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The potential of Calcium-Vanadium garnet loaded binary composites for use in the production of planar frequency agile microwave devices has been investigated. A WR90 rectangular waveguide system using the transmission/reflection technique has been used to compare effective medium theory predicted permittivities and permeabilities for unmagnetised and transversely magnetised composites with actual measured composite properties. Use of the the Bruggeman effective medium theory with manufacturer supplied garnet permittivity and values of garnet permeability calculated using simple empirical models were demonstrated to be as accurate as predictions made using the measured properties of the composites' individual constituents. Errors in predicted material properties for unmagnetised and transversely magnetised samples relative to measured data were less than 5% across almost half of the 8.2 -12.4GHz measurement band and within a worst-case error of 15% across the whole band. A series of end-coupled linear microstrip resonators using garnet-loaded composite substrates has been fabricated and tested. Tunabilities in resonance of up to 3.9% at 9.2GHz have been demonstrated for DC magnetic bias fields applied transverse to the microwave magnetic field component. An entirely new and previously unpublished broadband microstrip technique for the measurement of the effective permittivity and permeability of bulk gyromagnetic and gyromagnetic material loaded composite substrates subject to transverse DC magnetic bias fields is presented. This will have wide application in the design of frequency agile microwave integrated circuits.

Master of Science / Department of Biological & Agricultural Engineering / Naiqian Zhang / Permittivity is an important property of dielectric materials. By measuring the permittivity of a material, it is possible to obtain information about the material’s physical and chemical properties, which are of great importance to many applications. In this study, a realtime control system for a frequency-response (FR) permittivity sensor was developed. The core of the hardware was a kitCON167 microcontroller (PHYTEC America, LLC), which controlled and communicated with peripheral devices. The system consisted of circuits for waveform generation, signal conditioning, signal processing, data acquisition, data display, data storage, and temperature measurement. A C program was developed in the TASKING Embedded Development Environment (EDE) to control the system. The control system designed in this study embodied improvements over a previously designed version in the following aspects: 1) it used a printed circuit board (PCB); 2) the measurement frequency range was extended from 120 MHz to 400 MHz; 3) the resolution of measured FR data was improved by using programmable gain amplifiers; 4) a data storage module and a real-time temperature measurement module were added to the system; 5) an LCD display and a keypad were added to the system to display the FR data with corresponding frequencies and to allow users to enter commands. Impedance transformation models for the sensor probe, the coaxial cable that connects the control system with the sensor probe, and the signal processing circuit were studied in order to acquire information on the permittivity of measured materials from measured FR data. Coaxial cables of the same length terminated with different loads, including an open circuit, a short circuit, a 50 resistor, and a 50 resistor paralleled by a capacitor, were tested. The results indicated that the models were capable of predicting the impedances of these specific loads using the FR data. Sensor probes with different sizes and coaxial cables with two different lengths terminated with the same sensor probe were also tested. The results were discussed. Additional tests for the gain and phase detector were conducted to compare FR data measured by the gain and phase detector with those observed on an oscilloscope. The results were discussed.

Les propriétés électriques des matériaux sont des données indispensables dans les phases de conception de circuits micro-ondes. Ainsi, de nombreuses méthodes ont été mises au point en s’appuyant sur des mesures de paramètres «S», pour les systèmes de transmission-réflexion, ou de fréquences de résonance, pour les méthodes résonantes. Chacune d’entre elles présente des caractéristiques adaptées à un type de géométrie d’échantillon, à une bande de fréquence d’analyse, à une précision des résultats souhaitée... Dans tous les cas, les dimensions de l’échantillon doivent être au moins de l’ordre de grandeur de la longueur d’onde et donc, les caractérisations deviennent impossibles aux basses fréquences pour des échantillons de petites tailles. Un autre inconvénient de ces méthodes est qu’il est obligatoire de connaître parfaitement l’épaisseur de l’échantillon pour déterminer avec précision les caractéristiques électriques du matériau. L’objectif de ce travail de thèse a donc consisté à mettre au point une nouvelle méthode de caractérisation en s’appuyant sur une cavité de géométrie particulière. Celle-ci permet des mesures basses fréquences pour des dimensions très inférieures à la longueur d’onde. Avec un système de couplage original, nous avons pu également obtenir une réponse en transmission particulière, caractérisée par une fréquence de résonance et une fréquence d’antirésonance. Par rapport aux méthodes classiques qui ne travaillent que sur la fréquence de résonance, cette double information permet de déterminer à la fois la permittivité du milieu mais également l’épaisseur de l’échantillon. / The electrical properties of the materials are essential data in the design phases of microwave circuits. Thus, many methods have been developed based on "S" parameter measurements, for transmission-reflection systems, or resonance frequencies, for resonant methods. Each of them has characteristics adapted to a type of the samplegeometry, to the frequency band of analysis, to a desired precision of the results... In all the cases, the dimensions of the sample must be at least of the order of the wavelength and therefore the characterizations become impossible at low frequencies for samples of small sizes. Another disadvantage of these methods is that it is mandatory to know perfectly the thickness of the sample to accurately determine the electrical characteristics of the material. The objective of this thesis work was therefore to develop a new method of characterization based on a cavity of particular geometry. This allows low frequency measurements for dimensions much smaller than the wavelength. With an original coupling system, we have also been able to obtain a particular transmission response, characterized by a resonance frequency and an antiresonance frequency. Compared to conventional methods that only work on the resonant frequency, this double information makes it possible to determine both the permittivity of the medium but also the thickness of the sample.

Neste trabalho pós de CaCu3Ti4O12 foram preparados por reação em estado sólido e por técnicas de solução: complexação de cátions e coprecipitação dos oxalatos. Foram realizados estudos de formação de fase, densificação e propriedades dielétricas das cerâmicas sinterizadas. Para efeito comparativo, ta is propriedades foram determinadas em amostras puras e contendo dissilicato de lítio (LSO) e fluoreto de lítio (LiF) como aditivos de sinterização. O principal objetivo foi verificar o efeito do uso dos diferentes aditivos de sinterização na microestrutura, densificação e propriedades dielétricas do CCTO. Os principais resultados revelaram que pós preparados por técnicas de solução apresentam fase única após calcinação em condições selecionadas. Foi verificado que os aditivos influenciam na densificação, possibilitando obter cerâmicas com 95% da densidade teórica do CCTO a 1025°C. As amostras preparadas por diferentes técnicas apresentam propriedades similares, com exceção das características microestruturais. A permissividade elétrica determinada à temperatura ambiente é da ordem de 104 independentemente do método de síntese. As menores perdas dielétricas foram obtidas para amostras contendo LiF como aditivo de sinterização. / In this work the effects of the method of synthesis and sintering additives on the microstructure and dielectric properties of CCTO were investigated. Powder mixtures were prepared by the cation complexation and coprecipitation methods, and by mixing of the starting oxides, for comparison purposes. Lithium dissilicate (LSO) and lithium fluoride (LiF) were used as sintering aids. The main results revealed that powders prepared by solution techniques have single phase after calcination at selected conditions. The additives were found to influence the densification allowing for obtaining high relative density (≥ 95%) at 1025ºC. Specimens prepared by different methods show similar properties except on microstructure features. The electric permittivity is of the order of 104 for all investigated specimens independent on the method of synthesis. The dielectric loss is found to be lower for specimens prepared with LiF as sintering aid.

O conhecimento das propriedades dielétricas do osso tem se mostrado importante na medicina ortopédica para aplicações em diagnóstico e tratamento da osteoporose, de fraturas, controle da osteonecrose e, também, na área de cerâmicas industriais (porcelana de osso). Neste trabalho, apresenta-se uma metodologia de avaliação das permissividades complexas de osso cortical de fêmur bovino desidratado, utilizando-se o método de impedância em uma linha de transmissão. Esta se constitui de um condutor coaxial, do tipo N, de uma porta, e um terminal aberto, que é conectado a um analisador de impedância. A faixa de freqüência considerada está compreendida entre 100 Hz e 1 MHz. Em particular, apresenta-se uma metodologia de caracterização dielétrica de osso, com ênfase nas avaliações das suas características anisotrópicas. Alguns resultados das propriedades dielétricas são comparados com os valores experimentais e teóricos disponíveis na literatura. Este procedimento é justificado, haja vista que os valores experimentais encontrados na literatura são esparsos e pontuais, quando se considera toda a faixa do espectro eletromagnético avaliado. Ressalta-se que não existe um consenso entre especialistas da área sobre a precisão e metodologia de obtenção destes. O mesmo ocorre com relação aos protocolos de medição propostos nas normas internacionais, em particular, quando se buscam padrões de avaliações de materiais biológicos sólidos. Os valores da permissividade obtidos com as medidas realizadas entre 100 Hz e 1 MHz evidenciam a presença de uma anisotropia efetiva, sendo esta característica ressaltada em freqüências da ordem de algumas dezenas de kHz. Embora o fenômeno de anisotropia não se manifeste nas faixas superiores à anteriormente mencionada, algumas medidas foram realizadas, também, numa faixa de freqüências superiores, entre 50 MHz e 3 GHz. Utilizou-se um analisador de redes conectado a um dispositivo coaxial de duas portas, visando avaliar a adequabilidade dos procedimentos de preparação do tecido ósseo na avaliação das características de materiais biológicos em altas freqüências, já que se dispunha da instrumentação necessária e de alguns resultados, obtidos na literatura, para sua validação. / The knowledge of the dielectric properties of bones has become important to orthopedic therapy, for applications in the diagnosis and treatment of osteoporosis, fractures, and osteonecrosis, as well as is the industrial ceramics field (bone china). This work proposes a methodology for the evaluation of the complex permittivity of a dehydrated cortical bone of bovine femur, using an impedance method in a transmission line. The transmission line is composed by an one-port open-ended N-type coaxial conductor, connected to an impedance analyzer. The frequency range studied was 100 Hz - 1 MHz. The methodology proposed is proper for the dielectric characterization of bone and this work emphasizes the evaluation of its anisotropic characteristics. Some dielectric properties experimentally found in this work are compared to the experimental and theoretical results available in literature, which are sparse and punctual in the considered electromagnetic spectrum. It is pointed out that there is no agreement among the experts when the subject is the proper measuring methodology and its precision. The same occurs when the subject is the measuring protocols proposed by the international standards, especially for solid biological materials. The permittivity results obtained in frequencies between 100 Hz and 1 MHz evince an effective anisotropy, which stands out in frequencies of a few tens of kHz. Although the anisotropy phenomenon does not occur in a frequency range higher than the one previously mentioned, some measures were taken in the 50 MHz - 3 GHz range for validation, based on results from literature. A network analyzer and a two-port coaxial device were then used in such measures, which aimed the evaluation of the adequacy of the procedure used in the preparation of the bone tissue in high-frequency measurements.

O conhecimento das propriedades dielétricas do osso tem se mostrado importante na medicina ortopédica para aplicações em diagnóstico e tratamento da osteoporose, de fraturas, controle da osteonecrose e, também, na área de cerâmicas industriais (porcelana de osso). Neste trabalho, apresenta-se uma metodologia de avaliação das permissividades complexas de osso cortical de fêmur bovino desidratado, utilizando-se o método de impedância em uma linha de transmissão. Esta se constitui de um condutor coaxial, do tipo N, de uma porta, e um terminal aberto, que é conectado a um analisador de impedância. A faixa de freqüência considerada está compreendida entre 100 Hz e 1 MHz. Em particular, apresenta-se uma metodologia de caracterização dielétrica de osso, com ênfase nas avaliações das suas características anisotrópicas. Alguns resultados das propriedades dielétricas são comparados com os valores experimentais e teóricos disponíveis na literatura. Este procedimento é justificado, haja vista que os valores experimentais encontrados na literatura são esparsos e pontuais, quando se considera toda a faixa do espectro eletromagnético avaliado. Ressalta-se que não existe um consenso entre especialistas da área sobre a precisão e metodologia de obtenção destes. O mesmo ocorre com relação aos protocolos de medição propostos nas normas internacionais, em particular, quando se buscam padrões de avaliações de materiais biológicos sólidos. Os valores da permissividade obtidos com as medidas realizadas entre 100 Hz e 1 MHz evidenciam a presença de uma anisotropia efetiva, sendo esta característica ressaltada em freqüências da ordem de algumas dezenas de kHz. Embora o fenômeno de anisotropia não se manifeste nas faixas superiores à anteriormente mencionada, algumas medidas foram realizadas, também, numa faixa de freqüências superiores, entre 50 MHz e 3 GHz. Utilizou-se um analisador de redes conectado a um dispositivo coaxial de duas portas, visando avaliar a adequabilidade dos procedimentos de preparação do tecido ósseo na avaliação das características de materiais biológicos em altas freqüências, já que se dispunha da instrumentação necessária e de alguns resultados, obtidos na literatura, para sua validação. / The knowledge of the dielectric properties of bones has become important to orthopedic therapy, for applications in the diagnosis and treatment of osteoporosis, fractures, and osteonecrosis, as well as is the industrial ceramics field (bone china). This work proposes a methodology for the evaluation of the complex permittivity of a dehydrated cortical bone of bovine femur, using an impedance method in a transmission line. The transmission line is composed by an one-port open-ended N-type coaxial conductor, connected to an impedance analyzer. The frequency range studied was 100 Hz - 1 MHz. The methodology proposed is proper for the dielectric characterization of bone and this work emphasizes the evaluation of its anisotropic characteristics. Some dielectric properties experimentally found in this work are compared to the experimental and theoretical results available in literature, which are sparse and punctual in the considered electromagnetic spectrum. It is pointed out that there is no agreement among the experts when the subject is the proper measuring methodology and its precision. The same occurs when the subject is the measuring protocols proposed by the international standards, especially for solid biological materials. The permittivity results obtained in frequencies between 100 Hz and 1 MHz evince an effective anisotropy, which stands out in frequencies of a few tens of kHz. Although the anisotropy phenomenon does not occur in a frequency range higher than the one previously mentioned, some measures were taken in the 50 MHz - 3 GHz range for validation, based on results from literature. A network analyzer and a two-port coaxial device were then used in such measures, which aimed the evaluation of the adequacy of the procedure used in the preparation of the bone tissue in high-frequency measurements.

Cemented Paste Backfill (CPB) is a relatively new backfilling technology for which a better understanding of binder hydration is required. This research uses electromagnetic (EM) wave-based techniques to non-destructively study a CPB consisting of tailings, sand, process water and binder (90% blast-furnace slag; 10% Portland cement). EM experiments were performed using a broadband network analyzer (20 MHz to 1.3 GHz) in the lab and capacitance probes (70 MHz) in the lab and field. Results showed that the EM properties are sensitive to curing time, operating frequency and specimen composition including binder content. The volumetric water content interpreted from dielectric permittivity varied little with curing. Temporal variations in electrical conductivity reflected the different stages of hydration. Laboratory results aided interpretation of field data and showed that a reduction in binder content from 4.5% to 2.2% delays setting of CPB from 0.5 days to over 2 days, which has important implications for mine design.

Cemented Paste Backfill (CPB) is a relatively new backfilling technology for which a better understanding of binder hydration is required. This research uses electromagnetic (EM) wave-based techniques to non-destructively study a CPB consisting of tailings, sand, process water and binder (90% blast-furnace slag; 10% Portland cement). EM experiments were performed using a broadband network analyzer (20 MHz to 1.3 GHz) in the lab and capacitance probes (70 MHz) in the lab and field. Results showed that the EM properties are sensitive to curing time, operating frequency and specimen composition including binder content. The volumetric water content interpreted from dielectric permittivity varied little with curing. Temporal variations in electrical conductivity reflected the different stages of hydration. Laboratory results aided interpretation of field data and showed that a reduction in binder content from 4.5% to 2.2% delays setting of CPB from 0.5 days to over 2 days, which has important implications for mine design.

The key features of dynamics of ultraslowing glass forming systems are their universality in diversity. Its origin is recognized as one of the greatest challenges of condensed matter physics and materials engineering in the XXI century. Similar phenomena are observed on approaching the glass transition in low molecular weight supercooled liquids, polymers, colloidal fluids as well as in solids, for instance in orientationally disordered crystals, spin glass-like magnetic, vortex glasses. Pre-vitreous dynamics is also proposed as a general reference for the category of complex liquids/soft matter systems. The upsurge of the primary relaxation time or related dynamical properties is the basic physical phenomena of the still mysterious previtreous behavior. This means a much more pronounced slowing down than the Arrhenius pattern observed far above the glass transition temperature. Portraying this behavior constitutes one of key checkpoints for theoretical models developed to unwind the glass transition puzzle. However, none of the aforementioned features can answer the understanding that governs the increase of relaxation time in liquids upon cooling. In this thesis we focus on the above questions studying the dynamics of some materials for which their molecules can retain a translational order being orientationally disordered between them upon cooling, which are referred to plastic phases or orientationally disordered (OD) crystalline phases. The work presented in this thesis potentially extends the knowledge of dynamics of OD phases and orientationally glasses (OG), a research topic which has gained interest during the last decades. Through this study, especial attention has been devoted to the phenomenological equations accounting to the temperature dependence of the mean relaxation time describing the orientational dynamics .The study was carried out by the use of BDS as well as two complementary experimental techniques. We show distortion-sensitive and derivative-based empirical analysis of the validity of leading equations for portraying the previtreous evolution of primary relaxation time. A new method for studying the dynamics of glass forming systems is introduced and the minimization procedure is validated and discussed. We present the results divided in two topics, the dynamics of the pure compounds and mixed crystals and the derivative analysis through different existing models. In the first topic we focus on the dynamics of the pure compounds and mixed crystals formed between cycloheptanol and cyclooctanol as well as the a-relaxation dynamics of 1-cyano-adamantane and its mixtures with 1-chloro-adamantane. The second topic is divided in two groups of models, linearized and non-linearized models. In the linearized models we show the application of the derivative based, distortion-sensitive analysis to liquid crystals (LC) and OD phases. We also discuss the results concerning to the cases of the olygomeric liquid epoxy resin (EPON828), neopentylalcohol and neopentylglycol mixture, isooctylcyanobiphenyl and propylene carbonate. The possible empirical correlations between one of the linearized models with the universal pattern for the high frequency wing of the loss curve for primary relaxation time for LCs and OD phases is also shown. In the final part we show that the form of the equation recently introduced by Mauro et al. does not allow a similar straightforward linearization procedure. Unlike the previous models, the involved parameters are not correlated with the slope and the intercept of a linear function. In order to solve this problem, we have introduced the concept of the enthalpy space. The evidences of the existence of crossovers as well as quantitative descriptions are discussed. We show also a new procedure for detecting the crossover in a very easy way. A new kind of crossovers which seems to be impossible to be detected by the classical Stickel transformation is presented. / La principal característica de la dinámica de sistemas vítreos viscosos, es su universalidad en la diversidad. Su origen es uno de los mayores desafíos de la física de la materia condensada y de la ingeniería de materiales en el siglo XXI. La fenomenología típica de las fases vítreas se observan cerca de la transición vítrea en líquidos subenfriados de bajo peso molecular, polímeros, fluidos coloidales, así como en los sólidos con fases orientacionalmente desordenadas. La imposibilidad de explicar las causas del gran aumento del tiempo de relajación al enfriar un líquido, constituye uno de los problemas más importantes no resueltos en materia condensada. Con el objetivo de dar respuesta a dicha interrogante, se han propuesto modelos termodinámicos y dinámicos que han resultado inconsistentes. En esta tesis nos centramos en dicha problemática, estudiando la dinámica orientacional de algunos materiales que al ser enfriados pueden conservar un orden traslacional mientras que se conserva el desorden orientacional de las moléculas que los forman. Dichas fases se conocen como fases plásticas u orientacionalmente desordenadas (OD). El trabajo presentado en esta tesis amplía el conocimiento de la dinámica de dichas fases, un tema de investigación cuyo interés ha aumentado durante las últimas décadas. Se ha dedicado una atención especial a las ecuaciones fenomenológicas que describen la dependencia del tiempo de relajación con la temperatura. El estudio se ha llevado a cabo mediante el uso de espectroscopía dieléctrica de banda ancha, así como mediante el uso de técnicas experimentales complementarias. Se ha introducido un nuevo método para el estudio de la dinámica de los sistemas que dan lugar a fases vítreas. El método ha sido validado y discutido. Los resultados de esta tesis se presentan divididos en dos temas, por un lado, la dinámica de compuestos puros y de los cristales mixtos y, por otro, el análisis mediante el método derivativo aplicado a los diferentes modelos físicos existentes. En el primer tema nos centramos en la dinámica de los compuestos puros y los cristales mixtos formados por cicloheptanol y ciclooctanol, así como la dinámica de la relajación alfa en 1-ciano-adamantano y sus mezclas con 1-cloro-adamantano. El segundo tema se divide en dos grupos de modelos, los modelos lineales y no lineales. En los modelos lineales se muestra la aplicación del procedimiento de derivativo en los cristales líquidos (CL) y las fases OD. También se discuten los resultados relativos a los casos de la resina líquida (EPON828), la mezcla neopentil-alcohol y neopentil-glicol, el carbonato de propileno, así como el CL isooctilcianobifenil. Se discute también la existencia de posibles correlaciones empíricas entre uno de los modelos lineales con el patrón universal para la parte de alta frecuencia de la curva de pérdidas dieléctricas de la relajación primaria para las fases CL y OD. En la parte final se muestra que la forma de la ecuación introducida recientemente por Mauro et al. no permite la linearización mediante el método derivativo. A diferencia de los modelos anteriores, los diferentes parámetros no están correlacionados con la pendiente y el origen de coordenadas de una función lineal. Para resolver este problema, hemos introducido el concepto del espacio entálpico. Se analiza también la existencia de cambios de comportamiento dinámicos y se aportan descripciones cuantitativas. Se muestra también un nuevo procedimiento para detectar los cambios dinámicos de una manera fácil, que permite incluso detectar aquéllos que son obviados mediante el método clásico de Stickel.