<p>Advances in modern technology and recent demand for high power applications have motivated great interest in power electronics. Power semiconductor devices are key components that have enabled significant advances in power electronic systems. Historically, silicon has been the material of choice for power semiconductor devices such as diodes, transistors and thyristors. However, silicon devices are now reaching their fundamental limits, and a transition to wide bandgap semiconductors is critical to make further progress in the field. Among them, SiC (silicon carbide) has attracted increasing attention as a power semiconductor to replace silicon due to its superior properties and technological maturity. In fact, SiC power MOSFETs have been commercially available since 2011, and are actively replacing their silicon counterparts at blocking voltages above 1 kV. At these voltages, the specific on-resistance of SiC MOSFETs is 200-300x lower than that of silicon devices. However, conventional vertical SiC MOSFETs are still far from their theoretical performance at blocking voltages below 2 kV. In this regime, the channel resistance is the dominant limitation due to the relatively low channel mobility at the SiO2/4H-SiC MOS interface.<br></p><p> </p><p>In this thesis, the first successful demonstration of a novel power device in 4H-SiC called the trigate power DMOSFET (double diffused metal oxide semiconductor field effect transistor) is presented. This device reduces the channel resistance by a factor of 3-5× compared with the state-of-art commercial power DMOSFETs, without requiring an increase in the channel mobility. The trigate structure is applied to a power MOSFET for the first time along with a self-aligned short channel process. This new structure utilizes both the conventional horizontal surface as well as the sidewalls of a trench to increase the effective width of the channel without increasing the device area. Conceptual design, optimization, process development and electrical results are presented. The trigate power MOSFET with a trench depth of 1 μm designed for a blocking voltage of 650 V has a specific on-resistance of 1.98 mΩcm²and a channel resistance of 0.67 mΩcm².This corresponds to a ∼2× reduction in the total specific on-resistance, and a 3.3× reduction in the specific channel resistance as compared to a conventional DMOSFET with the same blocking voltage rating. This demonstration is a landmark that could help SiC technology compete successfully in the lower blocking voltage regime below 600 V, and access for the first time a completely new segment in the power electronics application space.</p>

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The master’s thesis deals with the topic of electrical discharge machining. The first part of the thesis contains a study of the die-sinking EDM. The die-sinking EDM of the silicon carbide ceramic is realized in the experimental part of the thesis. The result of this work was to explore the influence of the EDM sinking parameters, specifically pulse current, open-voltage and pulse on-time, on the machined surface. Furthermore, the analysis of the tool electrode was made. This analysis was focused on the wear in the corners, which has key influence on accuracy of the machining. The machining time was also examined.

This thesis is about to introduce the development of switched power supply with output voltage of 5,5 kV and power of 4,3 kW. This thesis directly follows the outputs of two previous semester projects. Main task is about to finish the development of remaining printed circuit boards and perform launching of all parts of developed power supply. Next necessary task is about to assemble a functional prototype of the supply using the developed parts, performing a series of measurement supply’s parameters and creating of technical documentation of mechanical part. There are all stages of supply’s development included in this thesis. From the first part, that describes various types of converters, through the design of all the supply’s parts, to final implementation of functional prototype. There are the results of measurement supply’s parameters at the end of this thesis.

Diploma thesis deals with the determination of fracture toughness values of sintered silicon carbide and casted basalt using both the Single Edge V-Notch Beam (SEVNB) and the Chevron Notched Beam (CNB) methods at room and cryogenic temperatures. The first part of this thesis offers general overview and categorization of ceramic materials. Fracture mechanics of the ceramic materials and available fracture toughness testing methods are discussed in following chapters. The last section in the theoretical part is aimed to the microstructure and properties of the silicon carbide. Experimental part of the work summarizes methods used for characterization of selected materials from the microstructural and fracture point of view. Preparation of samples for microstructural observation and samples for fracture toughness determination are described in details. The results of the fracture toughness data for sintered silicon carbide and cast-basalt obtained at room temperature and at -100 °C are displayed. Consideration of possible measurements errors and application of various fracture toughness testing methods are discussed in the next chapter of this work. The difference in the fracture toughness values with the decrease of testing temperature was found. The difference depends on both, the used method of fracture toughness determination and the material used for the tests. The most important results gained during the experimental work are summarized in the chapter “Conclusions”.

Le développement de protections balistiques toujours plus légères et performantes reste un sujet de recherche très actif. Malgré de très hautes performances, la difficulté de mise en forme du SiC conduit généralement à l’utilisation d’aides au frittage en quantité importante, favorisant la formation de phases secondaires pouvant fragiliser le matériau. De plus, les hautes températures de mise en forme induisent la présence de phase α, conférant au matériau des propriétés mécaniques anisotropes et inférieures à celles de la phase cubique β.Dans ces travaux de thèse, l’objectif a été d’élaborer un matériau SiC cubique de très haute pureté, avec une densité de 100% et une stœchiométrie Si/C idéale afin d’optimiser les performances de cette céramique. Deux types de précurseurs ont été envisagés : une poudre commerciale et une poudre issue de la conversion d’un précurseur polymère précéramique.Dans un premier temps, une étude paramétrique de frittage par SPS a permis d’atteindre des densités de 95% pour les 2 précurseurs, tout en conservant la phase cubique seule. Ces résultats, bien qu’encourageants mais n’étant pas suffisants pour l’application visée, l’étude s’est tournée vers l’ajout d’aides au frittage. Des densités de 100% ont ainsi été obtenues sur des échantillons préparés à partir de poudre commerciale, même pour de très faibles teneurs en additif. Un second aspect de ces travaux a permis de mettre en évidence une dépendance de la température de transition β -> α du SiC vis-à-vis de la pression de frittage mais également vis-à-vis du type de précurseur, l’utilisation du précurseur polymère étant plus favorable à la stabilité de la structure cubique. Enfin des mesures de dureté ont été réalisées sur les meilleurs échantillons et ont permis de souligner le rôle prépondérant de la densité sur cette propriété. / The development of light and high performance ballistic protections is currently a sensitive subject of research. Despite promising mechanical characteristics, the complexity of SiC shaping generally leads to the use of high content of sintering aids, favouring secondary phases formation which could weaken the material. Nevertheless, high sintering temperatures induce the presence of the α form of SiC, conferring to the material anisotropical and lower mechanical properties than the one obtained with the cubic β phase.The goal of this PhD work is the development of high purity cubic SiC, with density close to 100% and perfect Si:C stoichiometry to optimize the performances of this ceramic. Two kinds of precursors were considered: a commercial powder and a powder from the conversion of preceramic polymer precursor.Firstly, the parametric study of SPS sintering allowed to reach densities of 95% for both precursors, while conserving only the cubic phase. These encouraging results being not sufficient, this study switched to the use of sintering aids. Densities close to 100% were thus reached on samples sintered with prepared mixtures from commercial powder, even for very low content of additive. The second subject of this thesis highlighted a dependence of the β -> α transition temperature of SiC as a function of sintering pressure, but also according to the kind of precursor. Indeed, the use of polymer precursor is favourable to cubic structure stability. Then, hardness measurements were performed on the most promising samples and allowed to highlight the major role of density on this property.

Le graphène est un matériau bidimensionnel appartenant à la famille des allotropes du carbone. Il consiste en une couche atomique restant stable grâce à des liaisons chimiques fortes dans le plan entre les atomes de carbone. C'est un semi-conducteur sans bande interdite (gap) avec une dispersion d'énergie linéaire près des points de Dirac, ce qui facilite le transport balistique des porteurs de charge. De plus, tout comme n'importe quel semi-conducteur, il est possible de contrôler ses propriétés électriques sous l'influence d'un champ électrique externe, ce qui permet de modifier la densité de porteurs et leur type (électrons ou trous). Le graphène peut être élaboré par différentes techniques, mais nous avons considéré la croissance directe sur le carbure de silicium (SiC) par dépôt chimique en phase vapeur (CVD) avec une source de carbone externe, technique développée dans notre laboratoire depuis 2010. Cette approche est attrayante car elle permet de contrôler les propriétés du graphène en modifiant les paramètres de croissance. Notre objectif dans ce manuscrit est de donner une idée plus approfondie de cette technique de croissance et d'étudier son potentiel pour la croissance du graphène. À cette fin, nous avons discuté en détail de différents aspects de la croissance, en commençant par des simulations thermodynamiques pour comprendre la chimie gouvernant cette méthode. Nous avons également étudié l'influence des différents paramètres de croissance sur la formation du graphène et sur ses propriétés, tels que le temps de croissance, le débit de propane et d'autres paramètres. Cependant, nous nous sommes principalement concentrés sur deux paramètres majeurs : la quantité d'hydrogène dans le mélange gazeux, surtout que la croissance se fait sous hydrogène et argon, et la désorientation du substrat. Nos recherches ont révélé que la structure du graphène peut être modifiée en fonction de la proportion de l’hydrogène dans le mélange des gaz utilisé pour la croissance. Pour une faible proportion d’hydrogène, la croissance du graphène est associée à une reconstruction d'interface de (6√3×6√3), alors que pour une proportion élevée d’hydrogène, la couche de graphène est désordonnée dans le plan. Ces observations sont liées à l'intercalation de l'hydrogène à l'interface entre la couche de graphène et le substrat SiC, ce qui peut favoriser ou interdire la formation de la reconstruction (6√3×6√3) comme nous l'avons discuté dans le manuscrit. On s'attend à ce que la présence des deux structures de graphène ait un effet sur la contrainte dans la couche de graphène. Pour cette raison, nous avons discuté en détail les origines de la contrainte dans le graphène et tenté de corréler l'intercalation de l'hydrogène à l’interface avec la contrainte. Aussi, nous avons montré que l'angle de désorientation du substrat a une influence directe sur la croissance du graphène, affectant principalement la morphologie mais également la contrainte dans la couche du graphène. Enfin, nous avons pu produire du graphène de haute qualité, tout en démontrant la possibilité de contrôler ses propriétés électriques avec les conditions de croissance. Dans la deuxième partie de ce travail, nous avons étendu notre étude à la croissance du graphène sur les semi-conducteurs de type nitrures d’éléments III et en particulier le nitrure d’aluminium (AlN) massif ainsi que des couches hétéroépitaxiées d’AlN/SiC et AlN/Saphir, ce qui ouvre de nouvelles opportunités pour des applications innovantes. La croissance du graphène a été précédée d'une étude de recuit sur les différents échantillons d’AlN, dans le but d'améliorer leur qualité de surface, mais aussi pour tester leur stabilité à la température nécessaire pour la croissance du graphène. Bien que le film d’AlN ait été incapable de résister à la température élevée dans certains cas, une amélioration de la qualité cristalline a été détectée, attribuée à l'effet de recuit. / Graphene is a two-dimensional material belonging to the family of carbon allotropes, consisting of a stable single atomic layer owing to strong in-plane chemical bonds between carbon atoms. It can be identified as a gapless semiconductor with a linear energy dispersion near the Dirac points, which facilitates ballistic carrier transport. In addition, similarly to any semiconductor, it is possible to control its electrical properties under the influence of an external electric field, resulting in the tuning of its carrier density and doping type, i.e. electrons or holes. Graphene can be elaborated by different techniques and approaches. In this present work, we have considered the direct growth on silicon carbide (SiC) by chemical vapor deposition (CVD) with an external carbon source. This approach which has started to be developed in our laboratory since 2010 is very promising since it allows to control the graphene properties by manipulating the growth parameters. Our objective in this manuscript is to give further insights into this growth technique and to study its potential for the growth of graphene. For this purpose, we have discussed in details different aspects of the growth, starting with thermodynamic simulations to understand the chemistry behind our distinct growth approach. We have also investigated the influence of the different growth parameters, such as the growth time, the propane flow rate and other parameters on the growth of graphene and its properties. However, we mainly focused on two major factors: the hydrogen amount in the gas mixture, especially since the growth is carried out under hydrogen and argon, and the substrate’s miscut angle. Our investigations revealed that the graphene structure can be altered depending on the hydrogen percentage in the gas mixture considered for the growth. For low hydrogen percentage, the graphene growth is associated with a (6√3×6√3) interface reconstruction, whereas for high hydrogen percentage, the graphene layer is dominated by in-plane rotational disorder. These observations are related to the hydrogen intercalation at the interface between the graphene layer and the SiC substrate, which can allow or prohibit the formation of the (6√3×6√3) interface reconstruction as we have discussed thoroughly in this manuscript. The presence of two graphene structures was expected to impact the strain within the graphene layer. For this reason, we have discussed in details the origins of the strain in graphene and attempted to correlate the hydrogen intercalation at the interface to the strain amount. Furthermore, the substrate’s miscut angle was also found to have a direct influence on the growth of graphene, mainly affecting the morphology but also the strain within the graphene layer. In light of the different studies and results, we were able to combine the ideal growth parameters to produce state-of-the art graphene, while demonstrating the possibility of tuning its electrical properties with the growth conditions. In a second part of this work, we extended our study to the growth of graphene on III-nitrides semiconductors. We have considered substrates and templates such as bulk aluminum nitride (AlN), AlN/SiC and AlN/sapphire, which opens new opportunities for innovative applications. The growth of graphene was preceded by an annealing study on the different AlN substrates, in an attempt to enhance their surface quality, but also to test their stability at the temperatures necessary for the growth of graphene. Although the AlN film was found to be unable to withstand the high temperature in some cases, an enhancement of the crystalline quality was detected, attributed to the annealing effect.

In the present work new methods were developed for preparation of novel nanosized and nanostructured ceramic materials. Ordered mesoporous silica SBA-15 was found to be useful as a hard template for the nanocasting of silicon carbide and allowed the preparation of high temperature stable mesoporous silicon carbide ceramics. Chemical vapor infiltration of SBA-15 with dimethyldichlorosilane at elevated temperatures yields SiC/SBA-15 nanocomposites. The subsequent HF treatment of those composites resulted in silica removal and preparation of mesoporous silicon carbide with surface areas between 410 and 830 m2g-1 and high mesopore volume (up to 0.9 cm3g-1). The pore size (between 3 and 7nm in diameter) and surface area of mesoporous silicon carbide were controlled by adjusting the infiltration conditions (time, atmosphere). The mesoporous silicon carbide prepared via this method showed high structural thermal stability at 1300 oC, exceeding that of the SBA-15 template. However, the ordering on the mesoscopic scale was low. Nevertheless, highly ordered mesoporous silicon carbide materials were obtained via polymer melt infiltration in SBA-15. The low molecular weight polycarbosilane used as a preceramic precursor was converted at 1300 oC to silicon carbide inside the SBA-15, and after subsequent silica removal by HF, a highly ordered mesoporous material was obtained. Ordered mesoporous silicon carbide prepared by the methods reported here, may be an interesting material as a support due to its high temperature stability, chemical inertness, high thermal conductivity and semiconductor properties. In contrast to the nanocasting approach, based on the complete pore filling, also a new in-situ procedure for the preparation of finely dispersed metal and metal oxide particles inside ordered mesoporous silica was developed. A swelling agent (toluene) was used to deliver a hydrophobic platinum precursor into the surfactant micelles before addition of silica source. Such an in-situ method resulted in very high platinum incorporation (80-100%), not achieved for any other in-situ preparation procedures. Additionally, the presence of platinum allowed to decrease the template removal temperatures. Moreover, the method was also extended to other metal or metal oxide/ordered mesoporous silica systems. This may be especially interesting for the preparation of ordered mesoporous materials with low melting points, where typically the structure collapses during the high temperature calcinations process. The in-situ synthesized V2O5/MCM-41 materials were used to prepare VN/MCM-41 composites via nitridation in ammonia at 800oC. This method allowed to prepare highly dispersed, X-ray amorphous vanadium nitride species, with high activity in the propane dehydrogenation. Compared to nitridation of supported vanadium oxide prepared via the ex-situ procedure, in-situ synthesized materials showed similar catalytic activity, in spite of having significantly lower vanadium loading. As an alternative for the preparation of supported nitride materials, a novel preparation procedure of bulk not supported nanocrystalline vanadium nitride with high surface area was presented. Instead of pure oxide powder (which was typically used in the preparation of high surface area vanadium nitride catalysts), a macroporous amine intercalated V2O5 was used as the starting material. The obtained nitride consisted of small crystallites and had a surface area up to 198 m2g-1. Moreover, this foam-derived VN showed significantly improved activity as a catalyst in propane dehydrogenation. This novel preparation method could also be extended to other systems such as ternary VMoxNy nitrides.

Les composites SiC/SiC à renfort fibreux à base de SiC, et à matrice SiC sont développés pour applications aéronautiques. En vue d’améliorer leur durée de vie en atmosphère oxydante à haute température, l’utilisation d’interphase BN est préconisée,puisque l’oxyde de bore liquide permet de protéger le matériau. Cependant, sous atmosphère humide, la volatilisation de B2O3 sous forme d’hydroxyde HxByOz est non négligeable. L’objectif de ce travail est d’optimiser l’organisation structurale de BN élaboré par CVD/CVI, pour améliorer sa résistance à l’oxydation, et d’évaluer l’intérêt de l’ajout d’élément(s) au nitrure de bore permettant la stabilisation thermodynamique de B2O3 à haute température, en présence d’humidité. Ce travail a permis d’établir des liens entre composition chimique de la phase gazeuse, cinétique et mécanisme de dépôt, et degré d’organisation du nitrure de bore. Malheureusement, si la résistance à l’oxydation de BN augmente perpendiculairement à ses plans (002) avec son organisation structurale, elle est à peine améliorée le long des plans (002). Néanmoins, l’intérêt de l’ajout d’aluminium à l’interphase BN pour améliorer la stabilité chimique de B2O3 en présence d’humidité a été démontré à une température suffisamment élevée pour permettre la formation de cristauxAl4B2O9. Ainsi, il semble que ces cristaux permettent une cicatrisation efficace des fissures matricielles dans des composites SiC/SiC. Des essais supplémentaires d’oxydation dans des conditions plus complexes, comme sous cyclage thermique, sont nécessaires pour conclure catégoriquement en faveur de l’amélioration de la durée de vie de ces matériaux. / SiC/SiC composites with SiC-based fibres and SiC matrix are developed for aeronautic applications. In order to improve their life time in an oxidizing atmosphere at high temperature, the use of BN interphase is recommended, as far as liquid boron oxide can protect the material. However, this glassy material is known to be very sensitive to moisture because boron oxide volatilizes quickly under high temperature. The aims of this work are (i) to maximise the structural organization of BN deposited by CVD/CVI to improve its oxidation resistance and (ii) to assess the interest of elemental addition to boron nitride allowing thermodynamic retention for B2O3 under wet air. Relationships between gas phase composition, deposition rates, and microstructure have been established in this work. Unfortunately, if the oxidation resistance of BN perpendicular to its (002) crystal planes increases with its structural organization, it appears to be hardly improved along the (002) planes. Nevertheless, aluminium addition to BN has led to Al4B2O9 crystals generation, asAl2O3 reacts together with B2O3 under high temperature. These materials therefore appear tobe able to seal SiC matrix cracks. As a result, the global oxidation resistance under wet air of SiC/SiC composites with B(Al)N interphases can been significantly improved. Additional oxidation tests, especially under thermal cycling, are needed to definitively conclude about this point.

<p>QC 20140609</p>