Submitted by Lara Oliveira (lara@ufersa.edu.br) on 2017-05-26T20:13:25Z No. of bitstreams: 1 DiêgoPG_DISSERT.pdf: 3157583 bytes, checksum: 93d2e3a248fde9f22d2f942876892f0c (MD5) / Approved for entry into archive by Vanessa Christiane (referencia@ufersa.edu.br) on 2017-05-29T16:49:54Z (GMT) No. of bitstreams: 1 DiêgoPG_DISSERT.pdf: 3157583 bytes, checksum: 93d2e3a248fde9f22d2f942876892f0c (MD5) / Approved for entry into archive by Vanessa Christiane (referencia@ufersa.edu.br) on 2017-05-29T16:50:05Z (GMT) No. of bitstreams: 1 DiêgoPG_DISSERT.pdf: 3157583 bytes, checksum: 93d2e3a248fde9f22d2f942876892f0c (MD5) / Made available in DSpace on 2017-05-29T16:50:16Z (GMT). No. of bitstreams: 1 DiêgoPG_DISSERT.pdf: 3157583 bytes, checksum: 93d2e3a248fde9f22d2f942876892f0c (MD5) Previous issue date: 2016-06-17 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / In Brazil are located the two largest niobium reserves of the world – about 96% of the world production – and, for this reason, have been encouraged studies on its most diverse technological applications. Another aspect of prominent studies is currently the processing of ceramic materials with a microwave, which is presented as an alternative method of sintering in a muffle furnace – the use of microwave involves electromagnetic energy conversion instead of heat transfer, offering advantages when used for providing the obtainment of greater structural homogeneity of the material and a reduction of time and energy expended during processing. This work aims to perform the characterization of electrical properties of niobium pentoxide (Nb2O5) pure or doped with molybdenum (Mo) and to do an analysis of the influence of this doping when its sintering process occurs in muffle furnace or microwave. The properties characterized were the permittivity and loss tangent. Will be studied the viability of doping and/or processing the material for use as absorbent materials of electromagnetic radiation. The variation of concentrations in doping will indicate how effective, as a doping agent, molybdenum will be in the ceramic matrix, converting energy of microwave into heat energy. The results showed that the increase of doping of the niobium pentoxide with molybdenum (with 1% doping limit) combined with the sintering oven microwave increased the material conductivity values, making it more efficient in its use as absorber electromagnetic radiation / No Brasil estão localizadas as duas maiores reservas de nióbio do mundo – cerca de 96% da produção mundial –, e, por esta razão, têm sido incentivados os estudos sobre as suas mais diversas aplicações tecnológicas. Outra vertente de estudos em destaque atualmente é a do processamento de materiais cerâmicos com micro-ondas, que se apresenta como um método alternativo à sinterização em forno mufla – o uso de micro-ondas envolve conversão de energia eletromagnética, em lugar de transferência de calor, oferecendo vantagens ao ser usado por proporcionar a obtenção de uma maior homogeneidade estrutural do material e uma redução do tempo e da energia gasta durante o processamento. A proposta deste trabalho é a realização da caracterização de propriedades elétricas do pentóxido de nióbio (Nb2O5) puro ou dopado com molibdênio usando a tecnologia da metalurgia do pó e a análise da influência sobre estas dopagens quando seu processamento de sinterização se dá em forno mufla ou em forno de micro-ondas. As caracterizações feitas foram das propriedades elétricas de permissividade elétrica e tangente de perdas além de ter sido estudada a viabilidade da dopagem e/ou o tipo de processamento – na etapa de sinterização – do material para aplicação como materiais absorvedores de radiação eletromagnética. A variação das concentrações nas dopagens indicou o quão eficaz, como agente dopante, o molibdênio será na matriz cerâmica, convertendo a energia de micro-ondas em energia térmica. Os resultados mostraram que o aumento da dopagem do pentóxido de nióbio com molibdênio (com limite de dopagem de 1%) aliado à sinterização em forno de micro-ondas garantiu o aumento dos valores de condutividade do material, tornando-o mais eficiente para sua aplicação como absorvedor de radiação eletromagnética / 2017-05-26

Cette thèse est consacrée à la réalisation de composites constitués d’inclusions ferromagnétiques dispersées dans une matrice diélectrique en vue d’obtenir des absorbeurs hyper fréquences dans la gamme 1 GHz – 5 GHz. La principale originalité de notre étude repose sur l’utilisation de particules à forte anisotropie géométrique dites sous forme de «pétales». En raison de leurs bonnes propriétés magnétiques (perméabilité et aimantation à saturation élevées), notre choix s’est porté sur l’utilisation d’alliages NiFeMo et FeSiAl pour cette étude. Dans un premier temps, les particules sous forme de pétales sont obtenues par mécanosynthèse. Un ajustement des paramètres de broyage a permis d’obtenir des pétales avec différents rapports de forme (longueur latérale sur épaisseur). Les particules sont ensuite incorporées à une barbotine constituée d’un liant et d’un plastifiant qui est par la suite coulée en bandes selon le procédé Doctor Blade. Les propriétés structurales et magnétiques des particules broyées ainsi que l’orientation des particules dans le composite ont été caractérisées. Dans une seconde partie, les spectres de perméabilité et de permittivité des composites ont été mesurés en cellule monospire et en ligne coaxiale APC7. Les évolutions des spectres en fonction de la quantité de particules dans le composite ainsi qu’en fonction du rapport de forme des particules ont été étudiées. Il a été montré que la transformation en pétales permettait d’obtenir des niveaux élevés de perméabilité et de permittivité. Ainsi, afin d’avoir un absorbeur de qualité, il est nécessaire de limiter les niveaux de permittivité en enrobant les particules. Les pétales NiFeMo ont été enrobés par de la silice selon le procédé Stöber et ceux à base de FeSiAl par oxydation partielle. Les propriétés magnétiques et électriques dynamiques de composites chargées par des pétales enrobés ont également été étudiées. Des modèles analytiques (loi de mélange de Maxwell-Garnett pour la perméabilité et lois d’Odelevsky et de Mclachlan pour la permittivité) ont été utilisés pour reproduire les principales caractéristiques radioélectriques des spectres de perméabilité et de permittivité Enfin, les performances électromagnétiques de ces composites ont été évaluées en considérant le problème générique de la réflexiond’une onde plane sur des revêtements recouvrant un support métallique. Le passage sous forme de pétales a permis de gagner en taux de charge et en épaisseur de couche absorbante par rapport aux composites chargés par des sphères. Cependant, un taux de charge élevé en pétales entraine une augmentation importante de la permittivité réelle et nuit à la condition d’accord. L’enrobage à la silice des pétales NiFeMo a permis de réduire la permittivité et d’atteindre un niveau d’absorption plus important. Ainsi, nous avons pu réaliser des matériaux composites plus légers et plus minces, absorbants dans la gamme de fréquence recherchée / This thesis deals with composites material containing ferromagnetic flaky-shaped particles (high length to thickness ratio) which exhibit improved microwave properties in terms of permeability spectra. It aims at obtaining effective absorbers in the 1 GHz – 5 GHz range. Because of their good magnetic properties (high permeability and saturation magnetization), NiFeMo and FeSiAl alloys were chosen as fillers. Firstly, composite sheets containing flaky-shaped particles were elaborated. Particles with different aspect ratios were obtained through a ball-milling process and then mixed with polymers in a slurry which is casted into sheets by using the Doctor Blade method. Structural and magnetic properties of milled particles and their orientation in the dielectric matrix were investigated. Then, permeability and permittivity spectra measurements were carried out using a single coil permeameter and a standard APC-7 coaxial line. Their evolutions with the particles aspect ratio and the particles volume content in the matrix were studied. It was shown that flaky shaped particles exhibit higher permeability and permittivity levels. Hence, to avoid impedance mismatch, lowering permittivity levels by using an insulating layer is necessary. Consequently,NiFeMo flakes were coated with a silica layer through the Stöber process and FeSiAl flakes with an oxide layer through oxidation. Electromagnetic properties of composites filled with coated flakes were also studied. In addition, permeabilityspectra were fitted combining the Landau-Lifshitz-Gilbert equation and the Maxwell-Garnet mixing rule. Permittivity spectra were fitted using Odelevsky and Mclachlan laws. Finally, their efficiency as a microwave absorber is estimated by calculating the reflection loss of a normal incident electromagnetic wave on an absorbing layer backed by a perfect conductor. Using flaky particles instead of spherical ones allowed the use of lighter and thinner layer. However, it resulted in high permittivity levels and lead to impedance mismatches. Insulating NiFeMo flakes with a silica layer reduced permittivity levels and allowed better absorbing properties. By using flaky shaped particles, we elaborated thinner and lighter microwave absorbers in the 1 GHz – 5 GHz range.