<p>The main objectives of this thesis were to develop a lowtemperature PECVD process suitable for optoelectronicintegration, and to optimize silica glass composition forUV-induced modifications of a refractive index in PECVDfabricated planar devices. The most important achievement isthe successful development of a low temperature silicadeposition, which for the first time makes it is possible tofabricate good quality low loss integrated components whilekeeping the temperature below 250oC during the entirefabrication process. Two strong absorption peaks thatappear at1.5 mm communication window due to N-H and Si-H bonds have beencompletely eliminated by process optimization. This openspossibilities for monolithic integration with other,temperature sensitive devices, such as semiconductor lasers anddetectors, or polymer-based structures on the common siliconplatform. PECVD technology for low loss amorphous silicon inapplication to SiO2/Si based photonic crystal structures hasbeen also optimized to remove hydrogen incorporated during thedeposition process, responsible for the porosity of thedeposited material and creation of similar to silica absorptionbands.</p><p>Change of the refractive index of germanium doped silicaunder UV irradiation is commonly used for fabrication of UVinduced fiber Bragg gratings. Here we describe our achievementsin fabrication of fiber Bragg gratings and their application todistributed sensor systems. Recently we have built up a laserlab for UV treatment in application to planar technology. Wehave demonstrated the high photosensitivity of PECVD depositedGe-doped glasses (not thermally annealed) even without hydrogenloading, leading to a record transmission suppression of 47dBin a Bragg grating photoinduced in a straight buried channelwaveguide. We have also used a UV induced refractive indexchange to introduce other device modifications or functions,such as phase shift, wavelength trimming and control ofpolarization birefringence.The developed low temperature technology and the UVprocessing form a unique technology platform for development ofnovel integrated functional devices for optical communicationsystems.</p><p>A substantial part of the thesis has been devoted tostudying different plasma deposition parameters and theirinfluence on the optical characteristics of fabricatedwaveguides to find the processing window giving the besttrade-off between the deposition rate,chamber temperatureduring the process, optical losses and presence of absorptionbands within the interesting wavelength range. The optimalconditions identified in this study are low pressure (300-400mTorr), high dilution of silane in nitrous oxide and high totalflow (2000 sccm), low frequency (380 KHz) RF source and high RFpower levels (800-1000 W).</p><p>The thesis provides better understanding of the plasmareactions during the deposition process. RF Power is the keyparameter for increasing the rate of surface processes so as toaccommodate each atomic layer in the lowest energy statepossible. All the process conditions which favor a moreenergetic ion bombardment (i.e. low pressure, low frequency andhigh power) improve the quality of the material, making it moredense and similar to thermal oxide, but after a certain pointthe positive trend with increasing power saturates. As theenergy of the incoming ion increases, a competing effect setsin at the surface: ion induced damage and resputtering.</p><p>Finally, the developed technologies were applied for thefabrication of some test and new concept devices for opticalcommunication systems including multimode interference (MMI)-based couplers/splitters, state-of-the-art arrayed waveguidegrating-based multi/ demultiplexers, the first Bragg gratingassisted MMI-based add-drop multiplexer, as well as moreresearch oriented devices such as a Mach-Zehnder switch basedon silica poling and a Photonic Crystal-based coupler.</p><p><b>Keywords:</b>silica-on-silicon technology, PECVD, plasmadeposition, photonic integrated circuits, planar waveguidedevices, UV Bragg gratings, photosensitivity, arrayed waveguidegratings, multimode interference couplers, add-dropmultiplexers.</p>

Ce travail est consacré à la synthèse de nanotubes de carbone mono-parois et multi-parois orientés par dépôt chimique en phase vapeur assisté par plasma (PECVD). Des études cinétiques ont montré le rôle spécifique du plasma pour la croissance de nanotubes mono-parois (SWNT) ou possédant peu de parois (FWNT). En effet, les phénomènes de gravure physique et chimique, intrinsèques au procédé PECVD, favorisent la croissance des nanotubes multi-parois, structures plus robustes, au profit des SWNT/FWNT. En optimisant les paramètres du plasma (potentiel plasma, mélange des gaz) et le temps de dépôt, la croissance de SWNT/FWNT orientés peut être réalisée de manière contrôlée. De telles structures peuvent être obtenues à basse température (dès 450°C) sur des substrats recouverts d'aluminium. Les mesures d'émission par effet de champ des SWNT/FWNT orientés montrent des tensions de seuil peu élevées (~5 V.µm-1) corrélées avec la morphologie des nanotubes (longueur, rayon). De nombreuses techniques d'analyses ont été utilisées pour étudier la structure des nanotubes aussi bien à l'échelle locale (microscope électronique à transmission, spectroscopie de perte d'énergie des électrons) qu'à l'échelle macroscopique (microscope électronique à balayage, spectroscopie de photoélectrons ultraviolets/X, analyse par détection des atomes de recul, spectroscopie Raman).

Vibration control requires high dynamic stiffness in mechanical structures for a reliable performance under extreme conditions. Dynamic stiffness composes the parameters of stiffness (K) and damping (η) that are usually in a trade-off relationship. This thesis study aims to break the trade-off relationship. After identifying the underlying mechanism of damping in composite materials and joint interfaces, this thesis studies the deposition technique and physical characteristics of nano-structured HDS (high dynamic stiffness) composite thick-layer coatings. The HDS composite were created by enlarging the internal grain boundary surface area through reduced grain size in nano scale (≤ 40 nm). The deposition process utilizes a PECVD (Plasma Enhanced Chemical Vapour Deposition) method combined with the HiPIMS (High Power Impulse Magnetron Sputtering) technology. The HDS composite exhibited significantly higher surface hardness and higher elastic modulus compared to Poly(methyl methacrylate) (PMMA), yet similar damping property. The HDS composites successfully realized vibration control of cutting tools while applied in their clamping interfaces. Compression preload at essential joint interfaces was found to play a major role in stability of cutting processes and a method was provided for characterizing joint interface properties directly on assembled structures. The detailed analysis of a build-up structure showed that the vibrational mode energy is shifted by varying the joint interface’s compression preload. In a build-up structure, the location shift of vibration mode’s strain energy affects the dynamic responses together with the stiffness and damping properties of joint interfaces. The thesis demonstrates that it is possible to achieve high stiffness and high damping simultaneously in materials and structures. Analysis of the vibrational strain energy distribution was found essential for the success of vibration control.

Submitted by DIEGO GLAUCO AZARIAS DOS REIS null (diego.dgadr@gmail.com) on 2017-04-19T18:15:44Z No. of bitstreams: 1 Dissertação-Diego_Reis_2017.pdf: 2518961 bytes, checksum: a16c2b4a218332cdf0587afa47cadbff (MD5) / Rejected by Luiz Galeffi (luizgaleffi@gmail.com), reason: Solicitamos que realize uma nova submissão seguindo a orientação abaixo: O arquivo submetido está sem a ficha catalográfica. A versão submetida por você é considerada a versão final da dissertação/tese, portanto não poderá ocorrer qualquer alteração em seu conteúdo após a aprovação. Corrija esta informação e realize uma nova submissão com o arquivo correto. Agradecemos a compreensão. on 2017-04-19T19:55:04Z (GMT) / Submitted by DIEGO GLAUCO AZARIAS REIS (diego.dgadr@gmail.com) on 2017-04-20T13:12:56Z No. of bitstreams: 1 Dissertação-Diego_Reis_2017.pdf: 2653651 bytes, checksum: af70d0852f1dbed4cb80ba89720797f4 (MD5) / Approved for entry into archive by Luiz Galeffi (luizgaleffi@gmail.com) on 2017-04-25T17:14:34Z (GMT) No. of bitstreams: 1 azarias_dga_me_guara.pdf: 2653651 bytes, checksum: af70d0852f1dbed4cb80ba89720797f4 (MD5) / Made available in DSpace on 2017-04-25T17:14:34Z (GMT). No. of bitstreams: 1 azarias_dga_me_guara.pdf: 2653651 bytes, checksum: af70d0852f1dbed4cb80ba89720797f4 (MD5) Previous issue date: 2017-02-20 / O tratamento de materiais utilizando plasma tem sido utilizado amplamente nos dias atuais com o desenvolvimento de novas tecnologias baseadas em descargas elétricas a pressão atmosférica. Dentre os diversos métodos para produzir plasmas nestas condições destaca-se a descarga por microplasmas. No presente trabalho, um novo dispositivo foi desenvolvido e utilizado para deposição de filmes finos. Em estudos de arrasto de vapores no dispositivo foi verificado a relação linear entre a vazão do gás e a massa arrastada. Deposições poliméricas foram obtidas pela mistura de gás argônio com o monômero hexametildissiloxano (HMDSO) em substratos de vidro. A deposição de filmes ocorreu com a vazão de gás entre 0,07 L/min e 0,4 L/min para potências entre 100 mW e 650 mW. Para outras vazões, ocorreu a formação de material sólido em forma de grânulos submilimétricos. A caracterização dos filmes por espectroscopia infravermelha com transformada de Fourier (FTIR) mostrou a presença de grupos moleculares como trimetilsilil Si(CH3)3, siloxano SiOSi e metino CHx. Os testes de adesão realizados no padrão D3359 ASTM com fita Scotch 3M mostraram boa adesão dos filmes aos substratos. Medições de ângulo de contato mostraram a diminuição da hidrofilicidade da superfície dos substratos com valores variando de 40° sem tratamento para quase 90° com o filme fino. Os resultados mostraram que dispositivo desenvolvido foi utilizado com sucesso na deposição em pressão atmosférica de filmes de HMDSO indicando que pode ser empregado também com outros monômeros. / The treatment of materials using plasma has been used widely nowadays with the development of new technologies based on electrical discharges at atmospheric pressure. Among the various methods of producing plasma in these conditions, we gave attention to microplasmas. In this study, a new device was developed and applied to the deposition of polymeric thin films. The dragging of the vapour in the device was investigated for various organic compounds and gas flow rate. It was observed a linear relation between these parameters. The polymeric depositions were obtained with the mixture of argon gas and hexamethyldisiloxane (HMDSO) on glass slides. The thin film deposition occurred with gas flow rate between 0.07 L/min and 0.4 L/min with potencies around 100 mW and 650 mW. The formation of solid submilimeter grains was observed at others gas glow rates. The regular thin films was analysed by Fourier transform infrared spectroscopy (FTIR) and showed the molecular groups of trimethylsilyl Si(CH3)3, siloxane SiOSi and methyne CHx. The films had a good adhesion when subjected to the D3359 ASTM standard test using adhesive tape Scotch 3M. Contact angle characterization has shown a decrease of the hydrophilicity surface property with values changing from 40o without treatment up to 90o with thin film. The results has shown that the developed device was successfully used for deposition of HMDSO films at atmospheric pressure indicating that can be used with other monomers as well.

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.

O presente trabalho, realizado junto ao Grupo de Novos Materiais e Dispositivos (GNMD), no Laboratório de Microeletrônica do Departamento de Sistemas Eletrônicos da Escola Politécnica da USP, visou determinar algumas das propriedades termo-mecânicas de materiais depositados pela técnica de plasma enhanced chemical vapor deposition (PECVD) que são importantes para o desenvolvimento de sistemas microeletromecânicos (MEMS). O módulo de elasticidade, a tensão mecânica residual, o coeficiente de expansão térmica e a condutividade térmica de filmes finos de carbeto de silício amorfo hidrogenado (a-SiC:H) e de oxinitreto de silício (SiOxNy) foram estudados. Medidas de nanoindentação e ressonância de cantilevers foram utilizadas para a obtenção do módulo de elasticidade e os resultados obtidos foram similares (75 e 91 GPa) pelos dois métodos e compatíveis com valores encontrados na literatura. Além disso, obteve-se o módulo de elasticidade de filmes de cromo (285 GPa). A tensão mecânica residual dos filmes utilizados neste trabalho foi medida através da curvatura do substrato induzida pela deposição dos filmes e pela deformação de cantilevers. O valor médio da tensão mecânica, obtido pela curvatura do substrato, variou de -69 MPa até -1750 MPa, mostrando grande dependência das condições de deposição dos filmes. O método que utiliza a deformação de cantilevers possibilitou a obtenção do gradiente de tensão mecânica, que também mostrou uma dependência das condições de deposição, sendo sempre o a-SiC:H quase estequiométrico o menos tensionado. O coeficiente de expansão térmica foi medido utilizando a técnica do gradiente de temperatura e o valor obtido foi similar a valores reportados na literatura para o carbeto de silício cristalino. Para um a-SiC:H quase estequiométrico foi obtido um coeficiente de expansão térmica de 3,41 m/oC, enquanto para um a-SiC:H rico em carbono o valor foi de 4,36 m/oC. Também foi verificado que a variação da resistência do cromo em função da temperatura é pequena, não permitindo sua utilização como sensor de temperatura e inviabilizando a obtenção da condutividade térmica dos filmes estudados. Além disso, foram apresentados trabalhos promissores, mostrando o potencial dos materiais estudados para o desenvolvimento de MEMS. Nesses trabalhos, demonstrou-se a viabilidade de integrar microestruturas atuadas termicamente e guias de onda ópticos, utilizando os materiais estudados neste trabalho. Foram fabricados chaves ópticas, portas lógicas ópticas, fontes de luz integradas e acoplamento das fontes de luz com guias de onda. / This work, realized at the New Materials and Devices Group (GNMD) at the Microelectronics Laboratory of the Department of Electronic Systems of the Polytechnic School of the University of São Paulo, focused at the determination of thermo-mechanical properties of materials deposited by plasma enhanced chemical vapor deposition (PECVD) that are important for the development of microelectromechanical systems (MEMS). The Youngs modulus, the residual stress, the coefficient of thermal expansion and the thermal conductivity of amorphous hydrogenated silicon carbide (a-SiC:H) and silicon oxynitride (SiOxNy) thin films were studied. Nanoindentation and the resonance of cantilevers were used to obtain the Youngs modulus. The results were similar (75 and 91 GPa) with both methods and compatible with literature values. Further, the Youngs modulus of chromium films was also obtained (285 GPa). The residual stress of thin films was obtained through the substrate curvature induced by the film deposition and through the deformation of cantilever beams. The residual stress, obtained through the substrate curvature, varied between -69 MPa and -1750 MPa, showing great dependence on the deposition conditions of these materials. The deformation of cantilevers allowed the determination of the stress gradient and it was also affected by the deposition conditions. In all stress measurements the near stoichiometry a-SiC:H film was less stressed. The coefficient of thermal expansion was measured using the temperature gradient technique and the obtain values were similar to those reported in the literature for crystalline silicon carbide. For a near stoichiometry a-SiC:H film, a value of 3.41 m/oC was obtained, while a carbon rich film showed a thermal expansion coefficient of 4.36 m/oC. It was also verified that the variation of the chromium resistance as a function of temperature is small. This did not allow the utilization of chromium as a temperature sensor, which prevented the obtention of the thermal conductivity of the studied films. Also, some promising works were presented, showing potential applications of the studied materials for the development of MEMS. In these works, the viability of integration of thermal actuated microstructures and optical waveguides was demonstrated. In these works, optical switches, optical logic gates, integrated light sources and coupling of integrated light sources with optical waveguides were presented.

4H-SiC based Metal-Oxide Semiconductor(MOS) capacitors are promising key components for next generation power devices. For high frequency power applications, however, there is a major drawback of this type of devices, i.e. they have low inversion channel mobility that consequently affects the switching operation in MOS Field-Effect Transistors (MOSFETs). Carbon clusters or excess carbon atoms in the interface between the dielectric layer and SiC is commonly considered to be the carrier trapping and scattering centers that lower the carrier channel mobility. Based on the previous work in the research group, a new fabrication process for forming the dielectric layer with a lower density of the trap states is investigated. The process consists of standard semiconductor cleaning, pre-treatments, pre-oxidation, plasma enhanced chemical vapor deposition (PECVD) and post oxidation annealing. I-V measurements of the dielectric strength showed that the resulting layers can sustain proper working condition under an electric field of at least 5MV/cm. C-V characteristics measurements provided the evidence that the proposed method can effectively reduce the interfacial states, which are main culprit for a large flat band voltage shift of C-V characteristics, in particular under annealing at 900°C in nitrogen atmosphere.

The thesis describes surface topography of a-CSi:H films deposited by continuous wave plasma enhanced chemical vapor deposition (PECVD) based on tetravinylsilane monomer (TVS). Thin films are completely used in many fields of modern technologies and their physical and mechanical properties are affected by thin film preparation techniques. In this thesis the thin films were deposited by PECVD method on silicon wafers with the pure TVS monomer. Deposited samples were topographically described and analyzed using atomic force microscopy (AFM). The main characteristics which were described are RMS roughness, autocorrelation function and a size distribution of grains on the thin film surface. Analysis was realized with two sets of samples with different powers and thickness. The main results were statistically evaluated like a mixture of object on the surface prepared in different deposition conditions.

Cieľom diplomovej práce je príprava polymerných kompozitov vyztužených sklenenými vláknami s riadenou medzifázou za použitia metódy plazmochemickej depozície z plynnej fáze a monomeru tetravinylsilanu. Teoretická časť je zameraná na literárnu rešerš o plazme, plazmovej polymerácií, tenkých vrstvách a kompozitoch. Experimentálna časť popisuje použité materiály a aparaturu použitú na povrchovú modifikáciu sklenených vlákien a prípravu vláknom vyztužených kompozitov. Povrchová úprava sklenených vlákien prebiehala za rôznych depozičných podmienok. Chemické a mechanické analýzy vytvorenej medzivrstvy prebiehali za použitia FTIR spektrometrie a vrypového testu. Vliv povrchovej úpravy bol zistený pomocou získanej interlaminárnej šmykovej sily použítím testu krátkych trámečkov.

Diploma thesis deals with preparation of multilayered organic-inorganic nanostructures via PECVD technology and analysis of optical properties of these layers by spectroscopic ellipsometry. The theoretical part handles the definition of thin layers, layered and gradient nanostructures, plasma enhanced chemical vapor deposition and principles of spectroscopic ellipsometry. In the experimental part, used materials and chemicals are described, afterwards follow a complete description of the apparatus used for sample preparation and a description of the sample preparation procedure. The results part consists of methodology of preparing material models necessary for ellipsometric measurements and evaluation of optical properties of deposited nanolayers.