Les modèles basés sur la mécanique des milieux continus prévoient généralement une déformation à la rupture plus élevée, ainsi qu'une durée de vie en fluage beaucoup plus longue que les valeurs observées expérimentalement. Cette thèse met en évidence deux aspects de cette problématique en analysant l’endommagement à l'aide de tomographie in situ à rayons X de synchrotron et reconstruction 3D de la structure polycristalline par polissages successifs.L’endommagement en termes de fraction surfacique des cavités a été identifié dans les couches de reconstructions tomographiques perpendiculairement à l’axe de déformation. L'évolution de la fraction surfacique des cavités a été comparée avec le modèle de prédiction de Cocks et Ashby. Ce dernier surestime la durée de vie en fluage et sous-estime l’état de l’endommagement. L'importance de l'hétérogénéité initiale de l’endommagement et l’effet de localisation de l’endommagement est également souligné. L'amplitude de la plus grande fluctuation surfacique augmente de façon parabolique en fonction de la fraction surfacique moyenne.Une méthode de sectionnement sériel améliorée basée sur la profilométrie de surface a été développée. Elle permet la mesure précise de l'épaisseur du matériau enlevée localement. Les analyses ont montré que l'emplacement des cavités par rapport aux joints de grains et l’orientation cristallographique des grains au voisinage est similaire pour les échantillons déformé par différents mécanismes de fluage. La population relative des cavités de fluage présente aux joints de grains simples est supérieure à celle présente aux joints triples. Les cavités trouvées aux joints triples, cependant, sont plus grandes. / Power law creep damage is one of the most intriguing unsolved phenomena of materials science. Models based on continuum mechanics generally predict a much higher strain to failure, as well as a much longer creep lifetime than experimentally observed values. This thesis highlights two aspects of this problematic by analyzing creep damage in copper using in situ synchrotron tomography and 3D reconstruction of the damaged polycrystal structure by serial sectioning.Damage in terms of the area fraction of voids was first identified in slices of tomographic reconstructions of creep deformed copper. The local and global evolution of cavities area fraction was checked against the Cocks and Ashby model and it was found that the model overestimates creep lifetime and underestimates damage development. The importance of the initial damage heterogeneity and the role of damage localization are also emphasized. It was found that the amplitude of the largest damage fluctuation increases parabolically as a function of cavity’s mean area fraction.An improved serial sectioning method based on surface profilometry was developed, which allows the accurate measurement of the removed local material thickness. The 3D reconstructions enabled identifying the creep voids and the grains of the polycrystal. It was shown that with the exception of the void shape, the relationship between void location at a given grain boundary and crystallographic orientation of the neighbor grains is similar in samples deformed by different creep mechanisms. The relative population of creep voids is higher at simple grain boundaries than at triple junctions. Voids found at a triple boundary, however, are larger.

Vacuum-Arc Remelting (VAR) is an important process for manufacturing Ti- and Ni-based superalloys. Currently, the sources and mechanisms behind microstructural anomalies produced in VAR superalloy ingots are not well understood. In order to help understand formation processes, a method of characterizing specific anomalies in VAR ingots is desired. This paper presents a method of characterizing the composition and morphology of anomalies in VAR alloy ingots using a combination of serial sectioning and X-ray fluorescence (XRF) energy dispersive spectroscopy (EDS) techniques. This process is demonstrated on a dirty white spot from an Alloy 718 sample. The white spot of interest was serial polished and 2-D XRF EDS maps were acquired at each polish depth. The EDS maps were then stacked to form a 3-D representation of the white spot. In addition, SEM and optical microscopy techniques were used to further characterize the composition and morphology of the dirty white spot. The dirty white spot is composed of both Ti-enriched and Nb-depleted regions. The 2-D EDS maps acquired with the XRF equipment provided adequate contrast for creating a 3-D representation of the Ti-rich region of the dirty white spot. However, contrast was not sufficient to create a 3-D representation of the Nb-depleted region. The XRF EDS equipment combined with SEM and optical microscopy techniques provided valuable information about the morphology and composition of the Alloy 718 dirty white spot. It is concluded that this dirty white spot was produced by fall-in from either the crown or shelf regions during the VAR process. / text

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<p>  </p> <p>Transition to a sustainable power grid entails the use of all net-zero carbon emission technology that is currently available. Liquid metal-cooled fast nuclear reactors (LMFRs) are technologies capable of competitively providing power while attaining sustainability and reliability. Uranium-zirconium metallic alloys have been proposed as LMFRs fuels based on the performance of the fuel in experimental scale reactors, achieving up to 20 at.% burn-up. The following phenomena affects the irradiation performance of U-Zr fuels: constituent redistribution, swelling, fuel-cladding mechanical interaction (FCMI), and fuel-cladding chemical interaction (FCCI). Further understanding of these phenomena, and development of predictive models requires data collection of variables such as composition, morphology of the redistribution regions, porosity distribution, porosity morphology, fission gas release, and the relation between local composition and porosity evolution. </p> <p>To achieve this, focused ion beam-scanning electron microscopy (FIB-SEM) serial sectioning was applied to specimens from the different compositional regions developed during constituent redistribution of a U-10 wt.% Zr fuel neutron irradiated to 5.7 at.% burn-up. High-resolution backscattered electron (BSE) micrographs, and energy dispersive spectroscopy (EDS) spectra were obtained for several sections of each specimen. Each section was analyzed to identify the microstructural and compositional evolution in the specimen volume. Three-dimensional porosity and phase volume distribution was obtained using image processing and three-dimensional object classification. The study revealed local segregation of phases within each of the regions, porosity distribution dependency on temperature and local composition, preferential porosity nucleation sites, porosity evolution trends, interconnectivity, possible sinks/nucleation sites for porosity and precipitates, as well as possible mechanisms for fission gas release.</p>

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Die dreidimensionale Mikrostruktur, welche bei der Oberflächenkristallisation von Glaskeramiken entsteht, wird mittels einer neuartigen Methode zur Präparation von abgesenkten Probenoberflächen untersucht. Diese Initialkantensektionierungsmethode, welche auf der Erzeugung von Scharten in der Probenoberfläche und anschließender Glanzwinkelionenstrahlerosion basiert, erlaubt das rapide Freilegen von großflächigen Schichten in wohldefinierten Tiefen unterhalb der ursprünglichen Probenoberfläche. In dieser Dissertation werden mehrere Variationen der Technik durch Kombination von Laserablation, Ionenbreit- sowie Ionenfeinstrahlerosion untersucht und miteinander verglichen. Die in Bezug auf Schnittgeometrie und Probengüte relevanten, experimentellen Parameter werden bestimmt und bewertet. Ein Modell zur Beschreibung der zeitlichen Evolution der Probengeometrie während des Erosionsvorgangs wird auf Grundlage von Simulationen und analytischen Näherungen aufgestellt und mit experimentellen Ergebnissen verglichen. Schließlich wird die Initialkantensektionierungsmethode mit Elektronenrückstreubeugung kombiniert um Wachstumseffekte bei der Oberflächenkristallisation von Diopsid- und Ba2TiSi2O8-Fresnoitglaskeramiken zu untersuchen.:1 Introduction 1.1 Motivation 1.2 Aims and Objectives 2 Literature Review 2.1 Sample Preparation for Electron Backscatter Diffraction Studies 2.2 Serial Sectioning Methods 2.3 Microstructure Characterization of Glass Ceramics using EBSD 2.4 Interim Conclusion 3 Theory 3.1 Erosion of a Surface Under Ion Bombardment 3.1.1 Sputtering 3.1.2 Kinetic Theory of Surface Evolution 3.1.3 Numerical Simulation of Surface Erosion 3.1.4 Erosion of a Surface With Initial Notches 3.2 Electron Backscatter Diffraction 3.2.1 Measurement Principle 3.2.2 Representation of Orientations and Texture 4 Methods and Materials 4.1 Sample Preparation and Processing 4.2 Surface Metrology 4.3 Microstructure Analysis 4.4 Materials 5 Erosion of Surfaces With Initial Notches 5.1 Evaluation of Surface Processing Methods 5.1.1 Notch Creation 5.1.2 Terrace Formation by Glancing-Angle Ion Beam Erosion 5.2 Surface Properties in the Terrace Region 5.2.1 Terrace Roughness 5.2.2 Ion Beam Induced Amorphization 5.3 Evolution of Surface Geometry 5.3.1 Linear Model 5.3.2 Simulations 5.3.3 Experimental Results 5.4 Discussion 5.4.1 Sample Processing 5.4.2 Sample Quality 5.4.3 Kinetic Model of Surface Evolution 6 Depth-Resolved Microstructure Characterization Using Initial Notches 6.1 Diopside 6.2 Ba2TiSi2O8 fresnoite (BTS) 6.3 Discussion 6.3.1 Methodological Aspects of Initial Notch Sectioning 6.3.2 Microstructure Analysis on Surface-Crystallized Glass Ceramics 7 Summary and Outlook / Three-dimensional microstructures resulting from surface crystallization of glass ceramics are studied using a novel sample sectioning method. Based on the creation of notches on the sample surface and subsequent glancing-angle ion beam erosion, initial notch sectioning enables the rapid excavation of large subsurface layers at well-defined depths. In this thesis, several variations of this technique using different combinations of laser ablation, broad and focused ion beam erosion are realized and compared to each other. Relevant parameters controlling the section geometry and quality are determined. A model of the surface evolution kinetics is developed using simulations and analytical estimates, which is compared to experimental results. Finally, initial notch sectioning in combination with electron backscatter diffraction is applied to elucidate growth phenomena in the surface crystallization of diopside and Ba2TiSi2O8 fresnoite glass ceramics.:1 Introduction 1.1 Motivation 1.2 Aims and Objectives 2 Literature Review 2.1 Sample Preparation for Electron Backscatter Diffraction Studies 2.2 Serial Sectioning Methods 2.3 Microstructure Characterization of Glass Ceramics using EBSD 2.4 Interim Conclusion 3 Theory 3.1 Erosion of a Surface Under Ion Bombardment 3.1.1 Sputtering 3.1.2 Kinetic Theory of Surface Evolution 3.1.3 Numerical Simulation of Surface Erosion 3.1.4 Erosion of a Surface With Initial Notches 3.2 Electron Backscatter Diffraction 3.2.1 Measurement Principle 3.2.2 Representation of Orientations and Texture 4 Methods and Materials 4.1 Sample Preparation and Processing 4.2 Surface Metrology 4.3 Microstructure Analysis 4.4 Materials 5 Erosion of Surfaces With Initial Notches 5.1 Evaluation of Surface Processing Methods 5.1.1 Notch Creation 5.1.2 Terrace Formation by Glancing-Angle Ion Beam Erosion 5.2 Surface Properties in the Terrace Region 5.2.1 Terrace Roughness 5.2.2 Ion Beam Induced Amorphization 5.3 Evolution of Surface Geometry 5.3.1 Linear Model 5.3.2 Simulations 5.3.3 Experimental Results 5.4 Discussion 5.4.1 Sample Processing 5.4.2 Sample Quality 5.4.3 Kinetic Model of Surface Evolution 6 Depth-Resolved Microstructure Characterization Using Initial Notches 6.1 Diopside 6.2 Ba2TiSi2O8 fresnoite (BTS) 6.3 Discussion 6.3.1 Methodological Aspects of Initial Notch Sectioning 6.3.2 Microstructure Analysis on Surface-Crystallized Glass Ceramics 7 Summary and Outlook

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