FundaÃÃo Cearense de Apoio ao Desenvolvimento Cientifico e TecnolÃgico / CoordenaÃÃo de AperfeiÃoamento de Pessoal de NÃvel Superior / O progresso da indÃstria de telecomunicaÃÃes depende da fabricaÃÃo em larga escala de circuitos de baixo custo, alto desempenho elÃtrico, confiabilidade e passividade de miniaturizaÃÃo. Estas caracterÃsticas sÃo necessÃrias para garantir que os sinais transmitidos sejam confinados a uma freqÃÃncia bem definida, evitando assim sinais que possam interferir no desempenho satisfatÃrio de sistemas de telecomunicaÃÃes. As cerÃmicas dielÃtricas fornecem vantagens significantes em termos de compactaÃÃo, peso, estabilidade tÃrmica e custos de produÃÃo em dispositivos de micro-ondas, alÃm de possuir uma grande facilidade de integraÃÃo com outros circuitos integrados de microondas. Este trabalho consiste no desenvolvimento e caracterizaÃÃo de um novo tipo de material cerÃmico para ser utilizado como uma antena miniatura para aplicaÃÃes em Bluetooth (2.4 GHz). O trabalho està dividido em trÃs etapas. A primeira consiste em desenvolver um novo material que possua constante dielÃtrica (25 < Âr < 50), um alto fator de qualidade (Q > 5000) e um coeficiente de temperatura da freqÃÃncia de ressonÃncia (Âf ) prÃximo de zero. A segunda consiste em caracterizar o material desenvolvido atravÃs de DifraÃÃo de Raios-X e Espectroscopias Raman, Infra-vermelho e DielÃtrica. A Ãltima etapa consiste em fabricar e simular a antena feita com o material desenvolvido, comparando o desempenho teÃrico com o prÃtico. / The progress of telecommunication industry is highly dependent of the fabrication of low cost, quality factor and smaller size of the individual components for commercial applications. This kind of characteristics are necessary to warranty that the signal have well suited frequency, avoiding the noise interference signals, that could affect the performance of the telecommunication systems. Dielectric ceramics have significant advantages of light weight, low cost, small size, low profile, high radiation eficiency, low production cost and ease of integration with other active or passive microwave integrated circuit. This work will provide a new ceramic material that could be used in a miniature antenna for Bluetooth applications. This work is divided in three stages. The first one is develop a new material with a good dielectric permittivity (25 < Âr < 50), high quality factor (Q > 5000) and low temperature coeficient of resonant frequency (Âf ). The second one characterize the developed material by XDR, Raman, Infrared and dielectric spectroscopy in microwave region. The last one is build and simulate the antenna made with the developed dielectric material.

A dispersão e absorção das ondas eletromagnéticas que se propagam através de um material dielétrico podem ser medidas ao longo de uma ampla região do espectro que se estende desde a região de freqüências extremamente baixas até a região óptica incluindo as faixas das microondas, objeto de interesse do presente estudo. Dentre os dielétricos, incluem-se os materiais cristalinos e amorfos isolantes e semicondutores. Os vidros de composições (1-x)(60\'P IND. 2\'\'O IND.5\'.\'40\'BA\'\'O).x(\'M\'\'O\'), (1-X)(25\'LI IND. 2\'\'O\'.25\'NA IND. 2\'\'O\'.50\'P IND. 2\'\'O IND. 5\').x(\'M\'\'O\') e 60\'B IND. 2\'\'O IND. 3\'.30\'BA\'\'O\'.\'10\'AL IND. 2\'\'O IND. 3\' onde x é a concentração (mol%) de óxido do metal de transição \'FE\' ou \'CO\' (\'M\'\'O\'), foram escolhidos para representar o comportamento das propriedades dielétricas dos vidros óxidos, tanto na região das freqüências mais baixas (0 - 100 MHz), como na faixa de microondas (2 - 30 GHz). Os íons de metais de transição, quando ocupam posições intersticiais da rede vítrea, como ocorre com os elementos modificadores alcalinos e alcalinoterrosos atuam como compensadores de carga junto às unidades estruturais tetraédricas eletricamente carregadas, formando dipolos permanentes locais, contribuindo para a constante dielétrica do vidro. A polarização desses dipolos, quando submetido ao campo elétrico oscilatório de uma onda eletromagnética, atinge valores maiores às freqüências mais baixas decrescendo gradualmente à medida que estas atingem a região de microondas. Um novo método alternativo foi desenvolvido para a medida da temperatura da transição vítrea (\'T IND. g\') utilizando técnicas de microondas. Mostramos que a posição da inflexão do gráfico da constante dielétrica em função da temperatura do vidro 25\'LI IND. 2\'\'O\'.25\'NA IND. 2\'\'O\'.50\'P IND. 2\'\'O IND. 5\' medida em 9 GHz, na faixa de temperaturas em torno de \'(270 \'+ OU -\' 10) GRAUS\' C coincidiu com o valor da \'T IND. g\' deste vidro obtida por análise térmica diferencial (DTA). Outro método também foi desenvolvido para monitorar o resfriamento do vidro em função do tempo a partir do estado liquido até a solidificação, registrando o sinal de microondas refletido sobre o material vertido no interior de um guia de ondas. Pudemos observar, também, mudanças no espectro de ressonância paramagnética eletrônica (EPR) do vidro fosfato contendo níquel após ter sido irradiado com diferentes níveis de potência das microondas, por cerca de duas horas. Este efeito pode estar relacionado com mecanismos de acoplamento de spins paramagnéticos. Os espectros de transmissão de microondas das amostras de vidros fosfatos contendo diferentes concentrações de cobalto, bário, ferro e manganês, obtidos por meio de uma varredura de freqüências desde 7 até 13 GHz, mostraram a presença de uma intensa atenuação do sinal próximo de 9,7 GHz. Essa atenuação diminuiu conforme aumenta a concentração dos modificadores. / The dispersion and absorption of electromagnetic waves that propagate through a dielectric material can be measured along a wide spectral region ranging from extremely low frequency to the optical region, including microwaves one, which is the subject of interest of the present study. Among dielectrics, there are crystalline and amorphous materials that can be either insulators or semiconductors. Glasses of compositions (1-x)(60\'P IND. 2\'\'O IND.5\'.\'40\'BA\'\'O).x(\'M\'\'O\'), (1-X)(25\'LI IND. 2\'\'O\'.25\'NA IND. 2\'\'O\'.50\'P IND. 2\'\'O IND. 5\').x(\'M\'\'O\') and 60\'B IND. 2\'\'O IND. 3\'.30\'BA\'\'O\'.\'10\'AL IND. 2\'\'O IND. 3\', where x is the concentration (mol %) of the \'FE\' or \'CO\' (\'M\'\'O\') transition metal oxide, were selected to investigate the behavior of the dielectric properties of oxide glasses in the lower frequency range (0 - 100 MHz) and in the microwave region (2- 30 GHz). When transition metal ions occupy interstitial positions in the glass matrix, as it happens with the regular alkaline and alkaline-earth modifier ions, they compensate the electrically charged tetrahedral structural units. As a consequence, local permanent dipoles are formed, contributing to the dielectric constant of the glass. The polarization of these dipoles, when submitted to an oscillating electromagnetic field, is higher at lower frequencies and decreases gradual1y as the frequency approaches the microwave region. An alternative new method was developed to measure the glass transition temperature (\'T IND. g\') using microwave techniques. It was shown that the inflexion position of the dielectric constant of the glass 25\'LI IND. 2\'\'O\'.25\'NA IND. 2\'\'O\'.50\'P IND. 2\'\'O IND. 5\' measured at 9 GHz, in the temperature range about \'(270 \'+ OU -\' 10) GRAUS\' C, coincided with the \'T IND. g\' value obtained by differential thermal analysis (DTA). Another method was also developed for monitoring the melt cooling as a function of time from the liquid to the solid state, by recording the reflected microwave signal crossing the material poured inside the wave guide. We observed, also, changes in the electronic paramagnetic resonance (EPR) spectrum of phosphate glass containing nickel after being irradiated for two hours with several microwave power levels. This effect may be related with coupling and decoupling mechanisms among the spin clusters developed in the sample. The microwave transmission spectra of the phosphate glass samples containing different concentrations of iron, cobalt, barium, manganese and barium, obtained by a frequency sweep from 7 to 13 GHz, presented an intense attenuation of the signal near to 9,7 GHz. This attenuation was found to decrease with the increase of modifier content.

Certos solos não saturados ao serem umedecidos experimentaram bruscas reduções de volume, sob cargas praticamente constantes. O fenômeno é atribuído a um colapso de estrutura do solo, donde a designação de solo colapsível. Essa redução de volume pode ocorrer sob a ação do próprio peso do solo, mas é mais comum ocorrer quando o solo está sujeito a um carregamento adicional. Muitos dos problemas de recalques nas áreas urbanas e industrias na Região Sudeste do Brasil estão associados ao colapso dos solos. Deformações induzidas por umedecimento (colapso) têm sido reportados como decorrrentes de vazamentos oriundo das redes de esgoto e de abastecimento de água. Porém, pouco se sabe sobre a influência de vazamentos de diferentes efluentes químicos nesse fenômeno e em outros fenômenos eventualmente associados com a dispersão dos solos. Neste trabalho, analisa-se o comportamento colapsível de dois solos típicos do interior do Estado de São Paulo, considerando diferentes soluções como líquido inundante. Utilizaram-se substâncias orgânicas e inorgânicas com o intuito de verificar a interferência de algumas propriedades químicas destas soluções (pH, constante dielétrica, concentração e temperatura) no comportamento colapsível dos solos. Para evitar a ação dos fluídos químicos na dispersão dos solos, realizou-se o \"pinhole test\". Análises porosimétricas por intrusão de mercúrio foram utilizadas para identificar mudanças ocorridas nos poros das amostras após os ensaios edométricos. Para a análise estrutural, foram analisadas lâminas delgadas em microscópio óptico. Verificou-se que a presença de um agente dispersivo na solução tende a influenciar o potencial de colapso dos solos. A constante dielétrica, o pH e a concentração mostraram-se influentes para alguns fluídos de saturação. Os resultados dos \"pinholes tests\" revelaram que o fluxo das diferentes soluções não provocou a dispersão do solo. Ensaios de porosimetria ) por intrusão de mercúrio indicaram que as deformações por colapso resultam de uma redução do volume de macroporos. A análise das lâminas delgadas mostrou diferentes facetas dos processos ocorrentes em nível estrutural, como diminuição considerável dos poros e modificações no plasma para as amostras inundadas com as soluções defloculantes de hexametafosfato de sódio e hidróxido de sódio. / Some non saturated soils show considerable volume reduction when wetted under constant loads. The phenomenon is attributed to soil structure collapse, thus the designation collapsible soils;. Volume reduction upon wetting can arise under soil self weight, but it is more common when the soil is subjected to an additional load. Many settlement problems in urban and industrial areas in Southern Brazil are associated to soil collapse. Wetting induced strains (collapse) have been related to water and sewer leakage. However little is known about the influence of different effluent leakage from industrial plants in the phenomenon and in other related phenomenon such as soil dispersion. This work deals with the collapsible behavior of two typical soils from the state of São Paulo assessed by means of wetting both soils with different chemical solutions. Organic and inorganic solutions were applied, aiming to verify the interference of some physic-chemical properties of the solutions (pH, dielectric constant, concentration, temperature) in the collapse behavior of the soils. The soil dispersion was evaluated through pinhole tests, where the same solutions used in the collapse tests were applied in the leaching procedures. Thin sections and mercury porosimetry of the soils were used to study the soil structural features. It is shown that the dielectric constant and the pH tends to influence the collapse potential of the soils when some solutions are concerned. Mercury intrusion tests have revealed that collapse deformations are related to macropores volume reduction. Thin sections have shown some features of the occurring processes on a structural levei, such as pore reductions and changes in fine matrix for the soil samples soaked with sodium hexametaphosphate and sodium hydroxide solution.

A dispersão e absorção das ondas eletromagnéticas que se propagam através de um material dielétrico podem ser medidas ao longo de uma ampla região do espectro que se estende desde a região de freqüências extremamente baixas até a região óptica incluindo as faixas das microondas, objeto de interesse do presente estudo. Dentre os dielétricos, incluem-se os materiais cristalinos e amorfos isolantes e semicondutores. Os vidros de composições (1-x)(60\'P IND. 2\'\'O IND.5\'.\'40\'BA\'\'O).x(\'M\'\'O\'), (1-X)(25\'LI IND. 2\'\'O\'.25\'NA IND. 2\'\'O\'.50\'P IND. 2\'\'O IND. 5\').x(\'M\'\'O\') e 60\'B IND. 2\'\'O IND. 3\'.30\'BA\'\'O\'.\'10\'AL IND. 2\'\'O IND. 3\' onde x é a concentração (mol%) de óxido do metal de transição \'FE\' ou \'CO\' (\'M\'\'O\'), foram escolhidos para representar o comportamento das propriedades dielétricas dos vidros óxidos, tanto na região das freqüências mais baixas (0 - 100 MHz), como na faixa de microondas (2 - 30 GHz). Os íons de metais de transição, quando ocupam posições intersticiais da rede vítrea, como ocorre com os elementos modificadores alcalinos e alcalinoterrosos atuam como compensadores de carga junto às unidades estruturais tetraédricas eletricamente carregadas, formando dipolos permanentes locais, contribuindo para a constante dielétrica do vidro. A polarização desses dipolos, quando submetido ao campo elétrico oscilatório de uma onda eletromagnética, atinge valores maiores às freqüências mais baixas decrescendo gradualmente à medida que estas atingem a região de microondas. Um novo método alternativo foi desenvolvido para a medida da temperatura da transição vítrea (\'T IND. g\') utilizando técnicas de microondas. Mostramos que a posição da inflexão do gráfico da constante dielétrica em função da temperatura do vidro 25\'LI IND. 2\'\'O\'.25\'NA IND. 2\'\'O\'.50\'P IND. 2\'\'O IND. 5\' medida em 9 GHz, na faixa de temperaturas em torno de \'(270 \'+ OU -\' 10) GRAUS\' C coincidiu com o valor da \'T IND. g\' deste vidro obtida por análise térmica diferencial (DTA). Outro método também foi desenvolvido para monitorar o resfriamento do vidro em função do tempo a partir do estado liquido até a solidificação, registrando o sinal de microondas refletido sobre o material vertido no interior de um guia de ondas. Pudemos observar, também, mudanças no espectro de ressonância paramagnética eletrônica (EPR) do vidro fosfato contendo níquel após ter sido irradiado com diferentes níveis de potência das microondas, por cerca de duas horas. Este efeito pode estar relacionado com mecanismos de acoplamento de spins paramagnéticos. Os espectros de transmissão de microondas das amostras de vidros fosfatos contendo diferentes concentrações de cobalto, bário, ferro e manganês, obtidos por meio de uma varredura de freqüências desde 7 até 13 GHz, mostraram a presença de uma intensa atenuação do sinal próximo de 9,7 GHz. Essa atenuação diminuiu conforme aumenta a concentração dos modificadores. / The dispersion and absorption of electromagnetic waves that propagate through a dielectric material can be measured along a wide spectral region ranging from extremely low frequency to the optical region, including microwaves one, which is the subject of interest of the present study. Among dielectrics, there are crystalline and amorphous materials that can be either insulators or semiconductors. Glasses of compositions (1-x)(60\'P IND. 2\'\'O IND.5\'.\'40\'BA\'\'O).x(\'M\'\'O\'), (1-X)(25\'LI IND. 2\'\'O\'.25\'NA IND. 2\'\'O\'.50\'P IND. 2\'\'O IND. 5\').x(\'M\'\'O\') and 60\'B IND. 2\'\'O IND. 3\'.30\'BA\'\'O\'.\'10\'AL IND. 2\'\'O IND. 3\', where x is the concentration (mol %) of the \'FE\' or \'CO\' (\'M\'\'O\') transition metal oxide, were selected to investigate the behavior of the dielectric properties of oxide glasses in the lower frequency range (0 - 100 MHz) and in the microwave region (2- 30 GHz). When transition metal ions occupy interstitial positions in the glass matrix, as it happens with the regular alkaline and alkaline-earth modifier ions, they compensate the electrically charged tetrahedral structural units. As a consequence, local permanent dipoles are formed, contributing to the dielectric constant of the glass. The polarization of these dipoles, when submitted to an oscillating electromagnetic field, is higher at lower frequencies and decreases gradual1y as the frequency approaches the microwave region. An alternative new method was developed to measure the glass transition temperature (\'T IND. g\') using microwave techniques. It was shown that the inflexion position of the dielectric constant of the glass 25\'LI IND. 2\'\'O\'.25\'NA IND. 2\'\'O\'.50\'P IND. 2\'\'O IND. 5\' measured at 9 GHz, in the temperature range about \'(270 \'+ OU -\' 10) GRAUS\' C, coincided with the \'T IND. g\' value obtained by differential thermal analysis (DTA). Another method was also developed for monitoring the melt cooling as a function of time from the liquid to the solid state, by recording the reflected microwave signal crossing the material poured inside the wave guide. We observed, also, changes in the electronic paramagnetic resonance (EPR) spectrum of phosphate glass containing nickel after being irradiated for two hours with several microwave power levels. This effect may be related with coupling and decoupling mechanisms among the spin clusters developed in the sample. The microwave transmission spectra of the phosphate glass samples containing different concentrations of iron, cobalt, barium, manganese and barium, obtained by a frequency sweep from 7 to 13 GHz, presented an intense attenuation of the signal near to 9,7 GHz. This attenuation was found to decrease with the increase of modifier content.

Developments in micro and nano technology have great potential in many applications. Two applications that will be addressed in this work are self assembly of microdevices and Electrowetting in microfluidics. Capillary forces are the most critical factor in both of these techniques and need proper characterization. This thesis describes a detailed study of these forces and explains how they were utilized as an effective source of drive in high end applications. Self assembly is a promising alternative to conventional pick and place robotic assembly of micro components. Its benefits include parallel integration of parts with low equipment costs. Various approaches to self assembly have been demonstrated, yet demanding applications like assembly of micro-optical devices require increased positioning accuracy. This thesis proposes a new method for design of self assembly bonds that addresses this need. Current methods have zero force at the desired assembly position and low stiffness. The proposed method uses a substrate assembly feature to provide a high accuracy alignment guide to the part. The capillary bond region of the part and substrate are then modified to create a non-zero positioning force to maintain the part in the desired assembly position. Capillary force models show that this force aligns the part to the substrate assembly feature and reduces the sensitivity of part position to process variation. Thus, the new configuration analyzed proves substantial improvement in positioning accuracy of capillary self assembly. Guidelines are proposed for the design of an effective assembly bond using this new approach. Electrowetting is another application that has been successfully demonstrated as a means of drop manipulations in digital micro-fluidic devices. These demonstrations show that electrowetting actuation holds great promise, but there are also reports of erratic behavior and system degradation. While a method for electrowetting force measurement to track the degradation of the electrowetting response was demonstrated, this thesis analyzes some adverse effects in the electrowetting response due to variations during measurement of electrowetting forces, specially the variation of volume, the tilt in the part considered for measurements, and defective layer response.

Grid-scale integration of renewable energy sources and smart grid devices has created new demands in flexible power conversion. State-of-the-art semiconductor power switches present limitations in power handling capability, as well as forward and reverse breakdown voltages. Superconducting materials are a viable alternative due to their robustness against high ampacities, large electric fields and abrupt changes in power flow. This work pays focus to material testing and apparatus design for an antenna-coupled cryotron (ACC), which is a superconducting power switch.Design, fabrication and testing are examined for a longitudinal resonant cavity, paired with monopole transmit and modified slot receive antennae. These couple radio frequency (RF) energy into superconducting thin film niobium (Nb) carrying high current densities (∼105A/cm2), thereby creating an antenna-coupled cryotron.Induced electromagnetic field effects at the receive antenna alter superconductive fluid dynamics. The theorized quality in manipulating this mechanism is a rapid normal-conductivity transition (µs), which affects a switch "off" state. Functional evaluation of the device as a waveguide revealed evanescent mode resonance at frequencies below the waveguide cut-off of ∼18GHz. The thin film Nb was deposited on a quartz dielectric, which penetrated the waveguide and supported evanescent resonances within the structure.Altered resistivity and critical transition-point properties emerged from device testing at applied RF. When the Nb film temperature-dependent coherence length was comparable to its thickness, perpendicular magnetic field application generated an Abrikosov vortex state, energetically favoring a mixed domain condensate. Interaction of the magnetically-induced flux vortex lattice with Lorentz current forces gave rise to resistive changes within the metal. Three resistive transition mechanisms developed: a latch to normal state resistance, attributed to cooper-pair destruction avalanche induced near critical transition points; a small reversible increase in resistance (∼mV), arising from flux-flow within an intermediate state at peak resonance; as well as temporal alterations in superfluid dynamics from disequilibrium in the quasi-particle population. The RF induced superfluid effects were observable in separate terms of electric and thermodynamic fluctuations.Motivation for this work is the eventual design of a high voltage, high current and low cost power switch, able to function where existing semiconductor technology fails. Concentration is paid to the fundamental theory, physics and methodology in conceptual testing and design of prototype ACCs. Assessment focuses on preliminary findings and concludes with next stage design requirements.

Le PRC (Polyéthylène réticulé chimiquement) est utilisé comme matériau de base pour la fabrication de l’enveloppe à isolation électrique des câbles HTA en raison de ces propriétés thermiques et diélectriques remarquables. Afin d’améliorer la fiabilité de ces câbles, des études de vieillissement sous différentes contraintes (thermique, humidité, tension) ont été réalisées sur les différentes couches du câble, et en particulier sur l’isolant en PRC.Dans un premier temps, nous avons identifié un certain nombre de marqueurs chimiques et physiques pouvant donner des informations sur le degré de vieillissement de l’isolant PRC des câbles HTA. Ces différents marqueurs sont caractéristiques d’une dégradation multi-échelle (moléculaire, microscopique et macroscopique) et peuvent être utilisés pour établir le diagnostic d’un câble électrique et ainsi évaluer son état de dégradation général. Parmi ces marqueurs, l’existence d’un phénomène de migration d’espèces polaires des semi-conducteurs vers l’isolant du câble aura particulièrement attiré notre attention. Des analyses supplémentaires ont donc été réalisées afin de mieux appréhender ce phénomène.Ensuite, nous avons déterminé l’impact de contraintes thermique et électrique simultanées sur les propriétés physico-chimiques et diélectriques d’un isolant en PRC. Les analyses physico-chimiques ont montré que l’ajout d’une forte tension ne semble affecter ni l’oxydation, ni la diffusion. Des vieillissements sous contraintes importantes ont néanmoins permis d’identifier un signal particulier en spectroscopie diélectrique. La détection de ce signal pourra être utilisée pour anticiper des claquages de câbles sur le réseau électrique. Nous avons également réussi à établir un lien entre certains marqueurs chimiques et la dégradation des propriétés diélectriques des isolants pour des mises sous contraintes particulièrement extrêmes. / Due to its outstanding thermal and dielectric properties, XLPE (Chemically Crosslinked Polyethylene) is commonly used as a base material for manufacturing the electrical insulating jacket of MV cables. With a view to improve the reliability of these cables, aging studies have been carried out under different stress conditions (temperature, humidity, tension) on the different constituting layers, and in particular on the XLPE insulating one.First of all, we have identified several chemical and physical markers that can provide information on the aging degree of the XLPE insulation from MV cables. These different markers are representative of a degradation at different scales (molecular, microscopic and macroscopic) and they can be used to establish a diagnosis on an electrical cable, and thus evaluate its general state of degradation. Among these markers, the existence of a polar species’ migration phenomenon from semiconductors to the insulating layer had particularly attracted our attention. Additional analyzes were thus conducted to gain more insight on this phenomenon.Then, we have determined the impact of simultaneous thermal and electrical stresses on physico-chemical and dielectric properties of the XLPE insulating material. The physico-chemical analyzes have demonstrated that the addition of an important tension did not affect the oxidation and diffusion phenomena previously identified. Aging under high stress allowed us to identify a special signal in dielectric spectroscopy. The identification of such a signal could be used to anticipate cable breakdowns on the power grid. In addition, we were successful in establishing a clear link between some chemical markers and the degradation of the insulator dielectric properties in the case of extreme ageing conditions.

It is essential to properly monitor in-situ soil compaction properties during most earthwork construction projects. Traditional in-situ soil compaction monitoring methods are often limited in their application. As a result, new methods are being developed to more accurately measure in-situ compaction parameters. Time domain reflectometry (TDR) is one such method. Relying on the propagation of an electromagnetic wave through the soil sample, TDR can be used to measure both in-situ moisture content as well as soil dry density. Although TDR is relatively new to the field of geotechnical engineering, it has previously been implemented in other fields with success. Researchers at Purdue University have made several advances to further incorporate the use of TDR technology into the field of geotechnical engineering and as a result an innovative TDR measurement system has been developed for compaction control monitoring. The method was standardized in the form of ASTM D 6780 in 2002. Further advancements led to an improved method referred to as the Purdue one-step TDR method. Research has indicated that the ASTM TDR method is sufficiently accurate for application in compaction monitoring applications. A comparison between the ASTM TDR method and traditional methods was carried out to evaluate the accuracy of the TDR method to traditional methods. To further expand the application of the TDR method, a correlation was developed between the TDR spike driving process with the in-situ CBR test. A comprehensive review of previous research was conducted to examine recent advancements leading to the improved Purdue one-step method. A study was also performed to evaluate the effect of variable pore fluid conductivity on the calibration of the Purdue one-step method.

Les matériaux diélectriques sont présents dans de nombreux dispositifs en microélectronique. Ces derniers peuvent être soumis à de fortes contraintes électriques impactant leur durée de vie. Le stress électrique peut en effet provoquer le claquage du diélectrique ou la modification des performances des composants par accumulation de charges. Dans ces travaux de thèse, différentes méthodes de caractérisation et d'analyse physique ont été utilisées pour étudier la structure des échantillons et identifier les mécanismes en jeu dans le processus d'accumulation de charges dans des couches minces de nitrure de silicium. Puis un code de simulation modélisant les phénomènes de transport de charges dans les isolants a été développé. Le modèle prend en compte des phénomènes de transport par effet tunnel et par effet thermique, dans le volume du diélectrique et aux interfaces isolant-métal. Il permet d'étudier l'évolution de grandeurs physiques (courants, charge, champ électrique) en fonction du temps et de la profondeur dans la couche mince diélectrique. Des résultats de mesures sur des composants capacitifs ont pu être reproduits grâce aux simulations. Cet outil permet d'estimer l'intérêt d'un matériau diélectrique relativement à la fiabilité de composants capacitifs. Il peut également être utilisé en amont afin de définir un matériau aux propriétés idéales pour l'application visée ou aider au dimensionnement de dispositifs en microélectronique. / Dielectric materials can be found in numerous devices in microelectronics. They can be subjected to significant electrical stress, which impacts their lifetime. Indeed, this electrical stress can lead to dielectric breakdown or modify the component performances by charge storage. In this work, several characterization methods and physical analysis have been used in order to study the samples and identify mechanisms involved in charge transport in silicon nitride thin films. Then a simulation code has been developed to model charge transport phenomena in insulators. This model takes into account tunnel and thermal effects in the dielectric and at the dielectric-metal interfaces. The temporal and spatial evolution of physical quantities (currents, charge, electric field) in the dielectric film are calculated. Measurement results on capacitive components can be obtained thanks to simulations. This simulation tool allows testing dielectric materials according to capacitive component reliability. It may be used to define optimal properties for materials depending on applications or to assist in device design in microelectronics.

Dans un contexte où l’électronique est au centre de notre société, la productiond’appareils de plus en plus compacts et multifonctionnels concentre les efforts en rechercheet développement. Pour répondre à cette attente, une des options est d’augmenter lerendement volumique des composants passifs tels que les condensateurs, en se basant surl’utilisation de nanoparticules diélectriques du type BaTiO3. Dans un premier temps,l’objectif est d’optimiser la synthèse des nanoparticules de BaTiO3 et de comprendre leursmécanismes de formation en milieux fluides supercritiques. Pour ce faire nous avonscombiné des méthodes d’analyses ex situ telles que la microscopie électronique, ladiffraction des rayons X, et les spectroscopies Raman ou infra rouge à des mesures in situsynchrotron de diffraction des rayons X aux grands angles. L’étude a par la suite ététransposé à l’élaboration de la totalité des solutions solidesBa1-xSrxTiO3 (0 ≤ x ≤ 1) et BaTi1-yZryO3 (0 ≤ y ≤ 1). Une fois les synthèses optimisées, l’utilisation du spark plasma sintering(SPS) nous a permis de mettre en oeuvre des céramiques denses et nanostructurées,préservant la taille initiale des particules (20 nm), ceci afin d’étudier les propriétésintrinsèques des matériaux à l’échelle nanoscopique. Enfin, connaissant les propriétés debase de ces nanomatériaux, nous avons pu commencer à développer des matériauxhybrides diélectriques pour l’électronique flexible. / In a context where the electronic is at the center of our society, theproduction of more compact and multifunctional devices focuses the research efforts.To answer to the expectations, one option is to improve the volume efficiency ofpassive components such as capacitors using dielectric nanoparticles such asBaTiO3. First, the objective is to optimize the synthesis of BaTiO3 nanoparticles andunderstand their formation in supercritical fluids. To do this, we combinedconventional ex situ analyses such as X-ray diffraction, electronic microscopy,infrared and Raman spectroscopies with in situ synchrotron wide angle X-rayscattering analyses. This was then transferred to the development of Ba1-xSrxTiO3 (0≤ x ≤ 1) and BaTi1-yZryO3 (0 ≤ y ≤ 1) solid solutions. Once the syntheses wereoptimized, using spark plasma sintering (SPS), we processed the powders intodense and nanostructured ceramics keeping the starting particles size (20 nm), tostudy the materials intrinsic properties at the nanoscale. Finally, knowing thenanoparticles properties, we could start to develop hybrid dielectric materials forflexible electronics.