Ce travail de thèse porte sur le développement de films diamantés pour des applications de dissipation de chaleur dans les circuits électroniques de puissance. Dans le cadre d’un accord de cotutelle franco-américain, une approche duale a été adoptée. En France, la fabrication de films composites à matrice cuivre et renforts diamant par métallurgie des poudres a été privilégiée. Aux Etats-Unis, les efforts se sont concentrés sur la croissance de films de diamant par une méthode de combustion de flamme assistée laser. Dans chacune des approches, les corrélations entre microstructure et interfaces (microscopies à balayage et à transmission), composition chimique (spectroscopies Auger, Raman, XPS), et propriétés thermiques (radiométrie flash laser, radiométrie photothermique infrarouge, dilatométrie, cyclage thermique) ont été établies. Enfin, la simulation du comportement des matériaux en situation de fonctionnement opératoire à été abordée. / This PhD work deals with the development of diamond-based heat-spreading films for power electronic packaging applications. In the frame of a French-American dual PhD agreement, a double research approach was adopted. In France, the fabrication of copper-matrix diamond-reinforced composite films through tape casting and hot pressing has been endeavoured. In the US, the efforts were focused on the growth of diamond films through laser-assisted combustion synthesis. In both cases, relationships between the microstructure and the interfaces (scanning and transmission electron microscopy), the chemical composition (Auger, Raman, and XPS spectroscopy), and the thermal properties (flash laser radiometry, infrared photothermal radiometry, dilatometry, thermal cycling) of the final materials were established. Finally, the behaviour of the materials in operating environment was simulated.

Made available in DSpace on 2014-12-17T14:07:04Z (GMT). No. of bitstreams: 1 JulianaPN_DISSERT.pdf: 2953662 bytes, checksum: 47355bc7fed206f60c6c6b5d8565099b (MD5) Previous issue date: 2012-06-06 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / Nickel alloys are frequently used in applications that require resistance at high temperatures associated with resistance to corrosion. Alloys of Ni-Si-C can be obtained by means of powder metallurgy in which powder mixtures are made of metallic nickel powders with additions of various alloying carriers for such were used in this study SiC, Si3N4 or Si metal with graphite. Carbonyl Ni powder with mean particle size of 11 mM were mixed with 3 wt% of SiC powders with an average particle size of 15, 30 and 50 μm and further samples were obtained containing 4 to 5% by mass of SiC with average particle size of 15 μm. Samples were also obtained by varying the carrier alloy, these being Si3N4 powder with graphite, with average particle size of 1.5 and 5 μm, respectively. As a metallic Si graphite with average particle size of 12.5 and 5 μm, respectively. The reference material used was nickel carbonyl sintered without adding carriers. Microstructural characterization of the alloys was made by optical microscopy and scanning electron microscopy with semi-quantitative chemical analysis. We determined the densities of the samples and measurement of microhardness. We studied the dissociation of carriers alloy after sintering at 1200 ? C for 60 minutes. Was evaluated also in the same sintering conditions, the influence of the variation of average particle size of the SiC carrier to the proportion of 3% by mass. Finally, we studied the influence of variation of the temperatures of sintering at 950, 1080 and 1200 ? C without landing and also with heights of 30, 60, 120 and 240 minutes for sintering where the temperature was 950 ?C. Dilatometry curves showed that the SiC sintered Ni favors more effectively than other carriers alloy analyzed. SiC with average particle size of 15 μm active sintering the alloy more effectively than other SiC used. However, with the chemical and morphological analyzes for all leagues, it was observed that there was dissociation of SiC and Si3N4, as well as diffusion of Si in Ni matrix and carbon cluster and dispersed in the matrix, which also occurred for the alloys with Si carriers and metallic graphite. So the league that was presented better results containing Si Ni with graphite metallic alloy as carriers, since this had dispersed graphite best in the league, reaching the microstructural model proposed, which is necessary for material characteristic of solid lubricant, so how we got the best results when the density and hardness of the alloy / Ligas de N?quel s?o freq?entemente utilizadas em aplica??es que requerem resist?ncia mec?nica a elevadas temperaturas associada ? resist?ncia ? corros?o. Ligas de Ni-Si-C podem ser obtidas por meio de metalurgia do p? em que s?o realizadas misturas de p?s de n?quel met?lico com adi??es de p?s de diferentes portadores de liga, para tal foram utilizados neste trabalho SiC, Si3N4 ou Si met?lico com grafita. P?s de Ni carbonila com tamanho m?dio de part?culas de 11 μm foram misturados a 3% em massa de p?s de SiC com tamanho m?dio de part?culas de 15, 30 e 50 μm e foram obtidas ainda amostras contendo 4 e 5% em massa de SiC com tamanho m?dio de part?culas de 15 μm. Tamb?m foram obtidas amostras variando-se o portador de liga, sendo estes p?s de Si3N4 com grafita, com tamanho m?dio de part?culas de 1,5 e 5 μm, respectivamente. Assim como Si met?lico com grafita, com tamanho m?dio de part?culas de 12,5 e 5 μm, respectivamente. O material de refer?ncia adotado foi n?quel carbonila sinterizado sem adi??o de portadores. A caracteriza??o microestrutural das ligas foi feita por microscopia ?ptica e eletr?nica de varredura com an?lise qu?mica semi-quantitativa. Foram determinadas as densidades das amostras e obtidas medidas de microdureza Vickers. Foi estudada a dissocia??o dos portadores de liga ap?s sinteriza??o em 1200 ?C durante 60 minutos. Foi avaliada, ainda, para as mesmas condi??es de sinteriza??o, a influencia da varia??o do tamanho m?dio de part?culas do portador SiC, para a propor??o de 3% em massa. Por fim, foi estudo a influencia da varia??o das temperaturas de sinteriza??o em 950, 1080 e 1200 ?C sem patamar e, ainda, com patamares de 30, 60, 120 e 240 minutos para sinteriza??o cuja temperatura foi de 950 ?C. As curvas de dilatometria mostraram que o SiC favorece a sinteriza??o do Ni de forma mais eficaz que os demais portadores de liga analisados. O SiC com tamanho m?dio de part?culas de 15 μm ativa a sinteriza??o da liga de forma mais eficaz que os demais SiC utilizados. Por?m, com as an?lises qu?mica e morfol?gica para todas as ligas, foi poss?vel observar que houve dissocia??o do SiC e do Si3N4, assim como difus?o do Si na matriz de Ni e carbono aglomerado e disperso na matriz, o que tamb?m ocorreu para as ligas com portadores Si met?lico e grafita. Portanto, a liga que apresentou melhores resultados foi de Ni contendo Si met?lico com grafita como portadores de liga, j? que esta apresentou grafita melhor dispersa na liga, atingindo o modelo microestrutural proposto, do qual ? necess?rio para material com caracter?stica de lubrificante s?lido, assim como obteve os melhores resultados quando a densidade e dureza da liga

Made available in DSpace on 2014-10-09T12:49:13Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T13:57:43Z (GMT). No. of bitstreams: 1 09808.pdf: 15249724 bytes, checksum: 28b6b5cf9f351da89e42817bc182390d (MD5) / Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP / FAPESP:00/00255-9

O objetivo principal deste trabalho foi o desenvolvimento de um núcleo do rotor de um motor universal a partir dos processos da metalurgia do pó (M/P). O rotor desta máquina, cujo núcleo é originalmente fabricado em chapas laminadas, foi substituído por um rotor com núcleo em bloco maciço, mantendo-se as demais partes como eixo e escovas. A partir de simulações no software FEMM e dados existentes referentes ao desempenho de ligas metálicas sinterizadas como Fe-P, Fe-Si e Fe-Ni, foi selecionado o Fe1%P, que apresentou os melhores resultados para a aplicação na máquina elétrica em questão. Foram feitas simulações relacionadas às características eletromagnéticas e a partir dos resultados obtidos puderam-se fazer comparações entre um rotor convencional, fabricado com núcleo de chapas laminadas e o rotor com o núcleo maciço fabricado utilizando-se a metalurgia do pó. As etapas de fabricação consistem em mistura da liga, compactação, sinterização e forma final através de eletroerosão. A máquina foi montada utilizando a estrutura de um motor de furadeira manual comercial, mantendo-se todas as partes da máquina original com exceção do núcleo do rotor, e posteriormente foi testada em bancada, comparativamente a uma máquina convencional para análise dos resultados. Foi possível a substituição do rotor oriundo de placas laminadas por um rotor oriundo de metalurgia do pó. Os resultados dos ensaios com a máquina fabricada comprovaram que a liga Fe1%P é, comparativamente ao núcleo de chapas convencional, tecnicamente inferior para a fabricação de motores universais. Utilizando a liga Fe1%P seu rendimento foi de 7% contra 27% do motor convencional assim como torque e demais parâmetros ficaram abaixo do motor padrão. / The main objective of this work was the development of a rotor core of a universal motor from the processes of powder metallurgy (M/P). The rotor of this machine, whose core is originally manufactured in laminated plates, was replaced by a rotor core with solid block, keeping the other parts like shaft and brushes. From the software FEMM simulations and existing data regarding the performance of sintered alloys such as Fe-P, Fe-Si and Fe-Ni, was selected Fe1%P, which showed the best results for application in electric machine in question. Simulations were made related to the electromagnetic characteristics and from the results of comparisons could be made between a conventional rotor, made of rolled core and the solid core rotor is manufactured using powder metallurgy. The manufacturing steps comprise of mixing the alloy, compacting, sintering and final form by electro erosion. The machine structure was assembled using a hand drill motor trade, keeping all parts of the original machine except the rotor core, and thereafter the machine was tested on bench, compared to a conventional machine to analyze the results. It was possible to replace the rotor coming from a rotor laminated plates derived from powder metallurgy. The results of the tests made with the machine shown that the alloy Fe1% P is compared to a conventional core plates, technically inferior to manufacture universal motors. Using the league Fe1%P its yield was 7% versus 27% of the conventional engine as well as torque and other parameters were below the standard engine.

Este estudo identifica as vantagens do uso de um estator fabricado usando a tecnologia da metalurgia do pó, identificando suas vantagens e desvantagens. O motor elétrico utilizado é um motor do tipo universal originalmente o estator desta máquina, possui o núcleo fabricado em chapas laminadas, este foi substituído por um estator com núcleo em bloco maciço, mantendo-se as demais partes do motor originais, ou seja, nestes testes o rotor bobinado continuará a utilizar chapas laminadas e escovas originais. Motores elétricos foram desenvolvidos no início do século XIX e desde então vem sendo utilizado em larga escala com mudanças pouco significativas na sua forma construtiva, materiais e processo de fabricação. Neste trabalho o principal objetivo foi o desenvolvimento de um núcleo do estator para motor universal a partir dos processos da metalurgia do pó (M/P). Simulações com o software FEMM identificaram o comportamento de várias ligas (Fe-P, Fe-Si e Fe-Ni). Após análise dos dados da simulação foi selecionado o Fe1%P, por ter apresentado os melhores resultados para a aplicação na máquina elétrica em questão. As simulações permitiram comparações dos parâmetros eletromagnéticos e torque, entre estatores utilizando chapas de silício do motor original e estatores de núcleo maciço com dados das ligas experimentadas fabricadas através da metalurgia do pó. A fabricação destes núcleos consiste nas misturas da liga, compactação utilizando matriz para formato desejado, sinterização e acabamentos através de usinagem e eletroerosão. Foi utilizada uma furadeira manual comercial, testada em bancada para levantamento detalhado a fim de caracterizar as propriedades que definem a eficiência do equipamento com o estator original. Os mesmos testes foram conduzidos apenas substituindo o estator, agora de núcleo maciço. Processo de fabricação através da metalurgia do pó permite um menor consumo de material e energia, sendo este um processo muito mais eficiente quando comparado ao processo de fabricação das chapas laminadas de ferro silício. / This study will identify the advantages of using a fabricated stator using the technology of powder metallurgy, identifying its advantages and disadvantages. The electric motor used is a universal type motor, originally the stator core of this machine are made of laminated plates, this was replaced by a stator core with solid block , keeping the remaining parts of the original machine, ie these tests the wound rotor continued to use rolled sheet and original brushes. Electric motors were developed in the early of 19th century, and has since been used in large scale with little significant changes in its constructive form, materials and manufacturing process. This work has as main goal the development of a stator core for universal motor from the processes of powder metallurgy (M/P). Simulations with the FEMM software identified the behavior of various alloys (Fe-P, Fe -Si and Fe-Ni) .After data analysis of the simulation was selected Fe1%P, for having presented the best results for the application in the electric machine in question. The computer simulations of electromagnetic parameters and comparisons torque between stator plates using the original silicon motor stators and solid core of data experienced alloys manufactured by powder metallurgy. The manufacture of these core constitutes mix league, using compression matrix to desired shape, sintering and finishing by machining and EDM. Trade manual drill was used, tested on bench for detailed study to characterize the properties that define the efficiency of the equipment to the original stator. The same tests were conducted just by replacing the stator, now solid core. Manufacturing process by powder metallurgy allow less consumption of material and energy, this is a much more efficient process compared to the process of manufacturing the laminated silicon iron sheets.

O trabalho apresenta o desenvolvimento de uma metodologia denominada modelo de núcleo reduzido, aplicada para avaliar o desempenho de máquinas elétricas no que tange a geometria e materiais empregados na fabricação do núcleo completo. Para fins de validação da metodologia utiliza-se um Atuador Planar de Indução Trifásico com dois graus de liberdade, comparando os resultados numéricos e experimentais. Através desta metodologia, pode-se realizar a análise dos fenômenos eletromagnéticos ocorridos no núcleo completo por meio da avaliação de seu modelo reduzido, composto neste caso por 33% do núcleo completo empregado no Atuador Planar de Indução Trifásico. A comprovação da metodologia do modelo de núcleo reduzido ocorreu através da fabricação de uma bancada de testes, composta por uma célula de carga para realizar aquisição da força de propulsão planar, interface de potência e os núcleos reduzidos com seguintes materiais ferromagnéticos: compósitos SMC 1P Somaloy 500®, Ferro resinado e Aço ABNT 1020. Com auxilio da estrutura de testes, validou-se o modelo numérico dos três núcleos reduzidos quanto a força de propulsão planar. Na análise dos dados experimentais e numéricos, o material Ferro resinado apresentou a diferença 14% referente a força de propulsão planar, sendo a maior diferença entre os materiais estudados. Com a convergência dos resultados experimental e numéricos, realiza-se a comparação numérica entre os núcleos reduzidos e completos utilizando-se os três materiais ferromagnéticos. A análise numérica do núcleo reduzido com o material SMC 1P Somaloy 500® apresentou o fator de relação médio da força de propulsão planar de 2,65 em relação ao núcleo completo. O núcleo completo com Aço ABNT 1020 resultou no consumo médio de 56,7Watts para gerar a força de propulsão planar de 1 Newton. Dessa forma, proporciona-se uma ferramenta de maior rapidez para fabricação e avaliação do desempenho de materiais ferromagnéticos utilizados no núcleo completo da máquina elétrica. / This paper presents the development of a methodology denominated low core model applied to evaluate the performance of electrical machines with respect to geometry and materials used in manufacturing of the complete core. For validation purposes of the methodology is used a Planar Three-phase Induction Actuator with two degrees of freedom, comparing the experimental and numerical results. Through this methodology, it is possible to perform the analysis of electromagnetic phenomena occurring in the complete core based evaluation of the reduced model, made in this case with 33% of the full core employed in the Planar Three-phase Induction Actuator. The verification of the reduced core model methodology occurred through the manufacture of a testing bench, which is composed of a load cell to realize the acquisition of the planar propulsion force, potency interface and reduced cores with the following ferromagnetic materials: SMC 1P Somaloy 500® composites, resinated Iron and Steel ABNT 1020. With the help of the test structure, it was validated the numerical model of the three reduced cores regarding to the planar propulsion force. In the analysis of experimental and numerical data, the resinated Iron material showed a 14% difference concerning the strength of the planar propulsion, which is the biggest difference between the materials studied. With the convergence of the experimental and numerical results, a numerical comparison is performed between the reduced and complete cores using the three ferromagnetic materials. The numerical analysis of the reduced core with the SMC 1P Somaloy 500® material showed the average ratio of the planar factor propulsive force of 2.65 when compared with the complete core. The complete core with ABNT 1020 Steel resulted in an average consumption of 56.7 Watts to generate a planar propulsive force of 1 Newton. Thus, it is provided a faster tool for manufacturing and evaluation of ferromagnetic materials performance used in the complete core of the electric machine.

La récupération d’énergie par effet thermoélectrique est une technologie fiable avec un grand potentiel. Dans la gamme des hautes températures, il est nécessaire que les générateurs thermoélectriques soient fabriqués à partir d’un matériau massif pour gagner en puissance électrique. Dans la littérature, la nanostructuration baisse la conductivité thermique et permet d’augmenter le rendement de conversion. Par contre, l’effet de la porosité n’est pas clarifié. Par contre, l’effet de la porosité est sujette à controverse.Dans ce travail, l’alliage Si80Ge20 type n est élaboré par mécanosynthèse. Ce matériau est typique pour les applications aux hautes températures (vers 800◦C). La poudre nanocristalline est compactée en matrice, `a froid puis `a chaud. En plus de la caractérisation microstructurale, l’évolution de la microstructure est caractérisée par microscopie fine et par diffraction des rayons X. Les propriétés thermoélectriques et mécaniques sont identifiées expérimentalement. Cette étude montre que la nanostructuration du matériau est préservée et que le meilleur facteur de mérite obtenu est légèrement supérieur à l’unité pour un état dense. Cependant, les échantillons poreux ont une faible conductivité électrique dû à la taille macroscopique des pores, ce qui limite leurs rendu thermoélectrique final.Par la suite, le comportement mécanique de la poudre est modélisé au moyen de simulations fondées sur la méthode des éléments discrets (DEM, Discrete Element Method). Cette démarche permet de suivre l’évolution de l’empilement de particules pendant la densification et d’accéder aux paramètres microstructuraux clés. Les microstructures numériques obtenues par la DEM sont ensuite utilisées pour des calculs de conductivités thermiques et électriques. Les échantillons sont modélisés par trois phases dépendantes de leurs propriétés : la matrice SiGe, les pores et les joints de grains. Contrairement aux mesures expérimentales, le rendement thermoélectrique est maximal pour 30% de nanoporosité résiduelle. Ce résultat peut être expliqué par un modèle analytique qui prend en compte la résistance thermique des joints de grains ainsi que l’évolution de la microstrcuture pendant le procédé de densification. Une alternative au procédé de mise en forme actuel est proposée pour synthétiser la microstructure optimale. / Energy recovery by thermoelectric effect is a promising technology which offers greatreliability. In the range of high temperatures, it is necessary that the thermoelectric generatorshave to be made of bulk material to increase electrical power. In the literature,nanostructuring decreases the thermal conductivity and therefore enhances the conversionefficiency. On the contrary, the effect of porosity is a matter of debate.In this work, n-type Si80Ge20 alloy prepared by mechanical alloying is investigated. It isa typical material for high temperature applications (around 800◦C). The nanocrystallinepowder is compacted uniaxially at room temperature and then hot pressed. In addition tothe microstructural characterization, thermoelectrical and mechanical properties are identifiedexperimentally. This study shows that the grain size is kept below 200nm. The bestmeasured figure of merit is slightly slightly larger than one for dense specimens. However,the porous samples have low electrical conductivity which limits their final thermoelectricrendering.The mechanical behaviour of the powder is modelled through simulations using thediscrete element method (DEM). This approach has the advantage of following the evolutionof particle rearrangement during densification and provides useful information onmicrostructural parameters. Numerical microstructures obtained from DEM simulationsare then used for calculations of thermal and electrical conductivities. The samples aremodelled by three phases according to their properties : SiGe matrix, pores and grainboundaries. The conductivities ratio is maximal for 30% of residual porosity. This resultis explained by the analytical model that takes into account the thermal resistance ofthe grain boundaries as well as microstructure evolution during the densification process.Based on these findings, an alternative processing route is proposed to build an optimizedmicrostructure.

Made available in DSpace on 2016-06-02T19:12:21Z (GMT). No. of bitstreams: 1 4512.pdf: 12085865 bytes, checksum: 9c98b7edb2a0238a143b2c8e9469a515 (MD5) Previous issue date: 2012-03-06 / Ion nitriding is a process of thermo-physical-chemical treatment that provides a surface hardening, originated by interstitial diffusion of nitrogen on the ferrous and nonferrous alloys surfaces. Understanding and controlling the formation of the nitrided layer have considerable industrial interest due to the improvements regarding wear, corrosion and fatigue resistances on the metals and their alloys. In this work, it was performed the surface modification in sintered iron samples by ion nitriding process, with a gaseous mixture of 80% vol H2 and 20% vol N2, during times of 3 and 5 hours, using ion nitriding temperature of 500°C, 540°C and 580°C. The samples were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) analyses, and wear and micro-hardness tests, comparing the results with sintered and steam treatment samples. The results showed that both nitride thickness and wear resistance increased with higher nitriding time and temperature, where the temperature was the variable that most influenced the aforementioned characteristics. The XRD analysis indicated that the nitrided layer near to the surface, for all samples, consisted in a mixture of y-Fe4N and e-Fe3N phases. / A nitretação iônica é um processo de tratamento termo-físico-químico que consiste em um endurecimento superficial, provocado pela difusão intersticial de nitrogênio atômico na superfície de ligas ferrosas e não ferrosas. O entendimento e o controle da formação da camada nitretada apresentam considerável interesse industrial devido às melhorias alcançadas nas resistências ao desgaste, corrosão e à fadiga dos metais e suas ligas. Neste trabalho, promoveu-se a modificação superficial de amostras de ferro sinterizado por meio do processo de nitretação a plasma, com uma mistura gasosa de 80% vol H2 e 20% vol N2, nos tempos de 3 e 5 horas, e temperaturas de nitretação de 500°C, 540°C e 580°C. As amostras foram caracterizadas por meios de análise de microscopia eletrônica de varredura (MEV) e difração de raios X (DRX), e quantificadas quanto aos níveis de desgaste e microdureza, em comparação com amostras sinterizada e ferroxidada. Os resultados mostraram que tanto as espessuras das camadas de nitretos como as resistências ao desgaste das amostras aumentaram com o tempo e temperatura de nitretação, sendo a temperatura a variável que mais influenciou nas características mencionadas. A análise de DRX indicou que a camada nitretada próxima a superfície, para todas as amostras, consiste de uma mistura de fases de  -Fe4N e -Fe3N.

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