De nombreuses études ont prouvé l'affaiblissement de la résistance de l'alliage 600 lors de l'oxydation en milieu primaire des réacteurs à eau pressurisée. Celle-ci induit la rupture localisée du matériau notamment par fissure intergranulaire. La nature ainsi que la structure de l'oxyde se développant à la surface de l'alliage sont parfaitement connues. Cependant, l'influence mécanique de l'oxyde sur l'alliage n'a pas été explorée. L'objectif de cette étude est d'apporter des connaissances nouvelles sur l'impact de l'oxydation sur la réponse mécanique de l'alliage. Un système d'analyse, basé sur l'utilisation de nanoplots comme marqueurs de position, a été développé et mis en œuvre afin de mesurer des déformations engendrées par l'oxydation puis par une traction. Le traitement statistique de ces données a permis de déterminer des évènements rares de haute déformation. Les échantillons utilisés ont été caractérisés par MEB, TEM, XPS et ellipsométrie spectroscopique afin d'en déduire l'épaisseur de la couche d'oxyde interne contraignant l'alliage. De plus, le couplage de l'EBSD avec les nanoplots a permis de déterminer un ensemble de paramètres pouvant servir de critère d'alerte à l'initiation de la fissuration intergranulaire.

Technological advances results in the fact that quite a large number of electronic equipment interacts with its environment leading to the malfunction of the devices. This brings about the necessity of using proper electromagnetic (EM) wave absorbers/shields to avoid such interactions. In order to absorb EM waves in a large frequency band from several MHz to GHz, barium hexaferrite (BaHF) ceramics which are produced as textured ceramics as well as in multilayered form can be used. Textured ceramics are processed by tape casting using templated grain growth (TGG) phenomenon. In order to obtain textured ceramics, BaHF powders and platelets are required as raw materials in such a way that during sintering small size powders are directioned by large platelet surfaces. In this study, ferrite powders were synthesized by mixed oxide technique while the platelets were produced by both molten salt synthesis (MSS) and reactive templated grain growth (RTGG) methods. In the case of platelet synthesis by MSS, effects of calcination temperature and time as well as type and composition of the flux on the formation and morphology of platelets were investigated based on the XRD and SEM results. Studies have shown that KCl flux led to the formation of sharper platelet morphology, while NaCl resulted in more round shapes. However, extent of BaHF formation in the case of NaCl was higher when compared to KCl flux due to its higher wettability characteristic, and hence faster interaction with the raw materials. Since the aspect ratio of the synthesized platelets was only ca. 2-4, these platelets were not efficient for further TGG studies. Alternatively, BiFeO3 (BiF) particles having ~30-40 &mu / m average size were synthesized as seed crystals for the synthesis of BaHF platelets by RTGG method. After the washing of these platelets with dilute HNO3, pure BaHF powders and platelets were directed by tape casting which was followed by sintering using TGG phenomenon. Degree of achieved texturing in the processed ceramics was studied using Rietveld analysis, pole figure measurement and electron backscattered diffraction (EBSD).

No description available.

Co-20Cr-15W-10Ni alloy (L-605) is a cobalt-based superalloy combining high strength with keeping high ductility, biocompatible and corrosion resistant. It has been used successfully for heart valves for its chemical inertia, and this alloy is a good candidate for stent elaboration. Control of grain size distribution can lead to significant improvement of mechanical properties: in one hand grain refinement enhance the material strength, and on the other hand large grains provide the ductility necessary to avoid the rupture in use. Therefore, tailoring the grain size distribution is a promising way to adapt the mechanical properties to the targeted applications. The grain size can be properly controlled by dynamic recrystallization during the forging process. Therefore, the comprehension of the recrystallization mechanism and its dependence on forging parameters is a key point of microstructure design approach. The optimal conditions for the occurrence of dynamic recrystallization are determined, and correlation between microstructure evolution and mechanical behavior is investigated. Compression tests are carried out at high-temperature on Thermec-master Z and Gleeble forging devices, followed by gas or water quench. Mechanical behavior of the material at high temperature is analyzed in detail, and innovative methods are proposed to determine the metallurgical mechanisms at stake during the deformation process. Mechanical properties of the material after hot-working and annealing treatments are investigated. The grain growth kinetics of L-605 alloy is determined, and experimental results are compared with the static recrystallization process. Microstructures after hot deformation are evaluated using SEM-EBSD and TEM. Significant grain refinement occurs by dynamic recrystallization for high temperature and low strain rate (T≥1100 ◦ C, strain rate < 0.1s−1), and at high strain rate (strain rate > 10s−1). Dynamic recrystallization is discontinuous and takes place from the grain boundaries, leading to a necklace structure. The nucleation mechanism is most likely to be bulging from grain boundaries and twin boundaries. A new insight of the modeling of dynamic recrystallization taking as a starting point the experimental data is proposed. By combining the results from the mechanical behavior study and microstructure observation, the recrystallization at steady-state is thoroughly analyzed and provides the mobility of grain boundaries. The nucleation criterion for the bulging from grain boundaries is reformulated to a more general expression suitable for any initial grain size. Nucleation frequency can be deduced from experimental data at steady-state through modeling, and is extrapolated to any deformation condition. From this point, a complete analytical model of the dynamic recrystallization is established, and provides a fair prediction on the mechanical behavior and the microstructure evolution during the hot-working process.

Low temperature cleavage fracture behaviour was investigated using four experimental microalloyed bainitic plate steels. The four plate samples were produced by different thermomechanical processing (TMP) schedules and had yield strengths in the range 540 - 670 MPa. Microstructures were characterized by optical microscopy (OM), scanning electron microscopy (SEM) and electron back scattered diffraction (EBSD). Quantitative data was obtained for prior austenite grain (PAG) size, volume fractions of two bainite types (conventional bainite and acicular ferrite) and EBSD 15° domain size. Charpy impact tests (using two notch orientations) were carried out over a range of temperatures. Cleavage facet sizes were measured on -196°C Charpy samples. The range of TMP schedules produced variations in PAG width, type of bainite and 15° domain size. The effects of these three microstructural features on cleavage crack propagation are discussed. Results indicate that the microstructures are controlled by i) deformation below TNR and ii) accelerated cooling rate. Domain structure reflects TMP. There is no clear correlation between domain size and cleavage facet size. / Thesis (Master, Mechanical and Materials Engineering) -- Queen's University, 2009-07-30 19:17:01.25

L'amélioration des performances spécifiques des alliages métalliques de l'aéronautique est une démarche constante. Les alliages de titane sont des matériaux privilégiés par les constructeurs aéronautiques car ils allient hautes propriétés mécaniques et faible densité.Parmi ces matériaux, les alliages β-métastables qui ont pour particularité de retenir jusqu'à 40% de phase β connaissent un fort regain d'intérêt pour les motoristes (Ti-17) comme pour des applications de structure type trains d'atterrissage (Ti-5553 et Ti-10-2-3). Ce travail a pour but d'analyser le comportement mécanique et la durabilité de ces alliages soumis à des sollicitations monotones et cycliques en lien avec les microstructures.Des essais mécaniques ont pour cela été développés à partir de différentes microstructures métallurgiques qu'elles soient issues d'un traitement industriel ou spécifique visant à simplifier ces dernières. Les mécanismes de déformation (systèmes de glissement) et d'endommagement (amorçage de fissures) ont été identifiés et analysés à différentes échelles par microcopie optique et électronique à balayage en intégrant les notions d'orientation cristallographique (EBSD). Le recours à des essais réalisés in situ sous microscope (optique et MEB) et à une métrologie adaptée aux échelles pertinentes a permis d'identifier les éléments micro-structuraux clés et les cinétiques de développement de ces processus. Un des faits marquants est le rôle majeur de l'anisotropie de propriétés mécaniques de la phase β qui a également fait l'objet de simulations numériques.

A combined experimental and computational investigation of the deformation behavior of pure magnesium single crystal at the micron length scale has been carried out. Employing the recently exploited method of microcompression testing, uniaxial microcompression experiments have been performed on magnesium single crystals with [0001], [2-1-12], [10-11], [11-20] and [10-10] compression axes. The advantage of the microcompression method over conventional mechanical testing techniques is the ability to localize a single crystalline volume which is characterizable after deformation. The stress-strain relations resulting from microcompression experiments are presented and discussed in terms of orientation dependent slip activity, twinning mechanisms and an anisotropic size effect. Such a mechanistic picture of the deformation behavior is revealed through SEM, EBSD and TEM characterization of the deformation structures, and further supported by 3D discrete dislocation dynamics simulations. The [0001], [2-1-12], and [10-11] compression axes results show dislocation plasticity. Specifically, the deformation due to [0001] compression is governed by pyramidal slip and displays significant hardening and massive unstable shear at stresses above 500MPa. In the case of the two orientations with compression along an axis 45 degrees to the basal plane, unsurpringly it is found that basal slip dominates the deformation. In contrast, compression along the [11-20] and [10-10] directions show deformation twinning in addition to dislocation plasticity. In the case of compression along [11-20], the twinning leads to easy basal slip, while the twin resultant during compression along [10-10] does not lead to easy basal slip. In all cases, a size effect in the stress-strain behavior is observed; the flow stress increases with decreasing column diameter. Furthermore, the extent of the size effect is shown to depend strongly on the number of active slip systems; compression along the [0001] axis is associated with 12 slips systems and displays a saturation of the size effect at a diameter of 10μm, while the other orientations still show a significant size effect at this diameter. The experimental evidence of an orientation-dependent deformation behavior in flow stress has been investigated by 3D discrete dislocation dynamics simulations. Here, the code TRIDIS was modified for hcp structure and c/a ratio of Mg. By matching the simulation results to experimental results, some proper constitutive material parameters such as initial dislocation density, dislocation source length, the critical resolved shear stress were suggested. For the case of [0001] and [2-1-12] orientation, dislocation feature in the pillar during the deformation was exhibited and strain burst was discussed.

Submitted by Érika Aparecida da Silva null (erikametais@gmail.com) on 2016-07-15T22:12:15Z No. of bitstreams: 1 Versão final.pdf: 12982211 bytes, checksum: 38bfd8e2bd40ff36d58029a14bf04fba (MD5) / Approved for entry into archive by Felipe Augusto Arakaki (arakaki@reitoria.unesp.br) on 2016-07-18T14:18:45Z (GMT) No. of bitstreams: 1 silva_ra_dr_guara.pdf: 12982211 bytes, checksum: 38bfd8e2bd40ff36d58029a14bf04fba (MD5) / Made available in DSpace on 2016-07-18T14:18:45Z (GMT). No. of bitstreams: 1 silva_ra_dr_guara.pdf: 12982211 bytes, checksum: 38bfd8e2bd40ff36d58029a14bf04fba (MD5) Previous issue date: 2016-07-11 / Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / Diante da necessidade da produção de novos materiais para a indústria automotiva com melhores performances aliada à preocupação com as questões ambientais, visando a redução do consumo de combustíveis fósseis, surgiram, a partir da década de 1990, os aços avançados de alta resistência (AHSS), os quais conciliam uma pequena espessura da chapa e alta resistência mecânica. Porém, a produção em massa de componentes estruturais é limitada devido aos desafios na conformabilidade e união de chapas devido ao retorno elástico, conhecido como efeito springback. O presente trabalho avaliou 10 tipos de aços amplamente utilizados pela indústria automotiva, os quais estão agrupados em aços bifásicos, aços baixo carbono, aços endurecíveis após pintura e aços com interstícios livres. Todos esses materiais foram submetidos à caracterização mecânica e microestrutural por meio de determinação de composição química, ensaios de tração, ensaios de dureza e nanodureza, ensaios de dobramento de três pontos ao ar, análises de difração de elétrons retroespalhados (EBSD) e simulação de dobramento mecânico pelo método de elementos finitos (MEF) em software ABAQUS. Com os resultados provenientes do MEF, foi possível identificar as diferenças nos perfis anisotrópicos de cada material e correlacionar cada perfil com as características cristalográficas analisadas por meio de EBSD. Assim, foi possível compreender a variação no grau de springback com base na estrutura do retículo cristalino, uma vez que as diferenças estruturais do retículo cristalino são as responsáveis pelas diferentes respostas mecânicas. Concluiu-se que o modelo de encruamento isotrópico utilizado no MEF foi eficiente na determinação do perfil anisotrópico dos materiais, porém para uma perfeita acurácia na previsão e eliminação do springback, faz-se necessária a utilização do modelo de encruamento cinemático aliado ao uso de contrapunção nos ensaios experimentais. / In face of the need of the production of new materials for the automotive industry with better performance allied to the concern with environmental issues, aiming to reduce the consumption of fossil fuels, emerged from the decade of 1990, the advanced high-strength steels (AHSS), which reconcile a small sheet thickness and high mechanical resistance. However, the mass production of structural components is limited due to the challenges in conformability and union of sheets due to elastic return, known as springback effect. The present work has evaluated 10 types of steels are widely used in the automotive industry, which are grouped into biphasic steels, low carbon steels, bake hardening steels and interstitial free steels. All these materials were submitted to mechanical and microstructural characterization through determination of chemical composition, tensile tests, hardness Vickers tests and nanoindentation tests, sheet metal forming through three points bending in air, analyzes of electron backscatter diffraction (EBSD) and simulation of sheet metal forming by finite elements method (MEF) in ABAQUS software. With the results from the MEF, it was possible to identify the differences in anisotropic profiles of each material and correlate each profile with the crystallographic characteristics analyzed through EBSD. Thus, it was possible to understand the variation in degree of springback based on the structure of the crystal lattice, once the structural differences of crystal lattice are responsible for different mechanical responses. It was concluded that the model of isotropic hardening used in MEF was efficient in determining the anisotropic profile of materials, however for a perfect accuracy in prediction and elimination of springback, it is necessary to use a model of kinematic hardening allied to the use of counter-punch in experimental sheet metal forming. / 141827/2015-7 / CAPES: 99999.002440/2014-08

Placing recrystallization annealing in a manufacturing proces is often necessary in order to restore plasticity of worked blanks right before working products to its final shape. For better understanding of processes which are taking place in a material during annealing the use of in-situ techniques is favorable. Such observations enable us to watch changes in the materiál in real time at the original spot. Observations at grain-level are ideally made with scanning electron microscope – SEM by electron back-scattered diffraction – EBSD. The technique makes watching nucleation, growth and potential coarsening of recrystallized grains possible. Special construction of a tensile stage allows us to watch changes of a sample during tensile tests which can be used in observing influence of MnS inclusions on plasticity of free-cutting steels. Materials studied in this work are commonly used free-cutting steel 11SMnPb30 and its lead-free alternative 11SMnBi30.

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.