La propagation des fissures courtes de fatigue dans un matériau polycristallin dépend fortement de la microstructure. Bien que de nombreuses études de caractérisation et de modélisation existent sur le sujet, la prédiction du chemin et de la vitesse de propagation de ce type de fissure n'est pas encore possible aujourd'hui.Afin de bien comprendre les mécanismes de propagation, la caractérisation in-situ d'un échantillon par la tomographie aux rayons X a été réalisée à l'ESRF en combinant deux techniques de caractérisation. La tomographie par Contraste de Diffraction (DCT) qui est une méthode non destructive permettant de caractériser en 3D la morphologie et l'orientation des grains constitutifs de la microstructure, à l'état non-déformé, et la tomographie par Contraste de Phase (PCT) qui permet d'obtenir la forme de fissure à divers étapes de la vie de l'éprouvette. Grâce à ces informations, il est possible de simuler la propagation de fissure en utilisant un maillage réaliste reconstruit à partir des images tomographiques. Dans ce travail, une étude de l'anisotropie de comportement élastique est effectuée dans un maillage microstructural 3D reconstruit à partir des images tomographiques. Cette étude permet de comparer les tenseurs de déformation élastique moyennés à chaque grain avec les mesures expérimentale. Ensuite, une nouvelle méthodologie est proposée pour simuler la propagation de fissure. Issue d'une simulation en plasticité cristalline, la direction et la vitesse de la propagation de fissure est déterminée par un post-traitement, ce qui permet de propager la fissure par remaillage. Cette méthode est appliquée dans un premier temps à un monocristal pré-fissuré pour prédire le trajet de fissuration en fonction des systèmes de glissement activés. L'ensemble de la démarche est enfin appliqué au polycristal complet imagé par tomographie. Le rôle du joint de grains et la vitesse de propagation sont également analysés. En comparant les résultats de simulation avec les mesures expérimentales, le critère de la propagation de fissure est discuté. / The short fatigue crack propagation in polycrystal materials depends strongly on microstructure. Although numerous studies of characterisation and of simulation, the prediction of the short fatigue crack propagation remains a challenge.In order to understand the mechanisms of short fatigue crack propagation, an in-situ characterisation by X-ray tomography was carried out at ESRF, using two techniques of tomography. Diffraction Contrast Tomography (DCT) that is a non-destructive method can be used to obtain 3D morphology and grain orientations in an undeformed state of polycrystal materials. Couple with Phase Contrast Tomography (PCT), it allows to characterise the short fatigue crack propagation at different loading stages. Access to this information, it is possible to simulate the short fatigue crack propagation using a 3D reel microstructural mesh reconstructed from the tomographic images.In this work, the elastic anisotropic behaviour in a 3D microstructural mesh is performed. The elastic strain tensors averaged in grains are also compared to the experimental measurements. Then, a new numerical approach is proposed to simulate crack propagation. From a crystal plasticity FE simulation, the crack growth direction is determined by a post processing. Next, the crack is propagated through remeshing. This approach is firstly applied to the single crystals, then to the polycrystal mesh reconstructed from the tomographic images. The grain boundary effects and the crack growth rate are also analysed. By comparing between simulation and experimental crack, the damage indicator is discussed at the end.

Concrete substructures are often subjected to environmental deterioration, such as sulfate and acid attack, which leads to severe damage and causes structure degradation or even failure. In order to improve the durability of concrete, the High Performance Concrete (HPC) has become widely used by partially replacing cement with pozzolanic materials. However, HPC degradation mechanisms in sulfate and acidic environments are not completely understood. It is therefore important to evaluate the performance of the HPC in such conditions and predict concrete service life by establishing degradation models. This study began with a review of available environmental data in the State of Florida. A total of seven bridges have been inspected. Concrete cores were taken from these bridge piles and were subjected for microstructural analysis using Scanning Electron Microscope (SEM). Ettringite is found to be the products of sulfate attack in sulfate and acidic condition. In order to quantitatively analyze concrete deterioration level, an image processing program is designed using Matlab to obtain quantitative data. Crack percentage (Acrack/Asurface) is used to evaluate concrete deterioration. Thereafter, correlation analysis was performed to find the correlation between five related variables and concrete deterioration. Environmental sulfate concentration and bridge age were found to be positively correlated, while environmental pH level was found to be negatively correlated. Besides environmental conditions, concrete property factor was also included in the equation. It was derived from laboratory testing data. Experimental tests were carried out implementing accelerated expansion test under controlled environment. Specimens of eight different mix designs were prepared. The effect of pozzolanic replacement rate was taken into consideration in the empirical equation. And the empirical equation was validated with existing bridges. Results show that the proposed equations compared well with field test results with a maximum deviation of ± 20%. Two examples showing how to use the proposed equations are provided to guide the practical implementation. In conclusion, the proposed approach of relating microcracks to deterioration is a better method than existing diffusion and sorption models since sulfate attack cause cracking in concrete. Imaging technique provided in this study can also be used to quantitatively analyze concrete samples.

Manufacturing of light-weight materials is associated with several types of casting defects during solidification. Porosity defects are common, especially in aluminum and its alloys, which initiate crack propagation and thereby cause drastic deterioration in the mechanical properties. These defects, classified as micro and macro defects (based on their sizes), are mainly governed by release of hydrogen into the liquid at the solid-liquid interface, which triggers the nucleation and growth of hydrogen bubbles in the melt. Subsequently, these bubbles interact with solidifying interfaces such as dendritic arms and eutectic fronts, leading to the formation of pores. Macroscopic defects in the form of voids are created due to solidification shrinkage. The primary focus of the present work is to develop phenomenological models for the evolution of microporosity and microstructures during solidification. The issues outlined above typically occur in multi-phase environments comprising of solid, liquid and gaseous phases, and over a range of length and time scales. Any phenomenological prediction would, therefore, require a multi-phase-scale approach. Principles of volume averaging are applied to equations of conservation to obtain single-field formulations. These are then solved with appropriate interface tracking techniques such as Enthalpy, Level-set, Volume-of-fluid and Immersed-boundary methods. The framework is built up on a standard pressure based incompressible fluid flow solver (SIMPLER algorithm) and coupled modeling strategies are proposed to address the interfacial dynamics. A two-dimensional framework is considered with a fixed-grid Cartesian co-ordinate system. Scaling analyses are performed to bring out the relative effects of various competing parameters in order to obtain further insights into this complex phenomenon. The numerical results and scaling predictions are validated against experimental observations published in literature. In literature, numerical predictions of microporosity mainly include criteria based models based on empirical relations and deterministic/stochastic models based on diffusion driven growth assuming spherical bubbles. The dynamic evolution of non-spherical bubble-metal interface in a three-phase system is yet to be captured. Moreover, several in-situ experiments have shown elongated bubble shapes during the engulfment phase, therefore a criterion to define the dependence on cooling rates and the resulting bubble morphology can possibly deliver further practical insights. We propose a numerical model for hydrogen bubble growth, its movement and subsequent engulfment by a solidifying front, combining the features of level-set and enthalpy methods for tracking bubble-metal and solid-liquid interfaces, respectively. The influx of hydrogen into heterogeneously nucleated bubbles results in growth of bubbles to sizes up to a few hundreds of microns. In the first part of this numerical study, a methodology based on the level-set approach is developed to simultaneously capture hydrogen bubble growth and movement in liquid aluminum. The solidification is first assumed to occur outside the micro-domain providing a specified hydrogen influx to the bubble-in-liquid system. The level-set equation is formulated in such a way as to account for simultaneous growth and movement of the bubble. The growth of a bubble with continuous and fixed hydrogen levels in the melt is studied. The rates of growth of bubble-liquid and solidifying interfaces are compared using an order of magnitude analysis. This scaling analysis explains the thought experiment proposed in the literature, where difference in bubble shapes was attributed to the cooling rate. Moreover, it shows explicit dependence on bubble radius and cooling rate leading to a new criterion for bubble elongation proposed in this thesis. This also highlights the comparison between solidification and hydrogen diffusion time-scales which primarily govern the competitive growth behavior. The bubble-in-liquid model is coupled with microscopic enthalpy method to incorporate effects of solidification and study the interaction of solid-liquid and bubble-liquid interfaces. The phenomena of bubble engulfment and elongation are successfully captured by the proposed model. A parametric study is carried out to estimate the bubble elongation based on different initial bubble sizes and varying cooling rates encountered in typical sand, permanent mold and die casting processes. Although simulation of microstructures has been extensively studied in the literature, very few models address the phenomena of simultaneous growth and movement of equiaxed dendrites. The presence of different flow environments and multiple dendrites are known to alter the position and shape of the dendrites. The proposed model combines the features of the following methods, namely, the Enthalpy method for modeling growth; the Immersed Boundary Method (IBM) for handling the rigid solid-liquid interfaces; and the Volume of Fluid (VOF) method for tracking the advection of the dendrite. The algorithm also performs explicit-implicit coupling between the techniques used. Validation with available literature is performed and dendrite growth in presence of rotational and buoyancy driven flow fields is studied. The expected transformation into globular microstructure in presence of stirring induced flows is successfully simulated. A simple order estimate for time required for stirring is performed which agrees with numerical predictions. In buoyancy driven environment of a settling dendrite, the arm tip speeds show expected higher velocity of the upstream tip compared to its counterpart. The model is extended to study thermal and hydrodynamic interactions between multiple dendrites with appropriate considerations for different orientations and velocities of the dendritic solid entities. The present model can be used for the prediction of grain sizes and shapes and to simulate morphological transformations due to different melt flow scenarios. In the final part, the methodology presented for growth and engulfment of hydrogen bubbles is extended to study the phenomenon of diffusion driven bubble growth occurring in direct foaming of metals. The source of hydrogen is determined by the rate of decomposition of the blowing agent. This is accounted for by a source term in the hydrogen species conservation equation, and growth rate of hydrogen bubbles is calculated on the basis of diffusive flux at the interface. The level-set method is used for tracking the bubble-liquid interface growth, and the macroscopic enthalpy model is used for obtaining heat transfer and solid front position. The model is validated with analytical solution by comparing the front position and the solidification time. The variation of foam density with a transient hydrogen generation source is studied and qualitatively compared with results reported in literature. The modeling strategies proposed in this work are generic and therefore have potential in simulating a variety of complex multi-phase problems.

In this thesis, we present an experimental and numerical study of globularization during reheating of thixocast billet having non-dendritic microstructure. The process of reheating is an important step in the semisolid processing and is essential to control its microstructure and hence its mechanical properties. Material chosen for this study is Aluminum alloy, A356. The primary focus of this study is the heat treatment below eutectic temperature i.e. transformation in solid phase. It is found that during short duration heat treatment, globularization of primary α grains and spheroidization of eutectic Si flakes take place which improves the mechanical properties of semisolid cast products significantly. A prolonged heat treatment is found to degrade the properties of castings since it enhances the porosity and coarsening of Si. The study suggests that a precise heat treatment practice can be designed to improve the semisolid microstructure. A computational model based on Phase field approach has been proposed to study this phenomena. Predictions based on this model are qualitatively compared with corresponding experimental observations. Since eutectics form an important step in multiphase solidification, an attempt has been made to develop an enthalpy based explicit micro-scale model for eutectic solidification. In this preliminary study, growth of adjacent α and β phases in a two dimensional Eulerian framework has been simulated. The model is qualitatively validated with Jackson Hunt theory. Results show expected eutectic growth. This methodology promises significant saving in computational time compared to existing numerical models.

Filmes amorfos de nitreto de alumínio (AlN) foram preparados por sputtering de rádio frequência convencional em um alvo de Al+Cr e plasma de nitrogênio puro. A área relativa de Al-Cr determina o conteúdo de Cr, o qual esteve em um intervalo de concentração de ~ 0 3.33 at.% no presente estudo. A deposição dos filmes foi seguida por tratamento térmico das amostras até 1050 ºC e por caracterização espectroscópica através de medidas de EDS (Energy Dispersive Spectrometry), Foto-luminescência e Transmissão Óptica. De acordo com os resultados experimentais, as propriedades óptico-eletrônicas dos filmes de AlN contendo Cr são altamente influenciadas tanto pela concentração de Cr como pela temperatura de tratamento térmico. Na verdade, o tratamento térmico a 1050 ºC induz o desenvolvimento de estruturas que, devido ao seu tamanho típico e características espectrais exclusivas, foram designadas por micro-estruturas de rubi (RbMSs). Estas RbMSs são rodeadas por um meio rico em nitrogênio no qual os íons Cr3+ apresentam características luminescentes não encontradas na literatura. A emissão de luz apresentada pelas RbMSs e suas vizinhanças foram investigadas de acordo com o conteúdo de Cr e a temperatura de medida permitindo a identificação de várias linhas luminescentes relatadas do Cr3+. As principais características destas linhas luminescentes e correspondentes processos de recombinação-excitação são apresentados e discutidos tendo em vista uma análise espectroscópica detalhada. / Films of amorphous aluminum-nitride (AlN) were prepared by conventional radio frequency sputtering of an Al+Cr target in a plasma of pure nitrogen. The Cr-to-Al relative area determines the chromium content, which stayed in the ~ 0 3.33 at.% concentration range in the present study. Film deposition was followed by thermal annealing the samples up to 1050 ºC and by spectroscopic characterization through energy dispersive spectrometry (EDS), Photo-luminescence and Optical Transmission measurements. According to the experimental results, the optical-electronic properties of the Cr-containing AlN films are highly influenced by both the Cr concentration and the temperature of the thermal treatments. In fact, thermal annealing at 1050 °C induces the development of structures which, because of their typical size and unique spectral characteristics, were designated by ruby microstructures (RbMS\'s). These RbMS\'s are surrounded by a nitrogen-rich environment in which Cr3+ ions exhibit luminescent features with no counterpart in the literature. The light emission presented by the RbMS\'s and surroundings were investigated according to the Cr content and temperature of measurement allowing the identification of several Cr3+-related luminescent lines. The main characteristics of these luminescent lines and corresponding excitation-recombination processes are presented and discussed in view of a detailed spectroscopic analysis.

Epithelial tissues, one of the four primary tissue structures found in our human body, are known to comprise of tiny cells interconnected in a unique continuous pattern. In most cases, they serve a dual purpose of protecting the internal organs from physical damage, and at the same time, enable in facilitating inter-cellular activities and prevent pathogen break ins. While the tissue mechanics and its proliferation have been scrutinized to great detail, it is their geometric uniqueness, that has remained more or less unexplored. With an intent of doing the same, this thesis identifies and explores those geometric properties/parameters that have an influence on the micro structure’s homogenized and localized response. However, it does so by extracting the microstructures profile and representing its cell edges via three dimensional beam elements - hence the name, bio-inspired structures. The analysis is carried out by first developing a staggered Representative Volume Element (RVE)using finite elements, and identifying its appropriate size. The staggered assembly aids in minimizing boundary effects from creeping in, and at the same time, provides the requisite statistical homogeneity. This is followed by the geometry study. A wide range of epithelial geometries are considered for the study, ranging from completely isotropic skin models, to in plane anisotropic cuboidal structures and out of plane anisotropic stratified geometries. The effects of orientation, relative density and edge length are extracted and studied in great detail. It is observed that cell edges initial orientation has a direct dependence on the particle distribution, whereas the change in orientation is largely dependent on the deformation the microstructure is subjected to. Relative density is documented to show a direct correlation to a materials homogenized response i.e. larger the relative density, greater is the microstructures stiffness and homogenized stress response to the same deformation. Edge length, on the other hand is observed to showcase a downward trend on the cell edge’s axial stress. On average, in any kind of distribution and any kind of deformation, smaller cell edges are known to showcase larger stresses, as compared to the larger cell edges.

This master´s thesis focuses on duplex microstructures preparation by powder metallurgy. A hybrid material can be created by combining two or more existing materials in different geometries, and thus the newly formed composite can provide a superposition of the properties of the starting materials (powders). This means that it will have an improved combination of the required properties. The theoretical part describes in detail the hybrid materials and the architectured materials that contain highly controlled structures. Structure control allows to change the variety of possible geometries and opens up a number of other useful properties. Therefore, this thesis also deals with the mechanical alloying and SPS. The experimental part describes procedures of preparation of four samples of composites with a duplex structure from a powder of a significantly tough alloy (austenitic steel 316L) in combination with a powder of a significantly strong alloy (titanium carbonitride). A crucial part of this thesis is characterization of these four samples by electron microscopy methods (SEM, TEM, EDS) and supported by hardness measuring.

Photopolymerization is a technique used to create surface structures or microobjects from a photoresist. This process is started by illuminating the sample with a light of proper wavelength absorbed by the resist. After exposure, the sample is processed according to the type of the photoresist – be it heating, treating with developer or just washing the unaffected monomer with some reagent. Focused femtosecond laser beam with double wavelength can be used in the process. Short pulse length with high photon density starts two-photon absorption localized in the vicinity of focal point. The method resolution is thus increased and details with 1/10 micrometer size can be created. Moreover, very short laser pulse decreases the heat affected zone and the risk of thermal initiation is minimized. Manufacturing of larger structures composed of tiny details with two-photon photopolymerization is time-demanding process. Therefore, we have complemented the optical setup with spatial light modulator (SLM), which splits the incoming laser beam into several beams with holograms dynamically generated by a computer. Polymerization can be thus performed by multiple foci simultaneously which can be used to create separated microparticles or periodical surface structures. Additional speed improvement of the process can be substitution of static configuration, requiring sample replacement after each exposition, with continuous setup using microfluidic channel steadily supplied with photoresist transported to the active region of the sample.

Notre thèse porte sur l’histoire culturelle des dictionnaires bilingues français ↔ chinois. Notre but est d’examiner l’histoire des dictionnaires à travers les éditeurs, les lexicographes et les imprimeurs afin de trouver des caractéristiques du corpus sélectionné et d’établir une typologie des dictionnaires inventoriés. Cette étude apporte des éléments aux futurs travaux sur la lexicographie bilingue française et chinoise. Notre travail est divisé en deux parties : étude historique et étude métalexicographique. Dans l’analyse historique, un rappel de l’histoire de la Chine est donné dans un premier temps pour établir un panorama du contexte d’étude. Les chapitres suivants traitent de questions concernant l’apparition des dictionnaires bilingues en Chine et leur développement, les éditeurs et les imprimeurs, les lexicographes. Dans la partie métalexicographique, l’accent est mis sur les paratextes, les macrostructures, les nomenclatures et les microstructures. Notre recherche a porté sur l’ensemble des études lexicographiques bilingues françaises et chinoises. / Our thesis deals with the cultural history of the French ↔ Chinese bilingual dictionaries. Our aim is to examine the history of dictionaries through their publishers, lexicographers and printers in order to find characteristics of the selected corpus and to establish a typology of the inventoried dictionaries. This study provides ideas for future work on French and Chinese bilingual lexicography. Our work is divided into two parts : historical study and metalexicographical study. In the historical analysis, a reminder of the chinese history is given at the outset to expose a panorama of the study’s context. The following chapters deal with questions concerning the emergence of bilingual dictionaries in China and their development, publishers and printers, and lexicographers. In the metalexicographic part, emphasis is placed on paratexts, macrostructures, nomenclatures and microstructures. Our research has contributed to the study of French and Chinese bilingual lexicographic.

In der vorliegenden Arbeit wird ein neues Verfahren zur Dünnschichtverkappung von oberflächennahen Mikrostrukturen vorgestellt. Ausgehend von den speziellen Anforderungen an die Verkappung oberflächennaher Mikrostrukturen, insbesondere von Strukturen mit hohem Aspektverhältnis, wurden die Verwendung eines Fluor-Kohlenstoff-Polymers als Opferschichtmaterial und die Eignung unterschiedlicher Schichtstapel zur Realisierung der Dünnschichtkappe untersucht. Die resultierende Technologie ermöglicht eine durchgehend trockenchemische Prozessierung. Für die Abschätzung der notwendigen Schichtdicken und den geometrischen Entwurf der Kappenstrukturen, wurden auf Basis der Plattentheorie analytische und numerische Modelle erstellt. Verschiedene Materialkombinationen bestehend aus Siliziumoxid, Siliziumnitrid und Aluminium wurden hinsichtlich ihrer mechanischen und thermomechanischen Eigenschaften untersucht und bewertet. Ein weiterer Schwerpunkt lag auf der Entwicklung und Optimierung der Opferschichtprozesse, sowie deren Integration in die Gesamttechnologie. Die Eignung der plasmagestützten Prozesse zur Abscheidung und Strukturierung des Opferpolymers wurde durch die Fertigung von verkapselten Beschleunigungssensoren nachgewiesen. Ein ausreichender hermetischer Verschluss der Dünnschichtkappe konnte durch die Messung der viskosen Dämpfung an Feder-Masse-Schwingern bestätigt werden.