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Cette thèse présente la conception d'un microgyromètre MEMS triaxial. Les microgyromètres ont de nombreuses applications telles que le contrôle d'attitude de drones ou l'interfaces homme/machine. Les microgyromètres triaxiaux sont particulièrement avantageux car ils permettent de déterminer les trois composantes de la vitesse de rotation à partir d'un seule structure monolithique et planaire. Le principe de fonctionnement des gyromètres vibrants à effet Coriolis (CVG) a été étudié analytiquement, puis une structure originale de gyromètre triaxial monolithique et planaire a été conçue. Cette structure est constituée de quatre poutres encastrées sur un cadre déformable. Des prototypes en silicium ont été réalisés et caractérisés. L’arséniure de gallium (GaAs) a été sélectionné pour la réalisation en raison de ses propriétés piézoélectriques et de son fort potentiel de miniaturisation. Un système d’électrodes pour l'excitation et la détection des vibrations mécaniques a été mis au point. Deux procédés d'usinage du GaAs ont été développés, un procédé de gravure chimique et un procédé de gravure plasma permettant tous les deux de graver verticalement le GaAs sur 450 micromètres de profondeur. Le procédé de gravure plasma est compatible avec la réalisation du CVG triaxial. Des résonateurs de test en GaAs dopé Carbone ont été réalisés par gravure chimique pour mesurer l'évolution en température de la résistivité et des propriétés électromécaniques de ce matériau. Ces mesures ont permis d'estimer que les marches aléatoires angulaires du CVG triaxial sont inférieures à 0,025 degré par racine d'heure sur la gamme de température [-40°C +80°C] pour les trois axes de mesure. Ceci situe le potentiel du CVG triaxial conçu parmi les CVG MEMS les plus performants. / This PhD present the conception of a triaxial MEMS microgyro. Microgyros offer a wide range of applications varying from drones attitude control to human interface devices. The triaxial microgyros offer great benefits because they allow determination of the three rotation rate components with only one monolithic planar structure. The operating principle of Coriolis Vibrating Gyro (CVG) has been studied analytically and an original structure has been designed. This structure consists of four beam clamped into a deformable frame. Some silicon prototypes have been machined and characterised. The gallium arsenide (GaAs) has been chosen for the realisation because of its piezoelectric properties and its great miniaturization potential. A transduction system based on GaAs piezoelectricity was developed. Two GaAs machining processes have been developed: a chemical etching process and a plasma etching process which both enable 450 micrometers deep vertical etching. The plasma etching technique allows high fidelity enough machining to be compatible with the triaxial CVG realisation. Some C-doped GaAs test resonators have been realised to measure the resistivity temperature dependency and electromechanical properties of this material. Those characterisations lead to estimate the angular random walk for the three axis ranges below 0,025 degree per square root hour on the temperature range [-40°C +80°C]. This sets the triaxial CVG together with the best monoaxial MEMS CVG.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico / In this work, different sample preparation procedures for determining inorganic (in Hg2+ form) and organic mercury (in methylmercury form CH3Hg+) in edible mushrooms were evaluated. Conventional, microwave (MW) and ultrasound (US) assisted extractions combined with water, hydrochloric acid and L-cysteine solutions were tested. Liquid chromatography-chemical vapor generation-inductively coupled plasma mass spectrometry (LC-CVG-ICP-MS) was used for Hg species determination. Total Hg was determined by CVG-ICP-MS after sample decomposition. The influence of the main parameters on Hg species extraction, such as extraction solutions concentration, temperature, US amplitude and extraction time were investigated. Hg species conversion was observed in all conditions when HCl was used as extractor medium. Besides, Hg species extraction from the samples is not quantitative. No Hg species conversion was observed when water and 1.0% (m/v) L-cysteine solution were used. However, the extractions were not quantitative when water was used. Quantitative extractions were obtained only when 1.0% (m/v) L-cysteine was used as extraction solution for conventional and US assisted extractions. The optimized conditions for these procedures (US 20% for 1 min and conventional extraction for 12 h at 25 °C) provided extraction efficiencies higher than 86% for the sum of the Hg species, while only up to 88% of the Hg species were extracted when MW heating was used. The relative standard deviation (RSD) is lower than 8.0 and 13% for Hg2+ and CH3Hg+, respectively. Detection limits for US, MW and conventional extractions (using L-cysteine) were 0.41 and 0.35 ng g-1, 0.64 and 0.90 ng g-1, and 1.41 and 0.11 ng g-1 for Hg2+ and CH3Hg+, respectively. The procedures were evaluated using analyte recovery tests of Hg species and by analysis of certified reference material (DOLT-3). Recoveries in the range of 89 to 109% for Hg2+ and 96 to 113% for CH3Hg+ were obtained. The agreement of the obtained results for DOLT-3 were in the range of 88 to 93% for CH3Hg+ and 95 to 102% for total Hg, respectively. US assisted extraction was considered simpler and faster than the other procedures, being more suitable for Hg species extraction from edible mushrooms. / Neste trabalho foram avaliados diferentes procedimentos de preparo de amostra de cogumelo comestível para a determinação de espécies de mercúrio inorgânico (na forma de Hg2+) e orgânico (na forma de metilmercúrio - CH3Hg+). Para isso, foram avaliadas a extração convencional, a radiação micro-ondas (MW) e o ultrassom (US), combinados com diversos meios extratores (água, soluções de ácido clorídrico e L-cisteína). A cromatografia a líquido com geração de vapor químico acoplado a espectrometria de massa com plasma indutivamente acoplado (LC-CVG-ICP-MS) foi usada para a determinação das espécies de Hg. O Hg total foi determinado por CVG-ICP-MS. A influência dos principais parâmetros envolvidos na extração das espécies de Hg, como a concentração das soluções extratoras, a temperatura na extração por MW, a amplitude de US e o tempo de extração foram investigados. A conversão das espécies de Hg foi observada em todas as condições, quando o HCl foi usado como meio extrator, além de que essas soluções não possibilitaram extrair quantitativamente o Hg das amostras. Entretanto, não foi observada conversão das espécies de Hg em água e na solução de L-cisteína 1,0% (m/v), porém as extrações não foram quantitativas quando a água foi usada como meio extrator. Extrações quantitativas foram obtidas quando L-cisteína 1,0% (m/v) foi usada para os procedimentos de extração convencional e assistida por US. As condições otimizadas para esses procedimentos (US 20% por 1 min e extração convencional por 12 h a 25 °C) proporcionaram efici ências de extração superiores a 86% para a soma das espécies de Hg, com desvio padrão relativo (RSD) menor que 8,0 e 13% para Hg2+ e CH3Hg+, respectivamente. Por outro lado, as extrações assistidas por MW não tiveram eficiências de extração satisfatórias, uma vez que a eficiência máxima obtida foi de 88% para a soma das espécies de Hg. Os limites de detecção obtidos para os procedimentos empregando US, MW e extração convencional foram 0,41 e 0,35 ng g-1, 0,64 e 0,90 ng g-1, e 1,41 e 0,11 ng g-1, para Hg2+ e CH3Hg+, respectivamente. Os procedimentos de extração foram avaliados através de ensaios de recuperação das espécies de Hg, sendo que os mesmos ficaram na faixa de 89 a 109% para Hg2+ e 96 a 113% para CH3Hg+. A exatidão foi avaliada pela análise de material de referência certificado (DOLT-3), cuja concordância dos resultados obtidos em relação aos valores certificados ficou na faixa de 88 a 93% para CH3Hg+ e 95 a 102% para Hg total, respectivamente. A extração assistida por US foi considerada mais simples e rápida que os demais procedimentos, sendo, portanto, mais adequada para a extração das espécies de Hg em cogumelos comestíveis.

Cette thèse présente la conception d'un microgyromètre MEMS triaxial. Les microgyromètres ont de nombreuses applications telles que le contrôle d'attitude de drones ou l'interfaces homme/machine. Les microgyromètres triaxiaux sont particulièrement avantageux car ils permettent de déterminer les trois composantes de la vitesse de rotation à partir d'un seule structure monolithique et planaire. Le principe de fonctionnement des gyromètres vibrants à effet Coriolis (CVG) a été étudié analytiquement, puis une structure originale de gyromètre triaxial monolithique et planaire a été conçue. Cette structure est constituée de quatre poutres encastrées sur un cadre déformable. Des prototypes en silicium ont été réalisés et caractérisés. L'arséniure de gallium (GaAs) a été sélectionné pour la réalisation en raison de ses propriétés piézoélectriques et de son fort potentiel de miniaturisation. Un système d'électrodes pour l'excitation et la détection des vibrations mécaniques a été mis au point. Deux procédés d'usinage du GaAs ont été développés, un procédé de gravure chimique et un procédé de gravure plasma permettant tous les deux de graver verticalement le GaAs sur 450 micromètres de profondeur. Le procédé de gravure plasma est compatible avec la réalisation du CVG triaxial. Des résonateurs de test en GaAs dopé Carbone ont été réalisés par gravure chimique pour mesurer l'évolution en température de la résistivité et des propriétés électromécaniques de ce matériau. Ces mesures ont permis d'estimer que les marches aléatoires angulaires du CVG triaxial sont inférieures à 0,025 degré par racine d'heure sur la gamme de température [-40°C +80°C] pour les trois axes de mesure. Ceci situe le potentiel du CVG triaxial conçu parmi les CVG MEMS les plus performants.

Gyroscopes are inertial sensors that measure the rate or angle of rotation. One of the most promising technologies for reaching a high-performance MEMS gyroscope has been development of the micro-hemispherical shell resonator. (μHSR) This thesis presents the electronic control and read-out interface that has been developed to turn the μHSR into a fully functional micro-hemispherical resonating gyroscope (μHRG) capable of measuring the rate of rotation. First, the μHSR was characterized, which both enabled the design of the interface and led to new insights into the linearity and feed-through characteristics of the μHSR. Then a detailed analysis of the rate mode interface including calculations and simulations was performed. This interface was then implemented on custom printed circuit boards for both the analog front-end and analog back-end, along with a custom on-board vacuum chamber and chassis to house the μHSR and interface electronics. Finally the performance of the rate mode gyroscope interface was characterized, showing a linear scale factor of 8.57 mv/deg/s, an angle random walk (ARW) of 34 deg/sqrt(hr) and a bias instability of 330 deg/hr.