A combinatorial study was carried out for hydrogen storage alloys which involve processes similar to those normally used in their fabrication. The study utilized a single sample of combined elemental (or compound) powders which were milled and consolidated into a bulk form and subsequently deformed to heavy strains. Material library was obtained in a post annealing treatment carried out at elevated temperatures which brings about solid state reactions between the powders yielding equilibrium phases in the respective alloy system. A sample comprising the material library was then pulverized and screened for hydrogen storage composition. X-ray diffraction was used as a screening tool, the sample having been examined both in as-processed and hydrogenated state. The method was successfully applied to Mg-Ni, and Mg-Ni-Ti yielding the well known Mg2Ni as the storage composition. It is concluded that partitioning of the alloy system into regions of similar solidus temperature would be required to enrich the material library.

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES / This work investigated the effect of different types of homogenization on the microstructure and the cold deformation behavior of Ti-35Nb-0,15Si alloy. Homogenization was performed under two conditions. Condition 1: treatment in ambient air at 1000 °C for 8, 24, 48, 72, 96 and 120 hours. Condition 2: treatment in argon atmosphere at 1000 °C for 8 hours. For the cold deformation study samples of the Ti-35Nb-0,15Si alloy and samples of Ti CP were deformed by ECAP with up to 8 passes, using the routes A and BC in a matrix with angle of intersection between the channels of Φ = 120º. The microstructural characterization was performed in the internal and external regions with the aid of optical microscopy, scanning electron microscopy and X-ray diffractograms. Vickers microhardness measurements were performed to evaluate the changes caused by deformation. In the ambient air atmosphere the samples showed the presence of the oxide layer influencing the hardness and the level of cold deformation. With the deformation of Ti-35Nb-0,15Si by ECAP it was possible to refine the structure and increase the hardness with increasing the number of passes. XRD analysis showed the presence of the α” phase induced by deformation. With the Ti CP deformed by ECAP, it was possible to analyze the microstructural evolution throughout the sample. / Este trabalho investigou o efeito de diferentes tipos de homogeneização sobre a microestrutura e o comportamento em deformação a frio da liga Ti-35Nb-0,15Si. A homogeneização foi realizada em duas condições. Condição 1: tratamento em atmosfera de ar ambiente na temperatura 1000 °C por 8, 24, 48, 72, 96 e 120 horas. Condição 2: tratamento em atmosfera inerte de argônio de 1000 °C por 8 horas. Para o estudo de deformação a frio, amostras da liga Ti-35Nb-0,15Si e amostras de Ti CP foram deformadas via ECAP com até 8 passes, utilizando as rotas A e BC numa matriz com ângulo de intersecção entre os canais de Φ = 120º. A caracterização microestrutural foi realizada nas regiões internas e externas com o auxílio de microscopia óptica, microscopia eletrônica de varredura e difratogramas de raios-X. Medidas de microdureza Vickers foram realizadas para avaliar as mudanças ocasionadas pela deformação. Em atmosfera de ar ambiente as amostras apresentaram a presença da camada de óxido influenciando na dureza e no nível de deformação a frio. Com a deformação de Ti-35Nb-0,15Si por ECAP foi possível refinar a estrutura e aumentar a dureza com o aumento do número de passes. A análise de DRX mostrou a presença da fase α’’ induzida por deformação. Com o Ti CP deformado por ECAP foi possível analisar a evolução microestrutural ao longo da amostra. / São Cristóvão, SE

Ultrafeinkörnige metallische Werkstoffe haben verstärkt wissenschaftliche Bedeutung erlangt. Um dieser neuartigen Werkstoffklasse über die grundlagenorientierte Forschung hinaus einen Einsatz in technischen Anwendungen zu ermöglichen, ist es notwendig, deren Verhalten unter verschiedenen einsatzrelevanten Belastungsbedingungen vorhersagen zu können. In der vorliegenden Arbeit wird das Schädigungsverhalten einer ultrafeinkörnigen Aluminiumlegierung in den Bereichen der hochzyklischen (HCF) und niedrigzyklischen (LCF) Ermüdung sowie des Rissfortschritts untersucht. Im Mittelpunkt steht dabei die Identifikation der mikrostrukturell wirksamen Mechanismen bei der Entstehung und Ausbreitung von Ermüdungsrissen. Es werden ein homogen ultrafeinkörniger und ein bimodaler Zustand sowie verschiedene duktilitätsoptimierte Zustände betrachtet und systematisch der Einfluss der Korngröße, der Korngrößenverteilung, der Ausscheidungscharakteristik sowie der Festigkeit und Duktilität auf das Ermüdungs- und Rissfortschrittsverhalten ermittelt. Die Untersuchungen zeigen, dass das Schädigungsverhalten der ultrafeinkörnigen Aluminiumlegierung insbesondere durch die Korngröße und Korngrößenverteilung sowie den Kohärenzgrad der festigkeitssteigernden Ausscheidungen beeinflusst wird.

Made available in DSpace on 2016-03-15T19:36:54Z (GMT). No. of bitstreams: 1 Maria Claudia Lopes Guerra.pdf: 9968717 bytes, checksum: 7d0e4986884ffa382a835b641ed76573 (MD5) Previous issue date: 2015-06-12 / Fundo Mackenzie de Pesquisa / The ECAP (Equal Channel Angular Pressing) is a mechanical process of Severe Plastic Deformation (SPD) where a sample is subjected to a shearing force when passing through the region of intersection of two channels. The main goal of this method is Severe Plastic Deformation achieve a microstructure with ultrafine grains, which have much higher than the equivalent coarse grain materials physical properties, such as an increase in strength and toughness simultaneously. What makes this increasingly interesting technique is that as there is no reduction cross section is possible to obtain plastic strain accumulation and therefore gain in grain order of nanometer scale. The great advantage of ECAP is to achieve a much higher degree of strain hardening than obtained by conventional methods of plastic deformation, and consequently a grain refining much higher as well. The importance of the study of severe plastic deformation process is on improving the mechanical performance of the materials and the possibility of a better understanding of the mechanisms of strain hardening, which may indicate a new path for producing high-strength materials, possibly scaled industrial. In this work are presented the microstructural, mechanical and electrical analysis of the aluminum alloy AA 1050 samples, commonly used for electrical purposes, with ultrafine grains (typical grain size below a micron) resulting from processing by ECAP, based on the method of SPD. / A PCE (Prensagem em Canais Equiangulares) consiste num processo mecânico de Deformação Plástica Intensa (DPI) onde um corpo de prova é sujeito a um esforço de cisalhamento ao passar pela região de intersecção de dois canais. Os principais objetivos desse método de Deformação Plástica Intensa é alcançar uma microestrutura com grãos ultrafinos, os quais possuem propriedades físicas muito superiores aos equivalentes materiais de grãos grosseiros, como um aumento em resistência mecânica e tenacidade simultâneas. O que torna esta técnica cada vez mais interessante é que como não há redução da seção transversal é possível obter acumulo de deformação plástica e com isso obter grãos na ordem de escala nanométrica. A grande vantagem do PCE é alcançar um grau de encruamento muito superior do que obtido por métodos convencionais de deformação plástica, e consequentemente, um refino de grão muito superior também. A importância do estudo do processo de deformação plástica intensa está na melhoria do desempenho mecânico dos materiais e na possibilidade de uma melhor compreensão dos mecanismos de encruamento, fato que pode indicar um novo caminho para a produção de materiais de alta resistência mecânica, possivelmente em escala industrial. Nesse trabalho são apresentadas as análises microestruturais, mecânicas e elétricas de amostras de ligas de alumínio AA 1050, comumente utilizadas para fins elétricos, com estrutura de grãos ultrafinos (tamanho de grão típico abaixo de um micrometro) resultantes do processamento por PCE, baseada no método de DPI.

Ultrafeinkörnige metallische Werkstoffe haben verstärkt wissenschaftliche Bedeutung erlangt. Um dieser neuartigen Werkstoffklasse über die grundlagenorientierte Forschung hinaus einen Einsatz in technischen Anwendungen zu ermöglichen, ist es notwendig, deren Verhalten unter verschiedenen einsatzrelevanten Belastungsbedingungen vorhersagen zu können. In der vorliegenden Arbeit wird das Schädigungsverhalten einer ultrafeinkörnigen Aluminiumlegierung in den Bereichen der hochzyklischen (HCF) und niedrigzyklischen (LCF) Ermüdung sowie des Rissfortschritts untersucht. Im Mittelpunkt steht dabei die Identifikation der mikrostrukturell wirksamen Mechanismen bei der Entstehung und Ausbreitung von Ermüdungsrissen. Es werden ein homogen ultrafeinkörniger und ein bimodaler Zustand sowie verschiedene duktilitätsoptimierte Zustände betrachtet und systematisch der Einfluss der Korngröße, der Korngrößenverteilung, der Ausscheidungscharakteristik sowie der Festigkeit und Duktilität auf das Ermüdungs- und Rissfortschrittsverhalten ermittelt. Die Untersuchungen zeigen, dass das Schädigungsverhalten der ultrafeinkörnigen Aluminiumlegierung insbesondere durch die Korngröße und Korngrößenverteilung sowie den Kohärenzgrad der festigkeitssteigernden Ausscheidungen beeinflusst wird.

Industrial products of high-strength Al-alloys are currently manufactured by thermo-mechanical processes, which are only applicable in the integrated plants requiring high investment cost. Moreover, reduction of the average grain size not less than 10 &mu / m and re-adjustment of process parameters for each alloy type is evaluated as disadvantage. Therefore, recently there have been many research studies for development of alternative manufacturing techniques for aluminum alloys. Research activities have shown that it is possible to improve the strength of Al-alloys remarkably by severe plastic deformation which results in ultra-fine grain size. This study aims to design and manufacture the laboratory scale set-ups for severe plastic deformation of aluminum alloys, and to characterize the severely deformed samples. The stages of the study are summarized below: First, for optimization of die design and investigation of parameters affecting the deformation finite element modeling simulations were performed. The effects of process parameters (die geometry, friction coefficient) and material properties (strain hardening, strain-rate sensitivity) were investigated. Next, Equal Channel Angular Pressing (ECAP) system that can severely deform the rod shaped samples were designed and manufactured. The variations in the microstructure and mechanical properties of 2024 Al-alloy rods deformed by ECAP were investigated. Finally, based on the experience gained, a Dissimilar Channel Angular Pressing (DCAP) system for severe plastic deformation of flat products was designed and manufactured / then, 6061 Al-alloy strips were deformed. By performing hardness and tension tests on the strips that were deformed by various passes, the capability of the DCAP set-up for production of ultra-fine grain sized high-strength aluminum flat samples were investigated.

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES / This investigated the use of equiangular channel press (ECAP) in samples of pure niobium at room temperature up to 14 passes, using the Bc route, with a matrix with intersection angle between the channels of θ = 90º and 120º, with and curvature angle Ψ = 0°. During ECAP (equal channel angular pressing) deformation a bar is pressed through a rigid matrix consisting of two channels of the same cross-section, which intersect at an angle θ. The microstructure of the deformed samples has been analyzed with the aid of optic microscopy, scanning electron microscopy and Vickers Hardness (HV). With the deformation of pure niobium through ECAP, it was possible to refine the structure and increase the hardness due to the increase of the number of passes and the type of matrix. The results indicated that deformation of the niobium with a pass in the matrices of 90 ° and 120 ° was enough to produce the refinement of the microstructure and practically double the hardness values in relation to the material without deformation. The maximum microstructural refinement, steady state, occurred with 8 passes in the 120 ° matrix and 6 passes in the 90 ° matrix, indicating a higher deformation severity of the last matrix. The microstructures analyzed by scanning electron and optical microscopes revealed the microstructural changes with the increase of the number of passes and the type of matrix. / Este trabalho investigou o uso da prensagem em canais equiangulares (ECAP) em amostras de nióbio puro na temperatura ambiente até 14 passes, utilizando a rota Bc, com matrizes contendo ângulo de intersecção entre os canais de θ = 90º e 120°. Durante a deformação ECAP uma barra é pressionada através de uma matriz rígida consistindo de dois canais de mesma seção transversal, os quais se interceptam a um ângulo θ. A microestrutura das amostras deformadas foi analisada com auxílio de microscopia óptica, microscopia eletrônica de varredura e dureza Vickers (HV). Com a deformação do nióbio puro através do ECAP foi possível refinar a estrutura e aumentar a dureza em função do aumento do número de passes e do tipo de matriz. Os resultados indicaram que deformação do nióbio com um passe, nas matrizes de 90º e 120°, foi suficiente para produzir o refinamento da microestrutura e praticamente dobrar os valores de dureza em relação ao material sem deformação. O refinamento microestrutural máximo, estado estacionário, ocorreu com 8 passes na matriz de 120° e 6 passes na matriz de 90°, indicando maior severidade de deformação da última matriz. As microestruturas analisadas por microscopias ótica e eletrônica de varredura revelaram as mudanças microestruturais com o aumento do número de passes e com o tipo de matriz. / São Cristóvão, SE

Magnesium alloys have poor formability at room temperature, due to a limited number of slip systems owing to the hexagonal closed packed structure of magnesium. One possibility to increase the formability of magnesium alloys is to refine the grain size. A fine grain magnesium alloy shows high strength and high ductility at room temperature, hence an improved formability. In addition to grain refinement, the formability of Mg alloys can be improved by controlling crystallographic texture. Severe plastic deformation (SPD) processes namely, equal channel angular pressing (ECAP) and multi-axial forging (MAF) have led to improvement in room temperature mechanical property of magnesium alloys. Further, it has been reported that by adding rare earth elements, room temperature ductility is enhanced to nearly 30%. The increase in property is attributed to crystallographic texture. Many rare earth elements have been added to magnesium alloys and new alloy systems have been developed. Amongst these elements, Ce addition has been shown to enhance the tensile ductility in rolled sheets at room temperature by causing homogeneous deformation. It has been observed that processing of rare-earth containing alloys below 300°C is difficult. Processing at higher temperatures leads to grain growth which ultimately leads to low strength at room temperature. The present thesis is an attempt to combine the effect SPD and rare earth addition, and to examine the overall effect on microstructure and texture, hence on room temperature mechanical properties. In this thesis, Mg-0.2%Ce alloy has been studied with regard to the two SPD processes, namely, ECAP and MAF. The thesis has been divided into six chapters. Chapter 1 is dedicated to introduction and literature review pertaining to different severe plastic deformation processes as applied to different Mg alloys. Chapter 2 includes the details of experimental techniques and characterization procedures, which are commonly employed for the entire work. Chapter 3 addresses the effect of ECAP on the evolution of texture and microstructure in Mg-0.2%Ce alloy. ECAP has been carried out on two different initial microstructure and texture in the starting condition, namely forged and extruded. ECAP has been successfully carried out for the forged billets at 250°C while cracks get developed in the extruded billet when ECAP was done at 250°C. The difference in the deformation behaviour of the two alloys has been explained on the basis of the crystallographic texture of the initial materials. The microstructure of the ECAP materials indicates the occurrence of recrystallization. The recrystallization mechanism is identified as “continuous dynamic recovery and recrystallization” (CDRR) and is characterized by a rotation of the deformed grains by ~30⁰ along c-axis. The yield strengths and ductility of the two ECAP materials have been found quite close. However, there is a difference in the yield strength as well as ductility values when the materials were tested under compression. The extruded billet has the tension compression asymmetry ~1.7 while the forged material has the asymmetry as ~2.2. After ECAP, the yield asymmetry reduces to ~1 for initially extruded billet, while for the initially forged billet the yield asymmetry value reduces to ~1.9. In chapter 4, the evolution of microstructure and texture was examined using another severe plastic deformation technique, namely multi axial forging (MAF). In this process, the material was plastically deformed by plane strain compression subsequently along all three axes. In this case also two different initial microstructures and texture were studied, namely the material in as cast condition and the extruded material. The choice of initial materials in this case was done in order to examine the effect of different initial grain size in addition to different textures. By this method, the alloy Mg-0.2%Ce could be deformed without fracture at a minimum temperature of 350⁰C leading to fine grain size (~3.5 µm) and a weak texture. Grain refinement was more in the initial cast billets compared to the initial extruded billet after processing. The mechanism of grain refinement has been identified as twin assisted dynamic recrystallization (TDRX) and CDRR type. The mechanical properties under tension as well as under compression were also evaluated in the present case. The initially extruded billet has shown low tension compression asymmetry (~1.2) than cast billet (~1.9), after MAF. Chapter 5 addresses the exclusive effect of texture on room temperature tensile properties of the alloy. Different textures were the outcomes of ECAP and MAF processes. In this case, in order to obtain an exact role of texture, a third of deformation mode, rolling, was also introduced. All the processed materials were annealed to obtain similar grain size but different texture. A similar strength and ductility for ECAP and MAF, where the textures were qualitatively very different, was attributed to the fact that texture of both the ECAP and MAF processed materials, was away from the ideal end orientation for tensile tests. In chapter 7, the final outcomes of the thesis have been summarized and scope for the future work has been presented.