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Diagnosis of PEMFC stack failures via electrochemical impedance spectroscopyMérida Donis, Walter Roberto 15 November 2018 (has links)
Two failure modes related to water management in Proton Exchange Membrane fuel cells (dehydration and flooding) were investigated using electrochemical impedance spectroscopy as a diagnosis tool. It was hypothesised that each failure mode corresponds to changes in the overall stack impedance that are observable in different frequency ranges. This hypothesis was corroborated experimentally.
The experimental implementation required new testing hardware and techniques. A four-cell stack capable of delivering individually conditioned reactants to each cell was designed, built, tested, and characterised under a variety of operating conditions. This stack is the first reported prototype of its type.
The stack was used to perform galvanostatic, impedance measurements in situ. The measurements were made at three different temperatures (62, 70 and 80°C), covering the current density range 0.1 to 1.0 A cm−2 , and the frequency range 0.1 to 4 × 105 Hz. The recorded data represent the first reported set of measurements covering these ranges.
The failure modes were simulated on individual cells within the stack. The effects on individual cell and stack impedance were studied by measuring the changes in stack and cell impedances under flooding or dehydration conditions.
Dehydration effects were measurable over a wide frequency range (0.5 to 105 Hz). In contrast, flooding effects were measurable in a narrower frequency range (0.5 to 102 Hz). Using these results, separate or concurrent impedance measurements in these frequency ranges (or narrow bands thereof) can be used to discern and identify the two failure modes quasi-instantaneously. Such detection was not possible with pre-existing, do techniques.
The measured spectra were modelled by a simple equivalent circuit whose time constants corresponded to ideal (RC) and distributed (Warburg) components. The model was robust enough to fit all the measured spectra (for single cells and the stack), under normal and simulated-failure conditions.
Approximate membrane conductivities were calculated using this model. The calculations yielded a range from 0.04 to 0.065 S cm−1 (under normal humidification), and conductivities that deviated from these nominal range under flooding or dehydrating conditions. The highest conductivity value (was ∼0.10 S cm−1) was measured under flooding conditions at j = 0.4 A cm−2. The lowest conductivity (∼0.02 S cm−1) corresponded to a dehydrated cell at j = 0.1 A cm−2. These values fall within the ranges of published data for modern proton exchange membranes.
The phenomenological and numerical results reported in this work represent the first demonstration of these techniques on a PEMFC stack under real operating conditions. They are also the basis of ongoing research, development, and intellectual property protection. / Graduate
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A Multiplexing Immunosensor for the Quantification of Cytokine BiomarkersJanuary 2012 (has links)
abstract: Biosensors offer excellent diagnostic methods through precise quantification of bodily fluid biomarkers and could fill an important niche in diagnostic screening. The long term goal of this research is the development of an impedance immunosensor for easy-to-use, rapid, sensitive and selective simultaneously multiplexed quantification of bodily fluid disease biomarkers. To test the hypothesis that various cytokines induce empirically determinable response frequencies when captured by printed circuit board (PCB) impedance immunosensor surface, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) methods were used to test PCB biosensors versus multiple cytokine biomarkers to determine limits of detection, background interaction and response at all sweep frequencies. Results indicated that sensors for cytokine Interleukin-12 (IL-12) detected their target over three decades of concentration and were tolerant to high levels of background protein. Further, the hypothesis that cytokine analytes may be rapidly detected via constant frequency impedance immunosensing without sacrificing undue sensitivity, CV, EIS, impedance-time (Zt) methods and modeling were used to test CHITM gold electrodes versus IL-12 over different lengths of time to determine limits of detection, detection time, frequency of response and consistent cross-platform sensor performance. Modeling and Zt studies indicate interrogation of the electrode with optimum frequency could be used for detection of different target concentrations within 90 seconds of sensor exposure and that interrogating the immunosensor with fixed, optimum frequency could be used for sensing target antigen. This informs usability of fixed-frequency impedance methods for biosensor research and particularly for clinical biosensor use. Finally, a multiplexing impedance immunosensor prototype for quantification of biomarkers in various body fluids was designed for increased automation of sample handling and testing. This enables variability due to exogenous factors and increased rapidity of assay with eased sensor fabrication. Methods were provided for simultaneous multiplexing through multisine perturbation of a sensor, and subsequent data processing. This demonstrated ways to observe multiple types of antibody-antigen affinity binding events in real time, reducing the number of sensors and target sample used in the detection and quantification of multiple biomarkers. These features would also improve the suitability of the sensor for clinical multiplex detection of disease biomarkers. / Dissertation/Thesis / Ph.D. Bioengineering 2012
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Um método D-bar para estimar admitividade em 2-D através de tomografia por impedância elétrica. / A D-bar method for recovering admittivity in 2-D electrical impedance tomography.Claudia Natalia Lara Herrera 23 August 2012 (has links)
Propõe-se um novo método D-bar de Tomografia por Impedância Elétrica (TIE) para obter, simultaneamente, a condutividade e a permitividade de um domínio 2-D. O algoritmo direto baseia-se na prova de existência e unicidade do artigo de E. Francini [1]. A caracterização de tecidos biológicos é fortemente facilitada a partir do conhecimento de suas propriedades elétricas. Particularmente, nas aplicações médicas de TIE há grande interesse na permitividade, uma vez que, vários autores tem apresentado critérios para distinguir patologias baseados nesta propriedade, um exemplo constitui a determinação de presença ou ausência de sangue em líquidos acumulados no pulmão. Realizam-se testes com dados simulados numericamente e experimentais com o propósito de verificar e entender as propriedades, capacidades e limitações do algoritmo implementado. No caso dos testes numéricos, é desenvolvido um programa que resolve o problema direto da admitividade, o qual permite calcular conjuntos de dados de voltagem numéricos. São simulados dados aplicando padrões de corrente trigonométricos e por pares. As soluções exponencialmente crescentes do problema inverso são parte essencial do algoritmo e devem ser decompostas nas bases dos padrões de injeção de corrente. A compreensão da natureza destas decomposições para padrões de injeção trigonométricos e por pares, levou ao estabelecimento de especificações no projeto de um sistema de TIE para este algoritmo. Os resultados encorajadores numéricos e experimentais obtidos nas reconstruções de condutividade e permitividade, quanto à resolução espacial e às magnitudes, indicam que o algoritmo é promissor para uso clínico. / This work proposes a new D-bar method of Electrical Impedance Tomography (EIT) for reconstructing the conductivity and permittivity simultaneously in a 2-D domain. The direct algorithm presented is based on the existence and uniqueness proof by E. Francini [1]. Biological tissue characterization is strongly facilitated by the knowledge of its electric properties. In EIT medical applications there is great interest in the permittivity as an additional property for distinguishing pathologies. For instance, the determination of presence or absence of blood in fluid accumulation in the lung. Numerical and experimental data tests are carried out in order to verify and understand the properties, capabilities and limitations of the implemented algorithm. A numerical phantom to solve the forward admittivity problem is developed which allows to simulate voltage data sets. Trigonometric and pairwise injection current patterns are applied. Exponentially growing solutions of the inverse problem are a key part of the algorithm, which have to be expanded in terms of the current patterns. Understanding the nature of these expansions for trigonometric and pairwise injection current patterns leads to a set of specifications in the design of an EIT system for this algorithm. The encouraging numerical and experimental results obtained in conductivity and permittivity reconstructions, regarding the magnitude and spatial resolution, indicate that the algorithm is promising for clinical use.
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Reconstrução não-linear completa de imagens de tomografia por impedância elétrica utilizando o método D-bar 2D. / Reconstruction nonlinear full of images of electrical impedance tomography using the 2D D-bar method.Miguel Fernando Montoya Vallejo 16 October 2012 (has links)
Neste trabalho desenvolveu-se desenvolver uma versão sem linearizações do método D-bar para Tomografia por Impedância Elétrica (TIE). O problema inverso de TIE é não-linear e mal-posto. O algoritmo baseia-se na prova de existência e unicidade de Adrian Nachman [Ann. of Math. 143 (1996)] para domínios com distribuição de condutividade duas vezes diferenciáveis. O método faz uso de uma Transformada de Fourier não-linear chamada scattering transform, e o caráter mal-posto do Problema Inverso torna-se evidente no cálculo desta transformada, mais especificamente na determinação das soluções Complex Geometrical Optics (CGO). Atuais implementações práticas do método D-bar para padrões trigonométricos tem aproximado os valores na fronteira das soluções CGO por seu comportamento assintótico no cálculo da scattering transform, o que constitue uma linearização nesta etapa específica do método. Neste trabalho calcula-se a scattering transform a partir das soluções exponencialmente crescentes, o que implica calcular as funções Green de Faddeev, com o objetivo de encontrar imagens com maior resolução espacial e precisão nos valores de condutividade por ter resolvido o problema não-linear de forma completa. Dados de simulação numérica e experimentais usando padrões de injeção pula eletrodos e trigonométricos foram usados na avaliação do método. As imagens obtidas apresentam comportamento diferente em função do padrão de injeção utilizado. Do cálculo completo da transformada scattering resultam imagens com melhor resolução espacial. As imagens reconstruídas a partir de padrões de injeção trigonométricos apresentam também melhor resolução espacial comparadas as imagens reconstruídas a partir de padrões por pares, separados por três eletrodos. / This work proposes to develop a version of the D-bar method linearization for Electrical Impedance Tomography (EIT). The inverse problem of EIT is both nonlinear and very ill-posed. The version of the D-bar method implemented here is based on the existence and uniqueness proof of Adrian Nachman [Ann. of Math. 143 (1996)]. The method relies on the use of a nonlinear Fourier transform called the scattering transform, and the inherent ill-posedness of the inverse conductivity problem becomes evident in the computation of the scattering transform, more specifically in the determination of the Complex Geometrical Optics (CGO) solutions. Current practical implementations of the D-bar method using trigonometric patterns have replaced the boundary values of the CGO solutions by their asymptotic behavior in the calculation of the scattering transform, which is a linearization in this particular step of the overall method. This work proposes to calculate the scattering transform from exponentially growing solutions, which implies the calculation of the Faddeev Greens function, with the goal of obtaining images with higher resolution and accuracy in the conductivity values because the full nonlinear problem is solved. Numerical and experimental data using pairwise and trigonometric current injection patterns were used to evaluate the performance of the method. Better spatial resolution is obtained from the complete computation of the scattering transform. Reconstructed images from trigonometric current patterns also show better spatial resolution compared to pairwise current injection patterns, skipping three electrodes.
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Aplicação da teoria ac de eletrodos porosos na investigação da cinética de dispositivos eletrocatalíticos / Application of ac theory for porous electrode in the investigation in the kinetics of electrocatalytic devisesLiliane Aparecida de Carvalho 24 October 2008 (has links)
Este trabalho consiste em utilizar a técnica de Espectroscopia de Impedância Eletroquímica (EIE) na investigação da cinética de diferentes materiais eletrocatalíticos. O modelo de eletrodos porosos se apresenta como uma forma bastante promissora no tratamento das respostas em freqüência dos ADEs. Uma vez estabelecida a aplicação do modelo, pode-se chegar à obtenção de informações cinéticas importantes durante a análise de vários fatores que ocorrem no sistema em questão, sendo possível então, confirmar resultados obtidos por outras técnicas. Foram investigados eletrodos do tipo ADEs de composição Ti/Ru0,3Ti(0,7-x)SnxO2 (x = 0; 0,3 e 0,7), investigando o efeito da eletrodeposição de Pt na superfície do ADE de Ti/Ru0,3Ti0,7O2, a fim de comparar os resultados obtidos por EIE (ac) com o estudo cinético realizado por curvas de polarização de Tafel (dc) em meio ácido. Além destes realizou-se a investigação dos ânodos, aplicáveis a células a combustível de etanol (DEFCs), de composição: Ti/Pt, Ti/Pt:Ru (80:20), Ti/Pt:Sn (80:20) e Ti/Pt:Ru:Sn (80:10:10) em meio ácido e também de etanol, utilizando-se a EIE como elemento de diagnóstico da atividade da composição do ânodo. Os resultados de EIE confirmam que, o aumento da concentração de SnO2 na composição dos ADEs, favorece a formação de oxigênio, como o apresentado na literatura, por outras técnicas eletroquímicas. A linha de transmissão de um canal apresentou valores satisfatórios dos seus elementos, coerentes com os valores apresentados na literatura, quanto utilizada a técnica da EIE. Foi observado também que adição de Pt na composição do ADE Ti/Ru0,3Ti0,7O2 melhorou a eficiência do material, apresentando menores valores de resistência à transferência de carga, A resistência de transferência de carga (Rtc) diminui à medida que se aumenta o potencial, no sentido da RDO. Analisando-se aos valores de potencial em função das curvas de polarização de Tafel e EIE, pode-se concluir então que existe um relação entre o comportamento ac e dc do sistema. Nos estudos de materiais aplicados a DEFCs, confirmam os resultados que a introdução de Sn melhora a atividade para a oxidação do etanol. A composição Ti/Pt:Sn(80:20) apresentou os melhores resultados nos testes de EIE, obtendo-se valores menores de resistência a transferência de carga, concordando com os resultados obtidos no estudo de célula a combustível. / This work consists in using Electrochemical Impedance Spectroscopy (EIS) in the research of various electrocatalytic materials. The porous electrode model is a very promising approach to treat the frequency responses of Dimensionally Stable Anodes (DSA®). Once the application of the model is established, it is possible to obtain important kinetic information while various factors occurring in the system are analyzed. This allows confirmation results obtained by other techniques. Electrodes of the DSA® type with composition Ti/Ru 0,3Ti(0,7-x)SnxO2 (x=0; 0,3 e 0,7) were investigated. In order to compare the results obtained for DSA® Ti/Ru 0,3Ti0,7O2 electrodes by EIS (ac) with the kinetic studies by Tafel (dc) polarization curves performed in acid environment. Additionally, an investigation of the anodes, applicable to Direct Oxidation of Ethanol Fuel Cells (DEFCs), with composition Ti/Pt, Ti/Pt:Ru (80:20), Ti/Pt:Sn (80:20) and Ti/Pt:Ru:Sn (80:10:10) in acid environment and also in ethanol was carried out, using EIS as a diagnosis element for the activity of the anode composition. The EIS results confirmed that increasing concentration of SnO2 in the DSA® composition enhances oxygen formation, as reported in the literature, for other electrochemical techniques. The EIS technique revealed that the transmission line of one canal provided satisfactory data for its elements, in agreement with literature data. Pt addition to the DSA® Ti/Ru 0,3Ti0,7O2 improved the material efficiency, giving smaller resistance values for charge transfer. The resistance of the charge transfer (Rtc) lowered with increasing potential, in the direction of RDO. Analysing the potential values as a function of the Tafel polarization curves and EIS, it is possible to conclude that there is a relationship between the ac and dc behaviors of the system. In the studies of materials applicable to DEFCs it was confirmed that Sn improves the activity for ethanol oxidation. The composition Ti/Pt:Sn (80:20) led to the best results in EIS tests, revealing lower resistance values in the charge transfer, in agreement with results obtained in the study of fuel cells.
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Mecanismo de condução elétrica na interface do α-Ag2WO4 e do α-Ag2-xWO4 com nanopartículas de Ag na superfície / Electrical conduction mechanism at the interface of α-Ag2WO4 e do α-Ag2-xWO4 with Ag nanoparticles on the surface.Felipe Gollino 03 August 2015 (has links)
O projeto tem como proposito estudar o comportamento elétrico da microestrutura e interface de tungstato de prata e do tungstato de prata com nanoparticulas de prata focando em uma possível aplicação como dispositivo eletrônico. Os rods de α-Ag2WO4 foram sintetizadas utilizando o método hidrotermal assistido por microondas e posteriormente submetidas a um feixe de elétrons fazendo com que os íons de prata Ag+, dentro do bulk do cristal, sejam reduzidos e migrem para a superfície do material crescendo as partículas metálicas. A nucleação desses filamentos podem ser visualizado ao vivo e in situ acompanhando as imagens de MEV-FEG da matrix do material. A fase do material, posições atômicas e o entendimento da distrorção da rede foi confirmada pela difratometria de raio-X com o refinamento Rietveld. O material foi caracterizado, estruturalmente, pelas técnicas de espectroscopia Raman e infravermelho, na qual consegue entender quais são as ligações a curto alcance que os átomos estão fazendo. Foi estudado o seu comportamento eletrônico e espectroscópico, por medidas de espectroscopia de UV-Vis-NIR determinando o valor de bandgap do material. Por meio das medidas de XPS foi possível comparar o a pureza e o o grau de oxidação da superfície. E finalmente, foram realizadas medidas de espectroscopia de impedância e condutividade elétrica em regime DC do material não-irradiado e irradiado para com o feixe de elétrons para se entender o mecanismo de condução elétrica. Pelas curvas de impedância, é possível perceber que as amostras irradiadas possuem uma resistência maior causada pelos defeitos gerados dentro da estrutura dificultando a mobilidade dentro do cristal. Foi possível notar pelas medidas elétricas, que a formação dessa superfície com o nanoparticulas altera o o contato entre os cristais do material, apresenta um desvio da linearidade, essa a fase no contorno estaria permitindo a migração dos portadores de carga nos limites dos cristais de tungstato. / This project have to aim study the electrical conduction behavior of silver tungsten and silver tungsten with Ag nanoparticles microstructures and interface on focus in a possible application in electronic device. The rods of α-Ag2WO4 were synthetized using a microwave assisted method and then target by a electron beam, making the Ag+ ions inside of the crystal, reduce and go out to surface material as nanoparticles of Ag0 metallic. This growth can be view in situ by MEV-FEG. The phase of material, atomic position and structure distortion was confirmed by DRX pattern with Rietveld refinement. The material was structural characterized for Raman and infrared spectroscopy, which could be understood what bonds at short range the atoms was doing. The electronic behavior was study by UV-Vis-NIR spectroscopy for determine the bandgap. XPS measurements were performed to compare the purity of the surface and the degree of oxidation. Finally, the samples non-irradiated and irradiated were characterized electrical with impedance spectroscopy and electrical conductivity in DC to understand the electrical conduction mechanism. For the impedance curves, it was possible to notice that the samples irradiated have a higher resistance caused by the bulk defects difficult the mobility inside de crystal. Can be observed by electrical measures, that the formation of this surface with nanoparticles modify the contact between the crystal, showing a leak of linearity, this phase in the boundary could allow the migration of the charge transport.
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Sensor químico baseado em microponte de impedância = Chemical sensor based on impedance microbridge / Chemical sensor based on impedance microbridgeRibeiro, Luiz Eduardo Bento 21 August 2018 (has links)
Orientador: Fabiano Fruett / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Elétrica e de Computação / Made available in DSpace on 2018-08-21T04:02:00Z (GMT). No. of bitstreams: 1
Ribeiro_LuizEduardoBento_M.pdf: 4022818 bytes, checksum: d2a40b9cee4f59bc80ec0b09a97c31a8 (MD5)
Previous issue date: 2012 / Resumo: A integração de sistemas microeletrônicos em lab-on-a-chip está sendo cada vez mais necessária para concretizar novas aplicações dentro do emergente campo da microfluídica. Tanto na química quanto na bioquímica e até mesmo na medicina e bioengenharia, a microfluídica evolui conquistando um espaço crescente. Entretanto, desafios tecnológicos residem na sua complexa fabricação e integração com sistemas eletrônicos. Neste trabalho, foi desenvolvido um sistema sensor que emprega métodos de fabricação compatíveis tanto com a microeletrônica quanto com a microfluídica. Este sistema sensor é baseado em uma microponte de impedância composta por quatro capacitores interdigitados. Neste sistema, o fluido, guiado por um canal ou armazenado em um reservatório fabricado em polidimetilsiloxano (PDMS), passa sobre a microponte enquanto um termistor, fabricado no mesmo substrato, permite monitorar a temperatura do sistema durante a medida. A microponte é formada de eletrodos interdigitados arranjados de forma a permitir a utilização de um circuito eletrônico de condicionamento que pode ser construído bem próximo do elemento sensor. O trabalho foi validado comparando-se a função de transferência experimental do sensor, usando como analito a mistura etanol-água, com a função de transferência teórica obtida através de simulação baseada em elementos finitos. Identificamos a importância da deposição de um filme fino de boa qualidade para a proteção dos eletrodos de referência e sua influência na função de transferência experimental. Ainda, devido à utilização de materiais inertes como ouro, vidro e PDMS, o sistema sensor, com alguns ajustes, pode ser empregado para outras aplicações: desde o monitoramento da pureza e concentração de líquidos até a caracterização de filmes finos sensíveis a patógenos e fármacos / Abstract: The integration of microelectronic systems in lab-on-a-chip is being increasingly required to implement new applications on the emerging field of microfluidics. Both in chemistry and biochemistry, and even in medicine and bioengineering, microfluidics evolves gaining a growing space. However, technological challenges lie in its complex manufacturing and integration with electronic systems. In this work, we developed a sensor system that employs both fabrication methods compatible with microelectronics and with microfluidics. This sensor system is based on an impedance microbridge composed of four interdigitated capacitors. In this system, the fluid which is guided by a channel or is stored in a reservoir made of polydimethylsiloxane (PDMS), passes over the microbridge while a thermistor fabricated on the same substrate allows monitoring of the system temperature during the measurement. The microbridge is made of interdigitated electrodes arranged so as to allow the use of an electronic conditioning circuit that can be built very close to the sensor element. The study was validated by comparing experimental transfer function of the sensor, using the ethanol-water mixture as analyte, with the theoretical transfer function obtained by simulation based on finite element method. We identified the importance of depositing a good quality thin film for the protection of reference electrodes and its influence on experimental transfer function. Also, due to the use of inert materials such as gold, glass and PDMS, the sensor system, with some adjustments, can be used for other applications: from monitoring of the concentration and purity of liquid to the characterization of thin films sensitive to drugs and pathogenic agents / Mestrado / Eletrônica, Microeletrônica e Optoeletrônica / Mestre em Engenharia Elétrica
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[en] DETERMINATION OF THE INPUT IMPEDANCE OF AN ANTENNA IN AN OPEN RECTANGULAR CAVITY / [pt] DETERMINAÇÃO DA IMPEDÂNCIA DE ENTRADA DE UMA ANTENA INTERIOR DE UMA CAVIDADE RETANGULAR ABERTARAIMUNDO JOSE DOS SANTOS MOTA 20 October 2009 (has links)
[pt] O propósito deste trabalho é apresentar formulação para a determinação da impedância de entrada de uma antena colocada no interior de uma cavidade retangular com um dos lados aberto. O procedimento utilizado consiste na determinação da potência total irradiada da qual se obtém a impedância de entrada. A colocação do problema é feito utilizando o método do casamento de modos (Mode Match). Apresentam-se algumas considerações com relação ao erro surgido com as truncagens dos modos de índices elevados, aproximações da utilização em verificação experimental e aplicações. / [en] This work presents a formulation for determining the input impedance for an antenna located inside fo a rectangular cavity having one side open. The current distribution on the antena and the total power radiater are determined using and apropriate Green’s function and anatytic procedure from which the impedance is calculated. The problem is approchea and solved using the method of Mode Matching.
Some considerations concerning the erros due to the truncation of modes of larges index used in the aproximation method are presented as well as practical consideration for experimentally verifing and applying the results.
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Multi-functional epoxy/graphene nanoplatelet compositesCao, Gaoxiang January 2016 (has links)
Graphene nanoplatelets (GNP) with thickness of 6 ~ 8 nm and lateral dimension of 5 μm (M5) and 25 μm (M25) have been used to prepare epoxy composites. Epoxy composites were fabricated initially by shear mixing to investigate the effects of filler type on the structure and properties of composites. The complex viscosity of GNP-epoxy mixture was found to increase by almost three orders of magnitude going from the neat epoxy to the 8 wt.% loading, leading to difficulties in their processing. Scanning electron microscopy of the composites showed that both fillers aggregated at high loadings with the M25 buckling more easily due to its larger diameter, which compromises its aspect ratio advantage over M5, resulting in only slightly better mechanical performance. Polarized Raman spectroscopy revealed that both M5 and M25 were randomly distributed in the epoxy matrix, After adding M5 and M25 fillers, the storage modulus increase with the filler loadings, however, the glass transition temperature (Tg) drops slightly after initial incorporation, then rises with further filler addition attributed to the pin effects of filler aggregations. In terms of electrical property, M25 has lower percolation (1 wt.%) than M5 composites due to its bigger aspect ratio, which enable M25 to form a conductive network more efficiently. Furthermore, M25 composites also have slightly better thermal and mechanical properties over that of M5 composites. However, the difference is not significant considering the aspect ratio of M25 is five times of that of M5. The reason is that the aggregation and buckling of M25 compromise its advantage over M5. Due to the better performance of M25 as filler, M25/epoxy composites were prepared by shear mixing, solvent compounding and three-roll mill. Samples made by solvent compounding display the lowest percolation threshold (0.5 wt.%), related to its relatively uniform dispersion of M25 in matrix, resulting in higher thermal conductivity and better mechanical properties. Water uptake in a water bath at 50 °C took 75 days to be saturated. Higher loaded samples have lower diffusion coefficient because of the barrier effects of GNP fillers, but have higher maximum water absorbed, which is owing to filler aggregation. Properties test of aged and unaged specimens show thermal conductivity of the aged was enhanced due to water’s higher thermal conductivity than epoxy resin matrix, while electrical performance was compromised due to the swelling effects caused by absorbed water. The mechanical properties of aged samples also dropped slightly due to plasticization effects.
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Nouveaux matériaux sans plomb à base de bismuth : vers des composés de type (A,A') (B)O₃ et (A,A') (B,B') O₃ / Syntheses of new Bi-based lead-free materials : with the formula (A,A’)(B)O₃ and (A,A’)(B,B’)O₃Lelievre, Jerome 12 October 2017 (has links)
Ce travail est consacré à la recherche de nouveaux matériaux sans plomb à structure pérovskite, de formules (A⁺,Bi³⁺)BO₃ et (A⁺,Bi³+)(B,B’)O₃ où A⁺ = {Li⁺, Na⁺, K⁺, Rb⁺}. Le but visé est le remplacement des pérovskites à base de plomb actuellement utilisées dans les dispositifs électroniques. La possibilité de substitution du plomb par un pseudo-ion (A⁺,Bi³⁺) a été étudiée pour (i) les pérovskites simples PbTiO₃ et PbZrO₃ et (ii) les pérovskites complexes Pb(Mg⅟₃Nb⅔)O₃ et Pb(Zn⅟₃Nb⅔)O₃.La synthèse de la composition (Li⅟₂Bi⅟₂)TiO₃ (LBT) a conduit à un composé pyrochlore de type Bi₂Ti₂O₇. Les autres compositions ont permis d'obtenir les pérovskites (Na⅟₂Bi⅟₂)ZrO₃ (NBZ), (K⅟₂Bi⅟₂)ZrO₃ (KBZ), (Na⅟₂Bi⅟₂)(Mg⅓Nb⅔)O₃ (NBMN), (K⅟₂Bi⅟₂)(Mg⅟₃Nb⅔)O₃ (KBMN) et (K⅟₂Bi⅟₂)(Zn⅟₃Nb⅔)O₃ (KBZN). Un important travail de synthèse a été effectué, en utilisant plusieurs voies et différents précurseurs, afin d'essayer d'éliminer les phases secondaires qui accompagnent généralement ces pérovskites.Les structures cristallines ont été étudiées par diffraction de neutrons à l'aide de la méthode de Rietveld. Celles-ci ont été déterminées pour LBT, NBZ, KBZ et KBMN. Les propriétés électriques de ces matériaux ont également été étudiées. Aucun d'entre eux n'est ferroélectrique. KBZ est électrostrictif. Enfin, NBZ, NBMN et KBMN montrent d'intéressantes propriétés de relaxeurs. / The present work focused on the research of new lead-free perovskite materials with the formula (A⁺,Bi³⁺)BO₃ and(A⁺,Bi³+)(B,B’)O₃ with A⁺ = {Li⁺, Na⁺, K⁺, Rb⁺}. The aim of this study is to find potential candidates to replace the lead-based perovskite used in the electronic devices nowadays. The possibility to substitute the lead ion par a couple (A⁺,Bi³⁺) has been examined for (i) the simple perovskites PbTiO₃ and PbZrO₃ and (ii) the complex perovskites Pb(Mg⅟₃Nb⅔)O₃ and Pb(Zn⅟₃Nb⅔)O₃.The synthesis of the composition (Li⅟₂Bi⅟₂)TiO₃ (LBT) has led to a pyrochlore Bi₂Ti₂O₇-like compound. The other compositions have conducted to the perovskites compounds (Na⅟₂Bi⅟₂)ZrO₃ (NBZ), (K⅟₂Bi⅟₂)ZrO₃ (KBZ), (Na⅟₂Bi⅟₂)(Mg⅓Nb⅔)O₃ (NBMN),(K⅟₂Bi⅟₂)(Mg⅟₃Nb⅔)O₃ (KBMN) and (K⅟₂Bi⅟₂)(Zn⅟₃Nb⅔)O₃ (KBZN). A lot of work has been carried out for the syntheses, using different precursor or process, in order to suppress the secondary phases which are often obtained with these perovskites. The crystalline structures have been studied by neutron diffraction, using the Rietveld method. These have been determined for the LBT, NBZ, KBZ and KBMN compounds. The electrical properties of these materials have also been studied. None of them is ferroelectric. KBZ is électrostrictif. Finally, NBZ, NBMN and KBMN present some interesting relaxor properties.
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