This thesis investigated the microstructure and mechanical property of RRR( high purity) and RG (low purity) niobium (Nb) sheet material. RRR Nb is used in the fabrication RF cavities. Our method involves processing bulk niobium by equal channel angular extrusion (ECAE) and then cross rolling to obtain sheets. This work is a study of the effect different thermomechanical processing variables have on the microstructure niobium sheets. Recrystallization behaviors strongly depended on the purity levels. Tensile tests on sheets clearly indicated the anisotropy in the sheet material. The ductility of the sheet was found to be the largest at an angle of 45o to the rolling direction. There was no apparent relationship observed in the yielding behavior in the different samples. The formability of the sheet measured by the anisotropy ratio suggested a strong dependence of anisotropy on texture. Texture results obtained show that different routes of ECAE can lead to variety of textures in final sheet material. Correlations between the microstructure and the ECAE routes suggest that effective control of microstructure is possible by the thermomechanical steps followed in this study.

Modified 9Cr-1Mo ferritic-martensitic steel (T91) has been extensively investigated as a structural material for GenIV nuclear reactors and Accelerator Driven Transmutation systems. One attractive characteristic of this steel in these applications is its superior radiation damage tolerance in comparison to typical austenitic stainless steels such as 316L. In some GenIV applications, it also has a significantly higher corrosion resistance. Further improvement of both is necessary if GenIV designs are to become commercially viable. Other work has shown an improvement in radiation damage tolerance via cold rolling or sputtering nanoscale multilayered films. Additionally, corrosion resistance can be improved by homogenizing the microstructure. Further, these changes can improve the strength of the material. However, there has been no fabrication of bulk ultra fine grain ferritic-martensitic steel candidates that might offer these avenues of improvement. This work demonstrates the refinement and homogenization of T91 by Equal Channel Angular Extrusion (ECAE) and heat treatment. Processing temperature and strain level were varied to produce multiple levels of refinement. Materials were characterized by microhardness, tensile testing, x-ray diffraction and transmission electron microscopy. An ultra-fine, highly misoriented and homogeneous microstructure was achieved in the material. Refinement was demonstrated both in ferritic and ferritic-martensitic compositions of the steel. Microhardness increased by as much as 70% and ultimate tensile strength by 80%. More significantly, tensile strength was improved by 40% without decreasing ductility.

Ultrafine grained (UFG), and nanocrystalline (nc) materials are of interest because of the high strength, compared with coarse grained counterparts. Several current methods to fabricate UFG and nc materials result in samples too small for practical use. In addition, the fabrication of nc materials, in particular, is difficult, and defects in the material causes significant reduction in strength and ductility of these materials. The present study uses Equal Channel Angular Extrusion (ECAE) to produce relatively large consolidates of UFG and nc materials. ECAE has been used to consolidate micro and nanocrystalline powders. The behavior of consolidated pure Cu and aluminum alloys in the nano and micron size were explored. The effects of different routes, extrusion temperature, and post-ECAE processing on microstructure and mechanical behavior were studied. Processing parameters were explored to determine the influence of each parameter on the consolidation performance. The goals of experimenting with different processing parameters were to increase the ductility of the material, while maintaining relatively strong specimens. Comparisons were made with a recently developed powder compaction constitutive model and corresponding simulations. ECAE of microcrystalline powders produced relatively ductile materials, with high strength. Swaging of these consolidated powders produced samples which were softer and less ductile in tension, than the non-swaged samples. ECAE produced effective consolidation of Cu nanoparticles with average sizes of 100 nm, with an ultimate tensile strength of 680 MPa, with a fracture strain as much as 10%, which is higher than previously reported 7% [Haouaoui, 2005].

A thermodynamic framework was presented for the development of powderconstitutive models. The process of powder compaction through Equal ChannelAngular Extrusion (ECAE) at room temperature was modeled using the finiteelement analysis package ABAQUS. The simulation setup was used to conduct aparametric study involving varying the process parameters of ECAE, aimed ataiding the process design.Two powder compaction models, the Gurson model and the Duva and Crowmodel, were used to test their efficacy in modeling this process. Thethermodynamic framework was applied to derive the constitutive equations of theDuva and Crow model. Modeling parameters like friction coefficients, interactionconditions were determined by comparing the simulations for solid billet and anempty can with actual experimental runs for loads, shear angle and workpiece geometry. The simulations using the two powder constitutive models showed nosignificant difference in the stress in the powder during the extrusion.The results obtained from the 3-D simulations were also compared toexperiments conducted to compact copper powder with a size distribution of 10mto 45m. It was found through experiments that the powder does not fullyconsolidate near the outer corner of the workpiece after the first ECAE pass and theresults from the simulations were used to rationalize this phenomenon.Modifications made to the process by applying a back pressure during thesimulations resulted in a uniformly compacted powder region.Further, simulations were carried out by varying the process parameters likethe crosshead velocity, the friction coefficient between the walls of the die and thecan, can dimensions and material, shape of the can cross section etc and the effectof each of these parameters was quantified by doing a sensitivity analysis.

A thermodynamic framework was presented for the development of powderconstitutive models. The process of powder compaction through Equal ChannelAngular Extrusion (ECAE) at room temperature was modeled using the finiteelement analysis package ABAQUS. The simulation setup was used to conduct aparametric study involving varying the process parameters of ECAE, aimed ataiding the process design.Two powder compaction models, the Gurson model and the Duva and Crowmodel, were used to test their efficacy in modeling this process. Thethermodynamic framework was applied to derive the constitutive equations of theDuva and Crow model. Modeling parameters like friction coefficients, interactionconditions were determined by comparing the simulations for solid billet and anempty can with actual experimental runs for loads, shear angle and workpiece geometry. The simulations using the two powder constitutive models showed nosignificant difference in the stress in the powder during the extrusion.The results obtained from the 3-D simulations were also compared toexperiments conducted to compact copper powder with a size distribution of 10mto 45m. It was found through experiments that the powder does not fullyconsolidate near the outer corner of the workpiece after the first ECAE pass and theresults from the simulations were used to rationalize this phenomenon.Modifications made to the process by applying a back pressure during thesimulations resulted in a uniformly compacted powder region.Further, simulations were carried out by varying the process parameters likethe crosshead velocity, the friction coefficient between the walls of the die and thecan, can dimensions and material, shape of the can cross section etc and the effectof each of these parameters was quantified by doing a sensitivity analysis.

The purpose of this work was to study learn about grain refinement mechanisms and texture development in cast n-type Bi90Sb10 alloy caused by severe plastic deformation. The practical objective is to produce a fine grained and textured microstructure in Bi90Sb10 alloy with enhanced thermoelectric performance and mechanical strength. In the study, twelve millimeter diameter cast bars of Bi90Sb10 alloy were encapsulated in square cross section aluminum 6061 alloy containers. The composite bars were equal channel angular (ECAE) extruded through a 90 degree angle die at high homologous temperature. Various extrusion conditions were studied including punch speed (0.1, 0.3 and 0.6 in/min), extrusion temperature (220, 235 and 250oC), number of extrusion passes (1, 2 and 4), route (A, BC and C), and exit channel area reduction ratio (half and quarter area of inlet channel). The affect of an intermediate long term heat treatment (for 100 hours at 250oC under 10-3 torr vacuum) was explored. Processed materials were characterized by optical microscopy, x-ray diffraction, energy dispersive spectroscopy, wavelength dispersive spectroscopy and scanning electron microscopy. Texture was analyzed using the {006} reflection plane to identify the orientation of the basal poles in processed materials. The cast grains were irregularly shaped, had a grain size of hundreds-of-microns to millimeters, and showed inhomogeneous chemical composition. Severe plastic deformation refines the cast grains through dynamic recrystallization and causes the development of a bimodal microstructure consisting of fine grains (5-30 micron) and coarse grains (50-300 micron). ECAE processing of homogenizied Bi-Sb alloy causes grain refinement and produces a more uniform microstructure. Texture results show that ECAE route C processing gives a similar or slightly stronger texture than ECAE route A processing. In both cases, the basal-plane poles become aligned with the shear direction. Reduction area exit channel extrusion is more effective for both grain refinement and texture enhancement than simple ECAE processing.

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The objectives of this study were to examine the effect of strain and path change on the microstructural evolution of ultrafine grained interstitial free (IF) steel during equal channel angular extrusion (ECAE); to determine the mechanical properties; to observe the resulting texture; and to perform optical and electron microscopy of the resulting material. The effects of different routes of extrusion (A, B, C, C' and E), heat treatment and plastic strains from 1.15 to 18.4 were examined. Monotonous tensile testing was used to determine mechanical behavior of processed materials. X-ray diffraction and TEM analyses were performed to evaluate the effect of processing on texture and grain morphology. Hardness measurements were performed to determine recrystallization behavior of the processed material. Optical microscopy was conducted on heat treated samples to determine their grain size and refinement. Monotonous tensile testing of processed materials showed that there was significant strengthening after the first extrusion. Further processing resulted in increasing values of yield strength and ultimate tensile strength, with ductility at failure varying depending upon which processing route was used. The best tensile strength results were obtained after processing Routes 8C' and 16E, due to the significant grain refinement these routes produced. X-ray diffraction revealed increases in strength of preferred texture along the directions [111] and [001], perpendicular to the transverse plane, for all specimens that were processed using ECAE. TEM observations showed a consistent refinement of grain size as the amount of processing increased, especially within Routes C' and E. Hardness measurements of heat treated specimens showed that the onset of recrystallization occurred at approximately the same temperature of recrystallization as that of pure iron, 450°C. The recrystallization curves for all samples showed that grain growth begins at a temperature of around 700°C. The low carbon content of IF steel made optical microscopy challenging. The grain size of annealed materials becomes finer and more uniform, ranging between 60 and 90 μm2, at high strain levels under Routes C' and E, due to the many potential nucleation sites developed in highly worked material.

Nickel-Titanium (NiTi) shape memory alloys have been the focus of extensive research due to its unique characteristics such as high recoverable strain and ductility. However, solutionized samples of NiTi do not demonstrate good shape memory characteristics due to low strength for dislocation slip. Thermo-mechanical treatments are required to strengthen the matrix and improve the shape memory characteristics. Plastic deformation and the subsequent annealing is the common way to improve shape memory properties. In this case, deformation magnitude, temperature, rate, mechanism, and annealing temperature and time are all important parameters for the final shape memory properties. Equal channel angular extrusion (ECAE) is a well-known technique to severely deform materials by simple shear with no change in cross-section. In this study, Ti- 49.8 at% Ni samples are deformed by ECAE at three different temperatures near transformation temperatures. X-ray analysis, calorimetry, transmission electron microscopy and thermo-mechanical cycling techniques are utilized to investigate the effects of severe deformation and subsequent annealing treatment on shape memory properties. Martensite stabilization, formation of strain induced B2 phase, change in transformation temperatures, formation of new phases, recrystallization temperature, texture formation, and increase in strength and pseudoelastic strain are the main findings of this study. Co-32.9 at% Ni-29.5 at% Al is a newly found ferromagnetic alloy. Its low density, high melting temperature and cheap constituents make the alloy advantageous among other shape memory alloys. Although some magnetic properties of this alloy are known, there is no report on basic shape memory characteristics of CoNiAl. In this study, effect of thermo-mechanical treatments on the microstructure and shape memory characteristics such as transformation behavior, pseudoelasticity, stages of transformation, temperature dependence of the pseudoelasticity, response to thermal and stress cycling is investigated. Formation of second phase along the grain boundaries and inside the grains, about 4% pseudoelastic and two-way shape memory strain, very narrow stress hysteresis, large pseudoelastic window (>150°C), two-stage martensitic transformation, stable response to cyclic deformation, high strength for dislocation slip, slope of Clasius-Clapeyron curve, and twinning plane are determined for the first time in literature.

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.