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.

Atualmente existe um considerável interesse no processamento de materiais com estrutura ultrafina de grãos. Estes materiais podem ser obtidos por deformação plástica severa via extrusão por canal angular (ECAE). Durante ECAE, uma barra lubrificada é pressionada através de uma matriz rígida consistindo de dois canais de mesma seção transversal, os quais se interceptam a um ângulo ?. Cisalhamento simples é o mecanismo de deformação predominante e ocorre paralelamente ao plano de intersecção entre os dois canais. Este trabalho enfoca a estabilidade térmica e sua influência sobre as propriedades magnéticas de ferro puro severamente deformado por ECAE. Uma barra de ferro puro foi deformada em temperatura ambiente por múltiplos passes de ECAE (8 passes), usando uma matriz com ângulo de intersecção ??= 90º, resultando em uma deformação equivalente _N = 9,2. Esta barra foi girada de 90o depois de cada passe de extrusão. Amostras da barra deformada foram recozidas em várias temperaturas entre 100 e 800°C, variando-se o tempo de recozimento entre 1 e 120 min. Uma segunda barra de ferro puro foi deformada por um único passe de ECAE, com um ângulo ??= 120o, resultando em uma deformação equivalente _N = 0,67. Amostras retiradas desta barra foram recozidas em várias temperaturas entre 300 e 800°C por 15 min. Em uma condição correspondente à segunda barra, uma terceira foi deformada sendo o passe de ECAE interrompido. A caracterização microestrutural foi efetuada utilizando-se microscopias ótica e eletrônica de varredura, microdureza Vickers e textura via difração de raios X. Curvas de magnetização em função do campo magnético aplicado até cerca de 9 T foram obtidas para amostras representativas da barra deformada por múltiplos passes de ECAE. Foram determinados os intervalos de temperatura de recozimento em que ocorrem a recuperação e a recristalização para esta barra e para a barra deformada por um único passe de ECAE. Com relação à barra do ensaio interrompido, várias seções do plano normal à direção de extrusão da barra foram analisadas a fim de se investigar a evolução da textura durante extrusão em canal angular. Os resultados foram comparados com aqueles reportados para outros materiais deformados via ECAE com estrutura ccc e também com as texturas previstas pelo Modelo Visco-plástico Autoconsistente (do inglês VPSC model). / There is considerable current interest in fabricating ultrafine-grained materials. Such materials can be obtained by severe plastic deformation via equal-channel angular extrusion (ECAE). During ECAE, a lubricated billet is pressed through a rigid die consisting of two channels of the same cross section intersecting each other at an angle ?. Simple shear is the predominant deformation mechanism and occurs parallel to the intersecting plane of the channels. This work focuses on thermal stability and its influence on the magnetic properties of severely deformed pure iron via ECAE. A billet of pure iron was deformed at room temperature by multiple ECAE passes (8 passes), using a die angle ??= 90o, to a total equivalent strain of _N = 9.2. The billet was rotated by 90o after each extrusion pass. Samples of the deformed billet were annealed at several temperatures between 100 and 800oC, varying the annealing time from 1 to 120 min. A second billet of pure iron was deformed using 1-pass ECAE, with ??= 120o, with an equivalent strain of _N = 0.67. Samples of this billet were annealed at several temperatures between 300 and 800°C for 15 min. Corresponding to second condition, a third billet was deformed by interrupting the ECAE pass. Microstructural characterization was performed using optical and scanning electron microscopies, Vickers microhardness, and texture measurements via X-ray diffraction. Magnetization curves as a function of applied magnetic field up to 9 T were obtained for representative samples of the billet deformed by multiple ECAE passes. The annealing temperature ranges corresponding to recovery and recrystallization for this billet and 1-pass ECAE billet were determined. Regarding the interrupted 1-pass ECAE billet, several sections normal to the extrusion direction were analyzed in order to investigate the texture evolution during equal channel angular extrusion. The obtained results were compared to those ones found in other deformed bcc materials via ECAE and also by using the visco-plastic self-consistent (VPSC) model to predict the final texture.

Atualmente existe um considerável interesse no processamento de materiais com estrutura ultrafina de grãos. Estes materiais podem ser obtidos por deformação plástica severa via extrusão por canal angular (ECAE). Durante ECAE, uma barra lubrificada é pressionada através de uma matriz rígida consistindo de dois canais de mesma seção transversal, os quais se interceptam a um ângulo ?. Cisalhamento simples é o mecanismo de deformação predominante e ocorre paralelamente ao plano de intersecção entre os dois canais. Este trabalho enfoca a estabilidade térmica e sua influência sobre as propriedades magnéticas de ferro puro severamente deformado por ECAE. Uma barra de ferro puro foi deformada em temperatura ambiente por múltiplos passes de ECAE (8 passes), usando uma matriz com ângulo de intersecção ??= 90º, resultando em uma deformação equivalente _N = 9,2. Esta barra foi girada de 90o depois de cada passe de extrusão. Amostras da barra deformada foram recozidas em várias temperaturas entre 100 e 800°C, variando-se o tempo de recozimento entre 1 e 120 min. Uma segunda barra de ferro puro foi deformada por um único passe de ECAE, com um ângulo ??= 120o, resultando em uma deformação equivalente _N = 0,67. Amostras retiradas desta barra foram recozidas em várias temperaturas entre 300 e 800°C por 15 min. Em uma condição correspondente à segunda barra, uma terceira foi deformada sendo o passe de ECAE interrompido. A caracterização microestrutural foi efetuada utilizando-se microscopias ótica e eletrônica de varredura, microdureza Vickers e textura via difração de raios X. Curvas de magnetização em função do campo magnético aplicado até cerca de 9 T foram obtidas para amostras representativas da barra deformada por múltiplos passes de ECAE. Foram determinados os intervalos de temperatura de recozimento em que ocorrem a recuperação e a recristalização para esta barra e para a barra deformada por um único passe de ECAE. Com relação à barra do ensaio interrompido, várias seções do plano normal à direção de extrusão da barra foram analisadas a fim de se investigar a evolução da textura durante extrusão em canal angular. Os resultados foram comparados com aqueles reportados para outros materiais deformados via ECAE com estrutura ccc e também com as texturas previstas pelo Modelo Visco-plástico Autoconsistente (do inglês VPSC model). / There is considerable current interest in fabricating ultrafine-grained materials. Such materials can be obtained by severe plastic deformation via equal-channel angular extrusion (ECAE). During ECAE, a lubricated billet is pressed through a rigid die consisting of two channels of the same cross section intersecting each other at an angle ?. Simple shear is the predominant deformation mechanism and occurs parallel to the intersecting plane of the channels. This work focuses on thermal stability and its influence on the magnetic properties of severely deformed pure iron via ECAE. A billet of pure iron was deformed at room temperature by multiple ECAE passes (8 passes), using a die angle ??= 90o, to a total equivalent strain of _N = 9.2. The billet was rotated by 90o after each extrusion pass. Samples of the deformed billet were annealed at several temperatures between 100 and 800oC, varying the annealing time from 1 to 120 min. A second billet of pure iron was deformed using 1-pass ECAE, with ??= 120o, with an equivalent strain of _N = 0.67. Samples of this billet were annealed at several temperatures between 300 and 800°C for 15 min. Corresponding to second condition, a third billet was deformed by interrupting the ECAE pass. Microstructural characterization was performed using optical and scanning electron microscopies, Vickers microhardness, and texture measurements via X-ray diffraction. Magnetization curves as a function of applied magnetic field up to 9 T were obtained for representative samples of the billet deformed by multiple ECAE passes. The annealing temperature ranges corresponding to recovery and recrystallization for this billet and 1-pass ECAE billet were determined. Regarding the interrupted 1-pass ECAE billet, several sections normal to the extrusion direction were analyzed in order to investigate the texture evolution during equal channel angular extrusion. The obtained results were compared to those ones found in other deformed bcc materials via ECAE and also by using the visco-plastic self-consistent (VPSC) model to predict the final texture.

In this study, ultrafine-grained commercial purity AA1050 aluminum was produced by equal channel angular extrusion (ECAE).Annealing at 250¢J was able to give a grain size of 0.59£gm. Specimens were compressed along different ECAE axis under a strain rate of 7.1¡Ñ10-4 s-1at room temperature. Compression tests were also performed under 5¡Ñ10-5 s-1, 7.1¡Ñ10-4 s-1 ,and 10-1 s-1 strain rates at 100¢J,150¢J ,and 175¢J. Surface morphology of specimens was observed by optical and scanning electron microscopes to study the generation of shear bands. Texture within shear bands was analyzed by electron backscattered diffraction (EBSD). The present research found that, different compression direction has little effect on the generation of shear bands. Increasing compression temperature and decreasing strain rates have the effect of decreasing the degree of strain localization of shear bands. Shear band deformation is compatible with the uniform deformation occurred outside shear bands. Texture change within shear bands is rotated about an axis perpendicular to the specimen surface, and strengthens the texture component.

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Equal channel angular extrusion (ECAE) has attracted a substantial attention for it provides the opportunity to introduce large plastic strain into the material in the bulk form. Both die angles and processing routes have been recognized as the important parameters in applying ECAE to fabricate ultrafine-grained materials. Unfortunately, studies of different group provided inconsistent conclusions on the effectiveness of processing routes, which are believed to be due to the incomplete microstructural information obtained in each investigation. In the present work, quantitative analysis of the microstructure developed by different processing conditions were conducted using transmission electron microscopy (TEM), in which the morphology, size, and shape of subgrains as well as boundary misorientation were fully characterized. A commercial pure aluminum (AA 1050) was deformed by ECAE to strain of ~ 8 with different routes (A, Bc and C, in terms of reorientation angle 0o, 90o, and 180o respectively of the billet between two extrusion passes) and die angles. The results show that the effectiveness of high angle boundary (HAB) formation is in the sequence of route A¡ÜBc>C. However, in terms of grain refinement, the effectiveness is in the order of route Bc>A>C. In addition, route A produces subgrains with the most elongated shape, while route Bc produces subgrains with the most equiaxed shape. These results may be attributed to the different shear pattern introduced in each route. ECAE die angle determines both the strain per pass and the shear plane orientation. In route C, the shear is maintained in the same plane and the effect of strain per pass can be studied. With route C, both the 90o and 120o die produce microstructure with similar HAB proportions, but they result in different arrangement of HABs. The 120o die produces subgrains with larger size and higher aspect ratio than the 90o die does in route C. Generally speaking, for the die angle range studied, the different values of strain per pass used in ECAE mainly affect the morphology of the subgrains. On the other hand, the effect of die angle is weakened with route Bc as compared to route C, which may be attributed to the intersection of shear planes involved in route Bc.

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It has been shown that alloys with submicron-grained structure can be produced by severe plastic deformation (SPD). However, our understanding about the characteristics of mechanical behaviors of these materials is still limited. According to the literature, many alloys exhibit quite different mechanical properties as the grain size decreasing to submicrometer range. In this study, commercial purity aluminum (AA1050) of grain size ranging from 0.35 to ~ 45 mm was obtained by the proper combination of equal-channel angular extrusion (ECAE) and annealing treatment. The influences of grain size, testing temperature and boundary character on the mechanical properties were studied in this work. Generally speaking, the materials of grain sizes below 1mm have quite different mechanical properties than those of coarser grain sizes. In tensile tests, they exhibited yield drop immediately followed by work softening at RT, while they showed Lüders extension followed by work hardening at 77K. In addition, their yield strength at RT was about 20% higher in compression than in tension. The submicron-grained aluminum has much higher strength but lower tensile ductility than large grained aluminum at room temperature, while it exhibits both high strength and good ductility at 77K. This finding suggests that the poor tensile ductility of submicron-grained alloys at room temperature may be improved by reducing the dynamic recovery rate. The Hall-Petch slope in the submicrometer grain size range showed positive deviation from that extended from coarser grains at both room temperature and 77K. This might be arisen from the phenomenon of inhomogeneous yielding as grain size below 1 mm. In addition, the grain boundary character distribution was found to have influence on the tensile properties of matrials of submicrometer grain sizes. As the grain size increases to the range between 1 mm and 4 mm, the tensile deformation at RT proceeds by the propagation of Lüders band initially, and followed by strain hardening. For materials of grain sizes greater than 4 mm, a normal strain hardening behavior of coarse-grained aluminum resumes.

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NiTiHf alloys have attracted considerable attention as potential high temperature Shape Memory Alloy (SMA) but the instability in transformation temperatures and significant irrecoverable strain during thermal cycling under constant stress remains a major concern. The main reason for irrecoverable strain and change in transformation temperatures as a function of thermal cycling can be attributed to dislocation formation due to relatively large volume change during transformation from austenite to martensite. The formation of dislocations decreases the elastic stored energy, and during back transformation a reduced amount of strain is recovered. All these observations can be attributed to relatively soft lattice that cannot accommodate volume change by other means. We have used Equal Channel Angular Extrusion (ECAE), hot rolling and marforming to strengthen the 49.8Ni-42.2Ti-8Hf (in at. %) material and to introduce desired texture to overcome these problems in NiTiHf alloys. ECAE offers the advantage of preserving billet cross-section and the application of various routes, which give us the possibility to introduce various texture components and grain morphologies. ECAE was performed using a die of 90º tool angle and was performed at high temperatures from 500ºC up to 650ºC. All extrusions went well at these temperatures. Minor surface cracks were observed only in the material extruded at 500 °C, possibly due to the non-isothermal nature of the extrusion. It is believed that these surface cracks can be eliminated during isothermal extrusion at this temperature. This result of improved formability of NiTiHf alloy using ECAE is significant because an earlier review of the formability of NiTiHf using 50% rolling reduction concluded that the minimum temperature for rolling NiTi12%Hf alloy without cracks is 700°C. The strain level imposed during one 90° ECAE pass is equivalent to 69% rolling reduction. Subsequent to ECAE processing, a reduction in irrecoverable strain from 0.6% to 0.21% and an increase in transformation strain from 1.25% to 2.18% were observed at a load of 100 MPa as compared to the homogenized material. The present results show that the ECAE process permits the strengthening of the material by work hardening, grain size reduction, homogeneous distribution of fine precipitates, and the introduction of texture in the material. These four factors contribute in the increase of stability of the material. In this thesis I will be discussing the improvement of mechanical behavior and stability of the material achieved after various passes of ECAE.