[pt] Este trabalho mostra um estudo experimental realizado numa cavidade ressonante cilindra, dentro da qual, através de um tubo concêntrico à mesma, escoam fluídos. Dentro desta cavidade é inserida potência em microondas, que tem por objetivo aquecer o fluido escoante. Não é trivial prever-se a distribuição do campo elétrico dentro de uma cavidade ressonante, pois a forma geométrica da cavidade, conjuntamente com diversos parâmetros do material nela inserido, para absorver potência em microondas são variáveis que muito influenciam na intensidade e distribuição do campo eletromagnético interno à mesma. Por isso, ao se aquecer amostras cujas dimensões não permitem analisar-se o grau de absorção de energia através da teoria da perturbação em cavidades, faz-se necessário ema verificação experimental, além da teórica, no estudo do processo. O objetivo deste trabalho é analisar a influência de perturbações do interior da cavidade, visando-se a possibilidade de otimização prática do aquecimento de fluidos nesta. Tais alterações no interior da cavidade são três hastes metálicas localizadas numa seção transversal da mesma, além da variação do diâmetro externo do tubo pelo qual o fluido a ser aquecido escoará. O estudo das cavidades, em busca da otimização do aquecimento dentro das mesmas, traz, como retorno, menor desperdício de energia aplicada nestes sistemas de aquecimento. / [en] This work shows an experimental study accomplished on a cylindrical resonant cavity, inside of which, through a tube concentric to it, fluids flow. Inside the cavity is inserted microwave power, whose aim is to heat the flowing fluid. It s not trivial to foresee the electric field distribution inside a resonant cavity. Its geometric shape, together with several parameters, and the material in it inserted to absorb microwave power are variables that influence on the intensity and electromagnetic field distribution inside de cavity. Therefore, to heat samples whose dimensions don’t allow the absorption degree of energy through perturbation theory in cavities to be analyzed, it is necessary to verify both experimentally and theoretically all the process on study. The objective of this work is to analyze the influences of disturbances inside a cavity, seeking the practical possibility of heating optimization of the fluids inside of it. Such modification consists of three metallic stems placed on a transversal section of the cavity, besides the variation of the tubes external diameter where the fluid to be heated will flow. The cavitie s study, seeking for the optimization of the heating inside of it, has a result less waste of applied energy on these heating systems.

Ces dernières années, l’intérêt croissant porté aux considérations environnementales et à la sécurité des procédés pose la question de l’utilisation de solvants pétrochimiques nocifs non renouvelables tels que l’hexane, mais aussi de la quantité d’énergie investie dans le procédé de trituration des graines oléagineuses. L’objectif de cette thèse a donc consisté en la recherche et le développement de procédés d’éco-extraction d’huile végétale, issue de graines oléagineuses, grâce à des technologies innovantes (ultrasons et micro-ondes) et des solvants alternatifs plus respectueux de la santé et de l’environnement. La première partie de ce manuscrit propose en premier lieu l’optimisation du procédé d’extraction à l’hexane d’huile de colza à partir d’écailles de pression avec des ultrasons. Bien que ceux-ci aient un impact positif sur les rendements, le temps d’extraction et la consommation de solvant, l’utilisation de l’hexane reste problématique. Dans une deuxième partie, la substitution de l’hexane par des solvants alternatifs plus « verts » a donc été considérée. Une première approche expérimentale a été complétée par une approche prédictive grâce à l’utilisation d’outils d’aide à la décision : les paramètres de solubilité de Hansen et le modèle COSMO-RS. Cette démarche a conduit à la sélection d’un solvant, le 2-méthyltétrahydrofurane, pour la réalisation d’une étude complète allant de l’échelle laboratoire à l’échelle pilote. Dans une troisième et dernière partie, la combinaison de solvants alternatifs avec une technique innovante, les micro-ondes, pour l’extraction d’huile colza à partir d’écailles de pression a été envisagée. Cette étude a mis en évidence l’intérêt des micro-ondes dans le cas d’une sélectivité de chauffage entre la biomasse et le solvant. / In recent years, the growing interest in environmental considerations and process safety raises the issue of the use of non-renewable petrochemical harmful solvents such as hexane, but also the amount of energy invested in the process of oilseed crushing. The objective of this thesis has consisted in the research and development of green extraction processes of vegetable oil from oil seeds through innovative technologies (ultrasonic and microwave) and alternative solvents more respectful of health and environment. The first part of this manuscript describes the optimization with ultrasound of the extraction process, using hexane, of oil from rapeseed cake. Although ultrasound have a positive impact on extraction yield, extraction time and solvent consumption, the use of hexane remains questionable. In the second part, substituting hexane by "green" alternative solvents has been considered. A first experimental approach was supplemented by a predictive approach through the use of decision tools: Hansen solubility parameters and COSMO-RS model. This led to the selection of a solvent, 2-methyltetrahydrofuran, for conducting a comprehensive study from laboratory to pilot scale. In a third and final part, the combination of alternative solvents with an innovative technology, microwaves, for the extraction of oil from rapeseed cake was investigated. This study highlighted the benefit of microwaves in the case of a selective heating between biomass and solvent.

A series of experimental results about unusual heating of carbon nanotubes by microwaves is analyzed in this dissertation. Two of vibration types, cantilever type (one end is fixed and the other one end is free), the second type is both ends are fixed, have been studied by other people. A third type of forced vibration of carbon nanotubes under an alternating electromagnetic field is examined in this paper. Heating of carbon nanotubes (CNTs) by microwaves is described in terms of nonlinear dynamics of a vibrating nanotube. Results from the model provide a way to understand several observations that have been made. It is shown that transverse vibrations of CNTs during microwave irradiation can be attributed to transverse parametric resonance, as occurs in the analysis of Melde's experiment on forced longitudinal vibrations of a stretched elastic string. For many kinds of carbon nanotubes (SWNT, DWNT, MWNT, ropes and strands) the resonant parameters are found to be located in an unstable region of the parameter space of Mathieu's equation. Third order wave equations are used to qualitatively describe the effects of phonon-phonon interactions and energy transfer from microwaves to CNTs. This result provides another way to input energy from microwaves to carbon nanotubes besides the usual Joule heating via electron-phonon interaction. This model appears to be the first to point out the role of nonlinear dynamics in the heating of CNTs by microwaves.

[pt] A crescente demanda por dispositivos portáveis de tamanho e peso cada vez mais reduzidos vem estimulando a busca por materiais de alta constante dielétrica e baixas perdas na faixa de freqüência de microondas capazes de permitir a integração e miniaturização de circuitos. No presente trabalho foi realizado um estudo teórico e experimental sobre a utilização de filmes de alta constante dielétrica na fabricação de dispositivos passivos de microondas de tamanhos reduzidos. Foi feita uma análise no domínio da freqüência sobre a influência desses filmes nas características de diferentes configurações de linhas de transmissão planares com múltiplas camadas dielétricas. A partir dessa análise, foi escolhida a configuração, denominada aqui de QCPW (Quase-Coplanar Waveguide), que permite a realização prática de estruturas com diversos valores de impedância utilizando dimensões transversais confortáveis. Filmes espessos de compostos de titanato de cálcio e de titanato de magnésio depositados pelo método de screen-printing e filmes finos de titanato de estrôncio por RF Magnetron Sputtering foram fabricados e caracterizados. O método do ressoador linear CPW e da linha de transmissão CPW foram empregados para determinar o valor da constante dielétrica e da tangente de perdas desses filmes na faixa de freqüência de microondas e à temperatura ambiente. O método do ressoador linear CPW foi adaptado e aperfeiçoado para fornecer resultados satisfatórios para o caso dos filmes finos. Finalmente, foram projetados, analisados e fabricados, pela primeira vez, transformadores de impedância em linhas de transmissão (TLT) de tamanho reduzido e com resposta banda larga baseados na configuração QCPW utilizando filmes de alta constante dielétrica. / [en] The growing demand for portable devices with more reduced size and weight has stimulated the search for materials with high dielectric constant and low losses in the microwave frequency range allowing circuit integration and miniaturization. In this work, a theoretical and experimental study of the use of high dielectric constant films in the fabrication of microwave passive devices with reduced sizes has been made. A frequency domain analysis of the influence of these films on the characteristics of different configurations of multilayer transmission lines has been done. From this analysis, a configuration, called here as QCPW (Quasi-Coplanar Waveguide), that allows a practical implementation of structures with several values of impedance using comfortable transversal dimensions was chosen. Composite thick films of calcium titanate and magnesium titanate deposited by screen-printing and thin films of strontium titanate deposited by RF Magnetron Sputtering have been elaborated and characterized. CPW linear resonator method and CPW transmission line have been used to determinate the value of the dielectric constant and loss tangent of these films in the microwave frequency range at room temperature. The CPW linear resonator method was adapted and improved in order to provide satisfactory results for the case of thin films. Finally, for the first time, impedance transmission line transformers (TLT) with reduced size and wide-band response, based on the QCPW configuration using high dielectric constant films have been designed, analyzed, and fabricated.

Bearing in mind environmental concerns and global trends in ecology, biodegradable polyesters have gained enormous attention as alternative to non-biodegradable, commercial polymers used mainly in packaging industry contributing to the worldwide environment pollution. However, substitution of conventional polymers with biodegradable polyesters is limited due to their inferior mechanical and barrier properties, which can be improved by the introduction of relatively small content of non-toxic nanofillers. Nevertheless, environmental pollution is not only affected by material itself, but also manufacturing and processing sector in terms of energy sustainability. In case of the latter, low energetic processes are nowadays preferential. Thus, using microwave irradiation as the more efficient energy source, which can lead to shortening of process time, has become currently investigated subject. In this thesis, microwave-assisted in-situ synthesis of biodegradable nanocomposites based on polycaprolactone and non-toxic clay nanoparticles (layered double hydroxides) was studied and described in detail in four subsections (4.1-4.4). The first subsection (4.1) describes one-pot synthesis of Mg2+ /Al3+ layered double hydroxides functionalized with highly microwave-absorbing ionic liquids. In order to improve...

Les sulfoximines sont une famille de composés dont les domaines d’applications sont très variés. Elles sont utilisées comme auxiliaires, ou ligands pour la synthèse asymétrique et répertoriées comme groupements à forts potentiels dans des composés biologiquement actifs. Les sulfoximines fluorées sont bien plus rares et difficiles d’accès, mais de par les propriétés spéciales induites par le fluor, ont récemment attirées l’attention. Elles ont notamment été utilisées avec succès en tant que réactifs de (per)-fluoroalkylation ou comme groupements super-électroattracteurs. Cependant, il n’y a que de rares exemples de sulfoximines fluorées dans des composés bioactifs. De plus, à notre connaissance, les S-perfluoroalkyl sulfoximines n’ont encore jamais été utilisées comme ligands de métaux ou organocatalyseurs.La thèse porte sur le développement de la synthèse et la fonctionnalisation des sulfoximines fluorées pour la préparation de ligands et d’organocatalyseurs, notamment en version énantiopures. Elle est divisée en 3 chapitres.Le premier chapitre porte sur la synthèse des sulfoximines et des sulfilimines fluorées énantiopures. Sur différentes étapes de la synthèse de ces composés, plusieurs méthodes ont été utilisées, par exemple, la séparation de diastéréoisomères par l’acide de camphorsulphonique, l’oxydation asymétrique de Kagan, Modena, Uemura et aussi l’imination oxydante asymétrique. La CFS (Chromatographie par Fluide Supercritique) semi-préparative a permis de séparer les différents énantiomères des sulfilimines fluorées. L’oxydation des sulfilimines a permis d’obtenir les sulfoximines énantiopures avec de bons rendements. Ces sulfilimines et sulfoximines ont des configurations absolues stables, leurs caractéristiques optiques ont été mesurées ainsi que leurs structures ont été déterminées par diffraction des rayons-X. Le deuxième chapitre est principalement axé sur la N-fonctionnalisation des sulfoximines et leurs développements comme ligands et organocatalyseurs pour la catalyse. Nous avons pu montrer que l’utilisation des micro-ondes pour activer le couplage entre les sulfoximines libres et les aromatiques halogénés permettait d’obtenir de bons résultats et même de diminuer le temps de réaction par rapport à la méthode de chauffage conventionnel. Ce développement a également été utilisé pour préparer des ligands/organocatalyseurs chiraux. Ces nouveaux ligands, sulfoximines fluorées chirales, ont été appliqués dans des procédés de catalyse pour la réaction de Friedel-Crafts, de Biginelli et même comme réactif de Shibata asymétrique pour la trifluoromethylation. Nous avons montré également que ces composés peuvent être utilisés comme ligands ou organocatalyseurs chiraux dans la réaction de Mukaiyama ou de cycloaddition de Diels-Alder conduisant aux produits avec de bons rendements.Le dernier chapitre est basé sur la fonctionnalisation des sulfoximines fluorées par une réaction inédite d’ortholithiation. Dans cette partie, nous démontrons que la fonction sulfoximine fluorée joue le rôle de groupe ortho-directeur. Cela nous a permis d’accéder à une grande variété de sulfoximines orthosubstituées aux structures totalement nouvelles. Les produits dérivés ortho ont été utilisés comme réactifs dans de nombreuses réactions: dans la réaction de Sonogashira, dans la préparation de nouveaux réactif de trifluorométhylation et dans la synthèse d’analogues de composés biologiquement actifs. / Sulfoximines belong to a family of compounds with various application areas. They are used as auxiliaries or ligands for asymmetric synthesis and classified as high potential groups in biologically active compounds. Fluorinated sulfoximines are even more scarce and difficult to access, but special properties induced by fluorine, have attracted particular attention. They have been successfully used as (per)-fluoroalkylating reagent or as super-electron-withdrawing groups. However, there are only a few examples of fluorinated sulfoximines in bioactive compounds. To our knowledge, S-perfluoroalkylated sulfoximines have never been used as ligands of metals or organocatalysts so far.The Thesis focuses on the synthesis and functionalization of fluorinated sulfoximines for the preparation of chiral ligands and/or organocatalysts. It is divided into three chapters.The first chapter deals with the synthesis of enantiopure fluorinated sulfoximines and sulfilimines. During our synthesis, several methods were used, for example, separation of diastereoisomers by using camphorsulphonic acid, and the asymmetric oxidation of Kagan, Modena, Uemura as well as the asymmetric oxidizing imination. The SFC (Supercritical Fluid Chromatography) semi-preparative permits to separate the different enantiomers of fluorinated sulfilimines. Oxidation of sulfilimines led to the formation of enantiopure sulfoximines in good yields. These sulfilimines and sulfoximines are stable retaining their absolute configuration. Optical characteristics were measured and their structures were determined by X-ray diffractions. The second chapter focuses mainly on the N-functionalization of sulfoximines and their developments as organocatalysts and/or ligands for catalysis. Coupling reaction of free sulfoximines with halogenated aromatic under microwave activation led to the formation of products in good yields within short reaction time. This development has also been used to prepare chiral ligands/ organocatalysts. These new chiral fluorinated sulfoximines have been applied in catalytic processes for Friedel-Crafts reaction, Biginelli transformation and as Shibata’s asymmetric trifluoromethylation reagent. We also showed that these compounds may be used as chiral ligands or organocatalysts in Mukaiyama reaction or in Diels-Alder cycloaddition affording products in good yields.The last chapter is based on the functionalization of fluorinated sulfoximines by an ortholithiation reaction. In this part, we have demonstrated that the fluorinated sulfoximine function acts as ortho-directing group. This allowed us to access a wide variety of new ortho-substituted sulfoximine structures. Ortho-derivatives were used as reagents in Sonogashira reaction, in the preparation of novel trifluoromethylation reagents and in the synthesis of some biologically active compound analogues.

L’objectif de ce travail de thèse est d’étudier des lasers semi-conducteur issus de la plateforme d’intégration III-V sur Si et présentant un faible bruit d’intensité relatif (RIN) pour le transport de signaux RADAR par voie optique. Nous cherchons à obtenir des lasers de comportement dynamique dit de «Classe A», i.e. avec une réponse dynamique sans oscillations de relaxation. Dans ce cas, il a été précédemment montré qu’un tel comportement dynamique présente un RIN limité au bruit de grenaille sur une large bande de fréquences et est obtenu quand la durée de vie des photons dans la cavité est grande devant la durée de vie des porteurs dans la zone active. La plateforme photonique sur silicium est alors intéressante car elle permet de réaliser des cavités longues grâce aux guides optiques offrant de faibles pertes de propagation, i.e. de l’ordre du dB/cm. En première approche, nous avons étudié des lasers dont la cavité de longueur centimétrique est composée d’une partie active fournissant le gain optique et d’une partie passive composée de guide en silicium à faibles pertes de propagation. Nous avons proposé différentes optimisations des pertes optiques intra-cavité ainsi que différentes solutions de filtrage spectral à grande finesse nécessaire à une oscillation laser monomode. La seconde approcheétudiée repose sur le filtrage du RIN d’un laser hybride de longueur millimétrique en exploitant les effets de saturation du gain optique dans un amplificateur optique à SC (SOA). Nous avons présenté un modèle décrivant les différents mécanismes altérant le bruit du laser amplifié par un SOA. Une étudeexpérimentale a permis de mettre en évidence la réduction du RIN d’un laser hybride III-V sur silicium, allant jusqu’à 15 dB pour des fréquences allant jusqu’à quelques GHz. La dernière approche explorée dans cette thèse repose sur la conception de lasers DFB hybride III-V sur silicium à très haut facteur de qualité. L’utilisation d’un réseau de Bragg à pas variable permet de réduire les pertes radiatives, usuellement importantes dans les lasers DFB, et d’obtenir une cavité de facteur de qualité de l’ordre de quelques millions. Un premier composant réalisé présente un facteur de qualité de 65 000. / The objective of the present thesis is to investigate new laser architectures with low Relative Intensity Noise (RIN) using the Silicon Photonics integration platform. We intend to reach “class-A” dynamics, in which relaxation oscillations are eliminated. In this conditions, lasers with class-A dynamics exhibit shot-noise limited RIN over a wide frequency bandwidth, typically from 100 MHz to 20 GHz. Such behaviour can be obtained with high-Q laser cavities, i.e with long cavities or with ultra-low losses cavities. The silicon photonics platform is a good candidate for the desired dynamical behaviour as it makes possible the implementation of long cavities (ten’s of cm) based on low losses silicon waveguides (dB/cm). Three different approaches have been considered in the present work. In the first approach, we have developed centimetre long lasers, consisting of an active section providing the optical gain coupled to a passive section made with low losses silicon waveguides. We proposed different approaches to optimize the intra-cavity optical losses, and different architectures of high finesse optical filters allowing simultaneously single-mode operation and high side mode suppression. The second approach consists on filtering the laser RIN by taking advantage of the coherent population oscillations effects in a SC Optical Amplifier (SOA). We proposed a model for describing the different mechanisms altering the RIN of the amplified laser. We demonstrated 15 dB RIN reduction for frequencies up to a few GHz, using a hybrid III-V on Si laser and a “classical” SOA. The last approach explored in the present thesis is based on the use of hybrid III-V on silicon DFB lasers with a high quality factor. Using Silicon Bragg grating with a variable pitch can reduce the radiative losses, usually important in DFB lasers. In this case, we can obtain optical cavities with few millions quality factor, leading to few ns photon lifetime. We realize a first design of Si Bragg grating with a Q factor of 65 000.

This thesis aimed to investigate the relativistic magnetron (RM), which is a high-power microwave (HPM) source. Since the RM can generate high-intensity microwave radiation, it can be used as a pulsed electromagnetic weapon to target electronic systems in different objects, such as drones, missiles, or vehicles. Other applications include electromagnetic compatibility (EMC) testing. In this thesis, a novel design of an RM with a transparent cathode configuration was investigated. This RM, referred to as the FOI-magnetron, was developed with the goal of generating the more advantageous TE11 mode of microwaves. This thesis starts with an in-depth theoretical exploration of the physics surrounding the RM, followed by a proof-of-concept study, where we compare our simulation results against published data. We then investigate the FOI-magnetron to determine if the transparent cathode configuration is more favourable than a solid cathode configuration. Particle-in-cell (PIC) simulations in MAGIC3D were used to study the RM, and extensive parameter studies were conducted for the FOI-magnetron to optimise its performance. The simulations revealed that the FOI-magnetron suffered from leakage currents. Moreover, parameter studies of the FOI-magnetron with transparent cathode demonstrated favourable TE11-mode emission of microwaves with a peak output power reaching 590 MW after 15 ns, having a frequency of 2.56 GHz, and an efficiency of 37%. Comparisons between thetransparent and solid cathode for the FOI-magnetron showed a slightly lower output power and efficiency for the transparent cathode, with minimal difference in the rise time of microwaves. Additionally, the transparent cathode exhibits a higher overall impedance and leakage currents. On the other hand, a lower back-current density on the transparent cathode and emitter was shown, resulting in less damage to the material. In this study, we found that we could reduce leakage currents by extending the interaction region without impacting the performance of the FOI-magnetron. Also, the frequency was shown to change with either a shorter emitter or a longer interaction region, allowing for frequency control. Lastly, a modified design of an RM with a semitransparent cathode showed a promisingly high efficiency of 46% with an output power of 600 MW. This design utilised endcaps, which are useful for significantly reducing leakage currents

A relativistic magnetron (RM) is a high-power microwave (HPM) source. The main objective of the RM is to generate directed electromagnetic pulses with high power, which can be used in e.g. HPM weapons and for electromagnetic compatibility testing. These pulses can disturb or damage electronic equipment. One of the main challenges when designing an RM is to generate the advantageous TE11 wave mode to the circular waveguide and antenna with high efficiency and peak power. This thesis investigates a new design of the RM, developed at the Swedish Defence Research Agency (FOI), referred to as the FOI magnetron. This design is based on the A6-magnetron and employs four large and two small cavities in the diffraction output of the RM, compared to the conventional design that has six identical cavities. The FOI magnetron has previously shown results that indicate the possibility of generating the TE11 wave mode. In this thesis, a literature study was performed to better understand the governing physical laws of the RM. This was followed by parametric studies using the ​​particle-in-cell code MAGIC3D for simulating the RM. To validate the simulation models, a model of a conventional RM was constructed and the results were compared against the published simulation results by Daimon and Jiang (2008).  Lastly, different geometrical properties, applied magnetic field, and applied voltage of the FOI magnetron were studied to see how they impacted the RM performance. Apart from the diffraction output, the geometry of the interaction region was studied to investigate the effect on frequency and power. The goal was to generate a clean TE11 mode in the waveguide of the RM with high efficiency. The validation yielded results that were in good agreement with the ones obtained by Daimon and Jiang (beam-to-microwave efficiencies of 37% and 36% respectively). The parameter studies of the FOI magnetron gave results that indicate a clean TE11 mode with a beam-to-microwave efficiency of ∼35% and peak powers up to 1 GW at frequencies of approximately 2.5 GHz. The studies on the interaction region showed that a shift of approximately 0.12 GHz was possible when making the rear part of the interaction region 4.5 cm longer. It was found that the length of the front of the interaction region can to some extent affect the output power. Lastly, it was found that a fraction of the output power (∼10−17%) that leaves the interaction region propagates back toward the input region and the voltage source.

This thesis demonstrates the further development of an ultra-wideband (UWB) pulse generator and of an UWB antenna. Custom prototypes of these devices were initially developed for an ongoing research project. The project topic is a compact and portable concealed weapons detection (CWD) radar system to find objects such as firearms, knives, and grenades hidden on persons as they pass by. The system uses the UWB pulse generator as a transmitter, while the UWB antenna radiates the pulse and receives the corresponding backscatter from targets and other objects. Initial device prototypes do not perform adequately according to project specifications. A key specification is of adequate operation over the entire 0.5 GHz to 5 GHz frequency band, where adequate operation is defined distinctly for the antenna and pulse generator. In this work, empirical investigations of both devices are performed using techniques such as simulation, fabrication, and measurement. Through these investigations, the designs of the devices have been incrementally modified. Measured performance data suggest that the research has yielded designs with substantially improved bandwidth as a result. Bandwidth increases from 3.31 GHz to 4.36 GHz (31.7%) for the pulse generator and from 0.46 GHz to 4.98 GHz (983%) for the antenna are demonstrated. Future work is needed to establish the effects of fabrication tolerance, component tolerance, and human error on the variation of the observed device performance. / Thesis / Master of Applied Science (MASc) / This thesis is about the improvement of a radio antenna and a transmitter. These are ultimately intended as components in a system for detecting weapons (such as firearms, knives, etc.) concealed within the clothing or bags of nearby persons. The detection happens by transmitting specific radio signals which interact harmlessly with a person being scanned, and then are received back by the system. This is a form of radio detection and ranging (RADAR). The research on these devices has consisted of computer simulations and real-life measurements. As a result, it appears that the transmitter and radio antenna have been improved to be more suitable for the desired application than they were originally.