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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / This work is dedicated to investigate the spin relaxation in amorphous CoFeSiB glass-covered microwires and multilayered films of Permalloy/Cu. The microwires samples were Joule annealed and axially stressed in order to evaluate the modifications in the damping mechanisms due to the stress induced anisotropy. In the films we were interested in the observation of the modifications in the damping mechanisms imposed by the number of interfaces in the samples. We were able to identify the main damping mechanisms responsible for the spin relaxation in these materials by ferromagnetic resonance experiments. In order to explain the ferromagnetic resonance linewidth, we considered the extrinsic magnetic relaxation mechanisms in addition to the intrinsic Gilbert damping term, the intrinsic one. The extrinsic magnetic relaxation takes in to account the broadening induced by the magnetic inhomogeneities and is consistent with the two-magnon scattering model and anisotropy dispersions. The contribution from the intrinsic magnetization relaxation is constant in both systems of samples and is not sensible neither to Joule annealing and applied stress in microwires, nor to the increasing of the bilayers number in the films. The extrinsic contribution is very sensible to the anisotropy induction and is a signature of magnetic and structural inhomogeneities. / Este trabalho é dedicado ao estudo da relaxação de spin em microfios amorfos recobertos por vidro com composição nominal de CoFeSiB e em filmes multicamadas de Permalloy/Cu. Nos microfios, avaliamos o efeito da indução de anisotropia pela aplicação de tensão mecânica e o efeito do alívio de tensões internas promovido por tratamento térmico aos mecanismos de amortecimento responsáveis pela relaxação de spin. Nos filmes, avaliamos as modificações impostas aos mecanismos de amortecimento quando variamos o número de bicamadas. Identificamos e quantificamos os principais mecanismos responsáveis pela relaxação magnética, através da investigação da largura de linha de ressonância ferromagnética. Para explicar as larguras de linha de ressonância ferromagnética observadas consideramos como mecanismo intrínseco o mecanismo de amortecimento de Gilbert. Como mecanismos extrínsecos consideramos o alargamento da linha de ressonância devido a inomogeneidades magnéticas, consistente com o modelo de espalhamento de mágnons e com a presença de dispersões na anisotropia. O termo intrínseco de relaxação é constante em ambos os conjuntos de amostras estudados, não variando com o tratamento térmico ou tensão aplicada, no caso dos microfios, nem com o aumento do número de bicamadas, no caso dos filmes. A contribuição extrínseca de amortecimento mostrou-se bastante sensível à indução de anisotropias e é uma assinatura das inomogeneidades estruturais e magnéticas presentes nas amostras.

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / The possibility of exploring the magnetic properties of amorphous microwires in technological applications has attracted the attention of the scientific community in the last years. Beyond, the magnetoimpedance effect has been established as a powerful tool to study these properties. In this work we show a study of the magnetic properties of Joule heated glasscovered amorphous microwires, CoFeSiB, under applied stress. The stress modifies the anisotropy and the domain structure of the sample being studied by the magnetoimpedance measurements and the FMR dispersion relations. It was established a method to determine the permeability from the magnetoimpedance measurements, valid for a wide frequency range. From the study of the permeability curves parameters associated to the domain walls dynamic can be determined. From the FMR dispersion relations, the value and the direction of the transverse anisotropy field, as well as an estimative of the magnetic domain structure in these microwires were obtained. It can be concluded that the longitudinal anisotropy has the main role in the magnetic behavior of the microwire without stress. Also, it was verified the presence of an inner core with longitudinal anisotropy surrounded by an outer shell with circumferential anisotropy under applied stress. These magnetic configurations can be explained in terms of the frozen stress in the production process of the wire and the additional applied stress. / A possibilidade de explorar as propriedades magnéticas de microfios amorfos em aplicações tecnológicas tem atraído a atenção da comunidade científica nos últimos anos. Além disso, a magnetoimpedância foi estabelecida como uma ferramenta poderosa para estudar estas propriedades. Neste trabalho apresentamos um estudo das propriedades magnéticas de microfios amorfos, CoFeSiB, recobertos por vidro, tratados termicamente e sob aplicação de tensão. A tensão modifica a anisotropia e a estrutura de domínios presente na amostra de tal maneira que podem ser estudadas a partir das medidas de magnetoimpedância e da relação de dispersão de FMR (Ressonância Ferromagnética) extraída delas. Foi estabelecido um método para a determinação da permeabilidade a partir de medidas de magnetoimpedância, válido para uma ampla faixa de freqüências. A partir do estudo dessas curvas de permeabilidade pode-se determinar, por exemplo, parâmetros relativos à dinâmica de paredes de domínios. Do ajuste das relações de dispersão de FMR foram obtidos o valor e a orientação do campo de anisotropia transversal, bem como uma estimativa da estrutura de domínios dos microfios. Destes estudos, concluiu-se que a anisotropia longitudinal domina o comportamento magnético do microfio sem aplicação de tensão. Aplicando-se tensão aos microfios, verificou-se a presença de um núcleo interno com anisotropia longitudinal envolto por uma casca externa com anisotropia circunferencial. Estas configurações magnéticas podem ser explicadas em termos da tensão residual que surge no processo de produção do fio e da tensão adicional aplicada.

Magnetoimpedance has been proved to be an excellent tool to study the magnetization dynamics and the ferromagnetic resonance (FMR) linewidth provides a convenient way for measuring damping parameters in magnetic materials. The FMR linewidth depends on intrinsic magnetic damping and additional magnetic inhomogeneities, but complete understanding of the origin of these damping parameters is still unaccomplished. Besides the fundamental physics interest, the study of damping term and magnetization dynamics is very important for the development of any device which has its physical effect associated with the reversal of magnetization. Furthermore, the FMR linewidth is a very sensitive way to study the structural quality of magnetic samples, in both bulk and thin film geometries. In this work the magnetic relaxation of CoFeSiB glass-covered microwire was investigated by ferromagnetic resonance (FMR) linewidth measurements. We have identified the main damping mechanisms and quantified these damping terms, showing the effect of annealing temperature to them. The study have shown that there are three main damping mechanisms responsible for the FMR linewidth, the Gilbert damping parameter, a damping mechanism due to anisotropy dispersions and two-magnon scattering. The Gilbert damping parameter is almost constant and not influenced by the annealing. The FMR linewidth is very sensitive to anisotropy dispersions and this mechanism has a great contribution to the magnetic relaxation. The two-magnon scattering is an assignment of the inhomogeneities present in the samples and its contribution to the FMR linewidth decrease with the annealing temperature until a critical value, as a result of a decrease of inhomogeneities due to a reduction of the internal stress level. A further increase in the annealing temperature produces an increase in the two-magnon scattering contribution which is an indication of the growing of nanocrystals acting as scattering centers to the spin waves. / Magnetoimpedância tem provado ser uma excelente ferramenta para estudar a dinâmica de magnetização e a largura de linha da ressonância ferromagnética (FMR) fornece uma maneira conveniente para medir parâmetros de amortecimento em materiais magnéticos. A largura de linha FMR depende do amortecimento magnético intrínseco e adicionais inomogeneidades magnéticas, mas o completo entendimento da origem destes parâmetros de amortecimento ainda está inacabado. Além do interesse da física fundamental, o estudo da dinâmica de amortecimento e magnetização é muito importante para o desenvolvimento de qualquer dispositivo que tem seu efeito físico associado com a inversão da magnetização. Além disso, a largura de linha FMR é uma forma muito sensível para estudar a qualidade estrutural de amostras magnéticas. Neste trabalho é apresentado um estudo da relaxação magnética de microfios amorfos de CoFeSiB recobertos por vidro, mostrando o efeito da temperatura de recozimento sobre as propriedades magnéticas do microfio. Foram identificados e quantificados os principais mecanismos de amortecimento, mostrando o efeito da temperatura de recozimento para eles. Os estudos mostraram que existem três principais mecanismos de amortecimento responsável pela largura de linha FMR: o parâmetro de amortecimento de Gilbert; um mecanismo de amortecimento devido à dispersões na anisotropia; e o amortecimento devido ao espalhamento de magnons. O parâmetro de amortecimento de Gilbert é quase constante e não influenciado pelo recozimento. A largura de linha FMR é muito sensível a dispersões da anisotropia e esse mecanismo tem uma grande contribuição para o relaxamento magnético. A dispersão de magnons é uma atribuição de inomogeneidades presentes nas amostras e tem contribuição para a diminuição da largura de linha com a temperatura de recozimento até um valor crítico, como resultado de uma diminuição de inomogeneidades devido a uma redução do nível de estresse interno. Um aumento na temperatura de recozimento produz um aumento na contribuição de espalhamento dos magnons, que é uma indicação do crescimento de nanocristais atuando como centros de dispersão para as ondas de spin.

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / In this work, we have measured the domain wall velocity in the low field regime and studied the domain wall dynamics in Joule-annealed amorphous glass-covered microwires with positive magnetostriction. Such microwires are known to present magnetic bi-stability when axially magnetized. In order to measure of the single domain wall dynamics under different conditions, an electrical current was applied to the wire simultaneously to the mechanical stress and driving magnetic field. We have observed that the applied stress decreases the domain wall mobility. When the dc current is applied to the sample, an increase or a decrease is observed on the axial domain wall mobility, depending on the current direction. When we have treated the orthogonal motion of the domain wall, the current influence is not detected. On the other hand, it was verified a modification on the domain wall length. It was also observed a change in the domain wall shape from conical to parabolic one. These results are explained in terms of the change in the magnetic energy promoted by the additional Oersted field which, by its time, modifies the length and shape of the conical domain wall, in such a way that the orthogonal domain wall velocity is not changed by the applied current. / Nesse trabalho, foi medida a velocidade de paredes de domínios em regime de baixos campos e estudada a dinâmica dessas paredes em microfios amorfos recobertos por vidros com magnetostricção positiva tratados via efeito Joule. Tais microfios são conhecidos por apresentar biestabilidade magnética quando axialmente magnetizados. A fim avaliar a dinâmica de uma única parede de domínio sob diferentes condições, corrente elétrica DC foi aplicada simultaneamente a tensões mecânicas e campo magnético externo. Foi verificado que quando uma tensão mecânica externa é aplicada, a mobilidade da parede de domínio diminui. Já quando a corrente foi aplicada na amostra, um aumento ou decréscimo da mobilidade axial da parede foi observado, dependendo do sentido da corrente aplicada. Quando foi tratado da velocidade ortogonal da parede de domínio, não foi observada influência da corrente. Por outro lado, foi verificado uma modificação no comprimento da parede de domínios. Além disto, foi observado uma mudança na forma da parede de domínio, passando de um formato cônico para parabólico. Os resultados são explicados em termos da mudança na energia magnética promovida pelo campo de Oersted, gerado pela corrente aplicada, que por sua vez modifica o comprimento e a forma da parede de domínio sem que a velocidade ortogonal da parede de domínio seja alterada pela corrente aplicada.

Ce manuscrit est consacré à la croissance par HVPE et à la spectroscopie optique de nanofils d'InxGa1-xN et de microfils de GaN en vue de la réalisation de diodes électroluminescentes. Les microfils de GaN, épitaxiés par SAG-HVPE, ont été étudiés par micro-réflectivité et micro-photoluminescence. Un lien entre les différences de polarités au sein des fils et leurs propriétés optiques a été mis en évidence. De plus, il a été démontré que les microfils agissent comme des résonateurs optiques dans lesquels une émission stimulée de lumière a été observée. Des reprises de croissance par MOCVD ont permis de révéler le potentiel des microfils pour la réalisation de DELs sous forme d'hétérostructures coeur - coquille. Les nanofils d'InxGa1-xN ont été obtenus pour la première fois à l'Institut Pascal grâce à une étude thermodynamique et une étude expérimentale utilisant GaCl et InCl3 comme précurseurs en éléments III. Une variation de composition en indium de 0 à 100 % le long d'un unique échantillon a été rapportée dans un premier temps. L'optimisation du positionnement des échantillons par rapport à l'arrivée du flux d'indium associée à une étude systématique de l’influence des différents paramètres de croissance a permis de déterminer les facteurs contrôlant la composition et la morphologie des fils. Une étude par spectroscopie optique en fonction de la température a finalement montré une faible diminution de l'intensité de photoluminescence entre 20 K et 300 K. / This work is devoted to the HVPE growth and to the optical spectroscopy of InxGa1-xN nanowires and GaN microwires in order to realize light-emitting diodes.The GaN microwires, grown by SAG-HVPE, were studied by micro-reflectivity and micro-photoluminescence. A link between the polarity differences within wires and their optical properties has been highlighted. In addition, microwires have been shown to act as optical resonators in which stimulated light emission has been observed. Regrowth by MOCVD revealed the potential of microwires for LEDs realization with a core - shell structure.The InxGa1-xN nanowires were obtained for the first time at Institut Pascal thanks to a both thermodynamical and experimental investigations using GaCl and InCl3 as III element precursors. An indium composition variation from 0 to 100 % along a single sample was first reported. The optimization of the sample positioning regarding the indium flux arrival associated with a systematic study of the influence of growth parameters have allowed to determine influential factors on the composition and the morphology of wires. A temperature dependent optical analysis has finally shown a slight decrease of luminescence intensity between 20 K and 300 K.

Les microfils métalliques polycristallins produits par étirage à froid présentent une résistance mécanique significative en faisant des candidats idéaux pour les renforts de composites. Des études antérieures sur des fils de nickel polycristallin pur ont montré une dépendance importante par rapport à la taille de la limite d'élasticité et de la résistance à la traction, ainsi que de la ductilité.Le but de cette étude est de comprendre cet effet de la taille dans les microfils de nickel pur polycristallin par analyse de diffraction des rayons X in-situ (DRX) et simulations de la plasticité cristalline par éléments finis (CPFE). Des essais de traction monotone et cyclique in-situ sous rayonnement synchrotron ont été réalisés sur des microfils de diamètres allant de 100 à 40 μm. Les fils étirés à 100 micromètres obtenus dans le commerce présentent une architecture cœur-coquille avec une texture de fibre <111> dominante dans le cœur et une texture à double fibre hétérogène <111> et <100> dans la coquille. La réduction de la taille de l'échantillon par polissage électrolytique conduit à des fils ayant une microstructure homogène, tandis que la réduction de la taille de l'échantillon par un étirage à froid supplémentaire conduit à des fils avec une texture plus intense tout en conservant l'architecture cœur-coquille.La limite d'élasticité et la résistance à la traction des fils électropolis augmentent avec la diminution du diamètre, tandis que la ductilité diminue avec la réduction du diamètre. Dans le cas des fils étirés à froid, on observe que la limite d'élasticité et la résistance à la traction, ainsi que la ductilité, augmentent avec la diminution du diamètre. L'analyse DRX indique une plasticité successive des familles de grains sous iso-déformation. Nous avons observé que le gradient de la texture du microfil active des mécanismes de déformation qui ne sont pas observés pour les microfils à texture homogène. Pour comprendre l'influence de différents paramètres microstructuraux, notamment l'influence de la texture cristallographique, une microstructure représentative 3D a été générée et des simulations CPFE ont été réalisées. Le comportement simulé moyen des différentes familles de grains (<111>, <100>) concorde bien avec les résultats expérimentaux. La simulation CPFE indique une hétérogénéité du champ de contrainte à travers la microstructure en présence d'un gradient de texture cristallographique.Nous montrons que la micro-texture (texture simple ou double texture) et leur dispersion spatiale (homogène ou architecturée) peuvent être utilisées comme stratégie de conception pour obtenir une microstructure optimale en fonction de l’ensemble désiré de propriétés mécaniques. / Polycrystalline metallic microwires produced by cold-drawing exhibit significant mechanical strength that make them ideal candidates for reinforcement of composites. Previous studies on polycrystalline pure nickel wires have indicated a significant size dependence of their yield and tensile strength as well as their ductility. The aim of this study is to understand these size effects by in-situ X-ray diffraction (XRD) analysis and crystal plasticity finite element (CPFE) simulations. In-situ monotonous and cyclic tensile tests under synchrotron radiation were carried on microwires with diameters ranging from 100 to 40 µm. The commercially obtained 100µm as-drawn wires exhibit a core-shell architecture with <111> fiber texture dominant in core and heterogeneous dual fiber texture <111> and <100> in the shell. Reduction of specimen size by electropolishing leads to wires having a homogeneous microstructure, whereas reduction of specimen size by further cold drawing leads to wires with a sharper texture while retaining the core-shell architecture.The yield and tensile strength of the electropolished wires increase with decreasing diameter, whereas the ductility decrease with decreasing diameter. In the case of cold-drawn wires, the yield and tensile strength, and also the ductility was observed to increase with decreasing diameter. The XRD analysis indicates successive yielding of grain families under iso-strain condition. The gradient in the texture of the microwire was seen to activate deformation mechanisms which are not seen for microwires with homogeneous texture. To understand the influence of different microstructural parameters, and notably the influence of crystallographic texture, 3D representative microstructure was generated and CPFE simulations were carried out. The simulated average behavior of different grain families (<111>, <100>) agrees well with the experimental results. The CPFE simulations indicate heterogeneity in stress field across the microstructure in the presence of a gradient in crystallographic texture.We show that the microstructure engineering of micro-texture components (single- or dual-texture) and their spatial spread (homogenous or architectured) can be used as design guidelines for obtaining optimal microstructure in accordance with desired set of mechanical properties.

Cette thèse de doctorat porte sur la conception et la fabrication de microfils optiques de silice par la technique de fusion et d'étirage de fibres optiques standards, ainsi qu'une étude détaillée de leurs propriétés élastiques par spectroscopie Brillouin. Nous apportons une description complète, théorique et expérimentale, des spectres Brillouin rétro-diffusés par les microfils, révélant ainsi l'existence de plusieurs familles d'ondes élastiques, telles que les ondes hybrides et surfacique, ainsi que de nombreux anti-croisements. En exploitant l'ensemble de ces propriétés élastiques, nous démontrons ensuite une technique de mesure optique, simple et non-destructive, du diamètre des microfils et de leur uniformité, avec une très grande précision et une sensibilité de quelques nanomètres, comparable aux techniques conventionnelles comme la microscopie par balayage électronique. Nous réalisons en supplément une cartographie des ondes élastiques le long des microfils optiques par la technique de corrélation Brillouin de phase. Une autre étude majeure de cette thèse a porté sur la dépendance du spectre Brillouin en fonction d'une déformation axiale des microfils optiques qui présentent une très grande élasticité et des coefficients de contraintes élevés. Pour la première fois à notre connaissance, nous avons observé l’effet des non-linéaritiés des constantes élastiques de la silice dans un microfil optique fortement déformé sur les coefficients de contraintes. L'ensemble de ces travaux représente une étude fondamentale du processus de diffusion Brillouin dans les microfils optiques et permet également d'ouvrir la voie aux développements de dispositifs photoniques compacts dans le domaine des capteurs et des télécommunications. / This thesis reports the design and fabrication of subwavelength-diameter silica optical fibers, also known as optical micro and nanowires. These hair-like slivers of glass, manufactured by tapering optical fibers down to a size hundred times smaller than a strand of human hair, have a number of optical and mechanical properties that make them very attractive for both fundamental physics and technological applications. In addition to providing strong light confinement and enhanced nonlinear optical effects, they exhibit a large evanescent field, enabling applications not currently possible with comparatively bulky optical fibers.We here explore their elastic properties through Brillouin spectroscopy. We specifically provide a complete description, both theoretically and experimentally, of the backward Brillouin spectra including the observation of both bulk hybrid and surface acoustic waves with many anti-crossings. A very good agreement is found between numerical simulations of the elastodynamics equation and the experimental Brillouin spectra for a wide range of wire diameters. From this study, we demonstrate a simple and non-destructive in-situ technique for measuring the diameter of these ultra-thin fibers and their uniformity with a high sensitivity of only a few nanometers. A distributed measurement of both the surface and hybrid acoustic waves along an optical microwire was then performed using Brillouin optical correlation technique. We further investigate the tensile strain dependence of Brillouin scattering in optical microwires and report, for the first time to our knowledge, evidence of a strong elasticity and non-linearity of the elastic constants of silica. This thesis therefore demonstrates that optical microwires can find various potential applications for strain optical sensing.