Os aços de alta resistência e baixa liga (ARBL) utilizados em tubos para linhas de transmissão, ou seja, transferência e transporte de petróleo e gás, são especificados pela American Petroleum Institute (API) através da norma API 5L. Neste trabalho foi realizado um estudo da influência da têmpera e da nitretação no comportamento mecânico do aço API 5L X56. A microestrutura, os compostos formados com a nitretação e os mecanismos de fratura foram analisadas usando microscopia óptica, difração de raios X e microscopia eletrônica de varredura respectivamente. As amostras foram caracterizadas mecanicamente por testes de microdureza, tração, impacto e fadiga. Os resultados revelaram que apenas a têmpera promoveu modificações severas na microestrutura em relação à como recebida, formando bainita, martensita e constituinte M-A. A camada nitretada apresentou profundidade de 25 ?m e formação dos nitretos Fe3N e Fe4N. Houve aumento da microdureza, resistência mecânica com os tratamentos, juntamente com a diminuição da tenacidade e também houve um melhoramento na vida em fadiga para as duas amostras tratadas termicamente e superficialmente. Os mecanismos de fratura variaram de dúctil à frágil e em fadiga foi observado que as trincas nuclearam a partir da superfície para todas as amostras. / The high strength and low alloy steel (HSLA) used in pipeline for line transmission, there is transference and transportation of oil and gas, they are specified by American Petroleum Institute (API) through norm API 5L. In this work it was conducted a study of the nitriding and quenching influence on the mechanical behavior of API 5L X56. The microstructure, compounds made with the nitriding and the mechanisms failure were analyzed using optical microscopy, X-ray diffraction and scanning electron microscopy respectively. The samples were mechanical characterized by microhardness, tensile, impact and fatigue test. The results revealed that only quenching treatment promoted severe modifications in microstructure in relation to as received, making up bainite, martensite and M-A constituent. The nitriding layer showed depth of 25 ?m and formation of Fe3N e Fe4N nitrides. There was an increasing of microhardness and mechanical strength with the treatments, along with the decreasing of toughness and there was also an improvement in fatigue life for the two samples heat e surface treated. The failure mechanisms varied from ductile to brittle and in fatigue was observed that the cracks nuclear from the surface to all samples.

Aços microligados pertencem à classe dos aços ARBL contendo baixa ou média quantidade de carbono e pequena adição de elementos de liga tais como Mn, Nb, Mo, V e Ti. A variedade microestrutural desses aços pode ser obtida dependendo da temperatura de conformação, taxa de resfriamento e composição química. Os tratamentos intercríticos e isotérmicos produzem microestruturas multifásicas com diferentes quantidades de ferrita, martensita, bainita e austenita retida. A presença de diferentes fases nestes materiais, com morfologias distintas, pode afetar de modo significativo seu comportamento mecânico, afetando, por exemplo, o fechamento da trinca e resultando em mudanças na taxa de crescimento da mesma. O objetivo deste trabalho é avaliar as propriedades de tração e a resistência ao crescimento da trinca por fadiga de um aço microligado RD 480 com 0.08%C-1, 5%Mn (p), correlacionando-as com suas características microestruturais. Esse aço, desenvolvido recentemente pela CSN (Companhia Siderúrgica Nacional), é considerado promissor como alternativa para substituir o aço de baixo carbono utilizado em componentes de rodas na indústria automotiva. Distintas condições microestruturais foram obtidas por meio de tratamentos térmicos seguidos de resfriamento em água. As condições de tratamento intercrítico e têmpera simples foram escolhidas para se avaliar a resistência à propagação da trinca por fadiga. Os resultados dos ensaios foram sintetizados em termos da taxa de crescimento da trinca (da/dN) versus a variação do Fator Intensidade de Tensão (_K) no ciclo de carregamento. Para descrever o comportamento das trincas foram utilizados dois modelos: a equação convencional de Paris e um novo modelo exponencial que mostra o comportamento não linear das curvas de fadiga. Os resultados mostraram que uma microestrutura combinando ferrita de aspecto acicular e fases duras (martensita/bainita) resultou em menores taxas de crescimento da trinca. No entanto, a melhor combinação entre as propriedades de tração (limite de escoamento, resistência e ductilidade) e fadiga foi obtida com uma microestrura bifásica contendo martensita dispersa em uma matriz ferrítica. Observou-se uma transição nas curvas de crescimento da trinca para todas as condições tratadas termicamente e, por conta disto, as curvas das condições microestruturais bifásicas e multifásicas foram melhores modeladas quando divididas em duas regiões. As superfícies de fratura dessas amostras, bem como o caminho percorrido pela trinca, foram analisados via MEV e MO. / Microalloyed steels are a class of HSLA steels with low or medium carbon content and small additions of alloy elements such as Mn, Nb, Mo, V and Ti. A variety of microstructures in microalloyed steels can be obtained depending on the deformation temperature, cooling rate and chemical composition. Heat treatments and isothermal transformation on these materials, with various temperatures and holding times, produce multiphase microstructures with different amounts of ferrite, martensite, bainite and retained austenite. These different phases, with distinct morphologies, are determinant of the mechanical behavior of the steel and can, for instance, affect crack closure or promote crack shielding, thus resulting in changes on its propagation rate under cyclic loading. The aim of this study is to evaluate the tensile properties and resistance to fatigue crack growth in a microalloyed steel RD 480 with 0.08%C-1, 5% Mn (wt), correlating with their microstructural characteristics. This steel, recently developed by CSN (Companhia Siderurgica Nacional), is being considered as a promising alternative to replace low carbon steel in wheel components for the automotive industry. Distinct microstructural conditions were obtained by means of heat treatments followed by water quench. The intercritical treatment and quenching conditions were chosen to evaluate the strength to crack propagation. The crack propagation test results were summarized in terms of FCG rate (da/dN) versus stress intensity factor range (?K) curves. In order to describe the FCG behavior, two models were tested: the conventional Paris equation and a new exponential equation developed for materials showing non-linear FCG behavior. The results showed that a microstructure combining aspect acicular ferrite and hard phases (martensite / bainite) resulted in lower rates of crack growth. However, the best combination between the tensile properties (yield stress, tensile strength and ductility) and fatigue was obtained with a dual phase steel microstructure containing martensite dispersed in a ferrite matrix. It was observed a transition in the crack growth curves for all heat treated conditions, so the curves of the dual and multiphase microstructural conditions were better modeled by dividing them in two regions. The fracture planes of the fatigued specimens, as well as the crack path, were examined using a scanning electron microscope (SEM) and optical micrography (OM).

O uso das ligas de alumínio em aplicações estruturais tem crescido consideravelmente nas últimas décadas. Nos transportes, a baixa massa específica do alumínio resulta em uma alta razão resistência/ peso, favorecendo a fabricação de aviões, trens e automóveis. Com a crescente preocupação em reduzir a emissão de gases poluentes, vem tornando-se promissora a alternativa de reduzir o peso dos veículos substituindo peças convencionalmente produzidas com outros materiais por peças de alumínio. As ligas tratáveis termicamente da série 6xxx são frequentemente escolhidas para estas aplicações. Assim, para que o emprego dessas ligas seja otimizado, é importante um estudo mais detalhado de suas propriedades mecânicas, principalmente sob solicitações cíclicas. Neste trabalho foram estudadas ligas de Al-Si-Mg que são amplamente utilizadas nas indústrias automotivas, em especial na fabricação de componentes de carroçarias para caminhões e ônibus. Foi realizado o estudo do comportamento em fadiga de baixo ciclo e fadiga multiaxial das ligas AA6005 T6, AA6063 T6 e AA6351 T6, fornecidas pela CBA (Companhia Brasileira de Alumínio) visando caracterizar e comparar essas ligas em sua microestrutura, propriedades de tração e fadiga. As propriedades básicas de fadiga foram determinadas por meio do método ε-N (fadiga de baixo ciclo) e os ensaios foram realizados com controle de deformação total, onda triangular e taxa de deformação 0,005 seg-1. As análises dos laços de histerese elasto-plástica permitiram inferir sobre aspectos microestruturais relacionados às propriedades mecânicas das ligas estudadas. O comportamento em fadiga multiaxial foi avaliado por meio de carregamentos combinados axial-torcional em fase e fora de fase. Para ajustar os dados experimentais obtidos, foram testados alguns dos modelos encontrados na literatura. Os cálculos baseados no modelo de plano crítico, proposto por Fatemi e Socie, apresentaram resultados satisfatórios. Também foram realizadas análises microestruturais e fractográficas para as três ligas. As superfícies de fratura dos ensaios de fadiga multiaxial mostraram resultados diferentes de acordo com o carregamento adotado. A avaliação comparativa das três ligas estudadas fornece subsídios para fundamentar a seleção de materiais para a fabricação de componentes estruturais para o setor automotivo. / The use of aluminum alloys in structural applications has grown considerably in recent decades. In transportation, the low density of aluminum results in a high strength-to weight ratio, proving attractive for production of aircrafts, trains and automobiles. With a growing concern for the reduction of pollutant gas emissions, aluminum alloys are becoming a promising alternative to diminish vehicle weight through the replacement of conventionally produced parts made from other heavier materials for aluminum parts. The heat treatable alloys from the 6xxx series are often chosen for these applications. Therefore, to optimize the employment of these alloys, a detailed study of their mechanical properties, primary under cyclic solicitations is necessary For the present study Al-Mg-Si alloys were chosen, which are widely used in automotive industries, particularly in the manufacturing of components for trucks and bus bodies. The low-cycle fatigue behavior and multiaxial fatigue of the three following aluminum alloys: AA6005 T6, AA6063 T6 and AA6351 T6, provided by CBA (Brazilian Aluminum Company), were assessed, with the aim of characterizing and comparing these alloys in their microstructure, tensile properties and fatigue. The basic properties of fatigue were studied by ε-N method (low cycle fatigue) and the experiments were performed with total strain control, triangular waveform and with a constant deformation rate of 5.0x10-3 s-1. The analyses of hysteresis loops elasto-plastic provided insight about microstructural aspects, related to mechanical properties of the studied alloys. Multiaxial fatigue behavior was assessed in combined axial-torsion loading in phase and out of phase. To adjust the experimental data, some models found in the literature were tested. Calculations based on critical plane model, proposed by Fatemi Socie, presented satisfactory results. Furthermore, microstructure analyses and fractography were performed for these three alloys. The fracture surface of multiaxial fatigue assays demonstrated different results according to the adopted loading. Comparative evaluation of the three studied alloys provides support for the selection of materials for manufacturing structural components of the automotive sector.

A partir de mapeamento geológico, análises petrográficas, geoquímicas, geocronológicas e microestruturais em rochas metavulcânicas e metassedimentares, foi possível reconhecer duas sucessões de rochas metassedimentares - metavulcânicas de fácies xisto verde no sudoeste do Terreno Apiaí no cinturão Ribeira (entre Itapeva e Ribeirão Branco, SP): o Grupo Itaiacoca e a Formação Bairro dos Prestes. O Grupo Itaiacoca, datado pelo método U-Pb em zircão, apresentou idades neoproterozoicas entre 602,7 ± 24 (metabasito) e 613,4 ± 9,6 Ma (metatufo). É constituído por uma sucessão de metargilitos, filitos e quartzitos de granulação fina (Formação Água Nova), intercalados com metacalcários calcíticos e dolomíticos com estruturas estromatolíticas e pequenas camadas de tufo metavulcânico (Formação Bairro dos Campos) em contato transicional com rochas metabásicas, metadolomitos, e talco xisto e clorita xisto (Suíte Metabásica da Fazenda Velha) com quartzitos maciços (Formação Serra dos Macacos) sobrepondo todas as unidades. Com base na caracterização geoquímica, as metabásicas com assinaturas toleíticas e calci-alcalinas possuem padrões de manto tipo MORB com contribuição de componentes de subdução típicos de basaltos de bacias de retroarco. A Formação Bairro dos Prestes foi depositada entre 1761 ± 14 e ~ 1800 Ma (datada pelo metodo U-Pb SHRIMP em zircão de metariodacito e metavulcanossedimentar, respectivamente). A formação é composta por filitos, localmente com estruturas amigdaloides, em contato transicional com quartzitos de granulação fina a média, com camadas subordinadas de metaconglomerados e rohas metavulcânicas félsicas com assinatura calci-alcalina de alto K. Na área de estudo também estão presentes as rochas sedimentares paleozoicas do Grupo Itararé, os metarenitos quartzo-feldspáticos ediacaranos de granulação grossa da margem direita do rio Apiaí-Guaçu, a suite granítica ediacarana Três Córregos e o Complexo paleoproterozoico Apiaí Mirim. O Complexo Apiaí Miriam compreende paragnaisses e quartzitos micáceos de granulação média a grossa afetados por metamorfismo de fácies anfibolito, enquanto a Suite Granítica Três Córregos é constituída por monzogranitos porfiríticos e sienogranitos subordinados. A idade máxima de deposição obtida pelo método U-Pb LA-ICP-MS em zircões detríticos do Metarenito Apiaí-Guaçu foi de 588,4 ± 1,8 Ma, o que permite correlacioná-la com as bacias da fase de transição do ciclo Brasiliano. O arranjo estrutural compreende acamamento sedimentar (So) e três foliações tectônicas (Sn, Sn+1 e Sn+2). A foliação principal (Sn) é caracterizada por xistosidade ou clivagem ardosiana, geralmente paralelas a So, apresentando direções NE-SW e mergulhos elevados. Os planos Sn são deformados pelas clivagens de crenulação Sn+1 e Sn+2. A foliação Sn+1 está associada a dobras apertadas com planos axiais com direção NW desenvolvidas nos quartzitos, nas sequências metavulcanossedimentares e rochas pelíticas, enquanto a folição Sn+2 associa-se como dobras abertas com planos axiais com direção NE nos quartzitos e filitos. A área de estudo também é afetada por falhas NNW-SSE e NNE-SSW. A análise microestrutural realizada em amostras da Formação Bairro dos Prestes e do Complexo Apiaí Mirim através de técnicas de Orientação Preferencial de Forma (OPF) e Orientação Cristalográfica Preferencial (OCP), indica uma forma oblata para o elipsoide de deformação finita com planos XY na direção NE-SW e X-direções com alta obliquidade, correlacionadas com os dados estruturais medidos em campo. As temperaturas de deformação calculadas a partir do ângulo de abertura das estruturas dos eixos-c variam de 531 ° C - 593 ° C a 613 ° C -703 ° C. Foram influenciadas pela presençia de água e pelos processos de dissolução, sendo por vezes maior que as temperaturas indicadas pelas associações minerais metamórficas (fácies xisto verde). As temperaturas de deformação também exibem um gradiente regional, com as temperaturas mais altas a sul e mais baixas a norte. Um regime transpressivo com predominância de cisalhamento puro é sugerido com base na forma oblata e nas altas obliquidades dos eixos X do elipsoide de deformação finita. O contexto geológico, os dados geocronológicos e geoquímicos sugerem que o Grupo Itaiacoca e a Formação Bairro dos Prestes podem ser correlacionados às formações Pirapora do Bom Jesus e Boturuna do Grupo São Roque. O Grupo Itaiacoca é interpretado como depositado em uma bacia de retroarco associada ao oceano Adamastor, provavelmente representando uma sutura ediacarana entre o Terreno Apiaí e o Craton Paranapanema. / Field geological mapping, petrographic, geochemical, geochronological and microestrutural analysis obtained from metavolcanic and metasedimentary rocks led to the recognition of two greenschist facies metasedimentary-metavolcanic rock successions in Southwest of Apiaí Terrane in Ribeira belt (between Itapeva and Ribeirão Branco, SP): the Itaiacoca Group and Bairro dos Prestes Formation. The Itaiacoca Group dated by U-Pb method in zircon yield Neoproterozoic ages of 602.7 ± 24 (metabasite) and 613.5 ± 9.6 Ma (metatuff), it is constitute by a succession of metamudstone, phyllites and fine-grained quartzites (Água Nova Formation), intercalated with calcitic and dolomitic metalimestone with stromatolite structures and small beds of metatuff (Bairro dos Campos Formation) in transition contact with metabasites, metadolomites, talc schists and chlorite schists (Fazenda Velha Metabasic Suite), and massive quartzites (Serra dos Macacos Formation) overlapping all the units. Based on geochemistry characterization, the metabasites with tholeiitic and calc-alkaline signatures have patterns of MORB-type mantle with contribution of subduction components typically of back-arc basin basalts. The Bairro dos Prestes Formation was deposited between 1761 ± 14 and ~1800 Ma (Zircon SHRIMP U-Pb data of metarhyodacite and metavolcanosedimentary rock, respectively), it is composed of phyllites sometimes with amygdaloid structures in transitional contact with fine to medium grained-quartzites and restricted metaconglomerate and felsic metavolcanic rocks with high-K calc-alkaline signature. In the study area is also present the flat-lying sedimentary rocks of the Paleozoic Itararé Group, the Ediacaran fine to coarse-grained feldspathic quartz metasandstones of the Apiaí-Guaçu metasandstone, the Três Córregos Granitic Suite and the Paleoproterozoic Apiaí Mirim Complex. The Apiaí Miriam Complex comprises paragneiss and medium to coarse grained micaceous quartzite affected by amphibolite facies metamorphism, while the Três Córregos Granitic Suite consists of porphyritic monzogranite and subordinate sienogranite. The maximum depositional age calculated by U-Pb ICPMS- LA of detrital zircons of the Apiaí-Guaçu metasandstone was 588.4±1.8 Ma which allows to correlate it with the transition stage basins of the Brasiliano Cycle. The structural arrangement comprises relict bedding (So), and three tectonic foliations (Sn, Sn+1 and Sn+2). The main foliation (Sn) is characterized as a schistosity or slaty cleavage, generally parallel to So, presenting NE-SW strikes and steep dips, and it is deformed by Sn+1 and Sn+2 crenulation cleavages. The Sn+1 is associated with tight folds with NW axial-planes in quartzite metavolcanosedimentary and pelitic sequence, and the Sn+2 with open folds with NE axial-planes in quartzite and phyllite rocks. The study area is also affected by NNW-SSE and NNE-SSW faults. The microstructural analysis was performed in samples of Bairro dos Prestes Formation and Apiaí Mirim Complex through Shape Preferential Orientation (SPO) and Lattice Preferred Orientation (LPO) techniques, determinate an oblate shape for the finite strain ellipsoid with XY planes with NE-SW strike and X-directions with high rake, correlated with the structural data measured in field. The deformation temperatures calculated from opening-angle of c-axis structures vary from 531°C-593°C to 613°C-703°C, they were influenced by water weakling and solution-transfer process, being sometimes higher that the temperatures indicated by the metamorphic mineral assemblages (facies greenschists). The deformation temperatures also display a spatial gradient, in the south the highest temperatures are present, while in the north, the lowest temperatures were calculated. A transpressive regime with predominance of pure shear is suggested based on the oblate shape and high rake X axis of the finite strain ellipsoid. The geological context, geochronological and geochemical data suggest that the Itaiacoca Group and Bairro dos Prestes Formation can be correlated with Pirapora do Bom Jesus and Boturuna formations of São Roque Group. The Itaiacoca Group is interpreted as arc-back-arc basin system is associated with the large Adamastor Ocean, and probably represents an Ediacaran suture zone between the Apiaí Terrane and the Paranapanema Craton.

[pt] O presente trabalho compara os efeitos de dois parâmetros diferentes de curvamento a quente na microestrutura e nas propriedades mecânicas de um tubo de aço API 5L X80, com carbono equivalente Pcm de 0,17 porcento e sigma NbTiV de 0,11 porcento produzido pelo processo UOE e originado de chapa obtida por processamento termomecânico sem resfriamento acelerado, cujo limite de resistência é de 679 MPa. Os dois parâmetros de curvamento consideram potência de 105 kW e frequência de 2500 Hz, sendo que o segundo curvamento foi realizado com potência de 205 kW e freqüência de 500 Hz. O aumento da potência e a redução da freqüência promoveram um aporte térmico maior e uma camada de zona afetada mais espessa, onde o aquecimento ocorre por resistência à passagem das correntes induzidas, resultando em distribuição mais uniforme de tamanho de grão austenítico e aumento da temperabilidade. Durante o curvamento, um gradiente térmico é formado ao longo da espessura, onde a superfície externa é temperada em água e a superfície interna é resfriada ao ar calmo, resultando em alterações microestruturais e de propriedades mecânicas. Após curvamento com frequência de 500 Hz, os valores de limite de escoamento são limítrofes e os de resistência superiores aqueles normalizados pela API 5L, sendo estas variações creditadas a presença de uma maior fração volumétrica de ferrita bainítica através da espessura do tubo na curva. O tratamento térmico posterior a 600 graus C mostrou, em ambos os casos, que a temperatura otimizada melhora o limite de escoamento e a tenacidade do trecho curvado. / [en] The present work aimed to compare the effect of two different bending parameters on the microstructure and the yield stress of a API5L X80 steel pipe (679 MPa) with Pcm of 0.17 percent and sigma NbTiV of 0.11 percent produced by the UOE process and originated from a plate obtained by thermomechanical processing without accelerating cooling. The two bending parameters considered power of 105 kW and 2500 Hz of frequency and 205 kW and 500Hz. The increase in power lead to a higher heat input and a thicker layer of heat affected zone, due to the lower frequency and the resistance to the eddy currents which resulted in a more homogeneous distribution of the austenitic grain size increasing the hardenability. During the bending process, a temperature gradient is formed through the thickness, where this temperature gradient is formed, while the external surface is water quenched the internal surface is still air cooled, leading to a microstructural and mechanical properties changes. The strength values obtained after bent at 500Hz, closed to those determined by the API 5L, are credited to the presence of a higher depth and volume fraction of ferrite bainite through thickness. The post heat treatment at 600oC proved to be, in both cases, the optimized temperature in order to improve the yield stress and leading better values of toughness.

La thèse a pour but de caractériser les propriétés mécaniques de matériaux à base de fibres de bois en relation avec les propriétés intrinsèques des fibres et leur arrangement spatial complexe. Ce type de matériau, dont les caractéristiques dépendent de sa configuration, est hétérogène à différentes échelles : à l’échelle microscopique de la fibre, à l’échelle mésoscopique du réseau des fibres et à l’échelle macroscopique du matériau. Pour observer ces hétérogénéités, différents moyens expérimentaux de caractérisation sont utilisés, notamment la microtomographie aux rayons X et la corrélation d’images volumiques. Ces deux techniques permettent à la fois de visualiser et numériser la position spatiale des différentes fibres du matériau à l’échelle microscopique dans le volume, et d’obtenir le champ tridimensionnel de déformation à cœur. Comme résultats, le matériau étudié montre un comportement non-linéaire avec une déformation résiduelle et un effet d’hystérésis en charge/décharge, qui suit le modèle de Van-Wyk. A l’échelle microscopique, le champ de déformation 3D apparait fortement hétérogène et est intimement lié aux porosités locales. / This thesis aims at characterizing the mechanical properties of wood-based fibrous material in relation with the intrinsic properties of the fiber as well as the complex architecture of random fibrous assembly. This material, whose characteristics strongly depend on its configuration, is heterogeneous at different scales: microscopic scale of individual fibers, mesoscopic scale of fiber assembly and macroscopic scale of sample. In order to observe these heterogeneities, different experimental characterization methods are employed, especially X-ray microtomography and Digital Volume Correlation. These both techniques allow us to visualize and digitize the spatial position of different phases of material at microscopic scale as well as the full 3D strain field inside the material. The obtained results are following: the material shows a non-linear mechanical behavior with hysteresis and residual deformation during cyclic compression tests, which respects Van Wyk's model. At microscopic scale, the 3D strain field is strongly heterogeneous and deeply related to local porosities.

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.

Phase field models have played an important role in shaping our understanding of a variety of micro structural phenomena in materials. Their attractive features include (a) their ability to capture instabilities in microstructures, and (b) their ability to handle topological transitions { such as splitting or coalescence { gracefully. Therefore, we have chosen to use a phase field model in our study of instabilities in cylindrical pores in nanoporous membranes which eventually lead to their failure. Our study is motivated by recent studies on thermal stability of nanoporous membranes of alumina, titania and zirconia. The key feature in our model is its ability to incorporate surface discussion as the mechanism for mass transport. We first benchmark the model through a critical comparison of our results on early stages of surface evolution during Rayleigh instability and grain boundary grooving with those from linear theories of these phenomena. We have then used longer simulations (which go beyond early stages, and therefore, can incorporate non-lineare effects) to study instabilities in a hollow cylinder in three different systems: single crystal or amorphous solid (which fails through Rayleigh instability), a model sys-tem with parallel grain boundaries (which fails through grain boundary grooving), and a polycrystal (whose failure depends on a combination of grain growth and grooving). In all the cases, the surface energy is assumed to be isotropic, and the operative mechanism for mass transport is assumed to be surface discussion.

Le frittage par micro-ondes est une nouvelle technologie de chauffage rapide utilisée pour l’élaboration de matériaux par le procédé de métallurgie des poudres. Cette méthode de frittage est non seulement économique en temps et en énergie, mais peut aussi permettre d’améliorer les propriétés finales du matériau. Cependant, l’effet bénéfique que peut apporter le chauffage par rayonnement micro-ondes n'est pas encore complètement compris.Dans ce cadre, cette thèse porte sur la mise en œuvre et les comparaisons des comportements en frittages conventionnel et micro-ondes multimodes (2,45 GHz) de l’alumine. La densification et l'évolution de la microstructure des échantillons frittés ont été analysés et comparés entre ces deux processus de chauffage en relation avec la nature des poudres de l'alumine : surface spécifique et teneur en dopant magnésie.A partir du suivi dilatométrique du frittage au cours des traitements conventionnel et micro-ondes, nous déterminons en anisotherme les énergies d’activation apparentes, qui sont considérées comme les paramètres importants de la thermodynamique de frittage : les valeurs trouvées sont toujours plus faibles dans le cas du frittage sous champ électromagnétique, preuve que les diffusions conduisant à la densification sont favorisées. Le suivi in situ permet aussi de déterminer les mécanismes de frittage (étude cinétique), par exploitation des courbes obtenues en traitement isotherme : la diffusion aux joints de grains reste le mécanisme dominant dans la plupart des cas, sauf pour une nanopoudre où la réaction d’interface devient le mécanisme limitant sous champ micro-ondes, preuve là encore de l’influence du champ électromagnétique sur la diffusion.Nous avons ainsi mis en évidence et expliqué les effets d’un champ électromagnétique sur le phénomène de densification, contribuant à terme à la maîtrise de l’application du rayonnement micro-ondes dans l’industrie céramique. / Microwave energy has been successfully applied as a heating source in the field of powder metallurgy. Compared with conventional heating techniques, microwave sintering has a high potential to reduce the processing time as well as temperature, and to optimize functional properties. However, the detailed explanation of this enhanced effect underlying microwave sintering is still under debate.Taking into account those issues, the objective of this work was to investigate comparatively conventional and 2.45 GHz microwave multimode sintering of alumina. The densification behavior and microstructure evolution of alumina powders with different MgO doping levels as well as specific surface areas have been systematically and quantitatively studied.By the way of dilatometric measurements in both conventional and microwave processes, studies in terms of thermodynamics were carried out in non-isothermal conditions. The apparent activation energy values are significantly lowered when microwave is applied, indicating a microwave-induced enhancement on diffusion. Furthermore, densification kinetics was isothermally taken in order to study in more detailed manner the mechanism(s) involved during microwave sintering. It suggests that the grain boundary diffusion is the dominant mechanism in most cases, except for a nanopowder. In the case of fine-grained alumina, it was assumed that microwave-assisted densification is controlled by in-series “interface-reaction / grain-boundary diffusion” mechanism. But anyway, grain-boundary diffusion has been always enhanced by microwave non-thermal effect.This work will be meaningful to develop the in-depth understanding of the microwave sintering process at both the fundamental and the applied levels.

Cette thèse participe au développement d’un combustible particulaire uranium-molybdène dans le cadre de la conversion des réacteurs de recherche de haute-performance en France et à travers le monde, à l’utilisation de combustibles faiblement enrichis (LEU : Low Enriched Uranium à opposer à HEU : High Enriched Uranium). Ce dernier se présente sous la forme d’une dispersion de particules uranifères U(Mo) dans une matrice à base d’aluminium et une question majeure persiste quant à l’interaction se produisant entre le composé U(Mo) et la matrice d’aluminium. En effet, il a été constaté que sous certaines conditions d’irradiation, cette interaction donne lieu à un gonflement instable de la plaque combustible qui résulte d’une percolation accentuée et imprévisible de bulles de gaz de fission à l’interface entre une couche d’interaction formée autour des particules U(Mo) et la matrice aluminium. Cette thèse s’est attachée à développer plusieurs solutions « remèdes » visant à modifier et/ou diminuer, voire inhiber l’interaction combustible/matrice et à améliorer la rétention des bulles de gaz de fission. Pour atteindre ces objectifs, deux voies ont été testées au cours de la thèse, (i) l’amélioration des propriétés microstructurales intrinsèques de l’alliage U(Mo) et (ii) la modification de l’interface âme combustible / matrice, par le dépôt de couches à effet barrière. En ce qui concerne le premier axe de recherche, une campagne de caractérisation des poudres de référence a, au préalable, été réalisée, permettant d’identifier des paramètres clés pour le développement de produits à microstructure « optimisée ». Deux produits innovants ont ainsi été développés puis soumis à caractérisation : une poudre atomisée-broyée et une poudre obtenue par magnésiothermie. Nous avons démontré que ces produits peuvent être un atout vis-à-vis de la problématique de rétention des bulles de gaz de fission. En ce qui concerne la problématique de la formation d’une couche d’interaction, un troisième produit, reposant sur le génie des procédés, a été développé : une poudre U(Mo) atomisée, revêtue d’une couche type alumine. Nous avons démontré qu’une couche comprise entre 100 et 200 nm permettait d’inhiber la croissance d’une couche d’interaction activée thermiquement. Nos recommandations finales ont ainsi pu être données en vue de la réalisation de tests d’irradiation « en-pile » pour la qualification d’un combustible U(Mo) optimisé. / This thesis enters in the Material and Testing Reactors (MTRs) framework where the necessity to use a Low-Enriched Uranium (LEU) fuel has led to the development of a dense fissile material based on U(Mo) alloys. The designed fuel is a composite material, made of dispersed U(Mo) particles embedded in an Al based matrix. Post-Irradiation Examinations of these LEU fuel plates showed that the irradiation behaviour of the fuel is not fit for purpose yet. This is mainly due to the growth of an interaction layer between the fuel and the matrix and to the bad gas retention efficiency of the fuel particles. This thesis had for purpose the development of several solutions in order to modify and/or decrease or even inhibit the fuel/matrix interaction and to increase the gas retention capacities of the fuel. In order to achieve so, two solutions have been tested during this thesis, (i) optimization of the U(Mo) alloy intrinsic microstructural properties and (ii) modificationof the fuel meat/matrix interface, through the deposition of a layer acting as a ''diffusion barrier''. Concerning the first axe of study, a characterization campaign of the reference powders has been realized, as a first step, in order to identify the key parameters for the development of products showing an “optimized” microstructure. Two novel products have then been developed: one based on a combined process associating “atomization + grinding” and another, which consists in a magnesiothermy process. These products were subject to characterization: X-Ray and neutron diffraction, electron backscattered diffraction and transmission electron microscopy have been performed in particular. We managed to show that these powders can be an advantage concerning the issue with the gas retention capacities of the fuel. Concerning the growth of the interaction layer, a third product, using process engineering, has been developed: an U(Mo) atomized powder, coated with an alumina like layer. We managed to show that a thickness between 100 and 200 nm of the layer allowed inhibiting the growth of a thermally activated interaction layer. Finally, our recommendations have been given in order to realize irradiation tests “in-pile” for the qualification of an optimized U(Mo) fuel.