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Single-Chip Scanning Probe MicroscopesSarkar, Niladri January 2013 (has links)
Scanning probe microscopes (SPMs) are the highest resolution imaging instruments available today and are among the most important tools in nanoscience. Conventional SPMs suffer from several drawbacks owing to their large and bulky construction and to the use of piezoelectric materials. Large scanners have low resonant frequencies that limit their achievable imaging bandwidth and render them susceptible to disturbance from ambient vibrations. Array approaches have been used to alleviate the bandwidth bottleneck; however as arrays are scaled upwards, the scanning speed must decline to accommodate larger payloads. In addition, the long mechanical path from the tip to the sample contributes thermal drift. Furthermore, intrinsic properties of piezoelectric materials result in creep and hysteresis, which contribute to image distortion. The tip-sample interaction signals are often measured with optical configurations that require large free-space paths, are cumbersome to align, and add to the high cost of state-of-the-art SPM systems. These shortcomings have stifled the widespread adoption of SPMs by the nanometrology community. Tiny, inexpensive, fast, stable and independent SPMs that do not incur bandwidth penalties upon array scaling would therefore be most welcome.
The present research demonstrates, for the first time, that all of the mechanical and electrical components that are required for the SPM to capture an image can be scaled and integrated onto a single CMOS chip. Principles of microsystem design are applied to produce single-chip instruments that acquire images of underlying samples on their own, without the need for off-chip scanners or sensors. Furthermore, it is shown that the instruments enjoy a multitude of performance benefits that stem from CMOS-MEMS integration and volumetric scaling of scanners by a factor of 1 million.
This dissertation details the design, fabrication and imaging results of the first single-chip contact-mode AFMs, with integrated piezoresistive strain sensing cantilevers and scanning in three degrees-of-freedom (DOFs). Static AFMs and quasi-static AFMs are both reported.
This work also includes the development, fabrication and imaging results of the first single-chip dynamic AFMs, with integrated flexural resonant cantilevers and 3 DOF scanning. Single-chip Amplitude Modulation AFMs (AM-AFMs) and Frequency Modulation AFMs (FM-AFMs) are both shown to be capable of imaging samples without the need for any off-chip sensors or actuators.
A method to increase the quality factor (Q-factor) of flexural resonators is introduced. The method relies on an internal energy pumping mechanism that is based on the interplay between electrical, mechanical, and thermal effects. To the best of the author???s knowledge, the devices that are designed to harness these effects possess the highest electromechanical Qs reported for flexural resonators operating in air; electrically measured Q is enhanced from ~50 to ~50,000 in one exemplary device. A physical explanation for the underlying mechanism is proposed.
The design, fabrication, imaging, and tip-based lithographic patterning with the first single-chip Scanning Thermal Microscopes (SThMs) are also presented. In addition to 3 DOF scanning, these devices possess integrated, thermally isolated temperature sensors to detect heat transfer in the tip-sample region. Imaging is reported with thermocouple-based devices and patterning is reported with resistive heater/sensors.
An ???isothermal electrothermal scanner??? is designed and fabricated, and a method to operate it is detailed. The mechanism, based on electrothermal actuation, maintains a constant temperature in a central location while positioning a payload over a range of >35??m, thereby suppressing the deleterious thermal crosstalk effects that have thus far plagued thermally actuated devices with integrated sensors.
In the thesis, models are developed to guide the design of single-chip SPMs and to provide an interpretation of experimental results. The modelling efforts include lumped element model development for each component of single-chip SPMs in the electrical, thermal and mechanical domains. In addition, noise models are developed for various components of the instruments, including temperature-based position sensors, piezoresistive cantilevers, and digitally controlled positioning devices.
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Construção de um espectrômetro de absorção atômica e estudos de formação e evolução da nuvem atômica com atomização eletrotérmica em sistema de duplo filamento de tungstênio / Construction of an atomic absorption spectrometer and studies on the formation and evolution of the atomic cloud with electrothermal atomization in a double tungsten coil systemJora, Manassés Zuliani, 1987- 25 August 2018 (has links)
Orientadores: Celio Pasquini, Joaquim de Araújo Nóbrega / Dissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Química / Made available in DSpace on 2018-08-25T12:04:34Z (GMT). No. of bitstreams: 1
Jora_ManassesZuliani_M.pdf: 4929889 bytes, checksum: f8da5d6a35fbac5ae2d05d997971561a (MD5)
Previous issue date: 2013 / Resumo: A espectrometria de absorção atômica com atomização eletrotérmica (ET AAS) é adequada para a determinação de metais e semimetais, apresentando alta sensibilidade. Dentre os atomizadores eletrotérmicos, os fornos de grafite destacam-se por sua boa seletividade, exigência de pequenos volumes de amostra e baixos limites de detecção (i.e. 'mu'g L-1). Porém, esses atomizadores requerem fontes de alta potência (i.e. superiores a 2 kW), sistema de resfriamento e, ainda, apresentam alto custo. Como alternativa, o uso de superfícies metálicas têm sido objeto de pesquisa desde 1970. Dentre todos os metais empregados na fabricação de superfícies metálicas e utilizados para os estudos em ET AAS, o tungstênio é o que vem apresentando maior aplicação. Porém, a espectrometria de absorção atômica baseada em atomizadores de filamento de tungstênio (WC AAS) apresenta vários desafios relacionados ao entendimento da geração da nuvem atômica e dos efeitos de interferência observados. Dessa maneira, neste trabalho construiu-se um espectrômetro de absorção atômica com duplo filamento de tungstênio (DWC AAS), com duas configurações, uma empregando como sistema de detecção um sistema echelle/detector de carga acoplada intensificado (ICCD) e outra um sistema filtro óptico-acústico sintonizável (AOTF)/fotomultiplicadora. Essas duas configurações do equipamento foram empregadas em estudos de formação e evolução da nuvem atômica de elementos com características voláteis e refratárias (i.e. Pb e Cr). Além disso, estudou-se o efeito de Na, K, Ca e Mg, em três diferentes concentrações (i.e. 1, 10 e 100 mg L-1) sobre os perfis das nuvens atômicas de Pb e Cr. Esse estudo foi conduzido de tal forma que interferências em fase condensada e gasosa puderam ser avaliadas. Além disso, o equipamento foi empregado em medidas de temperatura na superfície do filamento e na fase gasosa / Abstract: Electrothermal atomic absorption spectrometry (ET AAS) is suitable for determination of metals and semimetals with high sensitivity. Among the existing electrothermal atomizers, graphite furnace stands out due to its selectivity, requirement of low volume of sample and low limits of detection (i.e. 'mu'g L-1). Notwithstanding, these atomizers present high cost and requires high power power supply (i.e. above 2 kW) and a cooling system. Alternatively, metallic surfaces have been studied since 1970. Among all metals employed as atomizers in ET AAS studies, tungsten has presented the best results and has found many analytical applications. However, tungsten coil atomic absorption spectrometry (WC AAS) presents several challenges related to understanding the atomic cloud generation and interferences effects. Thus, in this work, a double tungsten coil atomic absorption spectrometer (DWC AAS), with two different configurations was constructed. In one configuration, a detection system based on echelle/intensified charge-coupled device (ICCD) is employed and, in the other, an acousto-optic tunable filter (AOTF)/photomultiplier detection system is used. Both configurations were employed in the atomic cloud generation and evolution studies of Pb and Cr. Furthermore, interferences on the atomic cloud profile of Pb and Cr caused by Na, K, Ca and Mg, at three different concentrations (i.e. 1, 10 and 100 mg L-1), were studied. This study helped to evaluate the effect of condensed and gas phase interferences. Additionally, the equipment was employed to perform measures of surface and gas phase temperatures / Mestrado / Quimica Analitica / Mestre em Química
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Wide Bandgap Semiconductor Components Integration in a PCB Substrate for the Development of a High Density Power Electronics Converter / Intégration dans un substrat PCB de composants à semi-conducteur grand gap pour le développement d’un convertisseur d’électronique de puissance à forte densitéZhang, Shuangfeng 30 November 2018 (has links)
Les nouveaux composants à semi-conducteur de type grand gap ont été développés pour des applications de conversion de puissance en raison de leurs hautes fréquences de commutation (de centaine kHz à quelques MHz) et pertes faibles. Afin de bien profiter ses avantages, la technologie des circuits imprimés (PCB) est intéressante pour une intégration à haute densité de puissance grâce à sa flexibilité et son faible coût. Cependant, à cause de la mauvaise conductivité thermique du matériau FR-4 utilisé pour le substrat PCB et la haute densité de puissance réalisée, il est primordial de trouver des solutions thermiques pour améliorer les performances thermiques de la structure de PCB. Dans cette thèse, trois solutions thermiques pour les structures de PCB ont été proposées, y compris des solutions avec des vias thermiques, de cuivre épais sur le substrat de PCB ainsi que des dispositifs de refroidissement thermoélectrique (TEC). Nos études sont basées sur la modélisation électrothermique et la méthode d’éléments finis en 3D. Tout d’abord, l’optimisation des paramètres des vias (diamètre, épaisseur de placage, surface formée par des vias, la distance entre des vias etc.) a été réalisée pour optimiser l’effet de refroidissement. Ensuite, on constate que les performances thermiques des structures de PCB peuvent être améliorées en utilisant cuivre épais sur le substrat de PCB. Cuivre épais augmente le flux thermique latéral dans la couche de cuivre. Les influences de l’épaisseur de cuivre (35 à 500 µm) ont été étudiées. Cette solution est facile à réaliser et peut être combinée à d’autres solutions de refroidissement. Enfin, le dispositif thermoélectrique comme les modules Peltier est une technologie de refroidissement local. Les influences des paramètres de Peltier (Propriétés du matériau thermoélectrique, nombre d’éléments Peltier, distance entre la source de chaleur et les dispositifs Peltier, etc.) ont été identifiées. Il est démontré que des modules Peltier ont l’application potentielle pour le développement d’intégration de PCB attendu que son active contrôle des températures. / The emerging wide bandgap (WBG) semiconductor devices have been developed for power conversion applications instead of silicon devices due to higher switching frequencies (from few 100 kHz to several MHz) and lower on-state losses resulting in a better efficiency. In order to take full advantage of the WBG components, PCB technology is attractive for high power density integration thanks to its flexibility and low cost. However, due to poor thermal conductivity of the commonly used material Flame Retardant-4 (FR4), efficient thermal solutions are becoming a challenging issue in integrated power boards based on PCB substrates. So it is of the first importance to seek technological means in order to improve the thermal performances. In this thesis, three main thermal management solutions for PCB structures have been investigated including thermal vias, thick copper thickness on the PCB substrate as well as thermoelectric cooling (TEC) devices. Our studies are based on the electro-thermal modeling and 3D finite element (FE) methods. Firstly, optimization of the thermal via parameters (via diameter, via plating thickness, via-cluster surface, via pattern, pitch distance between vias etc.) has been realized to improve their cooing performances. We presented and evaluated thermal performances of the PCB structures by analyzing the thermal resistance of the PCB substrate with different thermal vias. Secondly, it is found that thermal performances of the PCB structures can be enhanced by using thick copper thickness on top of the PCB substrate, which increases the lateral heat flux along the copper layer. Influences of the copper thickness (35 µm to 500 µm) has been discussed. This solution is easy to realize and can be combined with other cooling solutions. Thirdly, thermoelectric cooler like Peltier device is a solid-state cooling technology that can meet the local cooling requirements. Influences of Peltier parameters (Thermoelectric material properties, number of Peltier elements, distance between the heating source and the Peltier devices etc.) have been identified. All these analyses demonstrate the potential application of Peltier devices placed beside the heating source for PCB structures, which is a benefit for developing the embedding technology in such structures.
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Electrokinetic Manipulation and Electrochemical Detection of Bacteria and Development of Hot-Square-wave VoltammetryFrkonja-Kuczin, Ariana 25 August 2020 (has links)
No description available.
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Design of Optical Measurements for Electrothermal Plasma DischargesHamer, Matthew David 23 June 2014 (has links)
Ablation controlled electrothermal (ET) plasma discharge devices consist of a small diameter capillary through which a large amount of energy is discharged. The high energy in the discharge ablates an inner sleeve material, ionizes the material, and a high energy-density plasma jet accelerates out the open end. ET devices can find applications in internal combustion engines, Tokamak fusion fueling and stabilization, hypervelocity launchers, and propulsion. The ballistic properties of an ET device are highly dependent on the propellant and ablated material. A useful noninvasive technique to characterize a propellant in these types of devices is spectroscopy. The purpose of this study is to design and conduct experiments on the ET facility called PIPE to verify results and assumptions in the ETFLOW simulation code as well as resolve data collection issues such as equipment triggering as spectrometer saturation. Experiments are carried out using an Ocean Optics LIBS2500plus high resolution spectrometer and a Photron FASTCAM SA4 high speed camera. Electron plasma temperatures are estimated using copper peaks in the UV region with the relative line intensity method, and electron plasma density is estimated by measuring the full width at half maximum (FWHM) of the stark broadened H--β line at 486 nm. Electron temperatures between 0.19 eV and 0.49 eV, and electron densities between 4.68*1022 m-3 and 5.75*10²² m⁻³ were measured in the expanding plasma jet about an inch outside the source with values as expected for this region. Velocity measurements of PIPE match well with simulations at around 5333 m/s. This study concluded that the assumption that the propellant Lexan is completely dissociated is a valid assumption, and that the ETFLOW results for electron temperature, density, and bulk plasma velocity match experimental values. / Master of Science
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Caractérisation de l'endommagement de composants électroniques de puissance soumis à des tests de vieillissement accéléré / Characterization of alterations on power electronic devices subjected to accelerated ageing testsMartineau, Donatien 17 March 2011 (has links)
L’intégration des dispositifs électroniques de puissance dans les véhicules automobiles nécessite une connaissance approfondie de leur fiabilité. Ces éléments sont soumis à des contraintes de fatigue électrothermique de plus en plus importantes. Cette étude vise à caractériser l’évolution de composants à base de MOSFET lors de tests de fatigue accélérés et contrôlés afin de déterminer les mécanismes physiques qui conduisent à sa dégradation.Nous décrivons d'abord l’évolution technologique des composants électroniques de puissance jusqu’à la technologie de type SmartMos utilisée par Freescale Semiconductor aujourd'hui. Les outils de caractérisation microstructurale (SAM, SAT, SEM, SIM, TEM, …) sont ensuite détaillés ainsi que l'échelle spécifique pour laquelle ils sont utilisés.Le vieillissement accéléré des composants est effectué sur un banc de fatigue pour déterminer la durée de vie d'un composant selon des paramètres donnés. L'analyse complète des composants détruits a permis de conclure que la zone affectée en priorité par le cyclage électro-thermique est le métal source qui comprend la métallisation en aluminium et les fils d'amenée de courants. Ces mêmes zones sont ensuite examinées après un vieillissement contrôlé correspondant à une fraction de la durée de vie. La fatigue du composant est essentiellement caractérisée par une forte augmentation de la résistance du métal source qui engendre l’augmentation de sa résistance drain-source (RdsON). Nous avons expliqué ce phénomène par une dégradation de la métallisation qui consiste en une division des grains d'aluminium et à l’apparition de fissures le long des joints de grains.Ces caractérisations sont corrélées à une étude par éléments finis (FEM) qui permet de simuler l’augmentation et le gradient de température dans un composant pendant un cycle de vieillissement, ainsi que l’impact de l’élévation de la résistance de la métallisation source sur le comportement thermoélectrique du composant / Integration of power electronic devices in automotive applications requires a perfect knowledge of their reliability as these components are subjected to more drastic electrothermal stresses. This study aims at determining the physical mechanisms responsible for degradation and failure of modern MOSFET-based power microprocessors during accelerated and controlled fatigue tests.After a description of the recent developments in power electronics that led to today's SmartMos technology from Freescale Semiconductor, the different microstructural characterizing techniques (SAM, SAT, SEM, SIM, TEM, …) and the specific scale for which they are used are detailed.The accelerated ageing of the components were carried out on a fatigue bench to evaluate the component lifetime according to parameters such as the temperature, current and pulse durations. A complete analysis of failed components showed that the area which is primarily affected by the electro-thermal cycling is the metal source that includes aluminum metallization and connection wires. In controlled ageing tests, we showed that the drain-source resistance (Rdson) increase was due to the metal source resistance augmentation. This phenomenon is linked to the degradation of the Aluminum layer that happens through grains division and crack propagation along the grain boundaries
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Avaliação da espectrometria de absorção atômica com atomização eletrotérmica em filamento de tungstênio para determinação de arsênio em águas / Evaluation of eletrothermal atomic absorption spectrometry with tungsten coil for the direct determination of arsenic in watersAntonio, Rosana Fernandes 19 September 2008 (has links)
A determinação direta de arsênio total em águas por espectrometria de absorção atômica com filamentos de tungstênio (150 W) modificados quimicamente com irídio ou ródio, representa uma alternativa para a atomização eletrotérmica de arsênio, que foi avaliada na presente dissertação. A utilização do revestimento com Ir como modificador químico proporcionou um aumento da massa característica de arsênio de 3,5 vezes. As medidas foram feitas com altura de observação selecionada para proporcionar a melhor razão sinal/ruído sem diminuir a sensibilidade do sinal analítico. Avaliaram-se dois programas de aquecimento: com temperatura de secagem constante (com diminuição gradativa da tensão aplicada) e com temperatura de secagem variável (com tensão aplicada de maneira constante). Não houve diferença na sensibilidade entre os dois programas estudados, indicando que a modificação química leva à formação de um precursor atômico com estabilidade térmica elevada. De fato, utilizando-se a modificação química permanente com 1000 müg Ir, e adotando-se programa de aquecimento com temperatura de secagem variável, a temperatura máxima de pirólise foi de aproximadamente 1700 °C ( temperatura de atomização de 2700 °C). Avaliou-se o comportamento eletrotérmico do As na presença dos concomitantes Na, K, Ca e Mg em 0,1% v/v HNO3. Interferências mais severas foram observadas na presença de cálcio acima de 10 \'mü\'g l-1, e acima de 100 \'mü\'g l-1 para os demais concomitantes. As interferências podem estar relacionadas com o elevado gradiente de temperatura entre a superfície do filamento e a fase gasosa do volume de observação, ou mesmo devido à formação de compostos refratários, particularmente para Ca e Mg, na fase condensada, ou seja, na superfície do atomizador. O emprego do método das médias móveis no tratamento dos sinais transientes gerados na atomização do arsênio também foi avaliada. Com o filamento posicionado na altura de observação 2 mm, foram utilizados os fatores 0, 3, 5, 7 e 9, observando-se melhora considerável nos limites de detecção instrumental e do método,utilizando-se média móvel com fator 7. Nestas condições, e depositando-se 20 \'mü\'l de amostra sobre o filamento, o limite de detecção foi de 3,2 \'mü\'g l-1 As e a massa característica de 37,0 pg As. A exatidão foi avaliada analisando-se diferentes amostras de águas provenientes da região do Quadrilátero Ferrífero do Estado de Minas Gerais, por espectrometria de fluorescência atômica com geração de hidretos e por espectrometria de absorção atômica com o filamento de tungstênio modificado com Ir. A comparação dos resultados mostrou que o método proposto pode ser utilizado para o controle de qualidade de águas desta região. Aproximadamente 150 queimas podem ser feitas com um único filamento de tungstênio / The direct determination of arsenic in waters by atomic absorption spectrometry with 150 W tungsten coils, treated with Ir or Rh, was evaluated as a possible alternative for the eletrothermal atomization of As. The use of iridium as a permanent chemical modifier did improve the characteristic mass of arsenic by 3.5 fold. Measurements were made by choosing an appropriate observation height in order to get the best signal to noise ratio. Two heating programs were tested, either by keeping the applied voltage constant or by using an inverted voltage ramp during the drying step. There were no significant differences in the sensitivities between both heating programs, indicating that the permanent modification lead to the formation of an atomic precursor of high thermal stability. Indeed, with the permanent chemical modification with 1000 \'mü\'g Ir, the maximum pyrolysis temperature was approximately 1700 °C (atomization temperature 2700 °C), allowing a heating program with temperature variation during the drying step. Method selectivity was carried out by evaluating the eletrothermal behavior of As in the presence of up to 1000 \'mü\'g l-1 Na, K, Ca and/or Mg in 0,1% v/v HNO3. The most serious interferences were observed with Ca in concentrations higher than 10 \'mü\'g l-1 and when the concentrations were higher than 100 \'mü\'g l-1 for Na, K or Mg, which can be attributed either to the gradient of temperature between the surface of the atomizer and the observation volume or to the formation of refractory compounds in the condensed phase, particularly with Ca and Mg. The absorbance transient signals treatment by the method of moving averages up to factor 9 was also evaluated, with a remarkable improvement in the instrumental and method detection limits. With the center of the observation volume 2 mm above the tungsten coil surface, and a moving average of factor 7, the limit of detection was 3,2 \'müg\' l-1 As and the characteristic mass 37,0 pg As. Accuracy was evaluate by analysing water samples collected in a contaminated area from the Quadrilátero Ferrífero, Minas Gerais State, by hydride generation atomic fluorescence spectrometry and by tungsten coil eletrothermal atomic absorption spectrometry. Results showed that the proposed method fits for the purpose of CONAMA 357 regulation for drinking water quality in the aforementioned contaminated area. Approximately 150 firings can be done with a single tungsten coil atomizer by using 20 \'mü\'l sample volume
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Applications de la vaporisation électrothermique couplée à la technique ICP-AES pour la détermination élémentaire dans les végétaux : une stratégie permettant l’analyse directe des échantillons à l’état solide / Application of the electrothermal vaporization method coupled with simultaneous inductively coupled plasma atomic emission spectrometry for the elemental determinations in plant samples : A strategy for the direct analysis of samples in the solid state.Masson, Pierre 19 May 2014 (has links)
Parmi les systèmes dédiés à l’analyse directe des solides, la vaporisation électrothermique occupe une place de choix. Elle offre plusieurs avantages. Le temps de préparation des échantillons est considérablement réduit. Il n’y a pas de dilution induite par la minéralisation et les risques de pertes ou de contaminations durant cette étape sont éliminés. Son principe de fonctionnement consiste à transformer, par chauffage, quelques milligrammes d’échantillon en un aérosol, qui est ensuite transporté dans un spectromètre d’émission atomique par plasma à couplage inductif, où la composition élémentaire est mesurée. Une première étude fondamentale a permis de mieux comprendre la dynamique de l’aérosol formé et de définir les meilleures conditions opératoires. L’utilisation de cette technique pour la détermination élémentaire dans les végétaux a présenté cependant des difficultés supplémentaires : difficulté d’étalonnage, effets de matrice et grandes variabilités sur les concentrations mesurées. L’utilisation d’un support de cellulose pour les solutions étalons a permis d’harmoniser les conditions de formation de l’aérosol pour l’échantillon et pour l’étalon, et d’obtenir ainsi des résultats justes. Les effets de matrices ont pu être considérablement réduits par une calcination préalable des échantillons. Le manque de précision des mesures, causée par le manque d’homogénéité des échantillons, a pu être limitée en de réduisant significativement la taille des particules solides. Ces résultats obtenus sur des poudres ont permis d’autres applications comme l’analyse d’échantillons entiers ou la cartographie de la composition chimique d’organes végétaux. / Among the systems dedicated to the direct analysis of the solids, electrothermal vaporization takes up a place of choice. It offers several advantages. The preparation time of the samples is considerably reduced. There is no dilution induced by the digestion and the risks of losses or contaminations during this stage are eliminated. Its functioning consists to convert, by heating, a few milligrams of sample into an aerosol which is then transported in an inductively coupled plasma atomic emission spectrometer, where the elemental composition of the sample is determinate. A first fundamental study allowed to better understand the dynamics of the formed aerosol and to define the best operating conditions. However, the use of this technique to determine the elemental composition of solid plant samples presented additional difficulties: difficulty of calibration, matrix effects and important imprecision on the measured concentrations. The use of a cellulose support for the standard solutions allowed to harmonize the formation of the aerosol between the sample and the standard, and to obtain accurate results. The matrix effects can be considerably reduced by a preliminary dry-ashing of the samples. The variability of measurements, caused by the lack of homogeneity of the samples, was limited by reducing significantly the size of the solid particles. These results, obtained on powders, allowed other applications as the analysis of whole plant samples or the imaging of the chemical composition of plant organs.
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Avaliação da espectrometria de absorção atômica com atomização eletrotérmica em filamento de tungstênio para determinação de arsênio em águas / Evaluation of eletrothermal atomic absorption spectrometry with tungsten coil for the direct determination of arsenic in watersRosana Fernandes Antonio 19 September 2008 (has links)
A determinação direta de arsênio total em águas por espectrometria de absorção atômica com filamentos de tungstênio (150 W) modificados quimicamente com irídio ou ródio, representa uma alternativa para a atomização eletrotérmica de arsênio, que foi avaliada na presente dissertação. A utilização do revestimento com Ir como modificador químico proporcionou um aumento da massa característica de arsênio de 3,5 vezes. As medidas foram feitas com altura de observação selecionada para proporcionar a melhor razão sinal/ruído sem diminuir a sensibilidade do sinal analítico. Avaliaram-se dois programas de aquecimento: com temperatura de secagem constante (com diminuição gradativa da tensão aplicada) e com temperatura de secagem variável (com tensão aplicada de maneira constante). Não houve diferença na sensibilidade entre os dois programas estudados, indicando que a modificação química leva à formação de um precursor atômico com estabilidade térmica elevada. De fato, utilizando-se a modificação química permanente com 1000 müg Ir, e adotando-se programa de aquecimento com temperatura de secagem variável, a temperatura máxima de pirólise foi de aproximadamente 1700 °C ( temperatura de atomização de 2700 °C). Avaliou-se o comportamento eletrotérmico do As na presença dos concomitantes Na, K, Ca e Mg em 0,1% v/v HNO3. Interferências mais severas foram observadas na presença de cálcio acima de 10 \'mü\'g l-1, e acima de 100 \'mü\'g l-1 para os demais concomitantes. As interferências podem estar relacionadas com o elevado gradiente de temperatura entre a superfície do filamento e a fase gasosa do volume de observação, ou mesmo devido à formação de compostos refratários, particularmente para Ca e Mg, na fase condensada, ou seja, na superfície do atomizador. O emprego do método das médias móveis no tratamento dos sinais transientes gerados na atomização do arsênio também foi avaliada. Com o filamento posicionado na altura de observação 2 mm, foram utilizados os fatores 0, 3, 5, 7 e 9, observando-se melhora considerável nos limites de detecção instrumental e do método,utilizando-se média móvel com fator 7. Nestas condições, e depositando-se 20 \'mü\'l de amostra sobre o filamento, o limite de detecção foi de 3,2 \'mü\'g l-1 As e a massa característica de 37,0 pg As. A exatidão foi avaliada analisando-se diferentes amostras de águas provenientes da região do Quadrilátero Ferrífero do Estado de Minas Gerais, por espectrometria de fluorescência atômica com geração de hidretos e por espectrometria de absorção atômica com o filamento de tungstênio modificado com Ir. A comparação dos resultados mostrou que o método proposto pode ser utilizado para o controle de qualidade de águas desta região. Aproximadamente 150 queimas podem ser feitas com um único filamento de tungstênio / The direct determination of arsenic in waters by atomic absorption spectrometry with 150 W tungsten coils, treated with Ir or Rh, was evaluated as a possible alternative for the eletrothermal atomization of As. The use of iridium as a permanent chemical modifier did improve the characteristic mass of arsenic by 3.5 fold. Measurements were made by choosing an appropriate observation height in order to get the best signal to noise ratio. Two heating programs were tested, either by keeping the applied voltage constant or by using an inverted voltage ramp during the drying step. There were no significant differences in the sensitivities between both heating programs, indicating that the permanent modification lead to the formation of an atomic precursor of high thermal stability. Indeed, with the permanent chemical modification with 1000 \'mü\'g Ir, the maximum pyrolysis temperature was approximately 1700 °C (atomization temperature 2700 °C), allowing a heating program with temperature variation during the drying step. Method selectivity was carried out by evaluating the eletrothermal behavior of As in the presence of up to 1000 \'mü\'g l-1 Na, K, Ca and/or Mg in 0,1% v/v HNO3. The most serious interferences were observed with Ca in concentrations higher than 10 \'mü\'g l-1 and when the concentrations were higher than 100 \'mü\'g l-1 for Na, K or Mg, which can be attributed either to the gradient of temperature between the surface of the atomizer and the observation volume or to the formation of refractory compounds in the condensed phase, particularly with Ca and Mg. The absorbance transient signals treatment by the method of moving averages up to factor 9 was also evaluated, with a remarkable improvement in the instrumental and method detection limits. With the center of the observation volume 2 mm above the tungsten coil surface, and a moving average of factor 7, the limit of detection was 3,2 \'müg\' l-1 As and the characteristic mass 37,0 pg As. Accuracy was evaluate by analysing water samples collected in a contaminated area from the Quadrilátero Ferrífero, Minas Gerais State, by hydride generation atomic fluorescence spectrometry and by tungsten coil eletrothermal atomic absorption spectrometry. Results showed that the proposed method fits for the purpose of CONAMA 357 regulation for drinking water quality in the aforementioned contaminated area. Approximately 150 firings can be done with a single tungsten coil atomizer by using 20 \'mü\'l sample volume
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Modélisation électrothermique de composants électriques et électroniques automobiles et estimation des résistances de contact dans les connecteurs / Electrothermal modeling of automotive electrical and electronic components and estimatation of contact resistance in connectorsChevrié, Mathieu 19 July 2016 (has links)
Un connecteur électrique automobile est le siège de points de contact électriques soumis à des échauffements supplémentaires par effet Joule provoqués par leurs résistances de contact. La dégradation d’une résistance de contact peut provoquer des échauffements critiques au niveau des points de contact. La présente étude propose deux approches pour détecter les variations anormales des résistances de contact. La première, appliquée à un connecteur de boîtier électronique automobile, repose sur un diagnostic à base de modèle afin de détecter les variations anormales de la résistance de contact par rapport à sa valeur nominale. La seconde approche,appliquée à un connecteur de recharge de véhicule électrique, consiste d’abord à estimer un flux de chaleur lié à l’effet Joule provoqué par la résistance de contact. La valeur de cette dernière est ensuite estimée grâce à la méthode des moindres carrés. Ces deux approches reposent sur des modèles électrothermiques des connecteurs considérés et de leurs environnements. Cette étude présente également le développement de ces modèles, et notamment l’optimisation du maillage d’un fil électrique basée sur la minimisation de la norme H2 de l’erreur entre un modèle maillé d’ordre entier et un modèle analytique de référence d’ordre non entier. / An automotive electrical connector contains electrical contact points subject to additional temperature rises by Joule effect caused by their contact resistances. The deterioration of a contact resistance can cause critical overheating at the contact points. This study proposes two approaches to detect abnormal changes in contact resistance. The first one, applied to an automotive electric case connector, relies on a model-based diagnosis to detect an abnormal variation in the contact resistance with respect to its nominal value. The second one, applied toan electric vehicle charging connector, consists in estimating a heat flow related to the Joule effect caused by the contact resistance. The value of the latter is then estimated using the least squares.These approaches rely on electrothermal models considered connectors and their environments.This study also presents the development of these models, including the optimization of the mesh of an electrical wire based on the minimization of the H2-norm of the error between ameshed integer order model and a reference analytical fractional order model.
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