The SIBM (Strain Induced Grain Boundary Migration) mechanism is the predominant mechanism for the EM721 material. For the other one (EM722), which has W precipitates, the SIBM mechanism is present, but a second one (PSN: Particle Stimulated Nucleation) has also been evidenced. Furthermore, regardless of the mechanism of recrystallization, once the nuclei are formed, they twin quickly. Therefore, a further study on the evolution of twin boundaries during primary recrystallization was performed, using EBSD and especially the ASTAR system installed in a TEM. It has been shown that the twin development depends both on the grain size and the stored energy during the deformation. Finally, a Monte Carlo simulation of the primary recrystallization was also implemented. Its originality lies especially on its ability to create coherent and straight twin boundaries.

La transition d’un comportement séismique/instable à un comportement aséismique/stable est observée dans la partie en aval des zones sismogéniques (12-15 km de profondeur). Cette transition est supposée être contrôlée par l’activation de la plasticité de basse température du quartz à ~350°C. À cause de la grande profondeur à laquelle cette transition a lieu, le seul moyen pour étudier les processus physiques qui agissent en ces contestés, est l’étude des anciens prismes d’accrétion exhumés actuellement dans des chaines de montagnes. Le mélange tectonique de Hyuga et l’unité de Morotsuka appartiennent au prisme fossile de Shimanto et sont des unités metasédimentaires déformées à des températures peu inférieures ou égales à la limite fragile/ductile (~250 et ~340°C respectivement). Les résultats des observations de microstructures en microscopie optique et en microscopie électronique à balayage (diffraction des électrons rétrodiffusés) confirment que 1) la pression dissolution et une intense microfracturation sont les mécanismes de déformation principaux du quartz dans le mélange de Hyuga et localement l’activation de la plasticité du quartz est aussi observée; 2) dans l’unité de Morotsuka la recristallisation dynamique du quartz est pleinement active. Ces considérations indiquent que la température n’est pas le seul paramètre qui control l’activation de la plasticité du quartz, et laisse supposer la participation de l’effet adoucissant de l’eau. Avec le but de mieux comprendre le rôle de l’eau sur la rhéologie quartz, des expériences en Presse Griggs ont été menées, le matériel du départ étant de porphyroclasts de quartz (immergés dans une matrice sec) à la fois très riches en eau (provenant du mélange tectonique de Hyuga) et secs (quartz du Brésil). Ces expériences montrent l’effet très adoucissant de l’eau, qui à parité de conditions de déformation, favorise la migration de joint des grains dans le quartz de Hyuga tandis que le quartz du Brésil reste indéformé à exceptions de ses bordures extérieures. L’eau « en excès » est expulsée dans la matrice pour le quartz de Hyuga et stockée dans des bandes de cisaillement C’; l’eau incorporée par le quartz de Brésil n’est pas suffisantes pour favoriser la recristallisation dynamique. / The trasition from instable seismic to stable aseismic behaviour is observed in at the lower limit of the seismogenic zones in subduction zones (12-15 km). This transition is supposed to be controlled by the onset of quartz low grade plasticity at about 350°C. Due to inaccessibility of these geodynamic contests, the only way to study the physical processes acting at these depth are exhumed accretionary prisms exposed in mountain chains. The Hyuga tectonic mélange and the Foliated Morotsuka are metasedimentary units constituting the Shimanto accretionary prism (Japan). They were deformed at temperatures of ~250°C and ~340°C respectively, so slightly lower or equal to the temperature transition. Results by optical microscopy and EBSD reveal that 1) quartz deformation mechanisms active in Hyuga Tectonic Mélange are pressure solution and microfracturation accompanied by local quartz low grade plasticity; 2) dynamic recrystallization is totally active in quartz of the Foliated Morotsuka. These considerations allow to consider the role of water in triggering quartz plasticity especially in such water-rich contest as subduction zones. With the aim to better understand the role played by water on quartz rheology, we deformed high hydrated (from Hyuga unit) and dry (classic Brazil) quartz porphyroclasts within a quartz matrix, with the Griggs apparatus. These experiments show the weakening water effect on quartz strength. At the same deformation conditions, the high hydrated Hyuga quartz show recrystallization by grain boundary migration while the dry Brazil porphyroclasts are mostly undeformed, at exception of the outer recrystallized rims. The exceeding water expulsed from Hyuga quartz is stored in C’ shear bands in the matrix; water absorbed by dry Brazil porphyroclasts is not enough to promote dynamic recrystallization.

[pt] O principal objetivo deste trabalho foi avaliar a evolução microestrutural de dois tipos de nanocompósitos metal/cerâmico: Cu-10(por cento)Ni-1(por cento)Al2O3 (Cu-rich) e Ni-10(por cento)Cu-1(por cento)Al2O3 (Ni-rich) consolidadas em forma de fitas. A obtenção de nanoparticulas precursoras às fitas se deu por uma rota química, (que compreende a decomposição térmica de nitratos metálicos, originando óxidos coformados (CuO-NiO-Al2O3), seguido da redução seletiva destes por hidrogênio). O pó constituído de nanopartículas metálicas CuNi de 20nm a 100nm, com dispersão de nanopartículas ainda mais finas de Al2O3, foi submetido a pressão uniaxial a frio, em forma de pastilhas, e posteriormente sinterizado por 30 minutos. As pastilhas foram laminadas a frio com redução de espessura em 40, 60 e 80 por cento. As fitas assim produzidas foram recozidas a 600 graus Celsius nas amostras Cu-rich e a 900 graus Celsius nas Ni-rich, durante 5, 30 e 300 minutos, gerando diferentes estados microestruturais em virtude de fenômenos de recuperação, recristalização e crescimento de grão, na presença do Al2O3 na matriz metálica. O estudo detalhado da evolução microestrutural foi realizado por Microscopia Eletrônica de Varredura, Feixe de Íons Focalizado e Microscopia Eletrônica de Transmissão (MET), nos modos convencional e transmissão varredura (STEM), e em alta resolução (HRTEM). Tanto no MEV como no MET/STEM analises composicionais foram sistematicamente conduzidas por espectroscopia de dispersão de energia característica de raios x (EDXS). A preparação das amostras para MEV foi realizada por metodos metalogarficos convencionais e também submetidas a polimento por feixe de íons no instrumento MEV/FIB, quando necessário. As amostras transparentes ao feixe de elétrons para MET foram preparadas por métodos eletrolíticos convencionais e seletivos como o denominado jato duplo, assim como por feixe de íons no instrumento de precisão (PIPS) e em regiões especificas selecionadas extraindo lamelas através do FIB. Foi observado que as partículas cerâmicas não se dispersam homogeneamente na matriz metálica policristalina, mas se auto segregam em finos aglomerados seguindo o sentido da laminação e servindo como sítios preferenciais para a nucleação heterogênea de novos grãos, durante o fenômeno de recristalização no recozimento. Observa-se que nos lugares que o Al2O3 está presente o tamanho de grão, TG, é bem menor quando comparado com os lugares em ausência de Al2O3. De fato, observou-se sistematicamente que, principalmente nas amostras com alto grão de deformação ocorreram recristalização e crescimento de grão, gerando microestruturas bastante heterogêneas em quanto ao tamanho de grão, dando lugar a regiões da mostra com TG variando de 10nm a 100nm e regiões vizinhas na amostra com TG entre 1 um e 10 um. Medidas de microdureza comprovaram que as nanopartículas de Al2O3 agem como eficiente reforço, pois aumentou em até 100 porcento a dureza do material, quando comparado ao mesmo sem Al2O3. / [en] In this work it is evaluated the microstructural evolution of two types of metal/ceramic nanocomposites, Cu-10(percent)wt(percent)Ni-1(percent)Al2O3 (Cu-rich) and Ni-10Cu-1(percent)Al2O3 (Ni-rich), consolidated in ribbons. Initially, the precursor nanoparticles were obtained by a chemical route synthesis based on the thermal decomposition of Cu and Ni metal nitrates solution, as it generates co-formed oxides (CuO-NiOAl2O3). This material was selectively reduced by hydrogen in order to produce the nanocomposites. The CuNi matrix with particle size of about 20-100 nm containing a dispersion of even finer Al2O3 was uniaxially cold pressed into pellets and then aggregated by heating for 30 minutes. The treated pellets were cold rolled aiming a thickness reduction of 40, 60 and 80 (percent). The produced ribbons were then annealed at 600 degrees Celsius for Cu-rich samples and at 900 degrees Celsius for Nirich samples for periods of 5, 30 and 300 minutes. This step has produced different microstructural states due to phenomena of recovery, recrystallization and grain growth. The microstructural analysis was performed by Scanning Electron Microscopy (MEV), Focused Ion Beam (FIB), and Transmission Electron Microscopy (MET). All of the studies included the conventional and scanning (STEM) modes and high resolution (HRTEM). Particularly, the SEM and TEM / STEM compositional analyzes were conducted by x-ray energy dispersive spectroscopy (EDXS). The preparation of the samples for MEV was performed by conventional metallography, if required, the samples were subject to ion beam polishing in the MEV / FIB instrument. Electron transparent samples were prepared by conventional double jet electropolishing of thin foils, ion milling in precision instrument (PIPS) as well as selected lamellae prepared by Focus Ion Beam (FIB).These studies indicate that the ceramic particles are not homogeneously disperse in the polycrystalline metal matrix, but they selfsegregate in fine agglomerates following the direction of the cold rolled, and serve as preferential sites for the heterogeneous nucleation of new grains, due to recrystallization phenomenon, during annealing. It has also been observed that in the regions with the presence of Al2O3 the grain size of the nanoparticles is smaller. Actually, in the samples with high grain of deformation, recrystallization and grain growth occurred, generating highly heterogeneous size for the microstructures (range about 50nm to 10um). Microhardness measurements have showed that Al2O3 is a good reinforcement, as it increased the hardness of the material by up to 100 percent when compared with the same material without Al2O3.

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.