High Pressure Torsion (HPT) is one of the most widely used severe plastic deformation methods which enable to obtain a crack free ultra-fine grained bulk material with improved mechanical properties like increased strength and toughness. In the process, a disc shaped sample is pressed between two anvils and deformed via surface friction forces by rotating one of the anvils. The aim of this study is to nondestructively characterize the variations in the deformation uniformity of the severely deformed steel disks. Two sets of low carbon steel samples were obtained by applying the unconstrained and constrained HPT process up to 6 turns. Magnetic Barkhausen Noise (MBN) method was used in order to evaluate the samples in a nondestructive manner via a commercial device. The results of the MBN measurements were verified with those of conventional methods such as / x-ray diffraction (XRD), metallographic examination and hardness measurements. The initial stages of HPT revealed the effects of conventional plastic deformation on MBN / however with further straining, grain size refinement prevailed and caused increase in MBN signals.

Kyoto University (京都大学) / 0048 / 新制・課程博士 / 博士(工学) / 甲第18986号 / 工博第4028号 / 新制||工||1620 / 31937 / 京都大学大学院工学研究科材料工学専攻 / (主査)教授 辻 伸泰, 教授 田中 功, 教授 乾 晴行 / 学位規則第4条第1項該当

京都大学 / 0048 / 新制・課程博士 / 博士(工学) / 甲第18986号 / 工博第4028号 / 新制||工||1620(附属図書館) / 31937 / 京都大学大学院工学研究科材料工学専攻 / (主査)教授 辻 伸泰, 教授 田中 功, 教授 乾 晴行 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DFAM

京都大学 / 0048 / 新制・課程博士 / 博士(工学) / 甲第20336号 / 工博第4273号 / 新制||工||1662(附属図書館) / 京都大学大学院工学研究科材料工学専攻 / (主査)教授 辻 伸泰, 教授 松原 英一郎, 教授 乾 晴行 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DFAM

Cette étude porte principalement sur l’influence de déformations plastiques sévères réalisées par torsion sous forte pression (ou HPT) sur différentes natures de poudres de magnésium pour la modification des propriétés d’absorption de l’hydrogène de Mg. La nature différente des poudres a été obtenue soit par un procédé d'atomisation de gaz, soit par un procédé d'évaporation/condensation par plasma d'arc. Ces poudres ont été consolidées en produits en vrac par un procédé HPT en deux étapes. Parmi les poudres composites étudiées, la poudre de magnésium contenant du graphène a montrée d’excellentes propriétés d’absorption de l’hydrogène correspondant à des cinétiques d’activation plus rapides. Un avantage significatif du procédé HPT est de briser les couches d’oxyde MgO, imperméables au passage de l’hydrogène et de venir les disperser uniformément avec les additifs dans le Mg. Par l’introduction de défauts cristallins associés à un affinement microstructural, le procédé HPT a permis d’obtenir des améliorations significatives dès le premier cycle d’hydrogénation pour les poudres consolidées de Mg par rapport aux poudre initiales, tandis que des résultats inverses ont été obtenus au sein de la poudre dopée au C et déformée par HPT. Un autre impact du procédé HPT a été de réduire l’hystérésis entre les plateaux de pression d’absorption et de résorption au cours des essais PCT (pressure-composition-temperature). De plus, il a été observé que le procédé HPT réduit de manière drastique la température de résorption pour toutes les combinaisons de poudres tandis que le taux de résorption de l’hydrogène a été légèrement diminué pour les produits consolidés. Toutefois, l’inconvénient majeur du procédé HPT, indépendamment de la nature des composés étudiés, est qu’il altère systématiquement la capacité de stockage maximum des poudres initiales. / The present work mainly focuses on the effects of severe plastic deformation through high-pressure torsion (HPT) of different nature of magnesium based powders on improving the hydrogen sorption properties of Mg. The different nature of powders was obtained by either a gas-atomization process or an arc-plasma evaporation/condensation method. These powders were consolidated into bulk products by a two-step HPT process. Among the studied powder composites, the Mg/graphene based powder demonstrated excellent hydrogen sorption properties representing faster activation kinetics. A significant advantage of the HPT processing was to break the impervious MgO oxide layers, and to disperse them uniformly along with catalytic additives within the Mg domains. Through the introduction of structural defects and microstructural refinement, the HPT processing has allowed significant improvements in the first hydrogenation kinetics for the consolidated Mg products compared to their initial powder precursors while it was reverse for the C-doped HPT products. Another significant impact of the HPT processing was to reduce the hysteresis between the absorption and desorption plateau pressures during the pressure-composition-temperature (PCT) experiments. Moreover, it was revealed that the HPT processing has drastically reduced the hydrogen desorption temperatures for all the powder combinations while the rate of dehydrogenation was slightly diminished for their consolidated products. Nevertheless, the major drawback of the HPT processing, irrespective of the nature of studied composites, was that it always impaired the maximum hydrogen storage capacity of the starting powder precursors.

Submitted by Aelson Maciera (aelsoncm@terra.com.br) on 2017-08-16T19:31:06Z No. of bitstreams: 1 DissDAGP.pdf: 24957220 bytes, checksum: d8c9cd6b22c7e40f1a1f5c7c88deb93a (MD5) / Approved for entry into archive by Ronildo Prado (bco.producao.intelectual@gmail.com) on 2018-01-30T16:50:04Z (GMT) No. of bitstreams: 1 DissDAGP.pdf: 24957220 bytes, checksum: d8c9cd6b22c7e40f1a1f5c7c88deb93a (MD5) / Approved for entry into archive by Ronildo Prado (bco.producao.intelectual@gmail.com) on 2018-01-30T16:50:13Z (GMT) No. of bitstreams: 1 DissDAGP.pdf: 24957220 bytes, checksum: d8c9cd6b22c7e40f1a1f5c7c88deb93a (MD5) / Made available in DSpace on 2018-01-30T16:57:24Z (GMT). No. of bitstreams: 1 DissDAGP.pdf: 24957220 bytes, checksum: d8c9cd6b22c7e40f1a1f5c7c88deb93a (MD5) Previous issue date: 2017-03-03 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / Biomedical devices currently in use (prostheses, implants) have satisfactory performance in many cases. However, sometimes the body reacts to the device insertion and may lead to its rapid replacement. Some of these disadvantages can be solved by the use of titanium and its alloys, due to their excellent combination of corrosion resistance, wear resistance and biocompatibility compared to other competing biomaterials. This work presents the possibility of obtaining near β titanium alloy with ultrafine grains produced by severe plastic deformation. For this, the Ti-13Nb-13Zr alloy was processed by high-pressure torsion processing method. Samples were processed with different loads and number of turns. The samples were evaluated by Vickers microhardness. As-received and deformed samples were analyzed through X-Ray diffraction. The microstructures were observed by optical microscopy and scanning electron microscope and the microtexture and phase mappings of the material evaluated through the ASTAR equipment in the transmission electron microscope. After characterization, it was observed that there is a refinement of the microstructure and increase of the microhardness of the Ti-13Nb-13Zr alloy deformed by HPT. Due to the superior microhardness of the deformed material and the results of phase transformations indicate a potential application as nanostructured biomaterial. / Os dispositivos biomédicos utilizados atualmente (próteses, implantes) possuem desempenho satisfatório em muitos casos. No entanto, às vezes, o corpo reage à inserção destes dispositivos exigindo a sua rápida substituição. Algumas destas desvantagens podem ser resolvidas pelo uso de titânio e suas ligas, devido à sua excelente combinação de resistência à corrosão, resistência ao desgaste e biocompatibilidade em comparação com outros biomateriais concorrentes. Este trabalho apresenta a possibilidade de obtenção de liga de titânio quase β com grãos ultrafinos produzidos por deformação plástica severa para três diferentes condições iniciais de microestrutura. Para isso, a liga Ti-13Nb-13Zr foi processada pelo método de processamento de torção sob alta pressão (High-Pressure Torsion - HPT). As amostras foram processadas com diferentes cargas e número de voltas e avaliadas por meio de microdureza Vickers. Amostras como recebidas e deformadas foram analisadas através de difração de raios X. As microestruturas foram observadas por meio de microscopia óptica e eletrônica de varredura. A microtextura e mapeamentos de fase do material foram avaliados através do equipamento ASTAR no microscópio eletrônico de transmissão. Após a caracterização, foi observado que existe um refinamento da microestrutura e aumento da microdureza da liga Ti-13Nb-13Zr deformada por HPT. A microdureza superior do material deformado e os resultados de transformações de fase apontam para uma potencial aplicação como biomaterial nanoestruturado.

Les procédés d’hyper-déformations (SPD) peuvent imposer de très grandes déformations à un métal et en transformer les propriétés métallurgiques de la matière en introduisant une forte densité de dislocations et un important affinement de la microstructure. Dans ce travail de thèse présenté, des expériences en torsion à haute pression (HPT) ont été réalisées pour la consolidation des différentes poudres de fer de taille à l’échelle nano et micrométrique. Ces expériences ont été effectuées avec succès à la température ambiante aboutissant à la fois à un faible niveau de porosité résiduelle et l'affinement significatif de la taille de grain, grâce à une importante déformation en cisaillement et à de la pression hydrostatique appliquée au procédé HPT. La compression a été faite en deux étapes: d'abord une compression axiale, puis déformation en cisaillement en tournant la partie inférieure de la filière HPT tout en maintenant constante la force axiale. L'homogénéité de la déformation en cisaillement à travers l'épaisseur du disque a été examinée par une mesure de déformation locale, qui montre une distribution du gradient. L'analyse par diffraction à rayons X a été réalisée sur des échantillons consolidés qui ont révélé une proportion peu importante d’oxydes. L'effet de la déformation en cisaillement sur la microstructure et la texture a été étudié par microscopie électronique à balayage et EBSD. La micro-dureté et la porosité moyenne des échantillons en fonction de la déformation en cisaillement, à pression hydrostatique constante, ont également été mesurées. Une trame de modélisation mise en œuvre dans le modèle de Taylor a été développée pour simuler l'effet du glissement aux joints de grains pour l'évolution de la texture cristallographique. Le principal effet constaté est un décalage des orientations idéales dans les conditions de cisaillement simple, ce qui a été vérifié expérimentalement. Le procédé de consolidation par HPT a été simulé numériquement en utilisant la méthode des éléments finis pour un modèle de plasticité des poudres. La simulation de ce dernier a permis de confirmer la porosité résiduelle moyenne observée expérimentalement et les différents gradients de la déformation plastique. La distribution de la densité locale a également été modélisée / Severe plastic deformation (SPD) processes can impose extremely large strains to a metal and transforming the metallurgical state of the material by introducing high dislocation density and high level of microstructure refinement. In the present thesis work High Pressure Torsion (HPT) experiments were performed for consolidation of different powders including Nano- and Micro- scaled iron powders. The experiments were carried out successfully at room temperature, achieving both low level of residual porosity and significant grain refinement, thanks to the intense shear strain and hydrostatic pressure applied in HPT. The compaction was done in two steps: first axial compaction, then shear deformation by rotating the bottom part of the HPT die while maintaining the axial force constant. The homogeneity of shear strain across the thickness of the disk was examined by local strain measurement, showing a gradient distribution. X-ray diffraction analysis was carried out on the consolidated samples which revealed no significant proportion of oxides. The effect of shear deformation on the microstructure and texture was investigated by metallographic scanning electron microscopy and electron backscattered diffraction (EBSD). The micro-hardness and average porosity of the samples as a function of shear strain at constant hydrostatic pressure were also measured. A modeling frame implemented into the Taylor model was developed to simulate the effect of Grain Boundary Sliding (GBS) on the evolution of crystallographic texture. The main effect found is a shift of the ideal orientations under simple shear conditions, which was verified experimentally. The consolidation process by HPT was simulated numerically using the finite element method together with a powder plasticity model. The simulation of the consolidation process permitted to confirm the experimentally observed average residual porosity and the different gradients in the plastic strain. The local density distribution was also modeled

This thesis is focused on processing of pure magnesium by high pressure torsion method (HPT). This process belongs to the group of intensive plastic deformation methods (SPD). SPD methods are in the centre of scientific interest for several decades. Theoretical part of this thesis puts an effort to summarize basic knowledge and principles of SPD methods with extra focus on method HPT. As theoretical part continues magnesium as technical material is presented. Influence of SPD on use and properties of pure magnesium is then presented. This trend is further developed in effort to describe the effect of individual HPT process variables on the properties of pure magnesium and its alloys. Focus of practical part of this thesis is in influence of number of revolutions. Samples were processed at 1/8, 1/4, 1/2, 1, 4 and 8 turns at room temperature. Speed of process was 1rpm and applied pressure was 6 GPa. The structure of commercially pure magnesium prepared by casting and moulding were observed with focus on differences caused by input material. The structure was observed by both light microscopy and back scattered electron diffraction (EBSD), focusing on structure development, grain size and grain orientation. Compared to other works on similar topic, the emphasis here is on observing the microhardness on the vertical edge of the sample. The hardness shows a steep increase right after 1/8 of a turn. With increasing number of turns gradual homogenization of microhardness is presented accompanied by slight decrease in microhardness. No trend in microhardness relative to the distance from anvil has occurred. Structure observed with EBSD shows a bimodal character with larger grains oriented in the same direction. The three-point bending test didn’t end up as expected, and the approach to evaluation of magnesium-based HPT needs to be re-evaluated for future work. A three-point bending test was designed for the initial assessment of the basic mechanical properties of the material.

Объект исследования – деформированные в результате интенсивной пластической деформации кручением под высоким давлением образцы на основе платины и алюминия. Цель работы – разработка технологии получения интерметаллида PtAl2 с последующим изучением микроструктуры и механических свойств полученных образцов. Методы исследования – проведение механосинтеза, изучение микроструктуры, измерение микротвердости. Результаты работы – методом кручения под высоким давлением из исходных металлических порошков получены образцы в виде пластин, содержащие интерметаллическую фазу. Образцы были исследованы в сканирующем электронном микроскопе и в рентгеновском дифрактометре. Произведены испытания микротвердости образцов. Рентгенофазовый анализ, показал наличие интерметаллида в продеформированных образцах. Новизна исследования состоит в способе получения интерметаллида PtAl2 путем механосинтеза при комнатной температуре (методом кручения под высоким давлением). Область применения – полученные результаты могут быть использованы при создании покрытий на основе интерметаллидов PtAl2 для авиастроения и машиностроения. / Subject of the research are samples based on platinum and aluminum and deformed by using high pressure torsion. The purpose of the work is to develop a technique to produce PtAl2 intermetallic compounds with subsequent study of the microstructure and mechanical properties of the obtained samples. Research methods: carrying out mechanical alloying, studying the microstructure, conducting mechanical hardness tests of samples. As a result of the research samples in the form of plates containing an intermetallic phase were obtained by high pressure torsion the starting metal powders. Samples were examined using a scanning electron microscope and an X-ray diffractometer. The microhardness of the samples was tested. X-ray phase analysis showed the presence of intermetallic in deformed samples. The novelty of the study is to obtain intermetallic using high pressure torsion. Application field: the obtained results can be used to create PtAl22 intermetallic compounds for aircraft and machine building.