L’hydrogène constitue un vecteur d’énergie très important. En effet, il est abondant à l’état combiné et sa combustion est très énergétique et non polluante. En revanche, le mode de stockage le plus sécurisant de ce gaz explosif c’est dans les métaux sous forme d’hydrure. Parmi ces métaux, le magnésium est l’un des plus prometteurs car il possède une capacité massique de stockage élevée (7,6%), un faible coût et une abondance naturelle. Cependant ses cinétiques de sorption sont lentes et son hydrure MgH2 est très stable et mauvais conducteur. L’objectif de ce travail de thèse est de contribuer à la résolution des points faibles du magnésium, en lui ajoutant des fibres de carbone comme renfort soit par broyage énergétique pour assurer une bonne intimité entre les deux, soit par coulage en bande, une technique qui permet d’orienter les fibres, pour un maximum de conductivité thermique. Nous étions donc intéressés à l’étude des cinétiques d’absorption/désorption où une amélioration a été observée après l’ajout du carbone par broyage. Une étude de la conductivité thermique était encore intéressante où le matériau préparé par coulage en bande, comme prévu, a présenté un très bon résultat. D’autre part, nous avons effectué des tests d’hydrolyse pour la production délocalisée d’hydrogène. Ayant comme problème la formation d’une couche imperméable de Mg(OH)2 en surface qui bloque la réaction, différents paramètres ont été modifiés (pH, T°, taille des particules, US) et cela a donné un impact positif sur le rendement en hydrogène et la cinétique de la réaction. Finalement, deux procédés de déformation plastique sévère i) le laminage et ii) l’ECAP ont été appliqués sur du TiH2 et du MgH2. Ces deux techniques ont présenté un pouvoir de déstabilisation des hydrures et donc une diminution de la température de déshydruration. Ils ont encore montré un comportement différent du broyage mécanique de point de vue microcontrainte et orientation des plans cristallins. / Hydrogen is a very important energy carrier. Indeed, it is abundant in the combined state and its combustion, very energetic, is non-polluting. However, the safest storage mode of this explosive gas is in the metal hydride form. Among metals, magnesium is one of the most promising one because its high mass capacity storage (7. 6%), low cost and natural abundance. However its kinetics of sorption are slow and its hydride MgH2 is very stable and has a poor thermal conductivity. The objective of this thesis is to resolve most of the weaknesses of magnesium by adding carbon fibers as reinforcement using the ball milling process, a way to ensure a good contact between the two, either by tape casting, a technique to help in the fibers’ orientation, for a maximum of thermal conductivity. We were therefore interested in the study of absorption / desorption kinetics, where an improvement was observed after the addition of carbon by grinding. A study of the thermal conductivity was also interesting, and the material prepared by tape casting, as expected, gave a very good result. On the other hand, we performed some hydrolysis’ tests to produce hydrogen. Having the problem of Mg(OH)2 formation on the surface, that blocks the reaction; different parameters were modified (e. G. PH, T°, particle size, U. S. ), which showed a positive impact on the hydrogen yield and reaction kinetics. Finally, two severe plastic deformation methods: i) cold rolling and ii) ECAP were applied to the TiH2 and MgH2 samples. Both techniques showed a destabilizing power of hydrides and therefore a decrease in the temperature of dehydrogenation. They even showed different behaviors than the mechanical grinding from microstrain and planes orientation point of view.

La modélisation des efforts de coupe en usinage est nécessaire pour prédire certaines caractéristiques de la pièce usinée comme sa géométrie, son état de surface ou encore l'intégrité de la matière en sub-surface.Les nombreux modèles d'efforts de coupe déjà développés sont souvent appliqués dans le cas d'opérations d'usinage simples, ce qui limite leur diffusion vers le milieu industriel, alors qu'il existe un réel besoin de modélisation d'opérations d'usinage complexes et variées, et prenant en compte d'éventuels changements métallurgiques au niveau du matériau usiné.L'objectif de ces travaux est de proposer un modèle d'efforts de coupe appliqué à toute opération de tournage d'une part et considérant certaines propriétés mécaniques du matériau usiné d'autre part.Concernant l'aspect multi-opérations, un modèle géométrique utilisant des transformations homogènes a été développé et permet de décrire à la fois la trajectoire et la géométrie de l'outil. Les effets de paramètres originaux, tels que le diamètre de la pièce, l'angle de direction d'arête et le rayon de bec, sont étudiés, notamment à l'aide de nouvelles configurations de coupe élémentaires. La prise en compte de ces paramètres dans les relations de coupe locales permet finalement d'améliorer la simulation des efforts de coupe lors d'un contournage.L'approche utilisée pour l'aspect multi-matériaux consiste à modifier progressivement le matériau usiné. Ainsi, le matériau initial, le cuivre pur, a été étudié dans différents états métallurgiques, obtenus par des traitements thermo-mécaniques. En particulier, le procédé d'extrusion coudée à aires égales (ECAE) a été utilisé afin d'écrouir le matériau dans la masse. Ainsi, trois matériaux aux caractéristiques mécaniques différentes mais conservant plusieurs caractéristiques communes (thermiques notamment) ont pu être comparés en termes d'efforts de coupe. Les coefficients des relations de coupe sont finalement mis en regard des propriétés mécaniques obtenues par des essais de traction et de compression à grande vitesse. / The cutting forces have to be known as accurately as possible in order to predict the characteristics of the workpiece as the geometry, the roughness or the material integrity.Numerous models have been yet developed; however, the majority cannot be used for the various industrial cutting operations and remain confined for a single machined material.The objective of this study is to develop a cutting forces model applied to any turning operation and taking into account some mechanical characteristics of the machined material.First, a geometrical model based on homogeneous transformations is presented. Then, the effects of some parameters, like the workpiece diameter, the cutting edge angle and the nose radius, are studied by using new cutting configurations, in order to improve the cutting laws.The multi-material aspect is approached by modifying the metallurgical state with thermo-mechanical treatments, especially by using the equal channel angular extrusion process in order to harden the material in the mass. Finally, the coefficients of the local cutting relations are compared to mechanical characteristics obtained from tensile and high compression tests.

This master’s thesis deals with design and preparation of a new biodegradable magnesium alloy based on Mg-Ca-Zn. Based on information from literature, the Mg-3Zn-2Ca alloy was designed. The base material was produced by gravity casting and the evaluation in the as-cast and heat treated state was performed. For preparation of the experimental material, following methods were designed: squeeze casting, hot rolling and the ECAP. During preparation by hot rolling, no optimal conditions were found and significant cracks occurred in both as-cast and heat treated material. In the case of experimental material, prepared by the ECAP method with back-pressure, better combination of stress-strain properties was observed. Also the squeeze casting method showed improvement; especially the amount of casting defects was eliminated. The evaluation of microstructure and mechanical properties was performed by the light and scanning electron microscopy, RTG phase analysis and the tensile and compression tests.

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

Ultra-fine grained (UFG) materials have attracted considerable interest due to the possibility of achieving simultaneous increase in strength and ductility. Effective use of these materials in engineering applications requires investigating the processing-microstructure-property inter-relations leading to a comprehensive understanding of the material behavior. Research efforts on producing UFG hexagonal close packed (hcp) materials have been limited in spite of their envisaged utilization in various technologies. The present study explores multiple UFG hcp materials to identify the general trends in their deformation behaviors, microstructural features, crystallographic texture evolutions and mechanical responses under strain path changes. UFG hcp materials, including commercial purity Ti, Ti-6Al-4V alloy and high purity Zr, were fabricated using equal channel angular extrusion (ECAE) as a severe plastic deformation (SPD) technique following various processing schedules. Several characterization methods and a polycrystal plasticity model were utilized in synergy to impart the relationships between the UFG microstructure, the texture and the post-ECAE flow behavior. Pure UFG hcp materials exhibited enhanced strength properties, making them potential substitutes for coarse-grained high strength expensive alloys. Incorporation of post-ECAE thermo-mechanical treatments was effective in further improvement of the strength and ductility levels. Strong anisotropy of the post-ECAE flow response was evident in all the materials studied. The underlying mechanisms for anisotropy were identified as texture and processing-induced microstructure. Depending on the ECAE route, the applied strain level and the specific material, the relative importance of these two mechanisms on plastic flow anisotropy varied. A viscoplastic self-consistent approach is presented as a reliable model for predicting the texture evolutions and flow behaviors of UFG hcp materials in cases where texture governs the plastic anisotropy. Regardless of the material, the initial billet texture and the extrusion conditions, ECAE of all hcp materials revealed similar texture evolutions. Accurate texture and flow behavior predictions showed that basal slip is the responsible mechanism for such texture evolution in all hcp materials independent of their axial ratio. High strength of the UFG microstructure was presented as a triggering mechanism for the activation of unexpected deformation systems, such as high temperature deformation twinning in Ti-6Al-4V and room temperature basal slip in pure Zr.

Ultra-fine grained (UFG) materials have attracted considerable interest due to the possibility of achieving simultaneous increase in strength and ductility. Effective use of these materials in engineering applications requires investigating the processing-microstructure-property inter-relations leading to a comprehensive understanding of the material behavior. Research efforts on producing UFG hexagonal close packed (hcp) materials have been limited in spite of their envisaged utilization in various technologies. The present study explores multiple UFG hcp materials to identify the general trends in their deformation behaviors, microstructural features, crystallographic texture evolutions and mechanical responses under strain path changes. UFG hcp materials, including commercial purity Ti, Ti-6Al-4V alloy and high purity Zr, were fabricated using equal channel angular extrusion (ECAE) as a severe plastic deformation (SPD) technique following various processing schedules. Several characterization methods and a polycrystal plasticity model were utilized in synergy to impart the relationships between the UFG microstructure, the texture and the post-ECAE flow behavior. Pure UFG hcp materials exhibited enhanced strength properties, making them potential substitutes for coarse-grained high strength expensive alloys. Incorporation of post-ECAE thermo-mechanical treatments was effective in further improvement of the strength and ductility levels. Strong anisotropy of the post-ECAE flow response was evident in all the materials studied. The underlying mechanisms for anisotropy were identified as texture and processing-induced microstructure. Depending on the ECAE route, the applied strain level and the specific material, the relative importance of these two mechanisms on plastic flow anisotropy varied. A viscoplastic self-consistent approach is presented as a reliable model for predicting the texture evolutions and flow behaviors of UFG hcp materials in cases where texture governs the plastic anisotropy. Regardless of the material, the initial billet texture and the extrusion conditions, ECAE of all hcp materials revealed similar texture evolutions. Accurate texture and flow behavior predictions showed that basal slip is the responsible mechanism for such texture evolution in all hcp materials independent of their axial ratio. High strength of the UFG microstructure was presented as a triggering mechanism for the activation of unexpected deformation systems, such as high temperature deformation twinning in Ti-6Al-4V and room temperature basal slip in pure Zr.

Severe plastic deformation (SPD) results in ultra-fine grain sizes in metals and alloys. Equal channel angular pressing (ECAP) is one of the special SPD methods aiming to introduce high plastic strains into the bulk materials without changing their cross section. ECAP results in improvement in hardness and strength while still satisfying acceptable ductility level. The combined effects of ECAP and subsequent heat treatments, i.e. post-aging and post-annealing, on the microstructure and hardness of the 2024 aluminum alloy were investigated. An ECAP die with 120&amp / #730 / channel angle was constructed. Subgrain formation, increase in dislocation density and dislocation tangling were observed after ECAP, and subgrain growth was detected after post annealing. The specimens revealed higher hardness values after ECAP at room temperature, and further increase in hardness was observed following post-aging at 80&amp / #730 / C, 100&amp / #730 / C and 190&amp / #730 / C. Effect of the aging temperature on the deformed specimens was investigated, and the aging behaviors of the severely deformed and undeformed samples at 190&amp / #730 / C were compared.

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

Bulk nanocrystalline 304L and 316L austenitic stainless steels (SS) were produced by equal channel angular pressing(ECAP) at elevated temperature. The average grain size achieved in 316L and 304 L SS is ~ 100 nm, and grain refinement occurs more rapid in 316 L SS than that in 304L. Also the structures are shown to retain a predominant austenite phase. Hardness increases by a factor of about 2.5 in both steels due largely to grain refinement and an introduction of a high density of dislocations. Tensile strength of nanocrystalline steels exceeds 1 GPa with good ductility in both systems. Mechanical properties of ECAPed 316L are also shown to have less dependence on strain rate than ECAPed 304L. ECAPed steels were shown to exhibit thermal stability up to 600oC as indicated by retention of high hardness in annealed specimens. Furthermore, there is an increased tolerance to radiation-induced hardening in the nanocrystalline equiaxed materials subjected to 100 keV He ions at an average dose of 3-4 displacement-per-atom level at room temperature. The large volume fraction of high angle grain boundaries may be vital for enhanced radiation tolerance. These nanocrystalline SSs show promise for further research in radiation resistant structural materials for next-generation nuclear reactor systems.

Submitted by GILSON SILVA JUNIOR null (gilson_feg@yahoo.com.br) on 2017-12-18T12:27:06Z No. of bitstreams: 1 Tese Doutorado Defesa - Versão Final.pdf: 8602731 bytes, checksum: 8f3cbfc632bdb7f8998d8a2a7aa87243 (MD5) / Approved for entry into archive by Pamella Benevides Gonçalves null (pamella@feg.unesp.br) on 2017-12-18T13:21:51Z (GMT) No. of bitstreams: 1 silvajunior_g_dr_guara.pdf: 8602731 bytes, checksum: 8f3cbfc632bdb7f8998d8a2a7aa87243 (MD5) / Made available in DSpace on 2017-12-18T13:21:51Z (GMT). No. of bitstreams: 1 silvajunior_g_dr_guara.pdf: 8602731 bytes, checksum: 8f3cbfc632bdb7f8998d8a2a7aa87243 (MD5) Previous issue date: 2017-11-10 / A obtenção de granulometria ultrafina em aços com baixo teor de carbono pode contribuir para ampliação de suas aplicações na indústria, devido as propriedades mecânicas superiores que podem ser alcançadas com o refinamento de grãos, tais como: resistência mecânica, dureza, e tenacidade. O processo conhecido como Equal Channel Angular Pressing (ECAP) induz deformações plásticas severas suficientes para alterar as características microestruturais dos metais reduzindo seu tamanho de grão, e consequentemente melhorando algumas propriedades mecânicas, sem alterar a composição química dos materiais, ao utilizar temperaturas abaixo do ponto de recristalização dos metais. Neste trabalho o processo ECAP foi conduzido com corpos de prova na temperatura de 550°C utilizando como material de estudo aço SAE 1020. Os corpos de prova foram separados em três grupos. No primeiro grupo as amostras não foram submetidas a nenhum tratamento térmico entre os passes, no segundo grupo foi aplicado tratamento de alívio de tensões após os passes, e por fim, no terceiro grupo e foi aplicado um tratamento de recozimento intercrítico após o primeiro passe. Ensaios mecânicos de tração, dureza e charpy foram realizados com objetivo de verificar a influência do processo ECAP no comportamento mecânico do aço. Com intuito de verificar as alterações microestruturais causadas pelo processo ECAP foram utilizadas as técnicas de microscopia óptica e eletrônica de varredura. O trabalho tem como objetivo principal induzir o refinamento dos grãos por meio do processo ECAP em matriz bipartida elaborada neste trabalho. Os resultados das análises microestruturais e dos ensaios mecânicos demonstraram que os tratamentos térmicos utilizados combinados ao processo ECAP influenciaram diretamente no comportamento do aço SAE 1020. Conforme o número de passes pela matriz ECAP ocorreu uma redução do tamanho dos grãos, assim como aumento do limite de resistência a tração e dureza do aço 1020. Com relação ao tratamento térmico de alívio de tensão, uma melhor combinação entre resistência mecânica e ductilidade foi encontrada. O tratamento de recozimento intercrítico foi suficiente para induzir a transformação de fases no aço SAE 1020, o qual proporcionou resultados positivo no que diz respeito a ductilidade e resistência mecânica. Por fim, a consistência das investigações da evolução microestrutural permitiu compreender os efeitos do ECAP no aço SAE 1020. / Ultrafine grained microstructures obtaining in low carbon steels may contribute to enlarge the application of this material in industry, due to superior properties that can be achieved, such as: mechanical strength, hardness, and toughness. The process known as Equal Channel Angular Pressing (ECAP) induces severe plastic deformation sufficient to modify metals microstructures characteristics, reducing its grains size, and consequently improve its mechanical properties without materials chemistry composition changes, under temperatures below to recrystallization point. At this work ECAP process was carried out with specimens at 550° C using steel SAE 1020 as material. The specimens were divided into three groups. The specimens in the first group none heat treatment was applied between and after ECAP passes, in the second group the specimens were submitted under stress relief heat treatment after ECAP passes, and in the third group, specimens were submitted under intercritical annealing after first pass. Mechanical tensile strength, hardness and charpy impact tests were used with aim to verify the ECAP influence in steel mechanical behavior. In order to verify microstructures evolution caused by ECAP were applied optical and scanning electron microscopy. The aim of this work is grain refining by means of ECAP process with two parts tool elaborated in this study. The microstructure analysis and mechanical tests results shown that the heat treatments applied, combined with ECAP process directly influenced on steel SAE 1020 behavior. According to the number of passes grains sizes were reduced, as well the ultima tensile strength and hardness were increased. In reference of stress relief heat treatment, better combination between mechanical strength and ductility was achieved. Intercritical annealing treatment was capable to induce phase transformation in steel SAE 1020, which provided positive results with respect to ductility and mechanical strength. In conclusion, the consistence of microstructure evolution investigation became possible to understand effects of ECAP in steel SAE 1020