Nous avons caractérisé de manière détaillée les  fortes hétérogénéités de texture et de microstructure (macrozones) par EBSD dans des zones déformées différemment d’un disque en IMI834 de structure bimodale αP/αS, utilisé en motorisation aéronautique. Des échantillons spécifiques ont permis de montrer que l’amplitude des signaux ultrasonores rétrodiffusés dans ces échantillons dépendait de la présence et de l’organisation des macrozones. Partant de ces observations, une analyse ultrasonore des signaux rétrodiffusés dans les parties du disque soumis à de fortes déformations lors du forgeage a permis de sélectionner un jeu d’éprouvettes ayant des caractéristiques microstructurales différentes et destinées à des essais en fatigue-dwell. Une forte dispersion des durées de vie liée aux microstructures présentes a été observée. L’analyse fractographique des surfaces de rupture et leurs études par EBSD ont permis de localiser les sites d’amorçage et les chemins de propagation des fissures ainsi que leurs caractéristiques cristallographiques. Les résultats des essais en fatigue-dwell montrent que la réduction de la tenue en service est fortement influencée par la présence de macrozones formées d’agglomérats de grains αP allongés associés à des lamelles αS plus épaisses et organisées en colonies et d’autre part présentant majoritairement des axes c à moins de 30° de l’axe de sollicitation / We have characterized in detail the strong heterogeneity of texture and microstructure (macrozones) by EBSD in areas, differently deformed, of a disk in IMI834 with a bimodal structure αP/αS, used in aircraft engines. Specific samples have shown that the amplitude of back-scattered ultrasonic signals depended on the presence and organization of macrozones. Based on these observations, an analysis of back-scattered ultrasonic signals in parts of the disc subject to strong deformation during forging led to select a set of specimens with different microstructural features for fatigue-dwell tests. A high dispersion of lifetimes associated with these microstructures was observed. The fractographic analysis of fracture surfaces and their EBSD studies were used to locate crack initiation sites and propagation paths and their crystallographic characteristics. The results of fatigue-dwell tests showed that the lifetime reduction is strongly influenced by the presence of macrozones formed by agglomerates of grains elongated αP associated with thicker αS lamellae, organized in colonies and with c-axis predominantly at less than 30 ° of the solicitation axis

This work was performed as part of the MUZIC-2 (Mechanical Understanding of Zirconium Corrosion) collaboration, established with the goal of understanding the mechanism of hydrogen pickup in zirconium alloys. Hydrogen pickup is one of the least understood and most significant degradation mechanisms affecting zirconium alloys in nuclear reactors. These alloys are used as cladding and structural materials in the reactor core, mainly due to their low thermal neutron absorption cross section and excellent corrosion resistance. This project aims to investigate the effect of oxide texture (i.e. the degree of preferred orientation) on the corrosion performance of zirconium alloys. The texture of the oxide is expected to affect the microstructural development of the oxide, the grain boundary distribution and the stress state. It is therefore considered to be one of the most important factors in determining how the corrosion process occurs, and why different alloys exhibit significantly different corrosion performance. It is hoped that this project will add to the current knowledge of the corrosion process, and in particular hydrogen pickup, so that the route of hydrogen through the protective oxide can be identified. This will lead to the development of a new generation of alloys that provide improved oxidation and hydrogen pickup performance, whilst maintaining the required mechanical properties. This work focuses on four zirconium alloys; Zircaloy-4, ZIRLO™, low-Sn ZIRLO™ and Zr-1.0Nb-0.1Fe. The alloys all have different chemical compositions and therefore exhibit different corrosion performance. The macrotexture of the oxide formed on different alloys was measured by glancing angle X-ray diffraction (XRD) and Electron Backscatter Diffraction (EBSD). A fibre texture was formed in all cases, with the (10-3) to (10-5) planes oriented parallel to the metal-oxide interface for the monoclinic phase. The major orientation was found to be independent of alloy chemistry, substrate orientation and oxidation conditions. The monoclinic texture strength was found to be weakened with increasing oxidation temperature, The major orientation of the tetragonal phase was also found to be a fibre texture, with the (001) planes oriented approximately parallel with the interface. Although significant variation from this texture component was observed. It is suggested that the main driving force for oxide texture development is the transformation stress induced by the Zr-ZrO2 transformation. The microtexture of the oxides was measured using two novel techniques, Transmission Kikuchi Diffraction (TKD) and automated crystal orientation mapping with transmission electron microscopy (TEM). The techniques revealed an oxide microstructure consisting of an outer layer of equiaxed grains with a large range of orientations and an inner layer consisting of well-aligned columnar monoclinic grains. This layer of equiaxed grains was observed to form again after the transition in corrosion kinetics. A large fraction of transformation twin boundaries were observed throughout the oxides. Some of these boundaries were observed to surround large monoclinic grains, providing evidence that the tetragonal grains from which they transformed had grown considerably larger than the critical grain size for stabilisation. Without the presence of Sn, larger monoclinic grains were observed to form with a greater degree of preferred orientation, and with a lower fraction of transformation twin boundaries than Sn-containing alloys. In addition, an increased number of well-oriented tetragonal grains was correlated with the presence of Sn. It is therefore concluded that a reduction in Sn will lead to the formation of an oxide microstructure that is more resistant to both oxidation and hydrogen pickup. An analysis of the crystallography and morphology of a ZrO phase present at the metal-oxide interface was also performed. Finally, the observations have been used to construct a model of the corrosion process.

Ti-6Al-4V is the most widely used titanium alloy and is typically used in stages of gas turbine engines, due to its high strength-to-weight ratio, corrosion resistance and high strength at moderate temperatures. However, the alloy is susceptible to the development of strong textures during thermomechanical processing that leads to a preferred crystallographic orientation. These are referred to as macrozones and are thought to develop during the β to α phase transformation, as a result of the retention of large prior β grains during processing and variant selection. Macrozones are clusters of neighbouring grains with a common crystallographic orientation that may act as one single grain during loading and have been shown to cause scatter in the fatigue life. The focus of the current work was based on the analysing the strain behaviour of soft, hard and no macrozones within the microstructure, during various loading conditions. The local strain behaviour was studied at a micro and nanoscale, using the digital image correlation (DIC) technique, which utilises microstructural images recorded during mechanical loading. On a microscale, the no-macrozone and strong-macrozone condition loaded at 0% exhibited homogeneous strain behaviour. The strong-macrozone condition loaded at 45% and 90% to the extrusion direction, respectively, developed pronounced high strain bands correlating to regions that were favourably oriented for prismatic and basal slip, respectively. Characterisation of the slip bands provided a detailed understanding of the deformation behaviour at the nanoscale and the slip system was subsequently determined for each grain using slip trace analysis. Prismatic slip was the dominant slip system in all conditions, particularly in the soft-oriented macrozone regions of the strong-macrozone condition loaded at 45 degrees. Shear strains of 10 times the appliedstrain were observed. Further investigations on the strong-macrozone condition loaded at 45 degrees to ED during standard and dwell fatigue demonstrated early failure in the dwell sample, with higher strain accumulation for dwell.

Les aciers bainitiques sans carbure font partie d'une nouvelle génération d’aciers à très haute résistance, présentant des limites d’élasticité élevées et un excellent compromis entre résistance mécanique et ductilité. Leurs propriétés sont liées à la spécificité de leur microstructure qui fait intervenir plusieurs constituants (bainite, austénite et martensite) imbriqués selon une topologie particulière (colonies lamellaires et ilots résiduels). De nombreuses questions restent cependant en suspens quant aux liens existant entre paramètres microstructuraux et propriétés mécaniques. Ce travail de thèse vise ainsi à explorer ces relations dans différents aciers bainitiques sans carbure élaborés par traitement de trempe étagée. Diverses techniques de caractérisation in situ et post mortem ont été mises en oeuvre pour analyser qualitativement et quantitativement les microstructures résultant de la décomposition de l'austénite en conditions isothermes. L'influence de la température de maintien isotherme et de la concentration en carbone sur la microstructure et la microtexture a ainsi été mise en évidence. Un traitement de trempe étagée réalisé sous Ms a également permis d'élaborer une microstructure composite constituée de martensite revenue, de ferrite bainitique et d'austénite résiduelle. Des essais de traction et de cisaillement ont permis d'évaluer les propriétés mécaniques de ces aciers et notamment d'estimer les contributions isotropes et cinématiques de leur écrouissage. Les résultats ont ensuite été analysés à la lumière des informations microstructurales et l'influence de certains constituants a été mise en évidence. Le comportement de la bainite sans carbure élaborée sous Ms a été appréhendé par une approche micromécanique basée sur une loi des mélanges entre la martensite revenue et le composé bainite – austénite résiduelle / Carbide-free bainitic steels are part of the 3rd generation of advanced high strength steels, which exhibit high yield strength and an excellent compromise between tensile strength and ductility. These ground – breaking properties are achieved thanks to the characteristics of their microstructure which is constituted of different phases (bainite, austenite and martensite) organized in a specific way (typical bainitic colonies and residual islands). However, relationships between microstructural features and mechanical properties are yet to be thoroughly established. In the frame of this PhD, we investigated these relationships in carbide-free bainitic steels elaborated by an austempering process. Various means of characterization were used in situ and post mortem to analyze qualitatively and quantitatively microstructures elaborated by the decomposition of the austenite in isothermal conditions. The influence of the austempering temperature and the carbon content on the microstructures has been highlighted. Moreover, austempering under Ms allowed elaborating a microstructure constituted of tempered martensite, bainitic ferrite and residual austenite. Tensile and shear tests were performed in order to evaluate their mechanical properties and to estimate the kinematical and isotropic contributions of the workhardening. Results were analyzed in the light of the microstructural characterizations and the effects of some microstructural features have been highlighted. The mechanical behavior of the bainite elaborated under Ms was estimated by a micromechanical approach based on a law of mixtures between the tempered martensite and the compound made of bainitic ferrite and residual austenite

Dans ce travail, les caractéristiques cristallographiques des martensites d’alliages Ni-Mn-Ga ont été étudiées en détail. En utilisant l’information de la superstructure de martensite 5M de Ni50Mn28Ga22 et de martensite 7M de Ni50Mn30Ga20 pour des mesures en EBSD, les structures cristallines ont été confirmées. Le nombre de variantes, les relations d’orientation entre les variantes adjacentes et les plans d’interface des variantes ont été déterminées sans ambiguïté. Sur la base de données d’orientations précises des variantes de martensite, les relations d’orientation de transformation de l’austénite en martensite 5M et de l’austénite en martensite 7M ont été déterminées, sans présence de l’austénite résiduelle. Pour la martensite NM de Ni54Mn24Ga22, les lamelles de macles à l’échelle nanométrique dans les platelets martensitiques ont été révélées. Les interfaces entre les platelets et entre les lamelles ont été analysées. Dans un alliage Ni53Mn22Ga25 avec coexistence de l’austénite et de la martensite à température ambiante, la formation de la microstructure martensitique en forme de losange avec quatre variantes lors de la transformation de l’austénite en martensite 7M a été mise en évidence. La nature de la martensite 7M a été clairement précisée dans ce travail. Elle est thermodynamiquement métastable et intermédiaire entre l’austénite parent et la martensite NM finale. La martensite 7M possède une structure cristalline indépendante, plutôt que la combinaison de macles nanométrique de martensite non modulée. Le rôle de la martensite 7M dans la transformation est d’atténuer le décalage important entre la maille de l’austénite cubique et celle de la martensite tétragonale et d’éviter la formation d’interfaces incohérentes entre les platelets de martensite NM, qui constituent une barrière énergétique infranchissable / In this work, the crystallographic features of martensites in Ni-Mn-Ga alloys were detailed studied. By using superstructure information for EBSD mapping on 5M martensite in Ni50Mn28Ga22 alloy and 7M martensite in Ni50Mn30Ga20 alloy, the crystal structures were confirmed and the variant number, twin orientation relationships of adjacent variants and twin interface planes were unambiguously determined. Based on the accurate orientation data of martensite variants, the transformation ORs for austenite-5M and austenite-7M were indirectly determined with no presence of initial austenite. For the NM martensite of Ni54Mn24Ga22, the nano-scale twin lamellae in martensitic plates were revealed, and the inter-plate interfaces and inter-lamellar interfaces were analyzed. In a Ni53Mn22Ga25 alloy with co-existence of austenite and martensite at room temperature, the formation of characteristic diamond-like martensite microstructure with four variants during the austenite-7M martensite transformation was evidenced. The 7M martensite occurs on cooling as a thermodynamically metastable phase that is intermediate between the parent austenite and the final NM martensite. 7M martensite possesses an independent crystal structure, rather than the nanotwin combination of normal non-modulated martensite. The role of 7M martensite in the transformation from the cubic austenite to the tetragonal NM martensite has been clarified, which is at the request of mitigating the large lattice mismatch between the cubic austenite and the tetragonal NM martensite and avoiding the formation of the incoherent NM plate interfaces that represent insurmountable energy barrier

The motivation to use lightweight materials in the construction of the automotive structure is the resultant increased fuel efficiency. However, these materials possess certain drawbacks that make it challenging to adopt them into current automobile manufacturing processes. In this dissertation the microstructural response observed in a magnesium alloy, AZ31, and an advanced high strength steel alloy, QP1180, to uniaxial deformation is analyzed and the results are presented. In AZ31 the required slip modes are not activated at room temperature leading to its low ductility at room temperature. The resulting activity of these twins in response to uniaxial tension is analyzed and its correlations with the microstructure features is reported. Additionally, a neighborhood viscoplastic self-consistent model is developed that will allow more accurate simulation of twin response to outside deformation. Furthermore, activity of slip modes that are usually observed at high temperatures (>200°C) are also observed at lower temperatures (<125°C) and they are compared to the relative twin activity at these temperatures. It is observed that larger grains, with high schmid factors, longer grain boundaries and have misorientation with its neighboring grain greater than 27° are more favorable for twin formation and transmission in the AZ31 microstructure in response to uniaxial tension. The nature of retained austenite (RA) transformation into martensite that gives QP1180 its enhanced ductility, is not clearly understood primarily because of challenges present in characterization of these metastable RA. Further, a 2 dimensional characterization method does not provide the complete information of the RA grain. These challenges are overcome by characterization of a 3 dimensional volume element using serial sectioning and EBSD followed by reconstruction using DREAM3D. The influence of 3d morphology and orientation direction on RA transformation is studied using as-is and uniaxially deformed samples. A novel shear affinity factor is introduced as a metric to describe the ease of RA transformation under uniaxial tension. The 3d nature of the information collected allows a new classification of disk shape in addition to globular and lamellar shapes for RA. It is found that RA that are low volume laths and have low shear affinity factor transform later compared to disk shaped RA’s. Through these guidelines the preparation of a microstructure that is conducive to RA transformation under uniaxial tension is possible.

The production and fabrication of semi-conductor core optical fibers was shown to be feasible and controllable. This was accomplished through the step sequence of fabrication and characterization of 4 fiber types, an experiment on controlling the grain length in the core and a simple model of the heat transfer during fabrication. Fibers were first made with a silicon core, followed by a phosphorous doped n-type silicon core, then a boron doped p-type silicon core, and a tellurium doped n-type gallium antimonide core. Characterization of the fibers was accomplished with energy dispersive spectroscopy (EDS) for compositional analysis, electron backscatter diffraction (EBSD) for crystal orientation and grain size, optical and electron microscopy for physical fiber quality and optical transmission for core optical quality. A model was developed to relate the heat transfer with the grain structure of the fiber core. All of the fibers fabricated had a polycrystalline core with either no detectable oxygen in the case of the silicon fibers or low amounts of oxygen diffusion into the core as in the case of the GaSb fibers. Fiber lengths ranged from 7 cm for the initial silicon fibers to 60 cm and outside diameters down to 100 µm for n and p type silicon fibers. Core diameters for all fiber types ranged from 10 – 200 µm depending on the fabrication parameters. Lengths of major grains in the core are dependent on the core diameter and the pulling speed. The grain lengths of the major grains in the core generally increase in length with an increase in core diameter. Grain lengths in all fibers are thought to be suitable for use in fabrication of electronic structures in the core region with even the smallest average grain length of around 300 µm. This grain structure satisfies the grain boundary requirements for fabrication of boundary free p-n junctions and other more complicated electronic structures. Small core diameter fibers had better physical quality with fewer cracks and longer continuous length than the larger core fibers. / Ph. D.

Magnesium alloys are excellent material candidate to reduce mass of automotive structures, and as such to meet the Department of Energy's targets in fuel economy and clean energy. However, magnesium alloys show poor ductility at room temperature, which is one of the most important impediments to achieving cost-effective manufacturing of wrought alloys and insuring good energy absorption in crash structures. This Master thesis aims to identify the mechanisms behind the low ductility of magnesium. Therefore, non-destructive EBSD analyses upon tension of both a strong and weak textured magnesium alloy were conducted with a focus on the role of twinning in fracture initiation. This study revealed five mechanisms responsible for early fracture, all of which relate to twinning activity. These mechanisms were involved directly in the shear incompatibility arising from interactions between twin-twin, twin-slip, twin-grain boundary, and double twinning. Backstress played a major role in twin-grain boundary and twin-twin boundary interactions.

The automotive industry's search for stronger lighter materials has been hampered in its desire to make greater use of Magnesium alloys by their poor formability below 150°C. One current challenge is to identify the complex structure and deformation mechanisms at work and determine which of these are primary contributors to the nucleation of defects. Orientation Imaging Microscopy has been the most accessible tool for microstructural analysis over the past 15 years. However, using OIM to analyze defect nucleation sites requires prior knowledge of where the defects will occur because once the defects nucleate the majority of microstructural information is destroyed. This thesis seeks to contribute to the early detection of nucleation sites via three mechanisms: 1. Detection of cracks that have already nucleated, 2. Detection of surface topography changes that may indicate imminent nucleation and 3. Beam control strategies for efficiently finding areas of interest in a scan. Successive in-situ OIM scans of a consistent sample region while strain is increased, while using the three techniques developed in this thesis, will be employed in future work to provide a powerful defect analysis tool. By analyzing retrieved EBSD patterns we are able to locate defect / crack sites via shadowing on the EBSD patterns. Furthermore, topographical features (and potentially regions of surface roughening) can be detected via changes in intensity metrics and image quality. Topographical gradients are currently only detectable in line with the beam incidence. It is therefore suggested that the tensile specimens to be examined are orientated such that the resulting shear bands occur preferentially to this direction. The ability to refine the scan around these areas of interest has been demonstrated via an off-line adaptive scan routine that is implemented via the custom scan tool. A first attempt at a defect detection framework has been outlined and coded into MATLAB. These tools offer a first step to accessing the information about defect nucleation that researchers are currently seeking.

Modeling of plasticity is often hampered by the difficulty in accurately characterizing dislocationdensity on the microscale for real samples. It is particularly difficult to resolve measureddislocation content onto individual dislocation systems at the length scales most commonly of interestin plasticity studies. Traditionally, dislocation content is analyzed at the continuum levelusing the Nye tensor and the fundamental relation of continuum dislocation theory to interpret informationmeasured by diffraction techniques, typically EBSD or High Resolution EBSD. In thiswork the established Nye-Kroner method for resolving measured geometrically necessary dislocationcontent onto individual slip systems is assessed and extended. Two new methods are alsopresented to relieve the ambiguity of the Nye-Kroner method. One of these methods uses modifiedclassical dislocation equations to bypass the Nye-Kroner relation, and the other estimates the bulkdislocation density via the entry-wise one-norm of the Nye tensor. These methods are validatedvia a novel simulation of distortion fields around continuum fields of dislocation density based onclassical lattice mechanics and then applied to actual HR-EBSD scans of a micro-indented singlecrystals of nickel and tantalum. Finally, a detailed analysis of the effect of the spacing betweenpoints in an EBSD scan (which is related to the step size of the numerical derivatives used in EBSDdislocation microscopy) on geometrically necessary dislocation measurements is conducted.