A obtenção de cerâmicas de SiC pela sinterização com a presença de aditivos que promovam a formação de uma fase líquida (SFL) durante o processo tem sido uma forma adequada para garantir a menor temperatura de sinterização. Pelo fato de o SiC ser frágil, a busca por melhores propriedades mecânicas e avaliação correta das mesmas, para ser aplicado em ambientes agressivos, é contínua. Com base nisso, na primeira etapa, foram estudados, quanto à molhabilidade sobre o SiC, os sistemas AlN/Re2O3 (Re = Dy, Yb) para serem utilizados como aditivos. Os ângulos de contato medidos foram menores que 10° e considerados adequados para a SFL. O SiC sinterizado com esses aditivos permitiu produzir microestruturas diferentes com o aumento da temperatura. Na segunda etapa, foram sinterizadas amostras na forma de pastilhas em várias temperaturas, cujas condições que apresentaram os melhores resultados de massa específica real e densidade relativa foram tomadas como referência para a sinterização na forma de barras prismáticas. Na terceira etapa, essas amostras foram avaliadas quanto à sua tenacidade à fratura (KIC) pelo método da barra entalhada em V, dureza e resistência à flexão. O comportamento de KIC foi avaliado em função da profundidade e raio de curvatura dos entalhes. Os valores variaram entre 2,59 e 3,64 MPam1/2. Verificou-se que os valores de KIC confiáveis foram aqueles encontrados com pequeno raio de curvatura na ponta do entalhe. Quando o raio foi grande, o mesmo não manteve a singularidade da raiz quadrada da ponta do entalhe, e forneceu valores de KIC superestimados. Foram realizados testes para determinar KIC em ar atmosférico e em água, cujos resultados foram menores em água que em ar, com queda entre 2,56 e 11,26%. A maior resistência sob flexão determinada em 4 pontos foi de 482 MPa. Observou-se correlação direta do tamanho dos grãos nos valores de KIC, dureza e módulo de ruptura das cerâmicas de SiC. / Obtaining SiC ceramics by sintering in the presence of additives that promote a liquid phase formation (LPS) during the process has been a proper manner to ensure the lowest sintering temperature. Because SiC is brittle, an ongoing search for better mechanical properties and proper evaluation of these properties for application in aggressive environments maintained. Thus, in the first stage we studied AlN/Re2O3 systems (Re = Dy, Yb), as to their wettability on SiC, for use as additives. The measured contact angles were smaller than 10° and considered suitable for the LPS. The sintered SiC with these additives allowed the production of different microstructures with the increase in temperature. In the second stage, pellet-shaped samples were sintered at various temperatures, and the conditions showing the best density results were taken as reference for sintering prism-shaped bars. In the third stage, these samples were evaluated for toughness (KIC) by single edge V-notched beam method, hardness, and flexural strength. The behavior of KIC was assessed for notch depth and notch radius of curvature. Values ranged between 2.59 and 3.64 MPa/m1/2. The reliable values of KIC were those found with small radius of curvature at the notch tip. When the radius was large, it did not maintain the singularity of the square root of notch tip and provided overestimated KIC values. Tests were performed to determine KIC in atmospheric air and water, and results were lower in water than in air, dropping between 2.56 and 11.26%. The greatest strength under the 4-point bending test was 482 MPa. We observed a direct correlation of grains size in KIC values, hardness and bending strength of SiC ceramics.

Materiais compostos de matriz metálica (CMM) vêm sendo estudados para diversas aplicações. Entretanto, pouco estudo é apresentado na sua confecção a partir de materiais reciclados. Este trabalho teve como objetivo a caracterização de um material composto de matriz metálica (CMM), utilizando material reciclado como matéria prima. Foram usados aparas de chapas de liga de alumínio 2024 descartados para a matriz e carbeto de silício (SiC) como reforço, sendo a produção realizada através do processo de fabricação com base na técnica de conformação por spray para possível aplicação em componentes automotivos. Foi realizado o tratamento térmico do material e a caracterização, determinando as propriedades de dureza, resistência mecânica, resistência ao desgaste, MEV e EDS. Foram ensaiadas amostras do material composto fundido e extrudado, bem como de ferro fundido de uma peça automotiva e da liga de alumínio 2024. Observou-se que o CMM ainda precisa de melhorias no processo de produção para obter propriedades de dureza e resistência que permitam que ele possa ser usado como um substituto para o ferro fundido, porém o mesmo apresentou melhores propriedades quando comparado com o material da matriz. / Metal matrix composites (MMC) have been studied for several applications. However, little study is presented in its manufacture from recycled materials. This study aimed to characterize a metal matrix composite (MMC), using recycled material as raw material. Were used aluminum alloy 2024 plates clippings discarded for the matrix and silicon carbide (SiC) as reinforcement, being the production accomplished through the manufacturing process based on the technique of spray forming for possible application in automotive components. The thermal treatment and the characterization of the materia was accomplished, determining the properties of hardness, mechanical strength, wear resistance, SEM and EDS. Were tested samples of the cast and extruded composite material, as well as cast iron of an automotive part and aluminum alloy 2024. It was observed that the MMC still needs improvements in the production process to obtain properties of hardness and strength that allows it to be used as a substitute forcast iron, but it presented better properties when compared with the matrix material.

Le carbure de silicium (SiC) est un matériau léger possédant de nombreuses propriétés avantageuses : forte résistance mécanique, bonne conductivité et faible expansion thermiques, ainsi que chimiquement inerte sur une large gamme de températures. Ces caractéristiques font de lui un matériau de choix pour de nombreuses applications dans des conditions extrêmes, allant de la catalyse au gainage de combustible nucléaire de génération IV. Pour satisfaire aux spécificités de ces applications, le SiC se doit de posséder une surface spécifique élevée, et une porosité contrôlée.Nous avons étudié la faisabilité de la synthèse de SiC mésoporeux par une voie dite de « soft templating » utilisant des semifluoroalcanes (SFA) linéaires pour structurer un précurseur moléculaire du SiC, le 1,3,5-trisilacyclohexane (TSCH). En effet, la polymérisation du TSCH en polycarbosilane autour d’assemblages de SFA permet de structurer la matrice, puis de créer de la porosité lors du retrait du template. Le polycarbosilane est ensuite converti en SiC par un processus de calcination au cours duquel la porosité doit être conservée.Dans un premier temps, nous avons temps étudié les capacités d’auto assemblage des SFA dans le cyclohexane comme solvant modèle, puis dans le TSCH, par des techniques de diffusion des rayons X et des simulations des diagrammes de diffusion. Nous en avons appréhendé le comportement et déterminé les paramètres contrôlant la taille des objets. Nous avons ensuite réalisé la synthèse de SiC à partir du TSCH en présence de SFA.Les matériaux obtenus ne présentant pas les caractéristiques de surface spécifique et de porosité visées, nous avons élargi nos recherches à d’autres templates, dont un copolymère tribloc styrène-butadiène-styrène, qui a permis d’obtenir des SiC mésoporeux, amorphes ou cristallins, par une voie impliquant le greffage des précurseurs de SiC sur le copolymère. / Silicon carbide (SiC) is a light material with numerous interesting properties: strong mechanical resistance, weak thermal expansion, good heat conductivity and chemically inert on a large range of temperatures. These characteristics make SiC an appropriate material for various applications in extreme conditions, from catalyst to generation IV nuclear fuel cladding material. Nevertheless, to fulfill these application specificities, SiC has to show high specific surface area, and a controlled porosity.We have studied the possibility to synthetize mesoporous SiC by a soft templating approach using semifluorinated alkanes (SFA) to structure a SiC molecular precursor, the 1,3,5-trisilacyclohexane (TSCH). The TSCH polymerization into polycarbosilane around SFA aggregates can structure the matrix, that will create porosity after the template removal. Then polycarbosilane is converted into a SiC by a calcination process conserving the porosity.In a first time, we studied the self-aggregation capacities of SFA in cyclohexane as model solvent, and then in TSCH, by X-ray scattering techniques and simulations of scattering patterns. We discussed the behavior of SFA and determined the parameters controlling the size of the aggregates. Then, we proceeded to SiC synthesis from TSCH in presence of SFA.As resulting materials didn’t show the expected specific surface area and porosity characteristics, we enlarged our studies to other templates such as a triblock copolymer styrene-butadiene-styrene, which finally allowed us to obtain mesoporous SiC, amorphous or crystalline, by an approach involving the grafting of the SiC precursor onto the copolymer.

Différents matériaux carbonés nanostructurés ont été synthétisés et mis en oeuvre comme matériaux supercapacitifs à double couche électrochimique (EDLC) ou comme substrats de matériaux pseudocapacitifs avec pour objectif d'augmenter leur densité de puissance. Nous avons ainsi développé une méthode de synthèse simple et originale de carbures de silicium (SiC) qui procède par une réduction topotactique d'un composite silice/carbon par le magnésium. Du fait de la température de synthèse inférieure à 800°C, SiC résultant conserve la morphologie et/ou la structure poreuse du précurseur composite. Par cette approche, nous pouvons moduler la structure poreuse ordonnée de SiC à façon, développer des porosités hiérarchiques méso/macro, préparer des feuillets ou des fibres de SiC. Les différentes formes de SiC ont été converties par chloration en autant de carbones, opération introduisant une microporosité supplémentaire. En électrolyte organique, ces carbones à porosité hierarchique combinent à la fois des capacités importantes issues de la microporosité mais également des performances inégalées en terme de puissance du fait de la méso ou macro-porosité associée. Dans une approche différente, des feuillet de graphène ont été décorés par voie sol-gel non-hydrolytique (micro-onde en milieu alcool benzilique) par des nanoparticules de FeOx. Le composite FeOx/graphene résultant combine simultanément les comportements EDLC et pseudocapacitif du graphène et de FeOx. Du fait de sa structure particulière, le composite FeOx/graphene conserve les performances en puissance du graphène auxquelles s'ajoutent celles d'énergie de FeOx. Nous avons également décoré des nanofibres de carbone avec des carbones mésoporeux. Après dépôt de MnO2 birnessite, les composites gagnent à la fois en capacité et en puissance en particulier avec des carbones présentant des pores supérieurs à 10nm. / Various nanostructured carbon materials were synthesized and further served as active materials of electrical double layer capacitor or substrates of pseudocapacitive materials in order to improve power capability of corresponding supercapacitor. On the one hand, a simple synthesis of porous silicon carbides (SiCs) was achieved by performing a topotactic thermal reduction by magnesium (Mg) of a silica/ carbon composite. Thanks to the low synthetic temperature (below 800 ºC), the SiCs well preserved the pristine skeletons of their silica/carbon precursors. Successively, the SiCs with diverse porous structures from their silica/carbon precursor emerged, e.g. ordered tunable mesoporous SiCs, 3D-hierarchical meso and macroporous SiC, SiC nanosheet and SiC nanofiber. Furthermore, the porous SiCs derived from magnesio-thermal reduction were reduced to hierarchical carbons with newborn narrow distributed microporosity by chlorination. In an organic electrolyte, the hierarchical carbon combines the high specific capacitance from narrow distributed microporosity and the outstanding rate capability from ordered-arranged meso or macroporosity that make it promising for high power and energy density capacitor. On the other hand, a “benzyl alcohol route” has been used to decorate RGO nanosheets with FeOx nanoparticles. The resulting FeOx/ RGO composite, due to their hybrid nanostructure, combine both EDLC capacitive and pseudocapacitive bahaviors of RGO and FeOx, respectively. Thanks to the laminated RGO and nano FeOx particles film, the resulting composite gains the same power capability as RGO and a higher energy density than raw FeOx. Furthermore, mesoporous carbon was introduced to adorn the CNF surface through self-assemble of resol, carbon nanofiber(CNF) and Pluronic@127. After further coating with birnessite-MnO2, the composite electrode gains extra capacitance and power improvement in presence of superficially coating mesoporous carbon with pore size larger than 10nm.

In 1972 Fujishima and Honda conceptualised a photoelectrochemical cell for hydrogen generation via PEC water splitting. Hydrogen as a clean energy carrier provides environmentally friendly energy storage solutions or can fuel certain applications. This idea has since then been further built upon with new materials and combinations with the aim of improving efficiency. In this project n-type cubic silicon carbide thick layers were grown by a sublimation method and characterised for water splitting performance. A generated photo-current density of 0.45 mA/cm2 was measured with no bias between the working and counter electrodes.

Face à la nécessité de trouver de nouvelles sources d'énergie, on assiste au développement des centrales solaires thermiques à concentration et plus particulièrement à tour. L'air est utilisé comme fluide caloporteur circulant dans un récepteur sur lequel sont concentrés les rayons solaires. L'absorbeur, situé dans le récepteur, est l'élément clé de ces dispositifs ; il doit absorber le rayonnement solaire tout en ayant une faible émissivité infrarouge pour limiter les pertes par rayonnement thermique observées. Le projet OPTISOL, dans lequel s'inscrivent ces travaux de thèse, a pour objectif d'optimiser les propriétés thermo-optiques d'un absorbeur volumique. Pour cela, une mousse en carbure de silicium a été choisie en tant que support mécanique de l'absorbeur, pour sa bonne tenue aux hautes températures, et pour sa capacité à absorber fortement le rayonnement solaire. Plusieurs laboratoires ont travaillé sur ce projet et le rôle du CIRIMAT fut, dans un premier temps, de caractériser ces mousses de carbure de silicium, par des techniques conventionnelles mais aussi par des techniques moins usuelles telles que la microtomographie X. Dans un second temps, les mousses de carbure de silicium ont été fonctionnalisées par un oxyde sélectif, YBaCuO, dans le but d'optimiser la sélectivité spectrale du système global. Pour cela, les techniques en voie liquide (sol-gel, suspensions, ...) ont été choisies et un procédé de fonctionnalisation a été développé, permettant de revêtir des substrats plans (pastille) et volumiques (mousse poreuse). La sélectivité spectrale du carbure de silicium ainsi fonctionnalisé a été étudiée par spectrométrie infrarouge-visible et les résultats obtenus sont prometteurs puisque une diminution de l'émissivité infrarouge a été observée tout en conservant une forte absorptivité du rayonnement solaire. / The necessity of finding new energy sources leads to the development of concentrated solar thermal power plants and more particularly the one using towers. Air is used as a heat transfer fluid flowing in a receiver heated by concentrated sunlight. The absorber, located in the receiver, is the key element of these devices; it must both absorb solar radiation and have a low infrared emissivity to limit thermal radiation losses. This work is part of the OPTISOL project, which aim is to optimize the thermo-optical properties of a volumetric absorber. For this purpose, a silicon carbide foam was selected as the mechanical support of the absorber for its good resistance to high temperatures and for its ability to be efficient to absorb sunlight. Several laboratories have worked on this project and the role of CIRIMAT was, at first, to characterize these silicon carbide foams using conventional and less conventional techniques such as X microtomography. Secondly, silicon carbide foams have been functionalized by a selective oxide, YBaCuO, in order to optimize the spectral selectivity of the system. For this, liquid routes such as sol-gel or suspension techniques have been selected and a functionalization process was implemented for coating planar (pellet) and volumetric (porous foam) substrates. The spectral selectivity of the functionalized silicon carbide was studied by infrared-visible spectrometry and the results are promising since a decrease in the infrared emissivity was observed while maintaining a high absorptivity of solar radiation.

Les détecteurs de radiations nucléaires sont des outils importants dans de nombreux domaines tels que dans les réacteurs nucléaires, la sécurité nationale, mais ils sont également primordiaux dans des applications médicales. Les progrès récents dans la technologie des semi-conducteurs permettent la réalisation de détecteurs très efficaces et quasi-insonores qui permettent la détection de différents types de radiations nucléaires. Le carbure de silicium (SiC) est une bande semi-conductrice large, grâce à sa conductivité thermique élevée et à une résistance élevée aux rayonnements, il est adapté pour les environnements difficiles où peuvent exister des flux élevés de température et de rayonnement. Le but du projet européen (I_SMART) est ainsi de prouver la fiabilité de nouvelles méthodes de réalisation de détecteurs de radiations nucléaires et d'étudier leur performance dans différents types d'irradiation (neutrons rapides et thermiques) et à différentes températures. Différentes méthodes ont été utilisées pour réaliser les détecteurs de rayonnement SiC. Par exemple l'implantation d'ions de bore a été utilisé pour créer la couche de conversion de neutrons soit dans le contact métallique ou directement en SiC. Les détecteurs fabriqués ont été testés dans le réacteur nucléaire BR1, mettant en lumière la présence de neutrons thermiques. En outre, ces détecteurs détectent des neutrons rapides sous n’importe quelle température. En outre, les détecteurs utilisés montrent leur stabilité sous différents flux de neutrons qui indiquent la fiabilité de ces nouveaux modes de réalisation de détecteurs de rayonnement qui pourraient remplacer ceux utilisés actuellement. / Nuclear radiation detectors are important tools in many fields such as in nuclear reactors, homeland security and medical applications. Recent advances in semiconductor technology allow construction of highly efficient low noise detectors for different nuclear radiations. Silicon carbide (SiC) is a wide band gap semiconductor with a high thermal conductivity and high radiation resistance. It is suitable for a harsh environment where high temperatures and radiation fluxes may exist. In the framework of the European project (I_SMART) the purpose of this work is to demonstrate the reliability of new methods of realizing nuclear radiation detectors and to study their performance under different types of irradiation (fast and thermal neutrons) and at elevated temperatures. Different methods have been used to realize SiC based-radiation detectors. For instance boron ion implantation has been used to create the neutron converter layer either in the metallic contact or directly in the SiC. The fabricated detectors have been tested in the BR1 nuclear reactor revealing the thermal neutron detection and the feasibility of gamma discrimination from thermal neutrons using one single detector. Such detectors are sensitive to fast neutrons with a stable response under elevated temperatures (up to 150 °C). Furthermore, the studied detectors show stability under different neutron fluxes, indicating a reliability of such new methods of realizing radiation detectors which could replace those of the current state of the art.

Ce travail s’inscrit dans le cadre de la caractérisation physique de nanofils (NF) semiconducteurs (SC) qui est un domaine en plein essor ces dernières années. Plus précisément, nous explorons l’émission de champ (EC) de NFs individuels de Carbure de Silicium (SiC) pour leur potentialité comme source d'électrons, mais surtout pour étudier leurs propriétés de transport électrique, optiques et mécaniques.Le rôle important joué par la surface dans ces NFs a été prouvé par des traitements in situ qui ont eu des conséquences radicales sur l’EC dévoilant ainsi des propriétés d’émission propres aux SCs. En particulier, un régime de saturation, en accord avec la théorie d’EC des SCs, associé à une forte dépendance de l'émission à la température et à l’illumination laser a été révélé pour la première fois pour un NF. Ces mesures ouvrent des perspectives importantes tant pour la recherche fondamentale que pour les applications telles que la réalisation de photocathodes et de sources d’électrons pilotées optiquement ou par la température. Les caractéristiques courant-tension-température associées à l’analyse en énergie des électrons émis nous ont permis de déterminer le mécanisme de transport dans ces NFs, qui est limité par le nombre de porteurs dans le volume et contrôlé par les pièges présents dans la bande interdite par l’effet Poole-Frenkel. Finalement, la caractérisation mécanique a révélé des valeurs du facteur de qualité élevé (160000) et du module de Young allant jusqu’à 700GPa. Ces valeurs sont très prometteuses pour l’utilisation de ces NFs dans les systèmes nano-électro-mécaniques et dans les composites. / We use field emission (FE) from individual silicon carbide nanowires (NWs) to explore their potential as electron sources, and especially as a versatile tool for studying transport, optical and mechanical properties of NWs. These studies fall within the larger framework of the physics of semiconducting (SC) nanowires, which is presently a large and rapidly expanding domain. The important role played by the surface in the transport and optical properties of NWs was clearly demonstrated by the radical consequences induced by in situ treatments on the FE properties. This permitted the observation of the specific behavior expected for SCs, particularly, a current saturation regime in agreement with the theory of FE for SCs. We found that the saturation was concomitant with a strong dependence of the emission on temperature and laser illumination, revealed for the first time for a NF. These measurements open important perspectives for both fundamental research and applications such as the realization of optically or thermally controlled FE electron sources. The current-voltage-temperature characteristics were carried out in parallel with measurement of the energy distributions of the emitted electrons, thus permitting the determination of the transport mechanism in the NWs. We found that the transport was limited by the carrier density in the volume and by the traps in the gap that generate current through the Poole-Frenkel effect. Finally, the mechanical characterization revealed high quality factors, as high as 160,000, and a Young’s modulus up to 700 GPa. These values are very promising for the use of these NWs in nano-electro-mechanical systems (NEMS) and composites.

This thesis evaluate the state of art ROHM SCT3080KR silicon carbide mosfet in a synchronous buck converter. The converter was using the ROHM P02SCT3040KR-EVK-001 evaluation board for driving the mosfets in a half bridge configuration. Evaluation of efficiency, waveforms, temperature and a theoretical comparison between a silicon mosfet (STW12N120K5) is done. For the efficiency test the converter operate at 200 V input voltage and 100 V output voltage at output currents of 7 A to 12 A, this operation was tested at switching frequencies of 50 kHz, 80 kHz and 100 kHz. The result of the efficiency test showed an efficiency of 98-97 % for 50 kHz, 97.7-96.4 % for 80 kHz and 97-96.2 % for the 100 kHz test. The temperature test shows a small difference in comparison of the best case scenario and the worst case scenario, temperature ranges from 25.5 to 33.5 °C for the high side mosfet while the low side mosfet temperature ranges from 29.8 to 35 °C. The waveform test was conducted at 50 kHz and 100 kHz for output currents of 4 A and 12 A (at 200 V input and 100 V output). The result of the waveform test shows a rise and fall time of the voltages in range of 10-12 ns while the current rise and fall time was 16 ns for the 4 A test and 20 ns for the 12 A test. Overall SiC mosfet show a clear advantage over silicon mosfet in terms of efficiency and high power capabilities.

This master thesis deals with design of DC-DC converter for onboard charging of electric vehicle. Developed converter will mainly be used for charging stationary traction battery in laboratory. Output voltage of this charger will be adjustable by user in between 200 V and 450 V depending on the current charged battery configuration. Output current limit is set at 8 A. Since the converter will be supplied from standard household socket, the problem of power factor correction must be solved during the design. That is because a large part of this thesis is focused on describing the problematics of power factor correction. After that, active PFC module is designed, completed and performance of this module is verified. To achieve low overall losses and thus be able to keep small volume of the system, modern switching components based on Silicon Carbide were preferred. Beside laboratory use, completed system will be used to emphasize volumetric difference between onboard chargers based on old versus modern switching components.