Microplasmas são plasmas gerados em espaços com dimensões reduzidas, tipicamente, de dezenas a centenas de micrômetros. Apresentam como principal vantagem a possibilidade de se obter plasmas frios com densidades elevadas com baixo consumo de energia em pressões maiores do que em reatores convencionais, reduzindo sensivelmente o custo do equipamento. Um gerador de microplasma inédito foi desenvolvido neste trabalho, utilizando a tecnologia LTCC. O dispositivo é constituído por dois eletrodos paralelos de prata-paládio perfurados por centenas de microfuros, formando microcanais. O microplasma é gerado na região entre os eletrodos e é conduzido para fora do gerador através dos microcanais, constituindo um plasma remoto que pode interagir com a superfície de um material a ser processado. Os microfuros formam a estrutura de um microcatodo oco. Na fabricação, as camadas de cerâmica verde foram usinadas com uma máquina de CNC e os eletrodos foram obtidos por serigrafia. O método de pós-sinterização utilizando a cerâmica de transferência mostrou ser bastante reprodutível e produziu eletrodos totalmente planos, sem arqueamento. O gerador de microplasma foi instalado dentro de um reator RIE convencional e o microplasma foi gerado em DC e RF. A caracterização dos microplasmas de Ar, O2, N2 e He foi realizada por meio de curvas VxI, sonda dupla de Langmuir e espectroscopia de emissão óptica. Para descargas DC, em condições de baixa vazão de gás e elevada pressão, as curvas VxI mostraram três modos de descarga: catodo oco, normal e anormal. O efeito catodo oco foi evidenciado também pelos espectros de emissão óptica que mostraram raias na faixa de 300 a 450 nm, que indicam a presença de elétrons de alta energia. Essas raias foram mais fortemente evidenciadas em descargas RF. Temperaturas de elétrons elevadas, na faixa de 10 a 30 eV, foram obtidas através de medidas com a sonda dupla de Langmuir, nas condições em que o efeito catodo oco foi observado. A aplicabilidade do gerador de microplasma foi testada com foco no tratamento de superfície de polietileno e os resultados mostraram alta capacidade de redução do ângulo de contato e aumento da molhabilidade superficial, demonstrando, conseqüentemente, substancial modificação da energia de superfície do material, através desse processo a microplasma. / Microplasmas are plasmas generated in spaces with reduced dimensions, typically ranging from tens to hundreds of microns. The major advantage of a microplasma generator is the possibility of glow discharge generation with high plasma density and low power consumption at pressures higher than usually observed in conventional plasma reactors, reducing considerably the equipment cost. A novel structure of microplasma generator was developed in this work, using the LTCC technology. The device is composed of two silver-palladium parallel electrodes perforated by hundreds of microholes, constituting microchannels. The microplasma itself is formed between the electrodes and the plasma species are carried through the microchannels to reach the processing chamber, where they can interact with the samples to be treated. The presence of microholes can promote microhollow cathode effect. In the fabrication process, green tapes were micromachined by using a CNC and the electrodes were obtained by screen printing. The post-fire method using transfer tapes has demonstrated to be very reproducible and produced very flat electrodes. The microplasma generator was mounted into a conventional homemade reactive ion etching (RIE) reactor and driven by DC and RF power supply. Characterization of Ar, O2, N2 and He microplasmas was performed by means of VxI characteristics, double Langmuir probe and optical emission spectroscopy. For DC discharges, the VxI characteristics revealed three distinct regions: microhollow cathode mode, normal glow and abnormal glow, for low gas flow rate and high pressure conditions. The microhollow cathode effect was evidenced by optical emission that presented lines in wavelengths between 300 and 450 nm, indicating the presence of high energy electrons. These emission lines have shown to be more intense in RF discharges. Double Langmuir probe diagnostic showed high electron temperatures ranging from 10 and 30 eV, under the microhollow cathode effect conditions. The microplasma generator applicability was tested focusing on the surface treatment of polyethylene film. The results showed high efficiency of this process in reducing water contact angle and thus substantially increasing the polyethylene wettability, thus demonstrating effective modification of surface energy of the material. One can conclude that among other potential applications for material processing, the microplasma generator has already shown to be a reliable tool to modify the surface energy of materials.

Microplasmas são plasmas gerados em espaços com dimensões reduzidas, tipicamente, de dezenas a centenas de micrômetros. Apresentam como principal vantagem a possibilidade de se obter plasmas frios com densidades elevadas com baixo consumo de energia em pressões maiores do que em reatores convencionais, reduzindo sensivelmente o custo do equipamento. Um gerador de microplasma inédito foi desenvolvido neste trabalho, utilizando a tecnologia LTCC. O dispositivo é constituído por dois eletrodos paralelos de prata-paládio perfurados por centenas de microfuros, formando microcanais. O microplasma é gerado na região entre os eletrodos e é conduzido para fora do gerador através dos microcanais, constituindo um plasma remoto que pode interagir com a superfície de um material a ser processado. Os microfuros formam a estrutura de um microcatodo oco. Na fabricação, as camadas de cerâmica verde foram usinadas com uma máquina de CNC e os eletrodos foram obtidos por serigrafia. O método de pós-sinterização utilizando a cerâmica de transferência mostrou ser bastante reprodutível e produziu eletrodos totalmente planos, sem arqueamento. O gerador de microplasma foi instalado dentro de um reator RIE convencional e o microplasma foi gerado em DC e RF. A caracterização dos microplasmas de Ar, O2, N2 e He foi realizada por meio de curvas VxI, sonda dupla de Langmuir e espectroscopia de emissão óptica. Para descargas DC, em condições de baixa vazão de gás e elevada pressão, as curvas VxI mostraram três modos de descarga: catodo oco, normal e anormal. O efeito catodo oco foi evidenciado também pelos espectros de emissão óptica que mostraram raias na faixa de 300 a 450 nm, que indicam a presença de elétrons de alta energia. Essas raias foram mais fortemente evidenciadas em descargas RF. Temperaturas de elétrons elevadas, na faixa de 10 a 30 eV, foram obtidas através de medidas com a sonda dupla de Langmuir, nas condições em que o efeito catodo oco foi observado. A aplicabilidade do gerador de microplasma foi testada com foco no tratamento de superfície de polietileno e os resultados mostraram alta capacidade de redução do ângulo de contato e aumento da molhabilidade superficial, demonstrando, conseqüentemente, substancial modificação da energia de superfície do material, através desse processo a microplasma. / Microplasmas are plasmas generated in spaces with reduced dimensions, typically ranging from tens to hundreds of microns. The major advantage of a microplasma generator is the possibility of glow discharge generation with high plasma density and low power consumption at pressures higher than usually observed in conventional plasma reactors, reducing considerably the equipment cost. A novel structure of microplasma generator was developed in this work, using the LTCC technology. The device is composed of two silver-palladium parallel electrodes perforated by hundreds of microholes, constituting microchannels. The microplasma itself is formed between the electrodes and the plasma species are carried through the microchannels to reach the processing chamber, where they can interact with the samples to be treated. The presence of microholes can promote microhollow cathode effect. In the fabrication process, green tapes were micromachined by using a CNC and the electrodes were obtained by screen printing. The post-fire method using transfer tapes has demonstrated to be very reproducible and produced very flat electrodes. The microplasma generator was mounted into a conventional homemade reactive ion etching (RIE) reactor and driven by DC and RF power supply. Characterization of Ar, O2, N2 and He microplasmas was performed by means of VxI characteristics, double Langmuir probe and optical emission spectroscopy. For DC discharges, the VxI characteristics revealed three distinct regions: microhollow cathode mode, normal glow and abnormal glow, for low gas flow rate and high pressure conditions. The microhollow cathode effect was evidenced by optical emission that presented lines in wavelengths between 300 and 450 nm, indicating the presence of high energy electrons. These emission lines have shown to be more intense in RF discharges. Double Langmuir probe diagnostic showed high electron temperatures ranging from 10 and 30 eV, under the microhollow cathode effect conditions. The microplasma generator applicability was tested focusing on the surface treatment of polyethylene film. The results showed high efficiency of this process in reducing water contact angle and thus substantially increasing the polyethylene wettability, thus demonstrating effective modification of surface energy of the material. One can conclude that among other potential applications for material processing, the microplasma generator has already shown to be a reliable tool to modify the surface energy of materials.

Orientador: Nilson Cristino da Cruz / Banca: Mario Antonio Bica de Morais / Banca: Tersio Guilherme de Souza Cruz / O Programa de Pós-Graduação em Ciência e Tecnologia de Materiais, PosMat, tem caráter institucional e integra as atividades de pesquisa em materiais de diversos campi da Unesp / Resumo: A proteção de superfícies metálicas é um assunto de grande interesse científico e econômico. As vultosas quantias empregadas regularmente em manutenção e conservação motivam estudos para a obtenção de materiais com maior durabilidade e manutenção de seu aspecto estético. Neste trabalho é proposto o desenvolvimento de um dispositivo de geração de plasma via eletrólise e a investigação de sua aplicabilidade no aumento da resistência a corrosão da liga de alumínio 2024. A alteração da resistência à corrosão conferida pelo filme ao substrato foi investigada através de ensaios de névoa salina e de impedâncias eletroquímica e de polarização. A composição e a estrutura química dos revestimentos foram analisadas por espectroscopia de absorção no infravermelho. Perfilometria e o método de correntes parasitas foram empregados na determinação da espessura das camadas depositadas, enquanto alterações da molhabilidade das superfícies foram avaliadas por medidas de ângulo de contato. Os resultadeos mostram que, sob determinadas condições, o tratamento aumentou em cerca de 145 vezes, em comparação com substratos sem tratamento, a resistência das amostras a exposição à névoa salina. / Abstract: The protection of metallic surfaces is a subject of great scientific and economical interests. The huge amounts of money regularly employed in maintenance and conservation motivate investigations on the production of materials with larger durability, preserving the esthetic aspect. In this work, it is proposed the development of an electrolytic plasma device and the investigation of its applicability on the improvement of the resistance to corrosion of 2024 aluminum alloy coupons. Modifications in corrosion resistance conferred by the films to the substrates have been evaluated through salt spray tests and electrochemical and polarization impedances. Fourier infrared absorption spectroscopy has been employed to assess composition and chemical structure of the coatings. Layer thickness has been determined by prolilometry and the eddy current method, while modifications in surface wettability have been evaluated through contact angle measurements. It has been observed that, under certain experimental conditions, the treatments have enhanced the resistance to salt spray corrosion up to 145 times, as compared to the pristine substrates. / Mestre

No description available.

Made available in DSpace on 2014-06-11T19:23:29Z (GMT). No. of bitstreams: 0 Previous issue date: 2010-01-18Bitstream added on 2014-06-13T18:09:40Z : No. of bitstreams: 1 oliveira_cr_me_bauru.pdf: 3505566 bytes, checksum: 468c32f115403697e311aca50569dd5e (MD5) / A proteção de superfícies metálicas é um assunto de grande interesse científico e econômico. As vultosas quantias empregadas regularmente em manutenção e conservação motivam estudos para a obtenção de materiais com maior durabilidade e manutenção de seu aspecto estético. Neste trabalho é proposto o desenvolvimento de um dispositivo de geração de plasma via eletrólise e a investigação de sua aplicabilidade no aumento da resistência a corrosão da liga de alumínio 2024. A alteração da resistência à corrosão conferida pelo filme ao substrato foi investigada através de ensaios de névoa salina e de impedâncias eletroquímica e de polarização. A composição e a estrutura química dos revestimentos foram analisadas por espectroscopia de absorção no infravermelho. Perfilometria e o método de correntes parasitas foram empregados na determinação da espessura das camadas depositadas, enquanto alterações da molhabilidade das superfícies foram avaliadas por medidas de ângulo de contato. Os resultadeos mostram que, sob determinadas condições, o tratamento aumentou em cerca de 145 vezes, em comparação com substratos sem tratamento, a resistência das amostras a exposição à névoa salina. / The protection of metallic surfaces is a subject of great scientific and economical interests. The huge amounts of money regularly employed in maintenance and conservation motivate investigations on the production of materials with larger durability, preserving the esthetic aspect. In this work, it is proposed the development of an electrolytic plasma device and the investigation of its applicability on the improvement of the resistance to corrosion of 2024 aluminum alloy coupons. Modifications in corrosion resistance conferred by the films to the substrates have been evaluated through salt spray tests and electrochemical and polarization impedances. Fourier infrared absorption spectroscopy has been employed to assess composition and chemical structure of the coatings. Layer thickness has been determined by prolilometry and the eddy current method, while modifications in surface wettability have been evaluated through contact angle measurements. It has been observed that, under certain experimental conditions, the treatments have enhanced the resistance to salt spray corrosion up to 145 times, as compared to the pristine substrates.

L'objectif de cette thèse est de fournir une meilleure compréhension des différents phénomènes physiques liés aux microplasmas/microdécharges. Pour cela, des matrices de microréacteurs sur silicium ont été étudiées. De nombreuses configurations ont été construites de manière à analyser l’influence de chaque paramètre physique sur le fonctionnement de ces dispositifs. Le présent travail porte sur l'élaboration et la caractérisation de dispositifs micro-décharge à base de silicium. Dans ce travail de thèse, les régimes de courant continu (DC) et de courant alternatif (AC) sont étudiés en utilisant des configurations de décharges différentes. Pour la fabrication de ces réacteurs, nous sommes partis de wafers de Silicium que nous avons structurés et traités en salle blanche. La technologie de fabrication utilisée est compatible avec les méthodes de fabrication de dispositifs CMOS. Les microréacteurs sont constitués d’électrodes de nickel et de silicium séparés par une couche diélectrique de SiO2 de 6 μm d’épaisseur. L’épaisseur du diélectrique est ici beaucoup plus faible que celle des microréacteurs étudiés jusqu’à présent. Les dispositifs sont constitués de cavités de 25 à 150 microns de diamètre. Les essais de microdécharge ont été effectués dans des gaz inertes à une pression comprise entre 100 et 1000 Torrs. Nous avons d’abord étudié les phénomènes d’allumage et d’extinction à partir de microdispositifs monocavité en alumine. Puis, nous avons étudié le fonctionnement en DC/AC de microréacteurs en silicium comportant un nombre de cavité compris entre 1 et1024. Les caractéristiques des microdécharges ont été étudiées grâce à des mesures électriques, des mesures de spectroscopie d'émission optique (OES), de spectroscopie d’absorption à diode laser (DLAS) et de spectroscopie d'émission optique résolue en temps (PROES). Ces différents diagnostics nous ont permis de mettre en évidence les phénomènes d’allumage, d’extinction, d’instabilité et les mécanismes de défaillance de nos microdispositifs. Ce travail de thèse a permis de tester les performances et les limites technologiques des matrices de microdécharges sur silicium. Une attention particulière a été portée sur leur durée de vie. / The objective of this thesis is to provide a better understanding of various physical phenomena related to microplasmas/microdischarges. For this purpose, arrays of microreactors on silicon were studied. Different array configurations were fabricated to analyse the influence of each parameter on the physical operation of these devices. The present work focuses on the development and characterisation of micro-discharge devices based on silicon. In this thesis, direct current (DC) and alternating current (AC) regimes are studied using different discharge configurations. For the fabrication of these reactors, Silicon wafers are structured and processed in a cleanroom. Fabrication technology used is compatible with the CMOS technology. The microreactors are fabricated with nickel and silicon electrodes, separated by a dielectric layer of SiO2 with a thickness of 6 μm. The thickness of the dielectric is much lower here than the microreactors studied so far. The devices consist of cavities with 25 to 150 μm in diameter. Experiments of the microdischarges are performed in inert gases at a pressure between 100 and 1000 Torr. We first studied the phenomena of ignition and extinction for the microdevices based on alumina. Then, we studied the microreactors based on silicon containing 1 to 1024 cavities under DC and AC regimes. Characteristics of microdischarges were studied by electrical measurements, measurements of optical emission spectroscopy (OES), laser diode absorption spectroscopy (DLAS) and phase resolved optical emission spectroscopy (PROES). These diagnostics allowed us to investigate the phenomena of ignition, extinction, instability and failure mechanisms of the microplasma devices. This thesis work allowed testing the performance and technological limitations of the silicon based microdischarge arrays. Particular attention was paid to their life time.

The objective of this thesis is to provide a better understanding of various physical phenomena related to microplasmas/microdischarges. For this purpose, arrays of microreactors on silicon were studied. Different array configurations were fabricated to analyse the influence of each parameter on the physical operation of these devices. The present work focuses on the development and characterisation of micro-discharge devices based on silicon. In this thesis, direct current (DC) and alternating current (AC) regimes are studied using different discharge configurations. For the fabrication of these reactors, Silicon wafers are structured and processed in a cleanroom. Fabrication technology used is compatible with the CMOS technology. The microreactors are fabricated with nickel and silicon electrodes, separated by a dielectric layer of SiO2 with a thickness of 6 μm. The thickness of the dielectric is much lower here than the microreactors studied so far. The devices consist of cavities with 25 to 150 μm in diameter. Experiments of the microdischarges are performed in inert gases at a pressure between 100 and 1000 Torr. We first studied the phenomena of ignition and extinction for the microdevices based on alumina. Then, we studied the microreactors based on silicon containing 1 to 1024 cavities under DC and AC regimes. Characteristics of microdischarges were studied by electrical measurements, measurements of optical emission spectroscopy (OES), laser diode absorption spectroscopy (DLAS) and phase resolved optical emission spectroscopy (PROES). These diagnostics allowed us to investigate the phenomena of ignition, extinction, instability and failure mechanisms of the microplasma devices. This thesis work allowed testing the performance and technological limitations of the silicon based microdischarge arrays. Particular attention was paid to their life time.