Granular materials are prevalent in the world at macro and micro scales, from the macro-scale of construction materials to the micro-scale of chemical powders. The properties of assemblages of grains are heavily controlled by the interparticle contacts. In order to assist with the better understanding of the means by which granular assemblages behave, this thesis seeks to develop understanding of the number, type and geometrical distribution of the contact points between individual grains.

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Made available in DSpace on 2014-12-17T14:06:59Z (GMT). No. of bitstreams: 1 MurilloMBMJ_DISSERT.pdf: 3939275 bytes, checksum: 05e057ccb01f46456e1e9588f664b52d (MD5) Previous issue date: 2011-02-17 / This masther dissertation presents a contribution to the study of 316L stainless steel sintering aiming to study their behavior in the milling process and the effect of isotherm temperature on the microstructure and mechanical properties. The 316L stainless steel is a widely used alloy for their high corrosion resistance property. However its application is limited by the low wear resistance consequence of its low hardness. In previous work we analyzed the effect of sintering additives as NbC and TaC. This study aims at deepening the understanding of sintering, analyzing the effect of grinding on particle size and microstructure and the effect of heating rate and soaking time on the sintered microstructure and on their microhardness. Were milled 316L powders with NbC at 1, 5 and 24 hours respectively. Particulates were characterized by SEM and . Cylindrical samples height and diameter of 5.0 mm were compacted at 700 MPa. The sintering conditions were: heating rate 5, 10 and 15◦C/min, temperature 1000, 1100, 1200, 1290 and 1300◦C, and soaking times of 30 and 60min. The cooling rate was maintained at 25◦C/min. All samples were sintered in a vacuum furnace. The sintered microstructure were characterized by optical and electron microscopy as well as density and microhardness. It was observed that the milling process has an influence on sintering, as well as temperature. The major effect was caused by firing temperature, followed by the grinding and heating rate. In this case, the highest rates correspond to higher sintering. / O presente trabalho apresenta uma contribui??o ao estudo da sinteriza??o de um a?o inox 316 L, com o objetivo de estudar o seu comportamento frente ao processo de moagem e o efeito da temperatura de isoterma na sua microestrutura e propriedades mec?nicas. O a?o inox 316L ? uma liga largamente utilizada pela sua propriedade de alta resist?ncia ? corros?o. Contudo a sua aplica??o ? limitada pela baixa resist?ncia ao desgaste, consequ?ncia da sua baixa dureza. Em trabalhos anteriores, foi analisado o efeito da sinteriza??o empregando aditivos como NbC e TaC. Assim, este estudo visa aprofundar o conhecimento da sinteriza??o analisando o efeito do tempo da moagem sobre o tamanho da part?cula e a microestrutura do sinterizado e o efeito da taxa de aquecimento e isoterma sobre a microestrutura do sinterizado e sobre a sua microdureza. Para isso foram mo?dos p?s de a?o 316L com NbC em tempos de moagens de 1, 5 e 24 horas respectivamente. Os particulados foram caracterizados por MEV e EDS. Amostras cil?ndricas, com altura e di?metro de 5,0 mm foram compactadas a 700MPa. As condi??es de sinteriza??o foram: taxa de aquecimento de 5, 10 e 15◦C/min, a temperatura de 1000, 1100, 1200, 1290 e 1300◦C, e tempos de isoterma de 30 e 60min. A taxa de resfriamento foi mantida em 25◦C/min. Todas as amostras foram sinterizadas em forno a v?cuo. Os sinterizados foram caracterizados na sua microestrutura atrav?s de microscopia ?tica e eletr?nica al?m de densidade e microdureza Vickers. Foi observado que o processo de moagem tem influ?ncia na sinteriza??o, assim como a temperatura. O efeito maior foi provocado temperatura de queima, seguida pela moagem e taxa de aquecimento. Neste caso, as maiores taxas corresponde a maior sinteriza??o.

Parmi les centrales solaires thermiques à concentration, la technologie des centrales à tour offre l'un des rendements les plus importants de production d'énergie. Néanmoins, l'efficacité et la sécurité de ces centrales sont améliorables. En effet, les sels fondus, généralement utilisés comme fluide de transfert thermique, présentent une plage limitée d'utilisation (200-550°C), à l'origine des limites d'efficacité de la conversion thermique-électrique, ainsi que de consommations parasites d'énergie de chauffage. De plus, leurs caractères corrosif et comburant sont à l'origine de sévères contraintes de sécurité. Un nouveau concept de récepteur solaire, dont les caractéristiques permettent de s'affranchir des contraintes associées aux sels fondus, est présenté dans ce manuscrit. Il utilise des suspensions denses de particules fluidisées par un gaz comme fluide de transfert et de stockage de l'énergie thermique. Ce concept, et la technologie de récepteur associée, a été brevetée par Flamant et Hemati dans le cadre d'une collaboration entre le Laboratoire CNRS-PROMES d'Odeillo, et l'Institut National Polytechnique de Toulouse. Son développement a reçu le soutien financier du CNRS, puis de la Commission Européenne. Les propriétés thermiques du carbure de silicium ont déterminé le choix de ce solide. Le diamètre moyen des particules utilisées avoisine 60 micromètres (groupe A). Ces particules présentent d'excellentes propriétés de fluidisation pour des vitesses de gaz faibles. La construction et l'exploitation d'une maquette froide transparente ont permis de démontrer la faisabilité hydrodynamique du concept. Cette maquette est un échangeur à deux passes. Chaque passe est constituée de deux tubes verticaux en parallèle. L'une est traversée par un débit vertical ascendant de solide, l'autre descendant. Un débit de solide continu, stable et équitablement réparti a été obtenu à l'intérieur des tubes. La caractérisation hydrodynamique détaillée de l'écoulement, et du comportement globale de la maquette, en fonction des conditions opératoires, a été effectué sur la partie ascendante de l'écoulement dans l'échangeur. La construction et l'exploitation d'une maquette chaude, constituée d'un seul tube traversé par une suspension dense en écoulement ascendant, chauffé par 3 fours d'une puissance totale de 5,6 kW, a permis d'estimer la capacité de transfert thermique de ce nouveau type d'échangeur. Le contrôle et la stabilité des conditions opératoires a permis d'évaluer l'effet de ces dernières sur le transfert thermique entre l'échangeur et la suspension dense de fines particules le traversant. La modélisation par 3 approches du transport ascendant de la suspension dense a également été réalisée. Une approche corrélative 1D basée sur le formalisme du modèle Bulle-Emulsion, adapté afin de tenir compte de l'entraînement des particules dans le sillage des bulles. Ce modèle permet de représenter la structure diphasique de l'écoulement. Une autre approche 1D a été utilisée. Elle repose sur la résolution des équations locales de conservation de masse et de quantité de mouvement sur chaque phase gaz et solide. Cette méthode permet de s'affranchir des hypothèses du modèle Bulle-Emulsion. Enfin, la simulation numérique 3D a été réalisée sur un maillage complet du système, de telle sorte que les conditions aux bornes imposées son identiques à celle imposée par l'opérateur (débit de fluidisation, débit d'aération, débit de solide, pression de la nourrice). Cette dernière apporte des informations sur la structure locale de l'écoulement, dont les caractéristiques permettent d'expliquer l'efficacité du transfert thermique entre la suspension et la paroi observé expérimentalement. / Among concentrating solar power plants, solar tower technology is one of the more power efficient. Nevertheless, their efficiency and safety can be improved. Indeed, molten salts, commonly used as heat transfer fluid, have a limited range of operating temperature (470-820K), thus lowering the thermal-electrical conversion efficiency, and increasing parasitic power consumption. Moreover, they are corrosive and combustion agent, leading to severe safety constraints. A new concept of solar receiver is presented in the present study, the characteristics of which avoid most of the molten salts drawbacks. It uses dense gas-particle suspension as heat transfer and storage fluid. This concept and the associated technology has been patented by Flamant et Hemati in the frame of a collaboration between the PROMES-CNRS Laboratory of Odeillo and the Polytechnic National Institute of Toulouse. Its development has been first supported by the CNRS, and later by the European Commission. Thermal properties of silicon carbide have determined the choice of this solid. The mean diameter of particles is around 64 microns (A group). These particles have excellent fluidisation properties at low gas velocities. The construction and the operation of a transparent cold mockup allowed demonstrating the hydrodynamic feasibility of this concept. This mockup is composed of two passes. Each pass is composed of two tubes in parallel. One pass is upward flow of solid, the other is downward flow. A steady, stable and evenly distributed solid flow has been set inside the tubes. The global behaviour of the system and the hydrodynamics of the suspension has been evaluated as a function of operating parameters on the upward pass. The construction and the operation of a hot mockup allowed estimating the heat transfer efficiency of this new kind of exchanger. On this mockup, the dense suspension flows upward inside a single tube, heated by three ovens of 5.6 kW total power. Thanks to the control and stability of the operating parameters, their effects on the heat transfer between the tube and the dense gas-solid suspension has been accurately determined. Modelling of the suspension upward flow has been performed using 3 approaches. The first one is based on the 1D Bubble-emulsion formalism, adapted to take into account the solid entrainment by the bubble wakes. It allows modelling the diphasic structure of the flow. The resolution of the local mass and momentum balance equation on each phase has also been performed. It allows to sidestep the Bubble-Emsulion assumptions, and to study the effects of drag models. 3D simulation has been performed on a complete mesh of the system, so that the boundary conditions are the same as those imposed by the operator (fluidisation flow rate, aeration flow rate, solid flow rate, dispenser pressure). These simulations give information on the local structure of the suspension flow, influencing on the heat transfer efficiency between the exchanger wall and the suspension.

La majeure partie des fibres optiques utilisées dans les domaines des sources optiques et des capteurs sont dites 'fonctionnalisées', c'est à dire qu'elles possèdent des propriétés nouvelles, de par leur nature et/ou leur structure, par rapport aux fibres standards. Pour ce faire, nous allons exploiter la technologie 'Poudre' pour la réalisation de fibres optiques utilisant les propriétés de matrices vitreuses originales développées lors de cette thèse. Trois familles de fibres seront étudier afin de démontrer le fort potentiel de cette association, matériaux – technologie. La première exploitera la structuration de la gaine optique à l'aide de deux barreaux de verre vitreux (type Panda), dopés ou non à l'aide d'oxyde de cuivre. L'étude de cette fibre sera faite depuis la synthèse du matériau jusqu'au test de cette fibre en tant que capteur. La seconde fibre nous amènera à concevoir un verre optique inédit à ce jour, à définir la composition optimale et la décliner sous forme d'une fibre optique incluant ce verre pour le cœur. Enfin le procédé de fabrication de fibres optiques sera utilisé pour réaliser de premières fibres optiques à cœur vitrocéramique, c'est à dire partant d'une matrice vitreuse spécialement développée pour cette application arriver à faire croitre les nanostructures dans le cœur de la fibre et obtenir ainsi une famille de fibre inédite. / The main part of optical fibers used in the fields of optical sources and sensors are called 'functionalised', i.e. they have new properties, due to their nature and/or structure, compared to standard fibers. To do this, we will use 'Powder' technology for the realization of optical fiber using properties of original vitreous glasses developed during this thesis. Three families of optical fibers will be studied in order to demonstrate the great potential of this association, materials - technology. The first exploit the structuring of the cladding with two vitreous glass rods (Panda type) doped or not with copper oxide. The study of this fiber is done from the synthesis of the material up to the test of this fiber as a sensor. The second fiber leads us to design a novel optical glass matrix, to define the optimal composition and decline form of an optical fiber including the glass for the core. Finally, the optical fiber manufacturing process is used to produce optical fiber with glass-ceramic core, i.e. starting from a vitreous matrix specially developed for this application happen to grow the nano-structures in the core of the fiber and obtain a novel fiber family.

The research presented in this work addresses open questions regarding (i) the fundamental understanding of powder compaction, and (ii) the complex mechanical response of particle-binder composites under large deformations. This work thus benefits a broad range of industries, from the pharmaceutical industry and its recent efforts on continuous manufacturing of solid tablets, to the defense and energy industries and the recurrent need to predict the performance of energetic materials. Powder compacts and particle-binder composites are essentially confined particulate systems with significant heterogeneity at the meso (particle) scale. While particle mechanics strategies for modeling evolution of mesoscale microstructure during powder compaction depend on the employed contact formulation to accurately predict macroscopic quantities like punch and die wall pressures, modeling of highly nonlinear, strain-path dependent macroscopic response without a distinctive yield surface, typical of particle-binder composites, requires proper constitutive modeling of these complex deformation mechanisms. Moreover, continued loading of particle-binder composites over their operational life may introduce significant undesirable changes to their microstructure and mechanical properties. These challenges are addressed with a combined effort on theoretical, modeling and experimental fronts, namely, (a) novel contact formulations for elasto-plastic particles under high levels of confinement, (b) a multi-scale experimental procedure for assessing changes in microstructure and mechanical behavior of particle-binder composites due to cyclic loading and time-recovery, and (c) a finite strain nonlinear elastic, endochronic plastic constitutive formulation for particle-binder composites.

Made available in DSpace on 2014-07-29T16:11:48Z (GMT). No. of bitstreams: 1 Dissertacaoo Rene Oliveira do Couto.pdf: 320246 bytes, checksum: 816190f5ad7a712d430d34f4a9536d4b (MD5) Previous issue date: 2011-02-24 / In this work, standardized spray-dried extracts of Rosmarinus officinalis L.(Lamiaceae), were obtained. The work started with the obtainment and characterization of the R. officinalis dried and powder leaves. A hydroalcoholic extract was obtained by percolation using as solvent ethanol at 80 % (v/v). The drying experiments followed a Box-Behnken (33) factorial design in order to obtain dry powders with optimized properties. In this way, the influence of several in-process parameters e. g. extract feed rate, drying air inlet temperature and spray nozzle airflow rate, on the dried extracts properties were investigated. The herbal raw material as well as both hydroalcoholic and dried extracts were analyzed by several physic-chemical and physical techniques. Additionally, the in vitro antioxidant activity from both hydroalcoholic and dried extracts were assessed by DPPH free radical scavenging test. Rosmarinic acid, the major component on the specie and one of the main compounds responsible for these pharmacological activities, was used as chemical marker in High Performance Liquid Chromatography (HPLC) coupled to photodiode array detection (PDA) quantification assays in all steps of this work. The analytical method was validated following Agência Nacional de Vigilância Sanitária (ANVISA Brazilian National Health Surveillance Agency) guidelines. This method proved to be simple, rapid, selective, linear, sensible, precise, accurate a robust. On the herbal raw material characterization, it were observed a swelling índex of 2.33 ± 0.11, a mean powder size of 437.94 ± 7.00 μm, as well as moisture, total ashes, acid insoluble ashes, total polyphenols, total tannins, total flavonoids and rosmarinic contents of 9.1 ± 0.23, 7.32 ± 0.045, 0.378 ± 0.016, 3.81 ± 0.043, 0.49 ± 0.01, 1.73 ± 0.07 and 1.05 ± 0.03% (w/w), respectively. The concentrated hydroalcoholic extract presented density of 0.964 ± 0.002 g/mL, solids content of 9.66 ± 0.07%, pH 5.106 ± 0.005, alcoholic content of 38.2 ± 0.53% and a viscosity of 5.2 ± 0.09 mPas. The levels of total polyphenols, total tannins, total flavonoids and rosmarinic contents were of 30.19 ± 0.24, 9.13 ± 0.01, 8.78 ± 0.1 and 10.68 ± 0.43% (w/w), respectively. Also, in the antioxidant assessment, the extract presented an inhibitory concentration (IC50) of 17.29 μg/mL. Results showed drying yields ranging from 17.1 to 74.96%. Also, all dried products showed moisture contents and water activities below 5% (w/w) and 0.5, respectively. Although dry products having lost some of their polyphenols they still presented antioxidant activities (IC50) ranging from 17.58 to 24.83 μg/mL. However, most recovered products presented inadequate flowability and compressibility. In general, the particles showed spherical shape and various sizes. Analysis of variance (ANOVAs) proved that the factors studied and some of their interactions significantly affected most of the investigated responses. Moreover, the best condition for obtaining dry extracts of rosemary with stability evidence as well as adequate physicochemical and functional properties is the one performed with a high extract feed rate, an intermediate drying air inlet temperature and a low spray nozzle air flow rate. Accordingly, spray drying technique may be an attractive and promising alternative to develop intermediate phytopharmaceutical products of rosemary. / A obtenção de extratos secos padronizados da Rosmarinus officinalis L. (Lamiaceae),por meio da técnica de spray drying, foi precedida de duas etapas, iniciando-se pela obtenção e caracterização do material de partida (pó das folhas da planta) e a partir desse, obtendo-se o extrato hidroalcoólico pelo método de percolação usando como solvente etanol a 80% (v/v).Os experimentos de secagem foram conduzidos seguindo um planejamento fatorial do tipo Box-Behnken (33) a fim de se obter produtos secos com propriedades otimizadas. Nesse sentido, foram investigadas as influências de alguns parâmetros envolvidos no processo, e. g. fluxo de alimentação de extrato, temperatura de entrada do ar de secagem e vazão do ar de aspersão nas propriedades dos extratos secos obtidos. Tanto o material de partida quanto os produtos obtidos através dele, foram caracterizados por vários ensaios físico-químicos e físicos. Ainda, foi avaliado o potencial antioxidante in vitro do extrato hidroalcoólico e dos extratos secos por meio de um método colorimétrico empregando o radical livre DPPH . O ácido rosmarínico, componente majoritário e um dos principais responsáveis pelas atividades farmacológicas da espécie, foi selecionado como marcador químico e, em todas as etapas do processo, foi quantificado por Cromatografia Líquida de Alta Eficiência (CLAE) acoplada a detector de arranjo de fotodiodos (DAD). Para tanto um método analítico foi validado seguindo os parâmetros e critérios de aceitação propostos pela Agência Nacional de Vigilância Sanitária (ANVISA), o qual provou ser de fácil execução, rápido, seletivo, linear, sensível, preciso, exato e robusto. Na caracterização da droga vegetal, foram verificados teores de voláteis, cinzas totais, cinzas insolúveis em ácido, polifenóis totais, taninos totais, flavonóides totais e ácido rosmarínico de 9,1 ± 0,23, 7,32 ± 0,045, 0,378 ± 0,016, 3,81 ± 0,043, 0,49 ± 0,01, 1,73 ± 0,07 e 1,05 ± 0,03% (m/m), respectivamente, além de índice de intumescência de 2,33 ± 0,11 e tamanho médio de partículas de 437,94 ± 7,00 μm. O extrato hidroalcoólico apresentou densidade de 0,964 ± 0,002 g/mL, resíduo seco de 9,66 ± 0,07%, pH 5,106 ± 0,005, teor alcoólico de 38,2 ± 0,53% e viscosidade de 5,2 ± 0,09 mPas. Ainda, foi obtida uma concentração inibitória (CE50) de 17,29 μg/mL nos ensaios de atividade antioxidante e os teores de polifenóis totais, taninos totais, flavonóides totais e ácido rosmarínico foram de 30,19 ± 0,24, 9,13 ± 0,01, 8,78 ± 0,1 e 10,68 ± 0,43% (m/m), respectivamente. Os rendimentos de secagem variaram de 17,1 a 74,96%, sendo que em todos os produtos secos, foram observados teores de voláteis e atividade de água abaixo de 5% (m/m) e 0,5, respectivamente. Apesar dos produtos secos terem perdido parte de seus compostos polifenólicos, eles ainda apresentaram CE50 variando de 17,58 a 24,83 μg/mL. Entretanto, a maioria dos extratos secos apresentou propriedades de fluxo e compressibilidade inadequadas para fins farmacêuticos. As fotomicrografias obtidas para esses produtos mostraram partículas de tamanho variável e formato esférico. Análises de Variância(ANOVAs) demonstraram que ambos os fatores estudados e algumas de suas interações afetaram significativamente a maioria das respostas investigadas, sendo que a melhor condição a ser empregada na obtenção de extratos secos padronizados com indícios de estabilidade, assim como propriedades físico-químicas e funcionais adequadas é aquela realizada com alto fluxo de extrato de alimentação, temperatura do ar de admissão intermediária e baixa vazão do ar de aspersão. Assim, a técnica de spray drying pode ser uma alternativa atrativa e promissora para a obtenção de produtos fitofarmacêuticos intermediários da R. officinalis.