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

Afin de comprendre les mécanismes de transport de la chaleur dans des films très minces des matériaux amorphes, nous avons proposé et démontré expérimentalement une nouvelle technique de mesure des propriétés thermiques de membranes très minces. Cette technique consiste à coupler la méthode 3 oméga avec la géométrie Völklein (membrane suspendue allongée). L'échantillon d'intérêt est alors monté dans un pont de Wheatstone spécifique afin d'éliminer le signal électrique 1 oméga. Cette technique permet de mesurer avec une très haute sensibilité le signal thermique 3 oméga et donc les propriétés thermiques des membranes. Le nitrure de silicium étudié dans ce travail constitue un matériau amorphe typique. Nous avons été intéressés par l'étude du transport thermique dans un tel système de dimensions réduites en fonction de la température et du stress intrinsèque qui présente dans les films. Afin d'atteindre cet objectif, les membranes de nitrure de silicium de stress élevé et de faible niveau de stress ont été mesurées respectivement pour une épaisseur de 50 nm et 100 nm. Le comportement global de la conductivité thermique mesurée est une croissance quand la température augmente, une tendance généralement constaté pour un matériau amorphe. Le data de membrane de 50 nm présente une conductivité thermique inférieure à celle du 100 nm, ce qui est en accord avec l'effet des dimensions réduites. La chaleur spécifique mesurée s'écarte sensiblement de la loi en T3 de Debye. Cela est particulièrement important en dessous de 100 K où la chaleur spécifique est plus élevé que celle prévue par la modèle Debye. Ces résultats expérimentaux sont en excellent accord avec les prévisions d'un model théorique qui tient en compte de l'effet TLS (Two Level System) qui présente dans le matériaux amorphe. Il a été montré expérimentalement que le stress n'a pas d'effet sur la chaleur spécifique de nitrure de silicium. De plus, nous avons démontré que le stress n'affecte pas la dissipation dans nitrure de silicium, et la dissipation par dilution semble être la cause de la réduction de la dissipation. Par conséquent, le stress ne devrait pas affecter la conductivité thermique du nitrure de silicium, ce qui est cohérent avec les résultats expérimentaux. En terme d'application de la méthode 3 oméga-Völklein, nous avons démontré que la membrane de SiN peut être utilisée comme capteur thermique spécifique pour caractériser un autre matériau déposée sur la face arrière de la membrane. Nous avons testé ce modèle pour mesurer les propriétés thermiques d'un film de 200 nm de Bi2Te3. Les résultats obtenus sont en excellent accord avec la littérature. Comme le SiN est un matériau isolant, ce modèle est capable de mesurer des films très minces quelle que soit sa nature, isolant, semi conducteur ou métallique. / In order to understand the mechanisms of the heat transport in very thin amorphous films, we have proposed and experimentally demonstrated a new technique to measure the thermal properties of very thin membranes. This technique consists in coupling the 3 omega method to the Völklein geometry (elongated suspended membrane). The sample of interest is then implemented into a specific Wheatstone bridge in order to eliminate the electrical 1 omega signal. This technique allows the measurement with very high sensitivity of the 3 omega thermal signal and therefore the thermal properties of the membranes. Silicon nitride membranes studied in this work constitutes a typical amorphous material. We have been interested in the study on the thermal transport in such system of reduced dimensions as function of temperature and intrinsic modified stress. In order to accomplish this goal, silicon nitride membranes of high stress and low stress have been measured respectively with the thickness 50 nm and 100 nm. The overall behaviour of the measured thermal conductivity is an increase as the temperature is increased, a trend commonly found for amorphous material. The 50 nm data show thermal conductivity less than that of the 100 nm, this is consistent of the effect of reduced dimensions. The measured heat capacity is apparently higher than what is expected from the Debye phonon heat capacity. This is especially significant below 100 K where the heat capacity deviates significantly from the T3 Debye law. A theoretical model taking into account the presence of TLS in amorphous materials is then used to fit the experimental data. The theoretical fits are in excellent agreement with the experimental results. It was seen experimentally that stress has no effect on the specific heat of silicon nitride. Moreover, we have demonstrated that stress does not affect the dissipation in silicon nitride, and the dissipation dilution seems to be the sole cause of the reduction of dissipation by an applied stress in high stress silicon nitride. Therefore, stress should not affect thermal conductivity of silicon nitride, and this is consistent with the experimental results. As application for the 3 omega-Völklein method, we have demonstrated that the SiN membrane can be used as specific thermal sensor to characterize another material deposited on the backside of the membrane. We have tested this model to measure thermal properties of Bi2Te3 film and the results are in excellent agreement with literature. As the SiN is an insulator, this model is able to measure very thin films whatever its nature, insulator, semi conductor or metallic.

Foram realizados ensaios tribológicos de deslizamento do par Si3N4-Al2O3, lubrificado com água, na configuração esfera contra disco, sendo a esfera de nitreto de silício e o disco de alumina para investigar a influência da velocidade de deslizamento, da carga aplicada e da temperatura no coeficiente de atrito. As esferas de nitreto de silício e os discos de alumina foram caracterizados determinando-se: densidades, dureza Vickers, módulo de elasticidade e tenacidade à fratura. Os ensaios foram realizados com rugosidade inicial nos discos de Rrms = 352 nm. O regime de ultra baixo coeficiente de atrito (UBCA, &#956; < 0,01) foi atingido após um período de running-in de aproximadamente uma hora e o coeficiente de atrito ficou na faixa de &#956; = 0,008 a &#956; = 0,002. Os resultados mostraram que este sistema deslizante tem características hidrodinâmicas, pois o coeficiente de atrito diminuiu com o aumento da velocidade de deslizamento. Uma variação suave da carga aplicada fez com que o coeficiente de atrito permanecesse no regime de UBCA, com a carga aplicada variando de 54 N até 94 N. Em temperaturas menores ou iguais a 11°C o sistema não atingiu o regime de UBCA e o coeficiente de atrito final ficou da ordem de centésimos. Foi observado o fenômeno de UBCA em temperaturas de 30 e 40°C. No entanto, nestas temperaturas, a baixa viscosidade da água não deveria permitir que o sistema atingisse o regime de UBCA. A análise dos dados possibilitou inferir que durante o regime de UBCA o sistema desliza num regime de lubrificação mista, sendo lubrificação hidrodinâmica, devido ao filme de água, somada a lubrificação limite, devido às camadas hidratadas formadas nas superfícies das cerâmicas. Os resultados mostraram que a temperatura influencia no desgaste das cerâmicas. A determinação do volume desgastado possibilitou observar que durante os ensaios a alumina sofre menos desgaste que o nitreto de silício e que o desgaste de ambas cerâmicas aumenta com o aumento da temperatura. / Tribological tests were conducted in a ball on disk setup, using water as lubricant. Were used a silicon nitride ball and alumina disk. The tests were conducted to investigate the effects of sliding speed, applied load and temperature on friction coefficient. The silicon nitride balls and alumina disks were characterized by determining density, Vickers hardness, elastic modulus and fracture toughness. The tests were conducted with initial roughness on the disk surface of 352 nm. The ultra low friction coefficient regime (ULFC, &#956; < 0.01) was reached after a running-in period of approximately one hour and the friction coefficient remains in the range of &#956; = 0.008 a &#956; = 0.002 during this steady state regime. The results showed that this sliding system has hydrodynamic characteristics, because the friction coefficient decreased with increasing of the sliding speed. With an smooth variation of the applied load the system remained in the ULFC regime, when the applied load varied from 54 N up to 94 N. At temperatures below or equal to 11°C the system did not reach the ULFC regime and the final friction coefficient was the order of hundredths. We observed the ULFC phenomenon at temperatures of 30 and 40°C. However, at these temperatures, the water viscosity is low and should not allow the system to reach the ULFC regime. The data analysis allowed infer that during the ULFC regime the system slides with a mixed lubrication regime, hydrodynamic plus limitrofe, the first due to water film and the second due to the hydrated layer formed on the ceramics surfaces. The results showed a influences of temperature in the ceramics wear. The results of the worn volume allowed to observe that during the tests alumina suffers less wear than the silicon nitride, and the ceramics wear increases with increasing temperature.

Orientador: Jose Alexandre Diniz / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Eletrica e de Computação / Made available in DSpace on 2018-08-05T17:29:59Z (GMT). No. of bitstreams: 1 Biasotto_Cleber_M.pdf: 4466326 bytes, checksum: 75500d469b99d21f5c40a3214a755168 (MD5) Previous issue date: 2005 / Resumo: Neste trabalho, filmes finos de nitreto (SixNy), oxido (SiOx) e oxinitreto (SiOxNy) de silicio sobre substrato de silicio, obtidos através da deposição química a partir da fase vapor auxiliada por plasma remoto (RPCVD), foram caracterizados e estudados para aplicações em micromáquinas (micromachining) ou sistemas micro-eletro-mecanico (MEMS). Os filmes de nitreto de silicio (SixNy) foram obtidos para aplicação em estruturas suspensas (pontes e membranas) e como mascara de proteção de dispositivos MOS para remoção do substrato, utilizando os processos de corrosão úmida do substrato de silicio pelas faces superior (front-side bulk micromachining) e inferior (back-side bulk micromachining), respectivamente. Os filmes de oxido de silicio (SiOx) foram aplicados como camada sacrificial em processos de obtenção de estruturas suspensas empregando a técnica de remoção de camadas sacrificiais na superfície (surface micromachining). Os filmes de oxinitreto de silicio (SiOxNy) foram obtidos como filmes alternativos para aplicação em estruturas suspensas (pontes e membranas), utilizando os processos de corrosão úmida do substrato de silicio pela face superior (front-side bulk micromachining). A fabricação destas estruturas e primordial para o desenvolvimento de micro-sensores e micro-atuadores. Neste trabalho foram revisadas as técnicas de processamento CVD (Chemical Vapor Deposition), apresentando a justificativa da escolha do reator ECR (Electron Cyclotron Resonance), que utiliza a tecnologia CVD com Plasma Remoto (RPCVD) para as deposições / Abstract: In this work, silicon nitride (SixNy), oxide (SiOx) and oxynitride (SiOxNy) thin films obtained by remote plasma chemical vapor deposition (RPCVD) on silicon substrate were studied and characterized for micromachining or micro electro-mechanical system (MEMS) applications. Silicon nitride films (SixNy) were used in suspended structures (membranes and bridges) and as MOS device protection mask against wet substrate etching, obtained by wet substrate etching processes using the front-side and back-side bulk micromachining techniques, respectively. Silicon oxide films (SiOx) were employed as sacrificial layers to obtain suspended surface structures using the surface micromachining technique. Silicon oxynitride (SiOxNy) films were used as alternative films in suspended structures (membranes and bridges), using the front-side bulk micromachining technique. The fabrication of these structures is primordial for the micro sensor and actuator development. In these work, CVD (Chemical Vapor Deposition) techniques are revised, presenting the choice justification of ECR (Electron Cyclotron Resonance) reactor, which uses RPCVD technology for the depositions / Mestrado / Mestre em Engenharia Elétrica

Orientador: Ioshiaki Doi / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Eletrica e de Computação / Made available in DSpace on 2018-08-08T12:57:52Z (GMT). No. of bitstreams: 1 Pereira_MarcusAnibal_M.pdf: 4318576 bytes, checksum: 61cdc38456d21cf10bf9ccfef5d0bff4 (MD5) Previous issue date: 2005 / Resumo: Isolantes de nitreto de silício (SiNx) para aplicação na tecnologia de isolação LOCOS foram depositados por ECR-CVD a temperatura ambiente e RP/RTCVD, a baixa pressão (5mTorr), com fluxos de gás de N2 de 2.5, 5, 10 e 20sccm, com fluxos de gases de SiH4/Ar fixos de 200sccm/20sccm, e potência de microondas de 1000W em substratos de SiO2-Pad/Si e Si. As estruturas de SiNx/SiO2-Pad/Si e SiNx/Si obtidas foram utilizadas para analisar as características físicas do nitreto de silício. Análises de espectroscopia de infravermelho (FTIR) revelaram a presença de trocas de posição do pico principal das ligações Si-N, das ligações N-H e das ligações Si-N (modo de vibração stretching) nos filmes de nitreto de silício, que está relacionado aos fluxos de N2 na mistura de gases. Os índices de refração entre 1.88 e 2.48 e as espessuras entre 120nm e 139nm foram determinados através de elipsometria. Com estes valores de espessura e com os tempos de ataque em Buffer de HF, foram determinadas as taxas de deposição de 9,6 a 11,1nm/min e taxas de corrosão de 2 a 86nm/min. O processo LOCOS, com etapas seqüenciais de fotolitografia e oxidação térmica, foi executado nas estruturas de SiNx/SiO2-Pad/Si e também de SiNx/Si (sem a presença de óxido "almofada"), com a espessura de cada tipo de nitreto entre 110nm a 215nm e espessura do óxido ?almofada? de 0 a 124nm. Análises de microscópio óptico e de microscopia eletrônica de varredura (SEM) foram utilizadas respectivamente para investigar a resistência dos nitretos de silício à oxidação térmica, executada sob altas temperaturas (1000ºC) e o efeito ?bico de pássaro? formado nas estruturas LOCOS. O nitreto depositado com fluxo de N2 de 10sccm (N10) foi o que apresentou a menor invasão lateral por parte do óxido de campo dentre os nitretos estudados, tanto com quanto sem a camada de óxido de ?almofada? sob o nitreto. O efeito "bico de pássaro" formado nas estruturas LOCOS teve comprimento de avanço lateral variando de 330nm a 2160nm tomando como base a oxidação local executada em temperatura de 1000ºC durante 180 minutos / Abstract: Silicon nitride (SiNx) insulators for LOCOS applications have been deposited by RP/RTCVD and ECR-CVD at room temperature, at low pressure (5mTorr), with N2 flows of 2.5, 5, 10 and 20sccm with fixed SiH4/Ar flows of 200/20sccm with a microwave power of 1000W on SiO2-Pad/Si and Si substrates. SiNx/Si structures were obtained to analyze the physical characteristics of silicon nitride. Fourier transform infrared (FTIR) spectrometry analyses revealed the main peak position shifts of Si-N, N-H and Si-N (stretching mode) bonds for each silicon nitride films, which is related to N2 flows in gas mixture. The refractive indexes between 1.88 and 2.48 and the thickness between 120nm and 139nm were determined by ellipsometry. With these thickness values and with buffered HF etching times, it was also determined the deposition rates of 9,6 - 11,1nm/min and etch rates of 2 -86nm/min. On the SiNx(110 -215nm)/SiO2-Pad(0 - 124nm)/Si and SiNx/Si (without pad oxide) structures, the LOCOS process, with sequential photolithography and thermal wet oxidation steps, was performed. Optical and scanning electron microscopy (SEM) analysis were used to investigate the silicon nitride to thermal oxidation accomplishement at high temperature of 1000 ºC, and bird's beak in the obtained LOCOS structures. On both structures (with and without pad oxide), the smallest lateral extension of the field oxide (bird's beak) was observed for the nitride films obtained with N2 flows of 10sccm (N10). The lengths of the bird's beak, in the obtained LOCOS structure, have resulted between 330nm and 2160nm / Mestrado / Eletrônica, Microeletrônica e Optoeletrônica / Mestre em Engenharia Elétrica

O objetivo deste trabalho, foi investigar o comportamento tribológico do par cerâmico alumina - nitreto de silício no deslizamento em água com pH controlado e em uma suspensão com diferentes concentrações de sílica coloidal em água, e verificar a possibilidade de atingir um coeficiente de atrito da ordem de milésimos (&#956; < 0,01), aqui chamado de ultra baixo coeficiente de atrito (UBCA) e verificar se a mudança do pH do meio, ou a alteração da concentração de sílica na água, diminui o runningin, tempo necessário para o sistema entrar em regime estacionário, do coeficiente de atrito. Os ensaios foram realizados na configuração de ensaio tribológico esfera contra disco, no qual a esfera foi de nitreto de silício e o disco de alumina, sob carga normal de 54 N e velocidade de deslizamento de 1 m/s. A água utilizada nos ensaios foi destilada e deionizada, e a sílica coloidal amorfa, sem porosidade e de tamanho médio de partícula de 12 nanômetros foi a Aerosil® 200. A esfera de nitreto de silício, adquirida comercialmente, e o disco de alumina, foi proveniente de trabalhos anteriores. Todos os materiais foram caracterizados quanto a densidade. Algumas propriedades mecânicas como dureza, módulo de elasticidade e tenacidade à fratura foram determinadas. Nos ensaios lubrificados com água onde o pH foi controlado, o sistema atingiu o regime com valores de coeficiente de atrito da ordem de milésimos, exceto quando o pH da água era muito baixo ou muito alto. Em hidrossol o coeficiente de atrito chegou a unidades de milésimos, mas quando se aumenta a concentração de sílica coloidal, também, aumenta o desgaste nas superfícies. O disco de alumina sempre apresentou menor desgaste do que a esfera de nitreto de silício, em todas as condições estudadas. / The objective of this work was to investigate the tribological behavior of the ceramic pair alumina-silicon nitride, sliding on the water with controlled pH and in a suspension with different concentrations of colloidal silica in water, and verify the possibility of achieving a friction coefficient in the order of thousandths (&#956; < 0.01), here called ultra low friction coefficient (ULFC) and verify if the change of pH or changing the concentration of silica in the water, decreases the running-in, time required for the system reach the steady state of friction coefficient. The tests were conducted in a pin on disc setup in which the ball was made on silicon nitride and the disc of alumina, under normal load of 54 N and a sliding velocity of 1 m/s. The water used in the experiments was distilled and deionized. The amorphous silica, without porosity and average particle size of 12 nanometers was Aerosil ® 200. The ball of silicon nitride, was purchased commercially, and the alumina disk was recycled from previous works, all materials were characterized by density. Some mechanical properties such as hardness, elastic modulus and fracture toughness were determined. In tests with controlled pH water the system has reached the friction coefficient of the order of thousandths, except when the pH of the water was too low or too high. In hydrossol the friction coefficient reached units of thousandths, but when increasing the concentration of colloidal silica also increases the wear in the surfaces. The alumina disc always showed less wear than the ball of silicon nitride, in all conditions studied.

Neste trabalho são apresentados resultados da caracterização estrutural e morfológica de filmes de oxinitreto de silício (SiOxNy) depositados pela técnica de deposição química a vapor assistida por plasma (PECVD) a baixa temperatura (320°C). O objetivo deste trabalho é relacionar a composição química de ligas amorfas de SiOxNy com suas propriedades ópticas, estruturais, morfológicas e mecânicas visando sua aplicação em dispositivos elétricos, optoeletrônica e microestruturas. A proposta é dar continuidade a trabalhos prévios desenvolvidos no grupo, que demonstraram a viabilidade de controlar a composição química e, como conseqüência, controlar as propriedades como o índice de refração, constante dielétrica e fotoluminescência de filmes de SiOxNy. As condições de deposição foram ajustadas de forma a obter dois tipos de material: filmes de SiOxNy de composição química controlável entre a do SiO2 e a do de Si3N4 e filmes de SiOxNy com composição rica em Si. O material foi caracterizado pelas técnicas de elipsometria, índice de refração por prisma acoplado, RBS (Rutherford Backscattering Spectroscopy), FTIR (Fourier Transform Infrared Spectroscopy), XANES (X-Ray Absorption Near Edge Spectroscopy) na borda K do Si, O e N, medida de stress residual e microscopia eletrônica de varredura (Scanning Electron Microscopy) e de transmissão (Transmission Electron Microscopy). Os resultados mostraram que os filmes com composição química intermediária entre a do SiO2 e a do Si3N4 apresentam arranjo estrutural estável com a temperatura, mantendo as ligações e a estrutura amorfa mesmo após tratamentos térmicos a 1000°C. Também fora demonstrada a possibilidade de obter um material com baixo stress residual e índice de refração ajustável entre 1,46 e 2, resultados ótimos para aplicações em MOEMS (micro-opto-electro- mechanical systems). Já nas amostras ricas em Si foi observada a formação de diferentes fases, sendo uma delas formada por aglomerados de Si e a outra por material constituído por uma mistura de ligações Si-O e Si-N. Este material apresenta a formação de nanocristais de Si, dependendo do conteúdo de Si e das condições do tratamento térmico, permitindo assim, sua aplicação em dispositivos emissores de luz. / In this work results on the morphological and structural characterization of silicon oxynitride (SiOxNy) films deposited by plasma enhanced chemical vapor deposition technique (PECVD) at low temperature (320°C) are presented. The main goal is to correlate the chemical composition of amorphous SiOxNy alloys to their optical, structural, morphological and mechanical properties intending applications on electrical, optoelectronic and micromechanical devices. The proposal is to continue previous research developed in this group, which demonstrated the possibility of tuning the chemical composition and, consequently, the SiOxNy films properties such as refractive index, dielectric constant and photoluminescence by the precise control of the deposition parameters. The deposition conditions were adjusted in order to obtain to material types, SiOxNy films with tunable chemical composition between SiO2 and Si3N4 and silicon-rich SiOxNy. The characterization was performed by elipsometry, refractive index by coupled prism, RBS (Rutherford Backscattering Spectroscopy), FTIR (Fourier Transform Infrared Spectroscopy), XANES (X-Ray Absorption Near Edge Spectroscopy) on K edge of Si, O and N, residual stress measurement and Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The films with chemical composition between SiO2 and Si3N4 presented stable structural arrangement with temperature, maintaining the chemical bonds and the amorphous structure after high temperature annealing. Also the results demonstrated the possibility of producing a low residual stress material and an adjustable refractive index since in the 1.46 to 2 range, excellent result for MOEMS devices (micro-opto-electro- mechanical systems applications. For silicon rich-samples the formation of different phases was observed, one formed by Si clusters and other one by a mixture of Si-O and Si-N bonds. Depending on the Si content and on the annealing conditions this material can present nanocristals, results which allowed us to understand and to optimize this material for light emitting devices applications.

Orientador: José Alexandre Diniz / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Elétrica e de Computação / Made available in DSpace on 2018-08-21T10:50:41Z (GMT). No. of bitstreams: 1 Silva_AudreyRoberto_M.pdf: 3023922 bytes, checksum: ee750f675d01f2b3ceebd5d74149b16e (MD5) Previous issue date: 2012 / Resumo: Este trabalho apresenta o desenvolvimento de células fotovoltaicas de junção n+/p em substratos de Si com processos de fabricação totalmente compatíveis com a tecnologia CMOS (Complementary Metal Oxide Semiconductor). Os processos compatíveis desenvolvidos neste trabalho sao as técnicas: i) de texturização da superfície do Si, com reflexao da superficie texturizada de 15% obtida com a formação de micro-pirâmides (alturas entre 3 e 7 ?m), utilizando-se solução alcalina de NH4OH (hidróxido de amônia), que e livre da contaminação indesejável por íons de Na+ e K+ quando se utiliza soluções tradicionais de NaOH e de KOH, respectivamente, e ii) de deposição ECR-CVD (Electron Cyclotron Resonance - Chemical Vapor Deposition) da camada antirrefletora (ARC) de SiNX (nitreto de silício), que e executada em temperatura ambiente, portanto pode ser feita apos a finalização da célula sem danificar trilhas metálicas e alterar a profundidade da junção n+/p. A caracterização desta camada ARC mostrou que o nitreto tem índice de refração de 1,92 e refletância mínima de 1,03%, o que e um excelente resultado para uso em células solares (ou fotovoltaicas). Foram fabricadas cinco series de células fotovoltaicas, utilizando-se a texturização com NH4OH e a camada antirrefletora de nitreto de Si. Em quatro series utilizou-se o processo de implantação de íons de fósforo (31P+), com posterior recozimento, para a formação da região n+, enquanto que na quinta serie foi utilizado o processo de difusão térmica. As eficiências máximas para as células fabricadas são de 9% e de 12%, respectivamente, para as células feitas utilizando os processos de implantação e de difusão térmica, indicando que a implantação de íons causa danos na rede cristalina do silício, que o posterior recozimento não consegue corrigir, o que reduz a eficiência da célula / Abstract: This work presents the development of photovoltaic cells based on n+/p junction in Si substrates, with fully compatible fabrication processes with CMOS technology. The compatible processes, which are developed in this study, are the techniques: i) of Si surface texturing, with the textured surface reflection of 15% obtained by the formation of micro-pyramids (heights between 3 and 7 ?m) using NH4OH (ammonium hydroxide) alkaline solution, which is free of undesirable contamination by Na + and K + ions, when NaOH and KOH traditional solutions are used, respectively, and ii) of the ECR-CVD (Electron Cyclotron Resonance - Chemical Vapor Deposition) deposition of SiNx (silicon nitride) anti-reflective coating (ARC), which is carried out at room temperature and can be performed after the end of cell fabrication without damage on metallic tracks and without variation of n+/p junction depth. The ARC coating characterization presented that the silicon nitride has a refractive index of 1.92 and a minimum reflectance of 1.03%, which is an excellent result for application in solar (or photovoltaic) cells. Five series of photovoltaic cells were fabricated, using the NH4OH solution texturing and the silicon nitride antireflective coating. In the first four series, phosphorus (31P+) ion implantation process, with subsequent annealing to get the region n+, was used, while, in the fifth series was used the thermal diffusion process. The maximum efficiency values are of 9% and 12%, respectively, for cells, which were fabricated using the ion implantation and thermal diffusion processes, indicating that the ion implantation damages the silicon crystal lattice and the subsequent annealing cannot rectify, which reduces the cell efficiency / Mestrado / Eletrônica, Microeletrônica e Optoeletrônica / Mestre em Engenharia Elétrica

Laser surface treatment of engineering ceramics offers various advantages in comparison with conventional processing techniques and much research has been conducted to develop applications. Even so, there still remains a considerable gap in knowledge that needs to be filled to establish the process. By employing a fibre laser for the first time to process silicon nitride (Si3N4) and zirconia (ZrO2) engineering ceramics, a comparison with the CO2 and a Nd:YAG lasers was conducted to provide fundamental understanding of various aspects of the laser beam-material interaction. Changes in the morphology, microstructure, surface finish, fracture toughness parameter (K1c) were investigated, followed by thermal finite element modelling (FEM) of the laser surface treatment and the phase transformation of the two ceramics, as well as the effects of the fibre laser beam parameter - brightness (radiance). Fibre and CO2 laser surface treatment of both Si3N4 and ZrO2 engineering ceramics was performed by using various processing gases. Changes in the surface roughness, material removal, surface morphology and microstructure were observed. But the effect was particularly more remarkable when applying the reactive gases with both lasers and less significant when using the inert gases. Microcracking was also observed when the reactive gases were applied. This was due to an exothermic reaction produced during the laser-ceramic interaction which would have resulted to an increased surface temperature leading to thermal shocks. Moreover, the composition of the ceramics was modified with both laser irradiated surfaces as the ZrO2 transformed to zirconia carbides (ZrC) and Si3N4 to silicon dioxide (SiO2) respectively. The most appropriate equation identified for the determination of the fracture toughness parameter K1c of the as-received, CO2 and the fibre laser surface treated Si3N4 and ZrO2 was K1c=0.016 (E/Hv) 1/2 (P/c3/2). Surfaces of both ceramics treated with CO2 and the fibre laser irradiation produced an increased K1c under the measured conditions, but with different effects. The CO2 laser surface treatment produced a thicker and softer layer whereas the fibre laser surface treatment increased the hardness by only 4%. This is inconsiderable but a reduction in the crack lengths increased the K1c value under the applied conditions. This was through a possible transformation hardening which occurred within both engineering ceramics. Experimental findings validated the generated thermal FEM of the CO2 and the fibre laser surface treatment and showed good agreement. However, a temperature difference was found between the CO2 and fibre laser surface treatment due to the difference in absorption of the near infra-red (NIR) wavelength of the fibre laser being higher than the mid infra-red (MIR) wavelength of the CO2 laser. This in turn, generated a larger interaction zone on the surface that was not induced further into the bulk, as was the case with the fibre laser irradiation. The MIR wavelength is therefore suitable for Viability and Characterization of the Laser Surface Treatment of Engineering Ceramics 3 the surface processing of mainly oxide ceramics and surface treatments which do not require deep penetration. Phase transformation of the two ceramics occurred at various stages during the fibre laser surface treatment. The ZrO2 was transformed from the monoclinic (M) state to a mixture of tetragonal + cubic (T+C) during fibre laser irradiation and from T+C to T and then a partially liquid (L) phase followed by a possible reverse transformation to the M state during solidification. The Si3N4 transformed to a mixture of α-phase and β-phase (α→ α+β) followed by α+β and fully transforms from α+β → β-phase. What is more, is a comparison of the fibre laser-beam brightness parameter with that of the Nd:YAG laser. In particular, physical and microstructural changes due to the difference in the laser-beam brightness were observed. This research has identified the broader effects of various laser processing conditions, as well as characterization techniques, assessment and identification of a method to determine the K1c and the thermal FEM of laser surface treated engineering ceramics. Also, the contributions of laser-beam brightness as a parameter of laser processing and the influence thereof on the engineering ceramics have been identified from a fundamental viewpoint. The findings of this research can now be adopted to develop ceramic fuel cell joining techniques and applications where laser beam surface modification and characterization of engineering ceramics are necessary.

Magister Scientiae - MSc / Amorphous silicon nitride (a-SiN:H) thin films has a multitude of applications, stemming from the tunability of the material properties. Plasma enhanced chemical vapour deposition (PECVD) is the industrial workhorse for production of device quality a-SiN:H. However, this technique has drawbacks in terms of film quality, rooting from ion bombardment, which then results in undesirable oxidation. Hot wire chemical vapour deposition (HWCVD) has shown to be a viable competitor to its more costly counterpart, PECVD. A thin film produced by HWCVD lacks ion bombardment due to the deposition taking place in the absence of plasma. This study will focus on optimising the MVsystems ® HWCVD chamber at The University of the Western Cape, for production of device quality a-SiN:H thin films at low processing parameters. The effect of these parameters on the structural, optical and morphological properties was investigated, for reduction of production costs. The films were probed by heavy ion elastic recoil detection, energy dispersive spectroscopy, Fourier transform infrared spectroscopy, atomic force microscopy, Xray diffraction, and ultraviolet visible spectroscopy. It was shown that silicon rich, device quality a-SiN:H thin films could be produced by HWCVD at wire temperatures as low as 1400 °C and the films showed considerable resistance to oxidation in the bulk.