The design and fabrication of porous ceramic materials with anisotropic properties has, in recent years, gained popularity due to their potential application in various areas that include medical, energy, defense, space, and aerospace. Freeze-casting is an effective, low-cost, and safe method as a wet shaping technique to create these structures. To control the morphology of these materials, many critical factors were found to play an important role. In this dissertation, the processing parameters of the magnetic field-assisted freeze-casting method were optimized with a focus on comparing the structure obtained using vertical and horizontal magnetic fields and understanding the mechanisms that occur under different freezing modes. More specifically, this processing method was used to produce Al2O3 and B4C porous ceramics materials with unidirectionally-aligned pore channels. The effect of the vertical and horizontal magnetic field strength and direction, concentration of magnetic material (Fe3O4), cooling rate, and freezing time were examined. The resulting ceramics with highly aligned pore channels were infiltrated with molten metal to create metal matrix composites. The mechanical properties of these structures were measured and were subsequently correlated to their morphology and composition.

CoordenaÃÃo de AperfeiÃoamento de Pessoal de NÃvel Superior / O interesse em cerÃmicas porosas vem aumentando, à medida que novos processos vÃo sendo desenvolvidos, e as aplicaÃÃes decorrentes representam oportunidades tecnolÃgicas e econÃmicas substanciais. Para cada aplicaÃÃo, hà pelo menos uma propriedade relevante e deve ser avaliada, dependendo da funÃÃo: fÃsica, quÃmica e biolÃgica. Dentre as vÃrias aplicaÃÃes de cerÃmicas porosas, podem ser citadas: separadores de cÃlula para bateria, queimadores, suportes para catÃlise, filtros, sensores de gÃs, dentre outras. A alumina se destaca como matÃria-prima para corpos cerÃmicos devido as suas propriedades, tais como alta dureza, elevada resistÃncia ao desgaste, baixo coeficiente de atrito, alta resistÃncia à corrosÃo tanto à temperatura ambiente quanto em altas temperaturas ao ar, ausÃncia de transformaÃÃes no estado sÃlido, e o fato de que o material mantÃm sua resistÃncia mesmo em altas temperaturas (1500ÂC-1800ÂC). O objetivo deste trabalho à avaliar algumas propriedades mecÃnicas da alumina (Al2O3) com diferentes nÃveis de porosidade. As amostras forma produzidas pelos mÃtodos da esponja polimÃrica, adiÃÃo de cera polimÃrica e barras cerÃmicas com e sem bicarbonato de sÃdio. A sinterizaÃÃo foi realizada em duas temperaturas: a 1450ÂC e 1550ÂC. As propriedades analisadas foram: resistÃncia à flexÃo e dureza atravÃs das normas da ASTM, porosidade aparente, densidade aparente, retraÃÃo linear de queima, retraÃÃo linear de secagem e absorÃÃo de Ãgua, mÃtodo de Souza Santos para argilas. Os resultados obtidos mostraram-se bastante satisfatÃrios, onde foi mostrado que os corpos cerÃmicos porosos obtiveram valores de resistÃncia à flexÃo e dureza coerentes com os da literatura. Realizou-se tambÃm uma caracterizaÃÃo via difraÃÃo de raios-x (DRX) e microscopia eletrÃnica de varredura (MEV) das amostrar confeccionadas pelos dois mÃtodos. / The interest in porous ceramics is increasing, as new processes and technologies are going to be developed and hence applications representtechnological and economical opportunities. For each application, there is at least one important property that must be evaluated, depending on its function: physical, chemical and biological. There are many applications for porous ceramics bodies, such as: battery fuel cell separators, burners, catalyst supports, filters, gas sensors, etc. Alumina is a wild raw material used because of its properties, such as high hardness, high wear resistance, low friction coefficient, high resistance to corrosion at room temperature and at high temperature on air, the absence of transformations within the entire temperature range of solid state, and the fact that the material retains its strength even at very high temperatures (1500ÂC â 1800ÂC). This research describes the evaluation of some mechanical properties of alumina (Al2O3) with different levels of porosity obtained by the polymeric sponge method and by adding polymeric wax at 1450ÂC and 1550ÂC. Flexural strength and hardness were assessed using ASTM specifications. Apparent porosity, apparent density, linear shrinkage after sintering, linear shrinkage after drying and water absorption by Souza Santos clay method. Data showed to be satisfactory, where it was shown that porous ceramic bodies had flexural strength and hardness values corroborating with literature. Analyses were performed by x â rays diffraction (XRD) and scanning electronic microscopy (SEM) for both samples made by each method. In a general way, both samples made by each method had a similar behavior; however, samples made by adding polymeric wax presented less porosity homogeneity than those made by polymeric sponge method, and showed better sinterization at both temperatures either.

Selective laser sintering is a rapid prototyping method (RP), which was originally developed, along with other RP methods, to speed up the prototyping stage of product design. The sole needed input for production being the solid model of the part, the mold/tool-free production characteristics and the geometric part complexity that can be achieved due to layer-by-layer production have extended the applicability/research areas of these methods beyond prototyping towards new applications and material development. Local pore formation in a part that occurs as a result of the discrete manufacturing nature of selective laser sintering is normally considered a defect. In the current research, this is viewed as an opportunity for material development: Exploitation of rapid prototyping methods to produce composites/functionally graded materials with controlled porous structures. That the material interior structure (porous structure) and exterior shape are formed during the same course renders selective laser sintering process as an attractive manufacturing alternative for producing complex-geometry composite/porous materials, which may be difficult or impossible to manufacture with other techniques. In this thesis, the use of selective laser sintering (a rapid prototyping method) in producing uniformly porous and graded polymeric graded porous structures is studied. The material used was polyamide powder (PA 2200) and the selective laser sintering machine used was the EOSINT P 380 system. In this research, three process parameters of the SLS system, the hatching distance, the laser power and the laser scanning speed were varied to produce parts that have different porosities. Porous parts with a homogenous porous microstructure (uniformly porous parts) could be produced, as well as graded porous parts. The results of uniformly porous structure production were utilized to build graded porous structures by imparting different porosities along a certain direction within a single part. Both, uniformly porous and graded structures were characterized physically and mechanically. The porous parts (both uniformly porous and graded porous) were infiltrated with epoxy resin to produce epoxy-PA composites and graded materials. The physical and mechanical properties of these parts were compared with those of the uninfiltrated (porous PA) structures

Selective laser sintering (SLS) is a rapid prototyping method in which three-dimensional objects are constructed by sintering thin layers of a variety of powdered materials via laser beam. In SLS, as in most other Rapid Prototyping methods, the produced parts exhibit varying degrees of intrinsic porosity due to the discrete nature of layer-by-layer production. Selective scanning and discrete bonding of individual particles or clusters of particles impart local porosity, which is mostly an undesired trait as the part integrity decreases with increased porosity. However, there are a number of emerging or potential applications as in tissue engineering and composite/functionally graded materials, in which part porosity and its control during production are needed. In this study, the manufacturing capabilities of selective laser sintering are investigated towards producing predesigned porous structures using a polymeric powder. The porous structures are characterized in two main categories: regular porous structures, which involve geometries such as predesigned holes and lattice structures that have orderly porous architecture, and irregular porous structures, which exhibit random pore architecture that is intrinsic in all SLS parts. The limitations of producing regular porous structures are investigated, identified and quantified, based on hole size and dimensional accuracy. An experimental analysis based on design of experiments is employed to investigate the effects of processing parameters on the resulting macroscopic pore properties of irregular porous structures. A mathematical relation is developed to quantify and predict the relations between the SLS process parameters: Laser power, hatching distance, laser scan spacing, and the resulting apparent mass density (as a measure of porosity). The subsequent tests verify accuracy of the developed empirical model.

Fundação de Amparo a Pesquisa do Estado de Minas Gerais / Hydrocyclones are equipments destined to solid-liquid separation broadly used in industry due to its advantages, including compact geometry, high separation efficiency, simple maintenance and low cost. Depending on the user desired finality (concentration or classification), it is possible to potentiate the hydrocyclones performance by the simultaneous use of new unit operations to hydrocycloning, for example, the filtration. The filtering hydrocyclone was an equipment developed and improved by FEQUI/UFU researchers. In this way the objective of this work was to experimentally study the effect of incorporating a porous cylinder and cone, together or separately, to the optimized geometry conventional hydrocyclone (H11). Experiments were done with aqueous suspension of phosphate rock in three different permeability values for the porous media and three underflow diameters. According to the main results, the hydrocyclones HCiF, HCoF and HCiCoF showed mean decrease in the energetic consume of 13, 32 and 35% respectively, in comparison to conventional hydrocyclone (HCon), in the lowest permeability used for the filtering medium. However the underflow-to-throughput ratio of the hydrocyclones HCiF, HCoF and HCiCoF increased in relation to the conventional hydrocyclone (HCon), regardless the permeability or the underflow diameter used. About the total efficiency of the filtering equipments, little differences in relation to the conventional separator were observed, and can be said that this variable remained practically constant for the same operational condition. From the experimental data it was possible to obtain the project equations and the total efficiency curves even for distinct granulometries of each hydrocyclone studied. In summary can be concluded that in the case of filtering hydrocyclones, it is not advisable to use filtering medium with permeability higher than 2,0.10-6 m2 because, in energetic terms, they will consume more energy than the conventional hydrocyclone, and in terms of separation they will be practically equal to the conventional separator. / Hidrociclones são equipamentos destinados à separação sólido-líquido amplamente utilizados na indústria devido a suas vantagens, incluindo geometria compacta, alta eficiência de separação, manutenção simples e baixo custo. Dependendo da finalidade almejada pelo usuário (concentração ou classificação), é possível potencializar o desempenho dos hidrociclones mediante o uso simultâneo de novas operações unitárias à hidrociclonagem como, por exemplo, a filtração. O hidrociclone filtrante foi um equipamento desenvolvido e aperfeiçoado por pesquisadores da FEQUI/UFU. Dessa maneira, o intuito deste trabalho foi estudar, experimentalmente, o efeito da incorporação do cilindro e cone porosos, conjunta ou separadamente, ao Hidrociclone Convencional de geometria otimizada (H11). Para tanto, os ensaios foram conduzidos com suspensão aquosa de rocha fosfática em três valores de permeabilidade para os meios porosos e três diâmetros de underflow. De acordo com os principais resultados, os hidrociclones HCiF, HCoF e HCiCoF apresentaram decréscimos médios no consumo energético de 13, 32 e 35% respectivamente, em comparação ao Hidrociclone Convencional (HCon), na menor permeabilidade utilizada para o meio filtrante. No entanto, a Razão de Líquido dos hidrociclones HCiF, HCoF e HCiCoF aumentou em relação à do Hidrociclone Convencional, independente da permeabilidade ou do diâmetro de underflow utilizados. Em se tratando da Eficiência Total dos equipamentos filtrantes foram observadas pequenas diferenças em relação ao separador convencional, podendo dizer que essa variável permaneceu praticamente constante para a mesma condição operacional. A partir dos dados experimentais, foi possível obter as equações de projeto, bem como as curvas de Eficiência Total para granulometrias distintas da utilizada para cada hidrociclone estudado. Em suma, pôde-se concluir que, em se tratando de hidrociclones filtrantes, não é aconselhável empregar meios filtrantes com o valor de permeabilidade maior do que aproximadamente 2,0.10-16 m2, já que, em termos energéticos, consumiriam mais energia do que a utilizada pelo Hidrociclone Convencional e em termos de separação, seriam praticamente idênticos ao separador convencional. / Mestre em Engenharia Química

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Les avalanches de plaque représentent un risque naturel majeur dont la prévision demeure très difficile. Le manque de lois constitutives fiables à l’échelle du matériau rend difficiles les tentatives de modélisation de ce phénomène. Plus spécifiquement, la réponse mécanique de la neige durant et après la rupture, dans des régimes de chargements rapides , demeure relativement méconnue. La nature particulièrement fragile du matériau au sein de ce régime de déformation rend ardue la réalisation d’expériences et complique l’observation à l’échelle microstructurale.Dans ce travail de thèse, un modèle numérique de neige fondé sur la Méthode des Éléments Discrets a été développé en tant qu’alternative aux expériences. Le modèle nous permet de simuler la réponse de la neige à des chargements mécaniques en tenant compte de la microstructure réelle du matériau grâce à l’intégration d’images acquises par microtomographie à rayons X en entrée du modèle. La neige est considérée comme un matériau granulaire cohesif, et une méthode originale a été développée afin de modéliser la forme de chaque grain. Les grains individuels sont ensuite assemblés pour reconstituer la matrice de la neige grâce à la prise en compte de lois de contact cohésives.Le modèle a été utilisé afin d’explorer la réponse mécanique macroscopique de différent échantillons de neige à un chargement mixte normal-cisaillant. Trois modes de rupture ont été observés dans tous les échantillons de neige testés, en fonction du niveau de contrainte normale appliquée : une rupture en cisaillement localisée pour des niveaux de contrainte normale faibles (mode A), un effondrement normal induit par rupture en cisaillement à des niveaux intermédiaires de contrainte normale (mode B) et un effondrement normal pour des valeurs de contrainte normale élevées (mode C). Ces différents modes de rupture produisent une enveloppe de rupture fermée dans l’espace des contraintes, ce pour les différents types de neige étudiés.Les mécanismes internes conduisant à l’effondrement normal des échantillons ont été étudiés plus en détail à l’échelle microscopique. Il a été montré que ce mode de rupture était associé à un mécanisme de flambement des chaînes de force. En outre, la stabilité de ces chaînes de force semble être contrôlée par les contacts entre les éléments des chaînes et les grains environnants. La rupture de ces contacts, observée dans les modes B et C, autorise le développement du flambement des chaînes de force et aboutit à l’effondrement volumique. / Dry slab snow avalanches represent a major natural hazard that is extremely difficult to manage. Attempts to model this phenomenon are hindered by the lack of a constitutive law that would describe the mechanical behaviour of snow on a material scale. In particular, relatively little is known on the failure and post-failure response of snow at high loading-rates. The highly fragile nature of the material in this deformation regimerenders experimental investigation difficult and complicates observation at the microstructural level.As an alternative to experiments, a Discrete Element Method-based numerical model of snow is developed in this thesis. The model enables us to simulate the response of snow to mechanical loading, while accounting for actual snow microstructure by using X-ray attenuation images of snow microstructure as input. Snow is considered as a cohesive granular material and an original methodology is developed in order to model the shape of each grain. Individual grains are bound into the snow matrix by modelling cohesion between neighbouring grains.The model is then used to explore the macroscopic mechanical response of different snow samples to mixed-mode loading. Three typical modes of failure are observed in all tested snow samples, depending on the level of applied normal stress: a localized shear failure at low normal stress (mode A), a shear failure-induced volumetric collapse at intermediate levels of normal stress (mode B), and a normal failure and collapse for high values of normal stress (mode C). The observed failure modes result in closed failure envelopes and no qualitative difference is observed between the mechanical responses of different snow types.The internal mechanisms that lead to volumetric collapse are further examined on the microscale. Force chain buckling is identified as a trigger of this material instability. Additionally, force chain stability appears to be controlled by the contacts between the force chain members and the surrounding grains. The failure in these contacts, which is evidenced in modes B and C, allows force chain buckling to develop and results in subsequent volumetric collapse.

Composite structures provide opportunities for weight reduction, material tailoring and integrating control surfaces with embedded transducers, which are not possible in conventional metallic structures. As a result there is a substantial increase in the use of composite materials in aerospace and other major industries, which has necessitated the need for structural health monitoring(SHM) of aerospace structures. In the context of SHM of aircraft structures, there are many areas, which are still not explored and need deep investigation. Among these, one of the major areas is the development of efficient damage models for complex composite structures, like stiffened structures, box-type structures, which are the building blocks of an aircraft wing structure. Quantification of the defect due to porosity and especially the methods for identifying the porous regions in a composite structure is another such area, which demands extensive research. In aircraft structures, it is not advisable for the structures, to have high porosity content, since it can initiate common defects in composites such as, delamination, matrix cracks etc.. In fact, there is need for a high frequency analysis to detect defects in such complex structures and also to detect damages, where the change in the stiffness due to the damage is very small. Lamb wave propagation based method is one of the efficient high frequency wave based method for damage detection and are extensively used for detecting small damages, which is essentially needed in aircraft industry. However, in order, to develop an efficient Lamb wave based SHM system, we also need an efficient computational wave propagation model. Developing an efficient computational wave propagation model for complex structures is still a challenging area. One of the major difficulty is its computational expense, when the analysis is performed using conventional FEM. However, for 1D And 2D composite structures, frequency domain spectral finite element method (SFEM), which are very effective in sensing small stiffness changes due to a defect in a structure, is one of the efficient tool for developing computationally efficient and accurate wave based damage models. In this work, we extend the efficiency of SFEM in developing damage models, for detecting damages in built-up composite structures and porous composite structure. Finally, in reality, the nature of variability of the material properties in a composite structure, created a variety of structural problems, in which the uncertainties in different parameters play a major part. Uncertainties can be due to the lack of good knowledge of material properties or due to the change in the load and support condition with the change in environmental variables such as temperature, humidity and pressure. The modeling technique is also one of the major sources of uncertainty, in the analysis of composites. In fact, when the variations are large, we can find in the literatures available that the probabilistic models are advantageous than the deterministic ones. Further, without performing a proper uncertain wave propagation analysis, to characterize the effect of uncertainty in different parameters, it is difficult to maintain the reliability of the results predicted by SFEM based damage models. Hence, in this work, we also study the effect of uncertainty in different structural parameters on the performance of the damage models, based on the models developed in the present work. First, two SFEM based models, one based on the method of assembling 2D spectral elements and the other based on the concept of coupling 2D and 1D spectral elements, are developed to perform high frequency wave propagation analysis of some of the commonly used built-up composite structures. The SFEM model developed using the plate-beam coupling approach is then used to model wave propagation in a multiple stiffened structure and also to model the stiffened structures with different cross sections such as T-section, I-section and hat section. Next, the wave propagation in a porous laminated composite beam is modeled using SFEM, based on the modified rule of mixture approach. Here, the material properties of the composite is obtained from the modified rule of mixture model, which are then used in SFEM to develop a new model for solving wave propagation problems in porous laminated composite beam. The influence of the porosity content on the parameters such as wave number, group speed and also the effect of variation in theses parameters on the time responses are studied first. Next, the effect of the length of the porous region (in the propagation direction) and the frequency of loading, on the time responses, is studied. The change in the time responses with the change in the porosity of the structure is used as a parameter to find the porosity content in a composite beam. The SFEM models developed in this study is then used in the context of wave based damage detection, in the next study. First ,the actual measured response from a structure and the numerically obtained response from a SFEM model for porous laminated composite beam are used for the estimation of porosity, by solving a nonlinear optimization problem. The damage force indicator (DFI) technique is used to locate the porous region in a beam and also to find its length, using the measured wave propagation responses. DFI is derived from the dynamic stiffness matrix of the healthy structure along with the nodal displacements of the damaged structure. Next, a wave propagation based method is developed for modeling damage in stiffened composite structures, using SFEM, to locate and quantify the damage due to a crack and skin-stiffener debonding. The method of wave scattering and DFI technique are used to quantify the damage in the stiffened structure. In the uncertain wave propagation analysis, a study on the uncertainty in material parameters on the wave propagation responses in a healthy metallic beam structure is performed first. Both modulus of elasticity and density are considered uncertain and the analysis is performed using Monte-Carlo simulation (MCS) under the environment of SFEM. The randomness in the material properties are characterized by three different distributions namely normal, Weibul and extreme value distribution and their effect on wave propagation, in beam is investigated. Even a study is performed on the usage of different beam theories and their uncertain responses due to dynamic impulse load. A study is also conducted to analyze the wave propagation response In a composite structure in an uncertain environment using Neumann expansion blended with Monte-Carlo simulation (NE-MCS) under the environment of SFEM. Neumann expansion method accelerates the MCS, which is required for composites as there are many number of uncertain variables. The effect of the parameters like, fiber orientation, lay-up sequence, number of layers and the layer thickness on the uncertain responses due to dynamic impulse load, is thoroughly analyzed. Finally, a probabilistic sensitivity analysis is performed to estimate the sensitivity of uncertain material and fabrication parameters, on the SFEM based damage models for a porous laminated composite beam. MCS is coupled with SFEM, for the uncertain wave propagation analysis and the Kullback-Leibler relative entropy is used as the measure of sensitivity. The sensitivity of different input variables on the wave number, group speed and the values of DFI, are mainly considered in this study. The thesis, written in nine chapters, presents a unified document on wave propagation in healthy and defective composite structure subjected to both deterministic and highly uncertain environment.