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The research described in this dissertation mainly covers the development of novel technologies for co-crystallisation along with the discovering of plumbagin co-crystal and thermodynamic interrelationship between the co-crystal polymorphs. Co-crystallisation is a fast growing field in the area of crystal design and has shown potential advantages in the field of pharmaceutical. Currently, many research groups are working on the development of new technologies for the synthesis of pure and stoichiometrically controlled co-crystals. In present study, three novel technologies have been developed for co-crystallisation, which include microwave assisted co-crystallisation, spherical crystallisation and microwave assisted sub-critical water processing. The microwave assisted co-crystallisation is a slurry based technology where, effects of drug solubility and dielectric properties of the solvent were investigated using caffeine / maleic acid as a model co-crystal pair. The mechanism of co-crystallisation under microwave irradiation has been proposed. The co-crystals of plumbagin with improved solubility were obtained with the coformers such as hydroquinone, resorcinol and urea using microwave assisted co-crystallisation technique. The spherical crystallisation technology was developed for co-crystallisation of carbamazepine / saccharin co-crystal pair and demonstrated its application for polymorphic control and as a potential technique for the purification of desired crystal form through surface energetic based separation. The thermodynamic interrelationship between Form I and Form II of carbamazepine / saccharin co-crystal was studied using different thermodynamic tests. The results obtained suggest that the carbamazepine / saccharin co-crystal polymorphs are monotropic. Microwave assisted sub-critical water processing has been explored as a green technology for the synthesis of co-crystals. Carbamazepine / saccharin co-crystal pair has been used as a model pair and effects of processing variables on the resulting crystal form and degradation of an API have been studied.

Mitt i Europas växande beroende av extern antimonproduktion har Europeiska kommissionen konsekvent betonat ett växande gap mellan utbud och efterfrågan sedan 2014. Som svar på denna utmaning riktade sig denna studie mot sekundära antimonkällor från underutnyttjade rester av guld, koppar och blymalm, som för närvarande utgör ett miljöproblem. Genom noggranna experiment, fastställde vi att optimal antimonurlakning uppnås vid 120 °C inom 2 timmar med en 250 g/L Na2S och 60 g/L NaOH-blandning. Detta tillvägagångssätt accentuerar selektiv extraktion, förbättrar antimonåtervinningen och minimerar kopparinterferens. En innovativ aspekt av denna studie var användandet utav mikrovågsassisterad urlakning, vilket visar fördelar i både utvinningseffektivitet och bevarande av mineralstrukturer jämfört med traditionella metoder. Våra resultat stöds av flera analytiska verktyg och ger en första förståelse, även om detaljerna kring mikrovågsassisterad urlakning och dess skalbarhet motiverar ytterligare utforskning. Denna studie introducerar en metod för urlakning av antimon från koppargruvavfall och föreslår ett motsvarande återvinningssystem som kan vara ekonomiskt lönsamt. Sådana ansträngningar kan ge ett blygsamt bidrag till att lindra den nuvarande situationen. / Amid Europe's growing reliance on external antimony production, the European Commission has consistently emphasized an expanding supply-demand gap since 2014. Responding to this challenge, our research targeted secondary antimony sources from underutilized residues of gold, copper, and lead ore processing, which currently pose environmental concerns. Through meticulous experimentation, we determined that optimal antimony leaching is achieved at 120°C within 2 hours, using a 250 g/L Na2S and 60 g/L NaOH mixture. This approach accentuates selective extraction, enhancing antimony recovery and minimizing copper interference. An innovative facet of this study was the adoption of microwave-assisted leaching, demonstrating advantages in both extraction efficiency and mineral structure conservation over traditional methods. Our results, backed by multiple analytical tools, provide an initial understanding, though areas like the specifics of microwave-assisted leaching and its scalability warrant further exploration. This study introduces a method for leaching antimony from copper mining waste and suggests a corresponding recycling system that may be economically viable. Such endeavors might offer a modest contribution to alleviating the present situation.

High-power microwave, HPM, systems can be used as non-lethal weapons with the ability to destroy or disturb electronics, by damaging internal circuits and inducing high currents. Today microwave sources are being developed with peak powers exceeding 1 GW, one of these devices is the vircator, a narrowband source which is unique to the HPM community. In order to understand and develop microwave sources like the vircator it is necessary to have computer models, as simulations gives an invaluable understanding of the mechanisms involved during operation, saving time and development costs.                                                                  This thesis presents the results from a theoretical analysis and a simulation study using a well known electromagnetic particle-in-cell code, Computer Simulation Technology Particle Studio. The results are then compared to measured data from a HPM system, the Bofors HPM Blackout. The results show that CST PS can be used to design and study the coaxial vircator with good results.

Les régions de haute latitude sont actuellement les plus sensibles aux effets du réchauffement climatique, et avec des élévations de température pouvant atteindre les 3 à 8 ◦C au niveau du pôle sur les 100 prochaines années. Les pergélisols (sols présentant des températures négatives deux années consécutives) sont présents sur 25 % des terres émergées de l’hémisphère nord et contiennent de grandes quantités de carbone « gelé », estimées à 1400 Gt (40 % de la quantité de carbone terrestre global). Des études récentes ont montré qu’une partie non négligeable (50 %) des premiers mètres des pergélisols pourraient fondre d’ici 2050, et 90 % d’ici 2100. Le but de l’étude est donc d’améliorer les moyens de suivi de l’évolution des températures du sol dans les zones arctiques, et plus particulièrement dans les régions couvertes de neige. L’objectif est de décrire la température du sol tout au long de l’année y compris sous un manteau neigeux, et d’analyser l’évolution de l’épaisseur de la couche active des pergélisols en relation avec la variabilité du climat. Nous utilisons des données satellites (fusion de données de température dans l’infra-rouge thermique “LST” et de température de brillance micro-onde AMSR-E « Tb ») assimilées dans le schéma de surface du modèle climatique canadien (CLASS, V 3.6) couplé à un modèle simple de transfert radiatif (HUT). Cette approche bénéficie des avantages de chaque type de donnée de manière à réaliser deux objectifs spécifiques : 1-construire une méthodologie solide permettant de retrouver les températures du sol, avec et sans neige, en zone de toundra, et 2-à partir de ces températures du sol, dériver la durée de fonte estivale et l’épaisseur de la couche active du pergélisol. Nous décrivons le couplage des modèles ainsi que la méthodologie permettant l’ajustement des paramètres météorologiques d’entrée du modèle CLASS (essentiellement les températures de l’air et les précipitations issues de la base de données des réanalyses météorologiques NARR) de manière à minimiser les LST et Tb simulées en comparaison aux mesures satellites. Par rapport aux données de mesures de sol de stations météorologiques prises comme référence pour validation dans les zones de toundra d’Amérique du Nord, les résultats montrent que la méthode proposée améliore significativement la simulation des températures du sol lorsqu’on utilise les données LST MODIS et Tb à 10 et 19 GHz pour contraindre le modèle, en comparaison avec les sorties du modèle sans les données satellites. Dans ce processus d’inversion, la correction de l’évolution des conditions de neige au cours de l’hiver contrainte avec le rapport de polarisation à 11 GHz constitue une approche originale. Une analyse de l’erreur pour 4 sites de toundra et sur plusieurs années (18 cas) est effectuée pour la période estivale (1,7 -3,6 K) ainsi que pour la période hivernale couverte de neige (1,8 -3,5 K). L’indice des degrés-jours de fontes annuel, dérivé des températures du sol simulés par notre approche, permet de cartographier les zones de pergélisols continu en accord avec les cartes actuelles. Un meilleur suivi des processus d’évolution des pergélisols, et tout particulièrement de l’impact de la couverture de neige, devrait permettre une meilleure compréhension des effets du réchauffement climatique sur la fonte des pergélisols et l’avenir de leurs stocks de carbone. / Abstract : High latitude areas currently are the most sensitive to global warming effects. In the next 100 years, temperature could rise up to 3 to 8 ◦C at the North Pole. Permafrost (ground with negative temperatures two years in a row) represents 25% of northern hemisphere lands, and contains huge quantities of "frozen" carbon estimated at 1400 Gt (40 % of the global terrestrial carbon). Recent studies showed that a part (50 %) of the permafrost first few meters could melt by 2050, and 90 % by 2100. The goal of our study is to improve our understanding of ground temperature evolution in arctic areas, especially in snow covered regions. The objective is to discribe the ground temperature all year long with and without a snow cover, and to analyze the evolution of the permafrost’s active layer in relation with the climate variability. We use remote sensing data (fuzzed of MODIS "LST" surface temperatures and AMSR-E "Tb" brightness temperatures) assimilated in the canadian landscape surface scheme (CLASS) coupled to a simple radiative transfer model (HUT). This approach takes into account the advantages of each kind of data in order to achieve two objectives : 1 - build a solid methodology allowing to retrieve ground temperatures, with and without a snow cover, in tundra areas ; 2 - from those retrieved ground temperatures, derive the summer melting duration which can be linked to the permafrost active layer thickness. We describe the models coupling as well as the methodology allowing the adjustement of CLASS input meteorological parameters (essentially the air temperatures and precipitations from the NARR meteorological data base) in order to minimize the simulated LST and Tb in comparison to remote sensing data. By using meteorological station’s ground temperature measurments as a reference for validation in North America tundra areas, results show that the proposed method improves the simulation of ground temperatures when using LST MODIS and Tb at 10 and 19 GHz data to constrain the model, in comparison with model outputs without satellite data. Using the Tb polarization ratio H/V at 10 GHz allows an improvement of the constrain on winter period simulations. An analyze of the error is conducted for summer (1,7 - 3,6 K) and winter (1,8 - 3,5 K). We present climatic applications for future work that meets the second objective of the Ph.D. A better understanding of evolution processes of permafrost, and particularly of the impact of the snow cover, should allow us a better understanding of global warming effects on the permafrost’s melting and the future of their carbon stocks.

Un nouveau procédé d'extraction des huiles essentielles a été développé, mis au point et optimisé nommé «Vapo-diffusion Assistée par Micro-ondes (MSDf)». Le procédé MSDf à été appliqué à l'extraction des huiles essentielles des peaux d'oranges et de fleurs de lavande. Ce procédé est basé sur la combinaison d'une technique d'extraction classique : l'hydro-diffusion et le chauffage micro-ondes comme technologie d'intensification. Une deuxième nouvelle approche pour l'extraction des huiles essentielles à partir de matrices aromatiques sèches et sans ajout de vapeur ni d'eau nommé «Diffusion à sec générée par micro-ondes (MDG)». Le procédé MDG à été appliqué à l'extraction des huiles essentielles des graines de carvi. Le MSDf et le MDG apparaissent comme des procédures «douces» permettant un gain de temps et d'énergie considérable et la diminution des rejets de CO2 dans l'atmosphère / Microwave steam diffusion (MSDf) was developed as a cleaner and new process design and operation for isolation of essentials oils and was compared to conventional steam diffusion (SDf). This green process has been applied and tested using two aromatic matrixes: fresh orange peels and dry lavender flowers. This process is based on the combination of a traditional technique of extraction: hydro-diffusion and the microwave irradiation energy. Without adding any steam or water, we proposed also a novel and green approach for extraction of secondary metabolites from dried plant materials. This “steam and water free” approach based on a simple principle involves the application of microwave irradiation and earth gravity to extract the essential oil from dried caraway seeds. MSDf and MDG were better than SDf in terms of energy saving, cleanliness and reduced waste water

A reciclagem de materiais poliméricos tem sido objeto de estudos a fim de poupar recursos naturais, principalmente de fontes não renováveis, com objetivo de minimizar os impactos causados ao meio ambiente. Nesse cenário, aparecem os materiais elastoméricos, como a borracha, principalmente na utilizada da fabricação de pneus, uma vez que a indústria pneumática consome aproximadamente 60% da produção de borracha. Como a destinação final de forma ambientalmente correta do pneu é uma exigência devidamente amparada por normas e leis nacionais e internacionais, o objetivo desse trabalho é desenvolver um estudo sobre a eficácia das irradiações das micro-ondas no processo de desvulcanização do pó de pneu. Para esse estudo as amostras de pó de pneu foram submetidas a irradiações de micro-ondas, e posteriormente incorporadas às matrizes poliméricas de NR (borracha natural) e SBR (borracha de butadieno-estireno), e caracterizadas para verificação de suas propriedades. Para caracterização das amostras foram utilizados os seguintes ensaios: Espectroscopia no Infravermelho (FTIR), Dureza, Resistência à Tração e Alongamento, Reometria, Índice de Inchamento, Análise Termogravimétrica (TGA) e Microscopia Eletrônica de Varredura (MEV). Verificou-se viabilidade técnica da incorporação do pó de pneu nas matrizes de NR e SBR, uma vez que alguns resultados mostraram que a adição do pó de pneu irradiado via micro-ondas não ocasionou perdas significativas nas propriedades mecânicas e térmicas dos compostos. / The recycling of polymeric materials has been studied in order to save natural resources, mainly from non-renewable sources, in order to minimize the impacts caused to the environment. In this scenario, there are elastomeric materials, such as rubber, mainly used in tire manufacturing, since the pneumatic industry consumes approximately 60% of rubber production. As the final destination of an environmentally correct tire is a requirement, duly supported by national and international laws and regulations, the objective of this work is to develop a study on the efficiency of microwave irradiation in the process of tire powder devulcanization. For this study the tire powder samples were subjected to microwave irradiation, and later incorporated into the polymer matrices of NR (natural rubber) and SBR (butadiene-styrene rubber), and characterized for verification of their properties. For characterization of the samples the following tests were used: Infrared Spectroscopy (FTIR), Hardness, Tensile Strength and Stretching, Rheometry, Swell Index, Thermogravimetric Analysis (TGA) and Scanning Electron Microscopy (MEV). It was verified the technical feasibility of the incorporation of the tire powder in the NR and SBR matrices, since some results showed that the addition of the tire powder irradiated by microwave did not cause significant losses in the mechanical and thermal properties of the compounds.

[pt] Esta Tese consiste na pesquisa, dimensionamento e desenvolvimento de estruturas de microondas que utilizam grafeno e nanotubos de carbono como componente fundamental. São apresentadas aplicações em dispositivos de micro-ondas e no domínio óptico, tais como filtros, conversores de frequência, antenas de microondas, absorvedores de microondas etc. Também são apresentados os resultados dos testes realizados em todos os dispositivos desenvolvidos. Alguns dispositivos contém inovações ainda não reportadas na literatura. / [en] This Thesis consists inthe research, dimensioning and design of microwave structures that use graphene and carbon nanotubes as fundamental component. Applications are presented in microwave devices and in the optical domain, such as filters, frequency converters, microwave antennas, microwave absorber etc. Besides that, the results of the tests performed in all designed devices are presented. Some devices have innovations not yet reported in the literature.

Este trabalho visou ao desenvolvimento de antenas de ressoador dielétrico de banda dupla em frequências de micro-ondas por meio do estabelecimento de uma metodologia de projeto para as mesmas e da proposição de configurações inéditas de antenas desse tipo. Estudos realizados sobre antenas de ressoador dielétrico e sobre suas técnicas de projeto forneceram a base para a elaboração de um procedimento de projeto para antenas de banda dupla que explora a flexibilidade das antenas de ressoador dielétrico. Empregando-se esse procedimento de projeto, duas antenas com configurações originais foram desenvolvidas para operar em frequências de micro-ondas. Uma delas é uma antena de ressoador dielétrico cilíndrica sobre plano de terra, destinada a operar nas frequências centrais de 3,94 GHz e de 5,42 GHz, com diagrama de radiação direcional e polarização circular na primeira banda de operação e com diagrama de radiação omnidirecional e polarização linear na segunda. A outra antena consiste em uma antena de ressoador dielétrico cilíndrica sobre substrato dielétrico aterrado, cujas frequências centrais de operação são 3,99 GHz e 6,20 GHz, com diagrama de radiação direcional e polarização circular em ambas as bandas de operação. O projeto das duas antenas também levou a contribuições novas adicionais em alguns temas específicos relacionados: estruturas de excitação para antenas de ressoador dielétrico, circuitos acopladores híbridos de 90° de banda dupla, circuitos de alimentação para antenas de banda dupla e modelos matemáticos para o ressoador dielétrico cilíndrico isolado no espaço livre. Os comportamentos previstos teoricamente para as antenas projetadas são confirmados por meio de resultados obtidos por simulação eletromagnética e por medição experimental, o que indica a validade das hipóteses adotadas, das configurações de antena propostas e da metodologia de projeto concebida, demonstrando também a flexibilidade desta para variadas especificações de antena. Os avanços obtidos com este trabalho e as melhorias que podem ser efetuadas sobre o mesmo são identificados examinando-se resultados recentemente publicados na literatura técnica. Este trabalho foi realizado na forma de uma pesquisa de doutorado sanduíche, desenvolvida parcialmente na University of Houston sob a supervisão do Prof. Stuart A. Long. / This work aimed at the development of microwave dual-band dielectric resonator antennas by means of establishing a design methodology for them and of proposing novel configurations of this antenna type. Studies on dielectric resonator antennas and on their design techniques provided the ground for elaborating a design procedure for dual-band antennas that exploits the flexibility of dielectric resonator antennas. By employing this design procedure, two antennas with original configurations have been developed for operation at microwave frequencies. One of them is a cylindrical dielectric resonator antenna on a ground plane, intended for operation at the center frequencies of 3.94 GHz and 5.42 GHz, with a directional radiation pattern and circular polarization in the first operating band and with an omnidirectional radiation pattern and linear polarization in the second one. The other antenna consists of a cylindrical dielectric resonator antenna on a grounded dielectric substrate, whose operating center frequencies are 3.99 GHz and 6.20 GHz, with a directional radiation pattern and circular polarization in both operating bands. The design of the two antennas also led to additional new contributions in some related specific subjects: excitation structures for dielectric resonator antennas, dual-band 90°-hybrid couplers, feeding circuits for dual-band antennas, and mathematical models for the cylindrical dielectric resonator isolated in free space. The behaviors theoretically expected for the designed antennas are confirmed by means of results obtained from electromagnetic simulation and from experimental measurements, which indicates the validity of the assumed hypotheses, of the proposed antenna configurations and of the conceived design methodology, also demonstrating the flexibility of the latter for various antenna specifications. The advances obtained with this work and the improvements that can be made on it are identified by examining results recently published in the technical literature. This work was carried out as a sandwich doctoral research, developed at the University of Houston under the supervision of Prof. Stuart A. Long.