O desempenho de componentes de engenharia está intimamente ligado a fenômenos de superfície, pois esta funciona como a interface entre o componente e o ambiente que o cerca. A escolha de um material com propriedades superficiais adequadas é fundamental para a sua funcionalidade. Neste trabalho as propriedades físico-químicas, estruturais e mecânicas do filmes de nitreto de silício depositados por magnetron sputtering reativo com uma fonte de radiofreqüência, antes e após tratamento térmico em 18O2, foram analisadas por diferentes métodos, tais como nanodureza, difração de raios X, perfilometria por reação nuclear ressonante, nanoindentação, espectrometria de retroespalhamento Rutherford, espectroscopia de fotoelétrons induzidos por raios X e reflectometria de raios X. Os filmes de Si3N4 depositados são essencialmente amorfos, estequiométricos e livres de contaminantes para vários parâmetros de deposição, com valores de dureza que variam de 16,5 GPa 22 GPa, dependendo principalmente da temperatura de deposição dos filmes. Depois de realizado o tratamento térmico em 18O2 a 1000 °C, a dureza de filmes converge para 21 GPa, independentemente da temperatura de deposição o que é explicado com base na cristalização dos filmes nesta temperatura de tratamento térmico. Além disso, o oxigênio é incorporado apenas 7,5 nm do filme de Si3N4, formando oxinitreto de silício na superfície do filme, indicando uma boa resistência à oxidação em altas temperaturas. Finalmente, a deformação elástica até a fratura H3/E2, que é um bom indicador da resistência ao desgaste do filme, dobra após o tratamento térmico a 1000 °C. Estas observações mostram o grande potencial do nitreto de silício como um revestimento duro para aplicações em altas temperaturas. / Submitted by Marcelo Teixeira (mvteixeira@ucs.br) on 2014-06-03T19:57:31Z No. of bitstreams: 1 Dissertacao Cristiane Marin.pdf: 10200632 bytes, checksum: 55a17a7df0f8900cefa2a80a1fe4c086 (MD5) / Made available in DSpace on 2014-06-03T19:57:31Z (GMT). No. of bitstreams: 1 Dissertacao Cristiane Marin.pdf: 10200632 bytes, checksum: 55a17a7df0f8900cefa2a80a1fe4c086 (MD5) / The performance of engineering components is closely tied to surface phenomena, because it acts as an interface between the component and the environment that surrounds it. The choice of a suitable material with surface properties is critical to its functionality. In this study the physicochemical, structural and mechanical properties of silicon nitride films deposited by radio frequency reactive magnetron sputtering before and after thermal annealing in 18O2 were analyzed using different methods, such as nanohardness, X-ray diffraction, profilometry resonant nuclear reaction, nanoindentation, Rutherford backscattering spectrometry, photoelectron spectroscopy and X-ray induced X-ray reflectometry The Si3N4 films deposited are essentially amorphous, stoichiometric and free of contaminants for various deposition parameters, with hardness values ranging from 16.5 GPa 22 GPa, depending mainly on the deposition temperature of films. After 18O2 annealing at 1000°C, films hardness converged to 21 GPa, independently of the deposition temperature, which is explained on the basis of crystallization of the films at this annealing temperature. Furthermore, oxygen is incorporated only in the 7.5 nm film of Si3N4, forming silicon oxynitride on the surface of the film, indicating good oxidation resistance at high temperature. Finally, the elastic strain to failure H3/E2, which mimics the wear resistance of the film, doubles after the 1000°C annealing. These observations show the great potential of silicon nitride as a hard coating for high temperature applications.

Neste trabalho, foi investigado o comportamento tribológico dos pares cerâmicos aluminanitreto de silício no deslizamento em água e em uma suspensão de sílica coloidal em água (hidrosol). O objetivo foi verificar a possibilidade de atingir um coeficiente de atrito da ordem de unidades de milésimos, aqui chamado de ultra-baixo coeficiente de atrito (UBCA), verificar se a mudança do meio, de água para hidrosol, diminui o running-in do coeficiente de atrito, e verificar o efeito da variação da rugosidade inicial da alumina no comportamento do atrito. Os ensaios foram realizados na configuração de teste esferasobre- disco, no qual a esfera foi de nitreto de silício e o disco de alumina, sob carga normal de 54 N e velocidade de 1 m/s. A água utilizada nos ensaios foi destilada e deionizada, e a sílica coloidal amorfa, hidrofílica, sem porosidade e de tamanho médio de partícula de 12 nm foi a Aerosil® 200, e o hidrosol foi preparado com pH 8,5 num eletrólito de NaCl de 1 mM. A esfera de nitreto de silício, adquirida comercialmente, e a alumina, sinterizada em laboratório, foram caracterizadas quanto a densidade, as fases foram determinadas por difração de raios X, microscopia eletrônica de varedura (MEV) observada em amostras ceramográficas atacadas. Algumas propriedades mecânicas como dureza, módulo de elasticidade e tenacidade à fratura foram determinadas. Duas condições de rugosidade dos discos de alumina foram utilizadas nos ensaios tribológicos, 350 nm e 10 nm RMS. Em todos os ensaios, em água, em hidrosol e independentemente da rugosidade inicial do disco o coeficiente de atrito no regime permanente apresentou pequena dispersão de valores de 0,002 a 0,006, e não foi possível estabelecer diferença entre elas. A menor rugosidade do disco de alumina acarretou menor desgaste e menor período de running-in de coeficiente de atrito, tanto em água quanto em hidrosol. Os ensaios em meio de hidrosol acarretaram menor desgaste das cerâmicas e apresentaram menor running-in de coeficiente de atrito, comparados aos ensaios com água. O disco de alumina apresentou menor desgaste do que a esfera de nitreto de silício, em todas as condições estudadas. Com a análise das perdas volumétricas, da rugosidade final das superfícies desgastadas, das curvas de coeficiente de atrito e das espessuras mínimas de filme lubrificante, calculadas com uso de modelo da literatura, foi possível relacionar a diminuição do desgaste e do running-in de coeficiente de atrito em meio de hidrosol, com a presença da sílica na superfície ou próxima dela. / In this work, the tribological behavior of the alumina-silicon nitride couple was investigated under water and hydrosol (colloidal silica suspensions in water) lubricated sliding. The purposes were to study how an ultra-low friction coefficient can be achieved and to analyze the effects of the environment, lubricant and alumina roughness changes on the friction behavior. Ball-on-disk tests with a normal load of 54 N and a sliding speed of 1 m/s were carried out, using a silicon nitride ball and an alumina disk. The water used as lubricant was distilled and deionized. The silica was amorphous colloidal and hydrophilic, without porous and with a 12 nm medium particle diameter, commercially named Aerosil ® 200. The hydrosol was obtained with a pH value of 8,5 and a 1mM NaCl electrolyte. To estimate the minimum film thickness, formed during the lubricated sliding tests, a theory model was used. The commercial silicon nitride balls and the alumina disks, which were conformed and sintered in laboratory, were characterized by density, X-ray diffraction and scanning electron microscopy measurements. The mechanical properties such as hardness, Young modulus and fracture toughness were determined. The friction coefficient values obtained in the steady state regime showed low standard deviations (0,002 to 0,006) under all conditions. A shorter period of running-in was observed with the lower disk roughness, both in water and hydrosol lubrication. The hydrosol lubricated sliding produced a lower wear and friction running-in comparing with the tests under water lubrication. The alumina disk always showed lower wear than the silicon nitride ball. The volume loss, friction coefficients, worn surfaces roughness and minimum film thickness results suggest that the wear and friction coefficient running-in decrease was caused by the presence of silica on the sliding surfaces or on the near surface regions.

O desempenho de componentes de engenharia está intimamente ligado a fenômenos de superfície, pois esta funciona como a interface entre o componente e o ambiente que o cerca. A escolha de um material com propriedades superficiais adequadas é fundamental para a sua funcionalidade. Neste trabalho as propriedades físico-químicas, estruturais e mecânicas do filmes de nitreto de silício depositados por magnetron sputtering reativo com uma fonte de radiofreqüência, antes e após tratamento térmico em 18O2, foram analisadas por diferentes métodos, tais como nanodureza, difração de raios X, perfilometria por reação nuclear ressonante, nanoindentação, espectrometria de retroespalhamento Rutherford, espectroscopia de fotoelétrons induzidos por raios X e reflectometria de raios X. Os filmes de Si3N4 depositados são essencialmente amorfos, estequiométricos e livres de contaminantes para vários parâmetros de deposição, com valores de dureza que variam de 16,5 GPa 22 GPa, dependendo principalmente da temperatura de deposição dos filmes. Depois de realizado o tratamento térmico em 18O2 a 1000 °C, a dureza de filmes converge para 21 GPa, independentemente da temperatura de deposição o que é explicado com base na cristalização dos filmes nesta temperatura de tratamento térmico. Além disso, o oxigênio é incorporado apenas 7,5 nm do filme de Si3N4, formando oxinitreto de silício na superfície do filme, indicando uma boa resistência à oxidação em altas temperaturas. Finalmente, a deformação elástica até a fratura H3/E2, que é um bom indicador da resistência ao desgaste do filme, dobra após o tratamento térmico a 1000 °C. Estas observações mostram o grande potencial do nitreto de silício como um revestimento duro para aplicações em altas temperaturas. / The performance of engineering components is closely tied to surface phenomena, because it acts as an interface between the component and the environment that surrounds it. The choice of a suitable material with surface properties is critical to its functionality. In this study the physicochemical, structural and mechanical properties of silicon nitride films deposited by radio frequency reactive magnetron sputtering before and after thermal annealing in 18O2 were analyzed using different methods, such as nanohardness, X-ray diffraction, profilometry resonant nuclear reaction, nanoindentation, Rutherford backscattering spectrometry, photoelectron spectroscopy and X-ray induced X-ray reflectometry The Si3N4 films deposited are essentially amorphous, stoichiometric and free of contaminants for various deposition parameters, with hardness values ranging from 16.5 GPa 22 GPa, depending mainly on the deposition temperature of films. After 18O2 annealing at 1000°C, films hardness converged to 21 GPa, independently of the deposition temperature, which is explained on the basis of crystallization of the films at this annealing temperature. Furthermore, oxygen is incorporated only in the 7.5 nm film of Si3N4, forming silicon oxynitride on the surface of the film, indicating good oxidation resistance at high temperature. Finally, the elastic strain to failure H3/E2, which mimics the wear resistance of the film, doubles after the 1000°C annealing. These observations show the great potential of silicon nitride as a hard coating for high temperature applications.

Orientador: Luiz Otávio Saraiva Ferreira. / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica / Made available in DSpace on 2018-08-21T04:03:41Z (GMT). No. of bitstreams: 1 Silva_MarioEduardodeBarrosGomeseNunesda_M.pdf: 3848213 bytes, checksum: ebb7fc7d814e03c6ae81ee577ddb158f (MD5) Previous issue date: 2012 / Resumo: A caracterização das propriedades mecânicas de filmes finos faz-se necessária para o projeto e fabricação de Microsistemas Eletromecânicos (MEMS - Micro-Electro-Mechanical Systems), que demanda dados precisos dos materiais. Esta pesquisa descreve um novo método de caracterização das propriedades mecânicas de filmes finos, barato e aplicávela uma ampla gama de materiais. Além do mais, este método também pode ser utilizado para avaliar a resistência das microestruturas durante cada etapa do processo de fabricação, e mesmo do sistema completo. Para realizar os experimentos de caracterização é utilizado um perfilômetro de superfície. Perfilômetros de superfície são dispositivos utilizados para medir a espessura e rugosidade de filmes, sendo essenciais em laboratórios de microfabricação. Tal fato permite que seja possivel repetir os experimentos deste trabalho em qualquer laboratório que possua um perfilômetro de superfície, sem a necessidade de investimento em novos equipamentos. O método de caracterização baseia-se na flexão de microestruturas suspensas. Os corpos de prova são fabricados no material em teste, e um perfilômetro de superfície é usado para defleti-los, e a partir dos dados desse experimento, pode-se calcular o módulo de Young. Caso os corpos de prova venham a se fraturar é possivel calcular a tensão de ruptura. Em uma primeira etapa do trabalho, foram caracterizados filmes de óxido de silício, fabricados por óxidação térmica de um substrado de silício monocristalino. Na segunda etapa, o método de caracterização foi expandido para filmes sobrepostos de materiais diversos e, foram caraterizados filmes de nitreto de silício, fazendo uso de microestruturas compostas de nitreto de silicio, depositado pelo método de vapor químico de baixa pressão (LPCVD), sobre o óxido de silício fabricado por óxidação térmica. O presente trabalho também sugere uma forma de utilizar o mesmo método de caracterização para determinar o coeficiente de Poisson, fazendo uso de várias amostras com expessuras diversas. Os corpos de prova foram fabricados no Centro de Componentes Semicondutores (CCS) da Universidade Estadual de Campinas (UNICAMP), e os experimentos de deflexão realizados no Laboratório de Microfabricação (LMF) do Laboratório Nacional de Nanotecnologia (LNNano) / Abstract: The mechanical properties characterization of thin films is necessary for MEMS (Micro-Electro-Mechanical Systems) design and manufacture, which requires accurate materials data. This research describes a new method for mechanical properties characterization of thin films, inexpensive and applicable to a wide range of materials. Also, this method can be used to evaluate the resistance of the microstructures during each step of the manufacturing process, and even the complete system. To perform the experiments of characterization is used a surface profilometer. Surface profilometers are devices generally used to measure the films thickness and roughness, and they are essential in microfabrication laboratories. This fact allows the possibility of repetitive the experiments of this work in any laboratory that has a surface profilometer, without the necessity to invest in new equipment. The characterization method is based on bending of suspended microstructures. The specimens are fabricated in the material under test, and a surface profilometer is used to deflect then, and from this experiment data, it's possible to calculate the Young's modulus. If the specimens fracture, it is possible to calculate the tensile strength. In a first step, were characterized films of silicon oxide, manufactured by thermal oxidation of a monocrystalline silicon substrate. In the second step, the characterization method has been expanded to superimposed films of various materials and films of silicon nitride were characterized, by making use of microstructures consisting of silicon nitride, deposited by the method of low-pressure chemical vapor (LPCVD), over the silicon oxide produced by thermal oxidation. The present work also suggests a way to use the same characterization method for determining the Poisson's ratio, using various samples with different thickness. The specimens were fabricated in the Center for Semiconductor Components (CCS) of University of Campinas (UNICAMP), and the deflection experiments performed in the Microfabrication Laboratory (LMF) of Brazilian Nanotechnology National Laboratory (LNNano) / Mestrado / Mecanica dos Sólidos e Projeto Mecanico / Mestre em Engenharia Mecânica

Doctorat en Sciences / info:eu-repo/semantics/nonPublished

Gallium Nitride (GaN) based transistors have been in the spotlight for power electronics due to promising properties like high bandgap, high breakdown field, high electron mobility, and high-frequency applications. While there are some commercial devices based on these transistors available, there is still room for improvement in these devices for widespread usage. In this project, GaN-based transistors fabricated at RISE AB were investigated. These devices had previously shown high leakage current. Different approaches taken to reduce the said leakage current were analysed. The main scope of the thesis was static electrical testing of a new batch of these transistors at room temperature, mainly investigating their leakage current. The new transistors were subjected to surface treatments and also a new in-situ dielectric layer was used. The surface treatments did not show much improvement but the in-situ grown dielectric showed almost half of the initial leakage current. In addition to this different device architectures with varying gate length, gate width, and gate to drain distance were tested and compared. It was found that devices with 3 μm gate length and 12 μm gate to drain distance showed the best performance. The blocking characteristic of the transistors was also tested and the devices could withstand up to 350V. Suggestions to further identify the sources of the leakage current are presented. Possible improvement in the design of the transistors to increase the blocking voltage is also described. / Transistorer baserade på galliumnitrid (GaN) har varit i strålkastaren för kraftelektronik på grund av lovande egenskaper som högt bandgap, högt nedbrytningsfält, hög elektronmobilitet. Dessa egenskaper gör materialet synnerligen lämpligt för komponentapplikationer vid höga effekter och, framför allt, höga frekvenser. Även om det finns några kommersiella applikationer baserade på dessa transistorer finns det fortfarande stort utrymme för förbättringar. I detta projekt undersöktes GaN-baserade transistorer tillverkade vid RISE AB. Dessa komponenter hade tidigare visat hög läckström och olika tillvägagångssätt för att minska nämnda läckström har analyserats. Transistorerna i detta projekt var ytbehandlade på ett nytt sätt och dielektirkat i styrelektroden var ocskå tillverkat på ett nytt sätt. Ytbehandlingarna visade inte mycket förbättring men det dielektrikat visade nästan hälften av den initiala läckströmmen. Utöver detta testades och jämfördes olika layouter med varierande geometri, gate-längd, gate-bredd och avstånd mellan gate/source. Det visade sig att komponenter med 3 μm gate-längd och 12 μm mellan gate och drain visade bästa prestanda. Transistorernas blockeringskaraktäristik testades också och visade sig tåla upp till 350V. Förslag för att ytterligare identifiera källorna till läckströmmen presenteras. Eventuell förbättring av utformningen av transistorerna för att öka blockeringsspänningen beskrivs också.

Silicon photonics (SiP) has evolved into a mature platform for cost-effective low power compact integrated photonic microsystems for many applications. There is a looming capacity crunch for telecommunications infrastructure to overcome the data-hungry future, driven by streaming and the exponential increase in data traffic from consumer-driven products. To increase data capacity, researchers are now looking at the wavelength window of the thulium-doped fiber amplifier (TDFA), centered near 2 µm as an attractive new transmission window for optical communications, motivated by the demonstrations of low loss, low nonlinearity, and high bandwidth transmission. Large-scale implementation of SiP telecommunication infrastructure will require light sources (lasers) and amplifiers to generate signals and boost transmitted and/or received signals, respectively. Silicon (Si) and silicon nitride (Si3N4) have become the leading photonic integrated circuit (PIC) material platforms, due to their low-cost and wafer-scale production of high-performance circuits. Silicon does however have a number of limitations as a photonic material, including that it is not an ideal light-emitting/amplifying material. This proposed research pertains to the fabrication of on-chip silicon and silicon nitride lasers and amplifiers to be used in a newly accessible optical communications window of the TDFA band, which is a significant step towards compact PICs for the telecommunication networks. Tellurium oxide (TeO2) is an interesting host material due to its large linear and non-linear refractive indices, low material losses and large rare-earth dopant solubility showing good performance for compact low-loss waveguides and on-chip light sources and amplifiers. Chapter 1 provides an overview of silicon photonics in the context of particularly rare earth lasers and amplifiers, operating at extended wavelengths enabled by the Thulium doped fiber amplifier. Chapter 2 presents a theoretical performance of waveguides and microresonators as the efficient structure for laser and amplifiers applications designed for optimized use in Erbium and Thulium doped fiber amplifier wavelength bands. Then spectroscopic study thulium (Tm3+) has been studied as the rare earth element for Thulium doped fiber amplifier wavelength bands. Chapter 3 presents an experimental study of TeO2:Tm3+ coated Si3N4 waveguide amplifiers with internal net gains of up to 15 dB total in a 5-cm long spiral waveguide. Chapter 4 provides a study of TeO2:Tm3+ -coated Si3N4 waveguide lasers with up to 16 mW double-sided on-chip output power. Chapter 5 presents an experimental study of low loss and high-quality factor silicon microring resonators coated with TeO2 for active, passive, and nonlinear applications. Chapter 6 represents the first demonstration of an integrated rare-earth silicon laser, with high performance, including single-mode emission, a lasing threshold of 4 mW, and bidirectional on-chip output powers of around 1 mW. Further results with a different design are presented showing lasers with more than 2 mW of double-sided on-chip output power, threshold pump powers of < 1 mW and lasing at wavelengths over a range of > 100 nm. Importantly, a simple, low-cost design was used which is compatible with silicon photonics foundry processes and enables wafer scale integration of such lasers in SiP PICs using robust materials. Chapter 7 summarizes the thesis and provides paths for future work. / Dissertation / Doctor of Engineering (DEng)

No description available.

This thesis aims to measure the mechanical properties of ceramics on the microscale using microcantilever beams. Focussed Ion Beam milled triangular cross-sectional beams (approximately 3 x 5 x 20µm) were fractured using a nanoindenter to measure the Young’s modulus, fracture strength, and fracture toughness. By developing the technique with a sapphire bicrystal, it was found that the mechanical properties could be successfully ascertained if correction factors were used. Experiments and theoretical work showed that sapphire and polycrystalline alumina beams undergo moisture assisted sub-critical crack growth when tested in air. Whilst corrections for the Young’s modulus have been previously reported, this is the first reported attempt to correct for the notch tip residual stress and the first to consider sub-critical crack growth. Once these factors were characterised using the sapphire bicrystal, the technique was applied to a range of different ceramics, such as polycrystalline α-alumina and silicon nitride. These are the first reported direct measurements the grain boundary toughness of these ceramics using microcantilever beams. The grain boundary toughness was correlated with the macroscopic fracture properties and the characteristics of the ceramic (grain boundary composition, impurities, and fracture mode). Two grades of α-alumina were used and the macro- and micro-scale properties extensively compared. The damage evolution during uniaxial compression of alumina was investigated in depth, and compared to a previous reported microcrack evolution model using the measured grain boundary toughness. Investigation of whether deformation twins formed during loading was undertaken and the phenomenon was shown to not occur.

Un nouvel essai mécanique a été développé pour répondre à la demande d'analyse des propriétés mécaniques des revêtements et films d'épaisseur nanométrique par essai de gonflement. La méthode utilisée est l'application d'une différence de pression sur une membrane non supportée, usinée en utilisant les techniques standards de gravure microélectronique. Le banc d'essai permettra d'effectuer des essais à haute température (au dessus de 900°C). La principale difficulté rencontrée a été la mise au point d'une méthode de mesure de la déflection de la membrane qui perturbe celle ci aussi peu que possible. Deux techniques ont été utilisées : capteur ponctuel et capteur interférométrique 2D avec référence sphérique. La première technique, plus simple, s'est révélée difficilement praticable, en particulier dans le cas de flambage de la membrane. La mise en place de la deuxième a nécessité une description fine du comportement du système optique (distorsion des images, calcul des interférogrammes) aboutissant à une méthode de mesure simple, susceptible d'être intégrée en ligne au système de contrôle de l'interféromètre, et complétée par un traitement complet des données après essai.Afin de valider l'essai, deux types de revêtements ont été caractérisés. Tout d'abord des films fragiles de nitrure de silicium et de silicium pour mettre en évidence la fiabilité et la reproductibilité des essais. Puis des films minces d'or pour observer l'influence de la microstructure sur le début de la déformation plastique / A new mechanical testing device of free standing membranes by Bulge Test has been built at Institute Jean Lamour in order to investigate the mechanical properties of thin films of nanometric thickness. The Bulge Test measures the deflection of a free standing membrane to which a differential atmospheric pressure has been applied. (The specimens are prepared from film on substrate deposits by cutting a window within the substrate by standard microelectronic techniques.) We aim of achieve tests from room temperature to ~ 900°C. The main technical difficulty met during this work was to develop a non perturbating method of measurement of the film bulge. Two different techniques were tested: point measurement and 2D interferometry using a spherical reference. The first technique, however simple, was difficult to practice, especially in the case of buckling membranes. The second method required a detailed analysis of the whole optical system (image distorsion, calculation of interferograms) leading to a simple measurement method, suitable for integration in the acquisition and command chain of the device, followed by an off line full treatment.The operating method was used on two different sets of specimens: fragile silicon nitride and silicon membranes in order to test the reproducibility of the device. Polycrystalline gold thin films were then used to study the early stage of plastic strain