Recovery, recrystallization, grain growth and precipitation constitute the fundamentals of thermomechanical controlled processing (TMCP) of microalloyed steels. In-depth understanding of these phenomena is indeed needed. In this work, the individual components and some of the potential mutual interactions have been investigated deliberately. The effect of alloying elements of Mn, Si, and Al on recovery and recrystallization has been systematically studied by conducting the stress relaxation tests on binary Fe-0.1%C and ternary Fe-0.1%C-X alloys. The effect of temperature on recovery kinetics was also investigated. The effects were considered by fitting the recovery model through the activation volume term. Higher temperature or lower solute content will accelerate the recovery process and then facilitate the onset of recrystallization. NbC precipitation behavior has been investigated using a nickel-based model alloy, having samples deformed at both room temperature and elevated temperature and subjected to annealing at 700℃ for different times, in order to elucidate the stages of nucleation, growth and coarsening for precipitation. The microstructures preserved by water quenching were examined using transmission electron microscopy (with both metal foil and carbon replica specimens). Results from mechanical response and microstructural evolution are linked and discussed. The precipitate number density and size evolution show good agreements with predictions from a classical strain-induced precipitation model. The in-situ laser-ultrasonics measurement of C-Mn steels provides a unique way to evaluate grain size evolution during TMCP, for different strains of 0.15, 0.25 and 0.35, at 950℃ and 1050℃. Effects of temperature and strain on recovery, recrystallization and grain growth have been covered and elucidated. Higher strains facilitate the onset of recrystallization and grain size refinement. However, higher temperatures only shorten the onset of recrystallization but lead to larger grain size. The effect of microalloying element of Nb on softening kinetics was also investigated by comparing C-Mn/C-Mn-Nb steels at the same conditions. The solute drag effect of Nb can be seen by the onset-delays of recrystallization and larger grain sizes. The laser-ultrasonics results can match well with stress relaxation measurements. The in-situ grain size evolution data has given the possibility to develop robust thermomechanical processing (TMP) models combining deformation, recovery, precipitation, recrystallization and grain growth. The application and validation of the TMP models have been attempted and remain ongoing. / Thesis / Doctor of Philosophy (PhD)

Ligas de Urânio são candidatas ao uso como combustível nuclear em reatores avançados, dentre essas ligas se destacam as ligas de Urânio com Nióbio e com Zircônio. Este trabalho investigou como os teores de Nb e Zr, assim como a processamento termomecânico afetam as microestruturas e as propriedades mecânicas de 3 ligas U-XNb-YZr onde X+Y=12. Duas amostras contendo 50g cada, foram fabricadas através de fusão à plasma nos teores U-3Nb-9Zr (liga 39), U- 6Nb-6Zr (liga 66) e U-9Nb-3Zr (liga 93). Uma das amostras de cada liga foi tratada termicamente por 5h a 1000°C para a realização de homogeneização química. A amostra homogeneizada e a amostra bruta de fusão de cada liga foram conjuntamente encapsuladas em aço para a realização de laminação a quente seguida de um recozimento final a 1000°C por 2h. À rota adotada pela amostra bruta de fusão chamou-se \" Rota C\" e a rota adotada pela amostra homogeneizada chamou-se \"Rota H\". A caracterização microestrutural foi feita por microscopia óptica e eletrônica de varredura. Todas as amostras, independente do processamento, apresentaram precipitados ricos em Nióbio e Zircônio em adição a uma matriz rica em Urânio. A caracterização das amostras brutas de fusão mostra que os teores de elementos de liga influenciam diretamente a morfologia das dendritas evidentes na microestrutura assim como das demais fases presentes em cada amostra. A liga 39 apresentou predominantemente fase ?\', a liga 66 a fase ?\" com traços de fase y e a liga 93 a fase y com traços de fase ?\". Após o tratamento térmico de homogeneização, a liga 39 apresentou fase ?\" na forma celular enquanto a liga 66 apresentou as fases y0 e y e a liga 93 apresentou apenas fase y. As propriedades mecânicas das ligas foram avaliadas por ensaios de dureza e de dobramento simples. As amostras da Rota C apresentaram redução de dureza em relação à condição inicial. Todas as microestruturas das amostras laminadas a quente exibiram duas fases ricas em U. A liga 39 apresentou as fases ?\" na forma celular e ?\' após a laminação a quente. Após o recozimento final na rota C, a liga 39 apresentou fase ?\" na forma acicular enquanto as ligas 66 e 93 apresentaram as fases ?\" e y após a laminação e fase y. A fração de área da amostra pobre em U elevou-se nas ligas 39 e 66 e reduziu-se na liga 93. As amostras da Rota H apresentaram redução de dureza em relação à condição bruta de fusão. A liga 39 apresentou fase ?\" na forma celular com orientação e traços da fase ?, a liga 66 exibiu as fases y0 e y e a liga 93 as fases y e y0. Após o recozimento final, a liga 39 mostrou-se novamente na forma ?\" na forma celular, mas sem orientação. A liga 66 apresentou fase y e a liga 93 fase y0. Os testes de dobramento simples mostraram que as ligas da Rota C exibem plasticidade, retendo parte da deformação plástica após a ruptura das amostras testadas. Já as amostras da Rota H mostraram comportamento super elástico, possibilitando maiores deformações mas sem reter deformação plástica após a ruptura das amostras. A melhor relação entre deformação total e residual foi observada na liga 93 fabricada pela Rota C. As análises nos perfis de fratura das amostras da Rota C mostram fraturas transgranulares em todas as amostras. O perfil de fratura de na amostra recozida liga 39 mostra que a fase ?\" na forma acicular tende a deforma-se por deslizamento. As análises dos perfis de fratura nas amostras da Rota H confirmaram a ausência de deformação plástica mesmo em escala microscópica. Para essa condição, a fase ?\" na forma celular com orientação (liga 39) aparenta deformar-se por maclação. As análises de superfície de fratura indicam que a fase pobre em U tem participação durante o processo de crescimento e propagação da fratura na Rota H, atuando como caminho para bifurcação de trincas acelerando o processo de ruptura, enquanto na Rota C, a fase pobre em U deforma-se conjuntamente com a matriz de U. Em uma segunda etapa do trabalho, a estabilidade das microestruturas resultantes na amostras processadas foi investigada por Ensaios de Calorimetria Diferencial Exploratória (DSC) e por calorimetria de queda livre (esta apenas para a amostra 93 da rota H). O teor de Nb e Zr também afeta a estabilidade das fases presentes em cada amostra. foram realizados com as amostras da condição homogeneizada e laminada. A quantidade de transformações assim como o estado final de cada liga diferiu de acordo com a razão Nb/Zr. Após o ciclo de aquecimento e resfriamento da análise térmica, a liga 39 apresentou fase ?\', a liga 66 fase ?\" e a liga 93 fase y. No ensaio de calorimetria por queda livre foi possível observar as diferentes etapas de reação de envelhecimento da matriz g, correspondendo a à transformação y -> y0 (entre 525 e 530 K), a transformação y -> ?\". (entre 623 e 651 K) e à transformação y\' -> y3+? (entre 825 e 925 K). / Uranium alloys are candidates to be used as nuclear fuel in research reactors, among the U alloys, the Nb and Zr containing alloys are promising. This work evaluated how the Nb and Zr content and the thermomechanical processing affects the microstructure and mechanical properties of 3 alloys U-XNb-YZr were X+Y=12. Two 50g slugs of each sample were fabricated using plasma arc melting according to U-3Nb-9Zr (alloy 39), U-6Nb-6Zr (alloy 66) and U-9Nb-3Zr (alloy 93). One slug of each alloy was heat treated for 5h at 1000°C to perform the chemical homogenization. The homogenized sample and the as-cast one were encapsulated in the same steel frame in order to perform hot rolling. After the rolling process, the samples were annealed by 2h at 1000°C. The route that uses only as-cast samples was nominated \"Route C\" and the route that uses the homogenized sample was nominated \"Route H\". The microstructural characterization was performed by optical and scanning electron microscopy. All samples, regardless the processing route, presented Nb and Zr rich precipitates in addition to U rich matrix. The characterization of as-cast samples shows that the content of the alloying element has a direct influence on dendrite morphology as in the phases presented for each alloy. The alloy 39 presented predominantly ?\' phase, the alloy 66 the ?\" phase with a small quantity of ? phase and the alloy 93 presented the ? phase with small quantity of ?\" phase. Afte the homogenization, the alloy 39 presented cellular ?\" phase, the alloy 66 presented ?0 and ?, the alloy 93 presented only ? phase. The mechanical properties were evaluated by hardness measurements and free bending tests. The Route C samples presented hardness reduction in comparison to the initial condition. All microstructures of hot-rolled samples of this route exhibit two U rich phases. The alloy 39 exhibited cellular ?\" and ?\', after the final annealing the alloy 39 presented acicular ?\". The alloys 66 and 93 exhibited ?+?\" after hot rolling and ? phase after the final annealing. The area fraction of poor U phase increased in the alloys 39 and 66, but reduced in alloy 93. The Route H samples presented hardness reduction in comparison to as-cast samples. The alloy 39 presented cellular oriented ?\" phase and a small quantity of ? phase. The alloy 66 exhibited ?0 and ?, the alloy 93 ? and ?0. After the final annealing, the alloy 39 presented the ?\" again, but without orientation. The alloy 66 presented ? phase and the alloy 93 presented ?0. The free bending tests show that Route C samples have real plasticity, retaining part of deformation after rupturing as plastic strain. The Route H samples exhibited superelastic behavior, allowing higher deformations but retaining no plastic strain after sample breaking. The better balance between total and residual strain was observed in alloy 93 fabricated by Route C. The cracking profile analysis of Route C samples shows transgranular fractures in all samples. The Cracking profile of final 39 sample shows that acicular ?\" tends to deform by slipping. The cracking profile analysis of Route H samples confirmed the absence of plasticity even on the microscopic scale. This condition, the oriented cellular ?\" phase (alloy 39) apparently deforms by twinning. The crack surface analysis indicates that the U poor phase has a direct participation in crack growing and propagation, acting as forking points to the fracture and accelerating the fracture process. In the Route C samples, the poor U phase deforms alongside the U matrix. The stability of resulting microstructures of homogenized and hot rolled samples was investigated by Differential Scanning Calorimetry (DSC) and Drop Differential Scanning Calorimetry (only for the homogenized hot rolled 93 sample). The Nb and Zr also affect the stability of present phases in each sample. The number of transformations and the final structure is directly influenced by the Nb/Zr ratio. After the thermal cycle imposed by the DSC analysis, the alloy 39 exhibited ?\' phase, the alloy 66 exhibited ?\" phase and the alloy 93 exhibited ? phase. The Drop-DSC allowed observing the different stages of reaction in ? matrix, corresponding to ? -> ?0 (between 525 and 530 K), ? -> ?\" transformation (between 623 and 651 K) and ?\' -> ?3+? transformation (between 825 and 925 K).

Ligas de Urânio são candidatas ao uso como combustível nuclear em reatores avançados, dentre essas ligas se destacam as ligas de Urânio com Nióbio e com Zircônio. Este trabalho investigou como os teores de Nb e Zr, assim como a processamento termomecânico afetam as microestruturas e as propriedades mecânicas de 3 ligas U-XNb-YZr onde X+Y=12. Duas amostras contendo 50g cada, foram fabricadas através de fusão à plasma nos teores U-3Nb-9Zr (liga 39), U- 6Nb-6Zr (liga 66) e U-9Nb-3Zr (liga 93). Uma das amostras de cada liga foi tratada termicamente por 5h a 1000°C para a realização de homogeneização química. A amostra homogeneizada e a amostra bruta de fusão de cada liga foram conjuntamente encapsuladas em aço para a realização de laminação a quente seguida de um recozimento final a 1000°C por 2h. À rota adotada pela amostra bruta de fusão chamou-se \" Rota C\" e a rota adotada pela amostra homogeneizada chamou-se \"Rota H\". A caracterização microestrutural foi feita por microscopia óptica e eletrônica de varredura. Todas as amostras, independente do processamento, apresentaram precipitados ricos em Nióbio e Zircônio em adição a uma matriz rica em Urânio. A caracterização das amostras brutas de fusão mostra que os teores de elementos de liga influenciam diretamente a morfologia das dendritas evidentes na microestrutura assim como das demais fases presentes em cada amostra. A liga 39 apresentou predominantemente fase ?\', a liga 66 a fase ?\" com traços de fase y e a liga 93 a fase y com traços de fase ?\". Após o tratamento térmico de homogeneização, a liga 39 apresentou fase ?\" na forma celular enquanto a liga 66 apresentou as fases y0 e y e a liga 93 apresentou apenas fase y. As propriedades mecânicas das ligas foram avaliadas por ensaios de dureza e de dobramento simples. As amostras da Rota C apresentaram redução de dureza em relação à condição inicial. Todas as microestruturas das amostras laminadas a quente exibiram duas fases ricas em U. A liga 39 apresentou as fases ?\" na forma celular e ?\' após a laminação a quente. Após o recozimento final na rota C, a liga 39 apresentou fase ?\" na forma acicular enquanto as ligas 66 e 93 apresentaram as fases ?\" e y após a laminação e fase y. A fração de área da amostra pobre em U elevou-se nas ligas 39 e 66 e reduziu-se na liga 93. As amostras da Rota H apresentaram redução de dureza em relação à condição bruta de fusão. A liga 39 apresentou fase ?\" na forma celular com orientação e traços da fase ?, a liga 66 exibiu as fases y0 e y e a liga 93 as fases y e y0. Após o recozimento final, a liga 39 mostrou-se novamente na forma ?\" na forma celular, mas sem orientação. A liga 66 apresentou fase y e a liga 93 fase y0. Os testes de dobramento simples mostraram que as ligas da Rota C exibem plasticidade, retendo parte da deformação plástica após a ruptura das amostras testadas. Já as amostras da Rota H mostraram comportamento super elástico, possibilitando maiores deformações mas sem reter deformação plástica após a ruptura das amostras. A melhor relação entre deformação total e residual foi observada na liga 93 fabricada pela Rota C. As análises nos perfis de fratura das amostras da Rota C mostram fraturas transgranulares em todas as amostras. O perfil de fratura de na amostra recozida liga 39 mostra que a fase ?\" na forma acicular tende a deforma-se por deslizamento. As análises dos perfis de fratura nas amostras da Rota H confirmaram a ausência de deformação plástica mesmo em escala microscópica. Para essa condição, a fase ?\" na forma celular com orientação (liga 39) aparenta deformar-se por maclação. As análises de superfície de fratura indicam que a fase pobre em U tem participação durante o processo de crescimento e propagação da fratura na Rota H, atuando como caminho para bifurcação de trincas acelerando o processo de ruptura, enquanto na Rota C, a fase pobre em U deforma-se conjuntamente com a matriz de U. Em uma segunda etapa do trabalho, a estabilidade das microestruturas resultantes na amostras processadas foi investigada por Ensaios de Calorimetria Diferencial Exploratória (DSC) e por calorimetria de queda livre (esta apenas para a amostra 93 da rota H). O teor de Nb e Zr também afeta a estabilidade das fases presentes em cada amostra. foram realizados com as amostras da condição homogeneizada e laminada. A quantidade de transformações assim como o estado final de cada liga diferiu de acordo com a razão Nb/Zr. Após o ciclo de aquecimento e resfriamento da análise térmica, a liga 39 apresentou fase ?\', a liga 66 fase ?\" e a liga 93 fase y. No ensaio de calorimetria por queda livre foi possível observar as diferentes etapas de reação de envelhecimento da matriz g, correspondendo a à transformação y -> y0 (entre 525 e 530 K), a transformação y -> ?\". (entre 623 e 651 K) e à transformação y\' -> y3+? (entre 825 e 925 K). / Uranium alloys are candidates to be used as nuclear fuel in research reactors, among the U alloys, the Nb and Zr containing alloys are promising. This work evaluated how the Nb and Zr content and the thermomechanical processing affects the microstructure and mechanical properties of 3 alloys U-XNb-YZr were X+Y=12. Two 50g slugs of each sample were fabricated using plasma arc melting according to U-3Nb-9Zr (alloy 39), U-6Nb-6Zr (alloy 66) and U-9Nb-3Zr (alloy 93). One slug of each alloy was heat treated for 5h at 1000°C to perform the chemical homogenization. The homogenized sample and the as-cast one were encapsulated in the same steel frame in order to perform hot rolling. After the rolling process, the samples were annealed by 2h at 1000°C. The route that uses only as-cast samples was nominated \"Route C\" and the route that uses the homogenized sample was nominated \"Route H\". The microstructural characterization was performed by optical and scanning electron microscopy. All samples, regardless the processing route, presented Nb and Zr rich precipitates in addition to U rich matrix. The characterization of as-cast samples shows that the content of the alloying element has a direct influence on dendrite morphology as in the phases presented for each alloy. The alloy 39 presented predominantly ?\' phase, the alloy 66 the ?\" phase with a small quantity of ? phase and the alloy 93 presented the ? phase with small quantity of ?\" phase. Afte the homogenization, the alloy 39 presented cellular ?\" phase, the alloy 66 presented ?0 and ?, the alloy 93 presented only ? phase. The mechanical properties were evaluated by hardness measurements and free bending tests. The Route C samples presented hardness reduction in comparison to the initial condition. All microstructures of hot-rolled samples of this route exhibit two U rich phases. The alloy 39 exhibited cellular ?\" and ?\', after the final annealing the alloy 39 presented acicular ?\". The alloys 66 and 93 exhibited ?+?\" after hot rolling and ? phase after the final annealing. The area fraction of poor U phase increased in the alloys 39 and 66, but reduced in alloy 93. The Route H samples presented hardness reduction in comparison to as-cast samples. The alloy 39 presented cellular oriented ?\" phase and a small quantity of ? phase. The alloy 66 exhibited ?0 and ?, the alloy 93 ? and ?0. After the final annealing, the alloy 39 presented the ?\" again, but without orientation. The alloy 66 presented ? phase and the alloy 93 presented ?0. The free bending tests show that Route C samples have real plasticity, retaining part of deformation after rupturing as plastic strain. The Route H samples exhibited superelastic behavior, allowing higher deformations but retaining no plastic strain after sample breaking. The better balance between total and residual strain was observed in alloy 93 fabricated by Route C. The cracking profile analysis of Route C samples shows transgranular fractures in all samples. The Cracking profile of final 39 sample shows that acicular ?\" tends to deform by slipping. The cracking profile analysis of Route H samples confirmed the absence of plasticity even on the microscopic scale. This condition, the oriented cellular ?\" phase (alloy 39) apparently deforms by twinning. The crack surface analysis indicates that the U poor phase has a direct participation in crack growing and propagation, acting as forking points to the fracture and accelerating the fracture process. In the Route C samples, the poor U phase deforms alongside the U matrix. The stability of resulting microstructures of homogenized and hot rolled samples was investigated by Differential Scanning Calorimetry (DSC) and Drop Differential Scanning Calorimetry (only for the homogenized hot rolled 93 sample). The Nb and Zr also affect the stability of present phases in each sample. The number of transformations and the final structure is directly influenced by the Nb/Zr ratio. After the thermal cycle imposed by the DSC analysis, the alloy 39 exhibited ?\' phase, the alloy 66 exhibited ?\" phase and the alloy 93 exhibited ? phase. The Drop-DSC allowed observing the different stages of reaction in ? matrix, corresponding to ? -> ?0 (between 525 and 530 K), ? -> ?\" transformation (between 623 and 651 K) and ?\' -> ?3+? transformation (between 825 and 925 K).

The effect of thermo-mechanical processing by deformation and annealing on the grain boundary configuration of commercially pure Ni-200 is reported in this thesis. Ni-200 is unalloyed, thus avoiding the complex effects associated with alloying elements on the formation and development of different types of grain boundaries. One step strain-recovery with strain levels in the range of 3% to 7.5% (with 1.5% intervals) and annealing temperatures in the range of 800ºC to 1000ºC (with 100ºC intervals) were used in processing. The effects of parameters such as strain level, annealing temperature, annealing time and grain growth on grain boundary configurations were studied. Using Orientation Image Microscopy (OIM) it was found that the Fsp (fraction of special grain boundaries) value of strained samples annealed in the range of 800ºC to 1000ºC began to increase after a critical length of time, after which the Fsp value increased quickly and becoming a maximum in 2~4 minutes. The length of the critical annealing time for the increase of Fsp was shorter in the material with the higher levels of strain at a constant annealing temperature. Also the critical annealing time was shorter when annealed at higher temperatures under a fixed level of strain. The Fsp value increased to 80% from an as received value of about 30% in the samples with varying strain levels. However, the Fsp values only increased from 30% to 45% in the material without strain. Due to grain boundary migration, the Fsp values increased with grain size and became a maximum during the heat treatment of the strained material. In the material without strain however even when grain growth occurred, limited improvement in Fsp values occurred showing that contribution of strain is very important to the formation of special boundaries. By varying the strain levels, annealing temperatures and times, material with high Fsp values in a wide range of grain size can be obtained. Under the present processing conditions used however, multi-cycle was not helpful to the improvement of Fsp. TEM observations indicated dislocation tangles occurred near the grain boundary of the 1x6% strained samples. These dislocation tangles decreased with time at 800˚C and were reduced considerably after 20 minutes. Thermodynamic and kinetic models were used in the calculations of twin density-grain size relationships. The results indicated that the contribution of strain is equivalent to the increase of grain boundary energy, which provided an extra driving force and improved probability of twin embryo formation. / February 2009

This book has the introduction of the friction stir welding and friction stir processing, and introduces the newest development in FSW.Finding out the appropriate paraments of the grain size refinement in AZ31 Mg. The relationship between the resulting grain size and the applied working strain rate and temperature for the friction stir processing in AZ31 Mg is systemically examined. The Zener-Holloman parameter is utilized in rationalizing the relationship. The grain orientation distribution is also studied using the X-ray diffraction.

The effect of thermo-mechanical processing by deformation and annealing on the grain boundary configuration of commercially pure Ni-200 is reported in this thesis. Ni-200 is unalloyed, thus avoiding the complex effects associated with alloying elements on the formation and development of different types of grain boundaries. One step strain-recovery with strain levels in the range of 3% to 7.5% (with 1.5% intervals) and annealing temperatures in the range of 800ºC to 1000ºC (with 100ºC intervals) were used in processing. The effects of parameters such as strain level, annealing temperature, annealing time and grain growth on grain boundary configurations were studied. Using Orientation Image Microscopy (OIM) it was found that the Fsp (fraction of special grain boundaries) value of strained samples annealed in the range of 800ºC to 1000ºC began to increase after a critical length of time, after which the Fsp value increased quickly and becoming a maximum in 2~4 minutes. The length of the critical annealing time for the increase of Fsp was shorter in the material with the higher levels of strain at a constant annealing temperature. Also the critical annealing time was shorter when annealed at higher temperatures under a fixed level of strain. The Fsp value increased to 80% from an as received value of about 30% in the samples with varying strain levels. However, the Fsp values only increased from 30% to 45% in the material without strain. Due to grain boundary migration, the Fsp values increased with grain size and became a maximum during the heat treatment of the strained material. In the material without strain however even when grain growth occurred, limited improvement in Fsp values occurred showing that contribution of strain is very important to the formation of special boundaries. By varying the strain levels, annealing temperatures and times, material with high Fsp values in a wide range of grain size can be obtained. Under the present processing conditions used however, multi-cycle was not helpful to the improvement of Fsp. TEM observations indicated dislocation tangles occurred near the grain boundary of the 1x6% strained samples. These dislocation tangles decreased with time at 800˚C and were reduced considerably after 20 minutes. Thermodynamic and kinetic models were used in the calculations of twin density-grain size relationships. The results indicated that the contribution of strain is equivalent to the increase of grain boundary energy, which provided an extra driving force and improved probability of twin embryo formation.

The effect of thermo-mechanical processing by deformation and annealing on the grain boundary configuration of commercially pure Ni-200 is reported in this thesis. Ni-200 is unalloyed, thus avoiding the complex effects associated with alloying elements on the formation and development of different types of grain boundaries. One step strain-recovery with strain levels in the range of 3% to 7.5% (with 1.5% intervals) and annealing temperatures in the range of 800ºC to 1000ºC (with 100ºC intervals) were used in processing. The effects of parameters such as strain level, annealing temperature, annealing time and grain growth on grain boundary configurations were studied. Using Orientation Image Microscopy (OIM) it was found that the Fsp (fraction of special grain boundaries) value of strained samples annealed in the range of 800ºC to 1000ºC began to increase after a critical length of time, after which the Fsp value increased quickly and becoming a maximum in 2~4 minutes. The length of the critical annealing time for the increase of Fsp was shorter in the material with the higher levels of strain at a constant annealing temperature. Also the critical annealing time was shorter when annealed at higher temperatures under a fixed level of strain. The Fsp value increased to 80% from an as received value of about 30% in the samples with varying strain levels. However, the Fsp values only increased from 30% to 45% in the material without strain. Due to grain boundary migration, the Fsp values increased with grain size and became a maximum during the heat treatment of the strained material. In the material without strain however even when grain growth occurred, limited improvement in Fsp values occurred showing that contribution of strain is very important to the formation of special boundaries. By varying the strain levels, annealing temperatures and times, material with high Fsp values in a wide range of grain size can be obtained. Under the present processing conditions used however, multi-cycle was not helpful to the improvement of Fsp. TEM observations indicated dislocation tangles occurred near the grain boundary of the 1x6% strained samples. These dislocation tangles decreased with time at 800˚C and were reduced considerably after 20 minutes. Thermodynamic and kinetic models were used in the calculations of twin density-grain size relationships. The results indicated that the contribution of strain is equivalent to the increase of grain boundary energy, which provided an extra driving force and improved probability of twin embryo formation.

Dual-phase (DP) advanced high-strength steels (AHSSs) are widely used in the automotive industry due to their excellent combination of strength, ductility, and work hardening properties. However, defects occurring during processing make these ferrous alloys expensive. Toward this ends, high-temperature tensile tests using a Gleeble thermomechanical simulator have been conducted to determine the stress/strain behaviour at temperatures between 1250 to 1480 C in order to quantify the tensile strength and ductility. The results of both as-cast and transfer-bar material will be presented as well as three different sample geometries in order to better understand the effects of starting microstructure, thermal gradient, and tress/strain distribution on the reproducibility of high temperature properties. Optical and scanning electron microscopy are then performed to further elucidate the structure/property relationships. The results show that the presence of preexisted prorosities in the as-cast structure decreases the high-temperature strength of the material, while the transfer-bar samples show lower ductility at ultra-high temperatures, (T 1450 C), due to their severe susceptibility to melting. In terms of the two mentioned thermomechanical characteristics, voids nucleation, growth, and coalescence initiated with porosity clustering are the main mechanisms behind the lower strength of the as-cast samples, whilst tearing apart of the melt plays an important role to drastically drop the ductility of transfer-bars at mentioned temperature interval. Moreover, the long-gauge-length (LGL) geometry proposes better reproducibility of data compared with the other geometries. This is attributed to a suitable combination between low stress localization and high thermal gradient during the Gleeble testing that provides a condition in which the samples experience sharp localized necking right on the hot-spot zone. The obtained data can be used as part of multi-physics process and microstructure continuous casting models. / Thesis / Master of Applied Science (MASc)

Metal additive manufacturing stands poised to disrupt multiple industries with high material use efficiency and complex part production capabilities, however many technologies deposit material with sub-optimal properties, limiting their use. This decrease in performance largely stems from porosity laden parts, and asymmetric solidification-based microstructures. Solid-state additive manufacturing techniques bypass these flaws, using deformation and diffusion phenomena to bond material together layer by layer. Among these techniques, Additive Friction Stir Deposition (AFSD), stands out as unique for its freeform nature, and thermomechanical conditions during material processing. Leveraging its solid-state behavior, optimized microstructures produced by AFSD can reach performance levels near, at, or even above traditionally prepared metals. A strong understanding of the material conditions during AFSD and the phenomena responsible for microstructure evolution. Here we discuss two works aimed at improving the state of knowledge surrounding AFSD, promoting future microstructure optimization. First, a parametric study is performed, finding a wide array of producible microstructures across two material systems. In the second work, a stop-action type experiment is employed to observe the dynamic microstructure evolution across the AFSD material flow pathway, finding specific thermomechanical regimes that occur within. Finally, multiple conventional alloy systems are discussed as their microstructure evolution pertains to AFSD, as well as some more unique systems previously limited to small lab scale techniques, but now producible in bulk due to the additive nature of AFSD. / Doctor of Philosophy / The microstructure of a material describes the atomic behavior at multiple length scales. In metals this microstructure generally revolves around the behavior of millions of individual crystals of metal combined to form the bulk material. The state and behavior of these crystals and the atoms that make them up influence the strength and usability of the material and can be observed using various high fidelity characterization techniques. In metal additive manufacturing (i.e. 3D printing) the microstructure experiences rapid and severe changes which can alter the final properties of the material, typical to a detrimental effect. Given the other benefits of additive manufacturing such as reduced costs and complex part creation, there is desire to predict and control the microstructure evolution to maximize the usability of printed material. Here, the microstructure evolution in a solid-state metal additive manufacturing, Additive Friction Stir Deposition (AFSD), is investigated for different metal material systems. The solid-state nature of AFSD means no melting of the metal occurs during processing, with deformation forcing material together layer by layer. The conditions experienced by the material during printing are in a thermomechanical regime, with both heating and deformation applied, akin to common blacksmithing. In this work specific microstructure evolution phenomena are discussed for multiple materials, highlighting how AFSD processing can be adjusted to change the resulting microstructure and properties. Additionally, specific AFSD process interactions are studied and described to provide better insight into cumulative microstructure evolution throughout the process. This work provides the groundwork for investigating microstructure evolution in AFSD, as well as evidence and results for a number of popular metal systems.

Additive friction stir deposition (AFSD) is an emerging solid-state metal additive manufacturing technology that uses deformation bonding to create near-net shape 3D components. As a developing technology, a deeper understanding of the processing science is necessary to establish the process-structure relationships and enable improved control of the as-printed microstructure and material properties. AFSD provides a unique opportunity to explore the friction stir fundamentals via direct observation of the material during processing. This work explores the relationship between the processing parameters (e.g., tool rotation rate Ω, tool velocity V, and material feed rate F) and the thermomechanical history of the material by process monitoring of i) the temperature evolution, ii) the force evolution, and iii) the interfacial contact state between the tool and deposited material. Empirical trends are established for the peak temperature with respect to the processing conditions for Cu and Al-Mg-Si, but a key difference is noted in the form of the power law relationship: Ω/V for Cu and Ω2/V for Al-Mg-Si. Similarly, the normal force Fz for both materials correlates to V and inversely with Ω. For Cu both parameters show comparable influence on the normal force, whereas Ω is more impactful than V for Al-Mg-Si. On the other hand, the torque Mz trends for Al-Mg-Si are consistent with the normal force trends, however for Cu there is no direct correlation between the processing parameters and the torque. These distinct relationships and thermomechanical histories are directly linked to the contact states observed during deformation monitoring of the two material systems. In Cu, the interfacial contact between the material and tool head is characterized by a full slipping condition (δ=1). In this case, interfacial friction is the dominant heat generation mechanism and compression is the primary deformation mechanism. In Al-Mg-Si, the interfacial contact is characterized by a partial slipping/sticking condition (0<δ<1), so both interfacial friction and plastic energy dissipation are important mechanisms for heat generation and material deformation. Finally, an investigation into the contact evolution at different processing parameters shows that the fraction of sticking is critically dependent on the processing parameters which has many implications on the thermomechanical processing history. / Doctor of Philosophy / Additive manufacturing or three-dimensional (3D) printing technologies have been lauded for their ability to fabricate complex geometries and multi-material parts with reduced material waste. Of particular interest is the use of metal additive manufacturing for repair and fabrication of industrial and structural components. This work focuses on characterizing the thermomechanical processing history for a developing technology Additive Friction Stir Deposition (AFSD). AFSD is solid-state additive manufacturing technology that uses frictional heat and mechanical mixing to fabricate 3D metal components. From a fundamental materials science perspective, it is imperative to understand the processing history of a material to be able to predict the performance and properties of a manufactured part. Through the use of infrared imaging, thermocouples, force sensors, and video monitoring this work is able to establish quantitative relationships between the equipment processing parameters and the processing history for Cu and Al. This work shows that there is a fundamental difference in how these two materials are processed during AFSD. In the future, these quantitative relationships can be used to validate modeling efforts and improve manufacturing quality of parts produced via friction stir techniques.