The ductile fracture process, which consists of the nucleation, growth and coalescence of microvoids, was extensively studied for materials deforming homogeneously. For materials with a non-homogeneous deformation behavior, such as those having hexagonal closed packed (HCP) crystal structure, experimental and numerical data is lacking. Therefore, the fracture properties of materials with such HCP structure, like titanium (used in aerospace and biomedical applications), zirconium (nuclear industry) and magnesium (manufacturing industry) are not well understood. The main research objective of this Ph.D. thesis is to better understand the mechanisms governing fracture in commercially pure (CP) titanium. In particular, the effect of grain orientation on void growth is investigated. The fracture process of CP titanium was visualized in model materials containing artificial holes. These model materials were fabricated using a femtosecond laser coupled with a diffusion bonding technique to obtain voids in the interior of titanium samples. Diffusion bonding was carried out either above or below the phase transformation temperature resulting in different microstructures. Changes in void dimensions during in-situ straining were recorded in three dimensions using x-ray computed tomography. Void growth obtained experimentally was compared with the Rice and Tracey model which predicted well the average void growth. However, a large scatter in void growth was observed experimentally and was explained in terms of differences in grain orientation which was confirmed by crystal plasticity simulations. It was also shown that grain orientation has a stronger effect on void growth than intervoid spacing and material strength. Intervoid spacing, however, appears to control whether the intervoid ligament failure is ductile or brittle. While this study showed a good agreement between experiments and simulations on average, there is no direct void growth comparison for particular grain orientations. In a follow-up study, an experimental approach was developed to directly relate the growth of a void to its underlying grain orientation. This is achieved by first annealing CP titanium samples below the α-β phase transformation temperature, then performing electron backscatter diffraction iii (EBSD) and finally diffusion bonding the samples together. Samples were then tested in x-ray tomography. This study showed the importance of the local state of strain on void growth. Crystal plasticity simulations that take into account the particular grain orientation and the local state of strain were found to predict well experimental void growth. Crystal plasticity simulations confirmed that the orientation of the voidcontaining grain is more important than the orientation of surrounding grains and more important than the volume fraction of voids, in order to determine void growth. This thesis on the growth and coalescence of voids is important to validate and improve the predictions of ductile fracture models and to design new materials with improved fracture properties.

<div> <div> <div> <p>Composite materials have become widely used in engineering applications, in order to reduce the overall weight of structures while retaining their required strength. Due to their light weight, relatively high stiffness properties, and formability into complex shapes, discontinuous fiber composites are advantageous for producing small and medium size components. However, qualifying their mechanical properties can be expensive, and therefore there is a need to improve predictive capabilities to help reduce the overall cost of large scale testing. To address this challenge, a composite material consisting of discontinuous glass fibers in a polypropylene matrix is studied at the microstructural level through coupled experiments and simulations, in order to uncover the mechanisms that cause microvoids to initiate and progress, as well as certain fiber breakage events to occur, during macroscopic tension. Specifically, this work coupled in-situ X-ray micro computed tomography (μ-CT) experiments with a finite element simulation of the exact microstructure to enable a 3D study that tracked damage initiation and propagation, and computed the local stresses and strains in the microstructure. In order to have a comprehensive 3D understanding of the evolution of the microstructure, high fidelity characterization procedures were developed and applied to the μ-CT images in order to understand the exact morphology of the microstructure. To aid in this process, ModLayer - an interactive image processing tool - was created as a MATLAB executable, and the 3D microstructural feature detection techniques were compared to traditional destructive optical microscopy techniques. For damage initiation, this work showed how high hydrostatic stresses in the matrix can be used as a metric to explain and predict the exact locations of microvoid nucleation within the composite’s microstructure. From a damage propagation standpoint, matrix cracking - a mechanism that has been notably difficult to predict because of its apparent stochastic nature - was studied during damage propagation. The analysis revealed the role of shear stress in fiber mediated flat matrix cracking, and the role of hydrostatic stress in fiber-avoidance conoidal matrix cracking. Overall, a sub-fiber simulation and an in-situ experimental analysis provided the microstructural physical phenomena that govern certain damage initiation and progression mechanisms, further enabling the strength and failure predictions of short fiber thermoplastic composites. </p></div></div></div>

Le bois possède des propriétés physiques remarquables mais qui dépendent étroitement du taux d’humidité dans le matériau. Du fait de sa structure multi-échelle et des différents états de l’eau dans le bois, les mécanismes de transferts d’eau dans le bois sont encore mal appréhendés. Nous étudions les phénomènes physiques essentiels à l’origine des propriétés d’imbibition et de séchage du bois de feuillu. On montre d’abord par des expériences macroscopiques classiques, que la dynamique d’imbibition d’eau dans le bois est significativement ralentie (plusieurs ordres de grandeur) par rapport aux prédictions du modèle de Washburn utilisant la perméabilité et la mouillabilité du bois mesurées indépendamment. Les distributions d’eau liée et d’eau libre obtenues par IRM au cours de l’imbibition montrent que l’eau liée adsorbée dans les parois cellulaires progresse en fait (par diffusion) plus vite que l’eau libre dans les pores. Il faut attendre que les parois soient saturées en eau liée pour que l’eau libre avance à son tour dans les lumens du bois. L’analyse des images tomographiques aux rayons X suggèrent que le ralentissement de la pénétration d’eau liquide dans le bois est dû à la modification des conditions de mouillage par la teneur en eau liée dans les parois. Les expériences d’imbibition avec un « bois artificiel » à base d’hydrogel confirment cette hypothèse. Finalement, l’étude du séchage du bois par IRM montre également différentes dynamiques de séchage pour l’eau liée et l’eau libre. Le séchage du bois est contrôlé par l’évaporation d’eau libre à partir d’un front sec à des teneurs en eau élevées. L’évaporation d’eau liée ne devient significative qu’à partir de la disparition totale de l’eau libre / Wood has excellent physical properties which however depend closely on the moisture content in the material. Because of its multi-scale structure and different states of water existing in the material, the mechanisms of water transfers in wood are still poorly understood. The essential phenomena at the origin of imbibition/drying properties of hardwood are studied in this thesis. We first show with classical macroscopic measurements that, water imbibition in wood is significantly damped compared to Washburn’s law which predicts the dynamic of capillary imbibition in the porous medium. The bound water and free water distributions obtained by MRI during imbibition show that, the bound water adsorbed in cell walls diffuses more quickly than the free water located in the pores. Free water cannot penetrate in the pores unless the cell walls have been saturated with bound water. The tomographic image analysis reveals that the damped dynamic of liquid water penetration in wood is due to the modification of wetting conditions by bound water content in the cell walls. Imbibition Tests with a hydrogel-based “artificial wood” confirm our hypothesis. Finally, the observations of wood drying by MRI show also different drying dynamics for bound and free water. At high moisture content, wood drying is controlled by the evaporation of free water from a dry front. Bound water starts to evaporate significantly only after the total disappearance of free water

There are many large-scale contacting methods for gas reactions requiring a solid catalyst. The catalytic gas-solid Fluidized Bed Reactor (FBR) is one of the popular methods in industry. In FBRs the bulk of the gas throughput is present as lean bubbles, mostly deprived of solids, bubbling through a solids-rich emulsion phase. The movement of gas into and out of the emulsion often dictates the performance of an FBR. During the past five decades major contributions have been made towards the understanding of FBRs, although numerous gaps still exist, especially at higher bubbling regime velocities. This work follows an integrated approach for the simultaneous measurement of hydrodynamics and reactor performance. Hydrodynamics are measured using fast X-Ray Tomography (XRT), pressure analysis techniques and an optical fibre probe. Reactor performance is measured by utilizing the ozone decomposition reaction. Performance is quantified using a basic two-phase reactor model with an apparent overall interphase mass transfer (K0) parameter. Two 14 cm (ID) fluidized bed columns are used, one setup supporting the ozone decomposition reaction and the other installed within a fast XRT facility. Special emphasis is placed on superficial velocities (U0) spanning the entire bubbling regime up to the onset of the turbulent regime (Uc). The particle types employed are Geldart B sand particles and highly dense ferro-silicon (FeSi) particles. Fines are added to both particle types, resulting in a total of four particle systems (sand baseline; sand with fines; FeSi baseline; FeSi with fines). Time constraints on the XRT equipment limited the tomography measurements to the sand baseline particle system. The hydrodynamics of the other particle systems were limited to the pressure signal and optical probe measurements of the ozone decomposition setup. The results of the sand baseline system suggest that a distinction should be made between the low-interaction bubbling regime and the high-interaction bubbling regime. A change in mass transfer behaviour occurs around a U0/Uc value of 0.25. Reactor performance increases up to U0/Uc = 0.7, after which a decreasing trend is observed. An empirical correlation is proposed for the specific interphase mass transfer (kbe) of the higher velocity bubbling regime. This correlation is based on the integration of the hydrodynamics determined by means of XRT and reactor performance: 4-12 The hydrodynamic parameter β gives the best fit for the entire velocity range with an average error of 8%, although it is not recommended for U0/Uc<0.17. It is observed that the classical approach of penetration theory for interphase mass transfer, performs exceptionally well at low velocities (U0/Uc<0.34). The addition of fines to the FeSi particle type decreases the overall reactor performance, despite decreased bubble sizes. The solids fraction, however, unexpectedly increases with the addition of fines and a collapse of the emulsion phase is measured. It is therefore postulated that though flow in the emulsion phase is much higher for the FeSi baseline system and decreases with the addition of fines. For the sand particle type, the behaviour expected from literature is observed: reactor performance increases, bubble sizes decrease and the solids fraction decreases. Very distinct hydrodynamic behaviour is observed for all the fluidization regimes with XRT. Probability density distributions show there are still two phases present in the turbulent regime and that the emulsion-phase solids fraction remains independent of velocity until fast fluidization sets in. The turbulent regime has unique hydrodynamic behaviour, although voids appear to be a transient structure between the structures of the bubbling and fast fluidization regimes. / Thesis (PhD)--University of Pretoria, 2013. / gm2014 / Chemical Engineering / unrestricted

In computed tomography (CT) cross-sectional images of the attenuation distribution within a slice are created by scanning radiographic projections of an object with a rotating X-ray source detector compound and subsequent reconstruction of the images from these projection data on a computer. CT can be made very fast by employing a scanned electron beam instead of a mechanically moving X-ray source. Now this principle was extended towards high-energy electron beam tomography with an electrostatic accelerator. Therefore a dedicated experimental campaign was planned and carried out at the Budker Insitute of Nuclear Physics (BINP), Novosibirsk. There we investigated the capabilities of BINP’s accelerators as an electron beam generating and scanning unit of a potential high-energy electron beam tomography device. The setup based on a 1 MeV ELV-6 (BINP) electron accelerator and a single detector. Besides tomographic measurements with different phantoms, further experiments were carried out concerning the focal spot size and repeat accuracy of the electron beam as well as the detector’s response time and signal to noise ratio.

<p>Meteorites fallen from the sky and surface particles of the moon gathered by lunar space missions, have distinct microstructure and properties that can provide unique insights on the origins and processes for the evolution of our solar system. These extraterrestrial materials contain highly complex microstructures due to the formation and structure evolution events spanning long periods of time. The comprehensive characterization on these samples, to extract multi-scale structural information, is especially crucial to support formation theories, understand material utilization possibility, and preparation for potential hazard mitigation. In addition to the microstructure, an understanding of the mechanical properties of these materials is also vital. Hence, an in-depth investigation on how microstructural phase distribution and their respective mechanical properties connect to macroscopic deformation behavior is required.</p> <p>In this study, a correlative microscopy-based methodology was used to study several celestial samples; meteorite Aba Panu (L3), meteorite Tamdakht (H5), and a lunar dust grain from mature sample 10084 returned by the Apollo 11 mission. X-ray microcomputed tomography (XCT) was utilized to acquire inherent 3D structural details from samples non-destructively. Scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) was used to further resolve finer structural features and compositional information to complete the correlative described above.</p> <p>Both ex situ and in situ compression experiments, in the XCT, were performed on machined cylindrical samples of Aba Panu meteorite. Structure development including crack initiation, propagation, and failure states were analyzed and correlated to the macroscopic stress-strain behavior. Direct 3D correlation on ex situ and in situ images of crack growth were used to obtain a comprehensive mechanistic understanding of crack development and deformation. Finally, nanoindentation was used to complement the 3D microstructural study, by acquiring mechanical properties of individual constituent phases.</p> <p><br></p>

The Polymer Electrolyte Membrane (PEM) fuel cell has a great potential in leading the future energy generation due to its advantages of zero emissions, higher power density and efficiency. For a PEM fuel cell, the Membrane-Electrode Assembly (MEA) is the key component which consists of a membrane, two catalyst layers and two gas diffusion layers (GDL). The success of optimum PEM fuel cell power output relies on the mass transport to the electrode especially on the cathode side. The carbon based GDL is one of the most important components in the fuel cell since it has one of the basic roles of providing path ways for reactant gases transport to the catalyst layer as well as excess water removal. A detailed understanding and visualization of the GDL from micro-scale level is limited by traditional numerical tool such as CFD and experimental methods due to the complex geometry of the porous GDL structural. In order to take the actual geometry information of the porous GDL into consideration, the x-ray tomography technique is employed which is able to reconstructed the actual structure of the carbon paper or carbon cloth GDLs to three-dimensional digital binary image which can be read directly by the LB model to carry out the simulation. This research work contributes to develop the combined methodology of x-ray tomography based the three-dimensional single phase Lattice Boltzmann (LB) simulation. This newly developed methodology demonstrates its capacity of simulating the flow characteristics and transport phenomena in the porous media by dealing with collision of the particles at pore-scale. The results reveal the heterogeneous nature of the GDL structures which influence the transportation of the reactants in terms of physical parameters of the GDLs such as porosity, permeability and tortuosity. The compression effects on the carbon cloth GDLs have been investigated. The results show that the c applied compression pressure on the GDLs will have negative effects on average pore size, porosity as well as through-plane permeability. A compression pressure range is suggested by the results which gives optimum in-plane permeability to through-plane permeability. The compression effects on one-dimensional water and oxygen partial pressures in the main flow direction have been studied at low, medium and high current densities. It s been observed that the water and oxygen pressure drop across the GDL increase with increasing the compression pressure. Key Words: PEM fuel cell, GDL, LB simulation, SPSC, SPMC, x-ray tomography, carbon paper, carbon cloth, porosity, permeability, degree of anisotropy, tortuosity, flow transport.

Les matériaux composites à renfort carbone dans une matrice époxy présentent des propriétés remarquables au regard de leur poids. Cependant, ces matériaux peuvent présenter des défauts qui peuvent significativement altérer leurs propriétés. Il est donc nécessaire de disposer d'un moyen de contrôle non destructif performant, afin de vérifier la structure interne de ces matériaux. Dans ce document, la tomographie X est utilisée. La distinction des défauts dans ces matériaux est cependant compliquée à cause de la proximité chimique entre le carbone et la résine. Dans le but d'améliorer la détection de ces défauts, ce document propose l'étude des différents phénomènes physiques entrant en jeu lors du procédé de tomographie X dont l'étude des paramètres d'acquisition et les phénomènes physiques dégradant la qualité de l'image. Afin d'aider à la compréhension des différents phénomènes physiques, l'outil de la simulation est utilisé, celle-ci permettant d'étudier de manière indépendante tous ces phénomènes. Après avoir présenté dans la première section les matériaux composites et la tomographie X, la deuxième section décrit les caractéristiques du système d'acquisition tomographique utilisé. Ensuite, les caractéristiques de la simulation du système d'acquisition sont également présentées. La troisième section propose une étude des différents phénomènes physiques contribuant à l'image. En effet, la comparaison des résultats entre la simulation et l'expérimental a permis de mettre en évidence qu'un phénomène de rétrodiffusion se produit à l'intérieur du détecteur. Un protocole est présenté afin de le déterminer expérimentalement et de l'ajouter aux projections simulées. De plus, la simulation ne prenant pas en compte le bruit sur les projections, un protocole est présenté afin de le déterminer expérimentalement. La quatrième section présente l'étude de l'optimisation de la qualité de l'image par simulation. Le choix de la tension accélératrice est étudié, ainsi que l'influence du rayonnement diffusé objet. La cinquième section propose une validation expérimentale des résultats, notamment en appliquant la correction du rayonnement rétrodiffusé aux pièces composites d'intérêt. / The carbon-fiber-reinforced-polymer (CFRP) materials display excellent properties considering their weight. However, they also can display defects that can significantly decrease their properties. In order to verify the internal structure of the composite materials, non destructive control is required. In this document, the X-ray computed tomography is used. Nevertheless, the distinction of the defects is difficult because of the chemical proximity between the carbon and the resin. In order to improve the detection of the defects, this document proposes to study the different physical phenomena happening during the tomography process such as the study of the acquisition parameters and the phenomena that decrease the image quality. In order to help to understand the different phenomena, the simulation tool is used. It allows to study the different phenomena independently to the others. After the presentation of the composite materials and the x-ray computed tomography in the first part, the features of the used acquisition system are presented in the second part. The features of the simulation of the acquisition system are also presented. The third part propose a study of the different phenomena contributing to the image. The comparison of the results between the simulation and the experimental allows to highlight a backscattering phenomenon happening inside the detector. A protocol allowing to determine these phenomena experimentally and to add it on the computed projections is presented. Furthermore, the simulation does not take the noise on the projection into account. Another protocol is presented, allowing to determine it experimentally. The fourth part displays the study of the optimization of the image quality using the simulation. The choice of the accelerating voltage is studied as well as the influence of the object scatter radiation. The fifth part proposes an experimental validation of the results. Especially, a correction of the backscattering is presented and applied to the composites objects.

La capacité opérationnelle axiale en service de pieux battus reste une zone d'incertitude, en particulier pour les structures offshore. La recherche sur le terrain a montré que le frottement latéral peut augmenter au cours des mois ou des années après le battage. Si des tendances similaires se retrouvent dans des ouvrages offshore, les avantages en terme d'ingénierie de réalisation peuvent être très importants. D'autre part, les fondations sur pieux de plates-formes de gaz, de pétrole sont soumises à des chargements cycliques à long terme qui peuvent influencer leur capacité à l'arrachement. Les pieux battus en eau profonde connaissent un grand nombre de cycles complets de charge-décharge pouvant contribuer à la dégradation du frottement latéral lors de l'installation. Cette thèse vise à mieux comprendre les principaux résultats obtenus avec des pieux réels en sable siliceux, par le biais d'une recherche à échelle de laboratoire sous conditions environnementales contrôlées. Ce travail fait partie d'un programme de recherche commun entre le Laboratoire 3SR de Grenoble, l'Imperial College London, et le projet français de recherche ANR- SOLCYP. La réponse de l'interface sol-pieu lors de l'installation ainsi que les périodes de vieillissement et de chargements cycliques axiaux ont été étudiés au laboratoire en utilisant des pieux-modèles installés dans la chambre d'étalonnage de Grenoble. Plusieurs essais avec le pieu modèle Mini-ICP (instrumenté avec des capteurs de tension totale à la surface du pieu (SST) pour les mesures de contraintes radiales de cisaillement à 3 sections) ont permis l'analyse de chemin de contrainte locale à l'interface du pieu. Des capteurs miniatures ont en outre été installés dans le massif de sable pour une mesure de contrainte lors de l'installation du pieu et son chargement ultérieur. Les effets des méthodes d'installation, de la taille des particules de sable, ou de la saturation du sable et du chargement de l'environnement, ont été pris en compte pour le vieillissement de la capacité. Les évolutions locales de l'interface radiale et du cisaillement sont en accord avec les prédictions des méthodes de conception modernes basées sur le CPT. Des preuves d'effets d'échelle soulignent l'importance des conditions aux limites appliquées à la modélisation physique. Des séries d'essais non-alternés purement en traction, ainsi que des essais alternés ont été réalisés sous contrôle en charge ou en déplacement. Les mesures locales effectuées dans les chemins de contraintes effectives montrent une contraction radiale de la masse de sable au voisinage du pieu. Les incréments de l'amplitude de charge et du déplacement imposé accélèrent les taux de dégradation cyclique. Un nouveau diagramme de stabilité cyclique a été réalisé, en résumant les essais de chargement cycliques axiaux pour les pieux foncés et battus dans du sable siliceux moyennement dense. Des mécanismes complexes comme la rupture des grains et des changements de densité locale à l'interface du pieu peuvent affecter la réponse des pieux. La cinématique derrière leur installation et l'interaction avec le sol environnant reste encore très limitée. Comprendre comment un matériau granulaire interagit avec le pieu est important pour étudier la réponse globale du pieu. Les observations globales du comportement des pieux dans la chambre d'étalonnage ont été modélisées à une échelle micro en utilisant la tomographie aux rayons X du Laboratoire 3SR à Grenoble. Le programme expérimental comprenait des essais sur une chambre d'étalonnage modèle afin d'analyser le champ de déplacement lors de l'installation d'un pieu modèle, à l'aide des techniques de corrélation d'images (DIC) en trois dimensions. Des analyses micromécaniques d'échantillons «intacts» récupérés post mortem à l'interface du pieu ont été également effectuées pour mettre en évidence de possibles changements radiaux de densité ainsi que la rupture des grains. / The operational in-service axial capacity of driven piles remains an area of uncertainty, especially for offshore structures. Field research has demonstrated that axial shaft capacities may increase over the months or years after driving. If similar trends apply offshore, the realisable engineering benefits are very significant. On the other hand, the piled foundations of oil/gas platforms and wind/water turbines are subject to long term environmental and in service cyclic loading due for example to waves, vibrations and storms that may also affect their shaft capacity. Deep driven piles experience large numbers of full load-unload cycles that contribute to shaft capacity degradation during installation. This thesis aims to improve understanding of the main results obtained with full-scale piles in silica sand through a laboratory scale investigation performed under controlled environmental conditions. This work was part of a joint research programme between the Grenoble Laboratory 3SR and Imperial College London, and the French National SOLCYP research project. The response of the soil-pile interface during installation, ageing periods and cyclic loading tests have been studied using laboratory model piles installed in the large Grenoble Calibration Chamber. Several tests with the Mini-ICP pile allow the analyses of local stress path at the pile's interface. This model pile is instrumented with surface stress transducers (SST) for local measurements of total and radial shear stresses at 3 different sections along the pile's shaft. In addition, miniature soil stress transducers were installed into the sand mass for total stress measurements during pile installation and loading. Possible ageing effects as installation methods, sand particle size, sand saturation and environmental loading were studied. Local evolution of interface radial and shear stresses agree with predictions from modern CPT based design methods. Evidence of possible scale effects remark the importance of the boundary conditions applied in physical modelling. Series of one-way purely tensile and two-way axial cyclic loading tests were performed under load and displacement control. Local measurements made of the effective stress paths shows radial contraction of the sand mass in the vicinity of the pile. Increments in loading amplitude and imposed displacements accelerate cyclic degradation rates. A new interactive shaft stability chart was produced as a summary of axial cyclic loading tests for both jacked and driven piles in medium dense silica sand. Laboratory tests confirm findings from field tests where one-way low amplitude cycles lead to beneficial increases in tensile pile capacity of up to 20%. Complex mechanisms as grain breakage and local density changes at the pile's interface. The kinematics behind the installation of piles and its interaction with the surrounding soil is still limited. Understanding how granular material interacts with the pile may reveal important to understand the global pile response. The global observations of the pile behaviour from calibration chamber tests were modelled at a micro scale using Micro Computed Tomography at the Grenoble Laboratory 3SR. The experimental campaign included tests on a model calibration chamber devoted to the displacement field analyses during the installation of a model piles using three dimensional (3D) digital image correlation (DIC). Micromechanical analysis of « intact » post-mortem samples recovered at the pille's interface were also conducted for evidences of radial density gradient and grain breakage.

La mise en forme par ice-templating est un procédé d’élaboration permettant via la congélation d’une suspension, d’obtenir des matériaux poreux à porosité contrôlée. L’analyse des mécanismes régissant la congélation de suspensions concentrées en particules et leurs conséquences sur les microstructures poreuses, est très peu développée dans la littérature du point de vue de l’influence de la composition de la suspension, en termes de nature et quantité d’additifs. Les objectifs de ces travaux de thèse sont d’observer et caractériser in situ et ex situ la formation des structures par ice-templating. Il s’agit également d’établir les liens entre la composition des suspensions, le procédé et la morphologie poreuse obtenue pour les structures congelées et frittées qui en découlent. L’évolution de l’avancée du front de congélation d’un panel de suspensions d’alumine aux propriétés caractérisées a été observée par radiographie X et la microstructure des échantillons congelés et frittés a été caractérisée par tomographie X ou par MEB. Nous avons ainsi pu caractériser les différentes étapes de la congélation par ice templating, les microstructures congelées associées, l’influence de la composition de la suspension ainsi que les mécanismes générateurs de défauts. La force ionique générée par la quantité de dispersant, la présence ou non de liant et la vitesse de refroidissement des suspensions sont trois paramètres ayant des conséquences critiques sur la microstructure et sur l’orientation ou la désorientation des cristaux. Nos résultats apportent un éclairage inédit sur les mécanismes de congélation des sols étudiés en géophysique et notamment la formation de glace lenticulaire. / Ice-templating is a processing route used to obtain porous material with a controlled porosity by freezing a suspension. Researches focused on this subject so far revealed a lack of information about mechanisms controlling the freezing of suspensions with a high solid loading and their consequences over porous microstructures, depending on the composition of the suspension in terms of additives nature and quantity. The objectives of this work are to observe and characterize in and ex situ the formation of structures by ice-templating and to establish the relationships between the composition of suspensions, process and porous morphology of frozen and sintered bodies. The advancement of the freezing front of a panel of alumina suspensions, with characterized properties was investigated by X-ray radiography and the microstructures of frozen or sintered samples were characterized by X-ray tomography and SEM. We have defined the different stages of the freezing by ice-templating, the associated frozen and sintered microstructures, the influence of the composition of the suspension and the mechanisms responsible for defects creation. The ionic strength generated by the dispersant quantity, the addition or not of a binder and the cooling rate of suspension are three parameters with critical consequences on microstructures, orientation and disorientation of ice crystals. Our results shed a new light on the freezing mechanisms of soils in geophysics and more particularly the ice lenses formation.