Dans le domaine des couches minces (épaisseur~Å) associant un métal magnétique (Fe, Co, Ni) et un élément non magnétique (essentiellement métallique ou isolant), de remarquables propriétés physiques (aimantation, transport) nécessitent des caractérisations structurales fines. En particulier, citons le cas de jonctions tunnel (métal/isolant/métal) à aimantation perpendiculaire qui sont en cours d'étude au laboratoire Spintec (UMR8191 (CEA/CNRS/UJF). Ces nanomatériaux sont déposés par voie physique (pulvérisation cathodique) au sein de ce laboratoire. Ces nanostructures sont également sondées par diffraction aux rayons X au sein de l'Institut Néel (UPR 2940) via une collaboration entre Spintec et une équipe de cet Institut (Surface, interfaces et nanostructures du Département MCMF, Matière Condensée, Matériaux, et Fonctions). Ces mesures de réflectivité X constituent la sonde privilégiée de choix dans la cadre de cette thèse. D'autres voies sont également exploitées: à l'aide des moyens de rayonnement synchrotron tels que la spectroscopie d'absorption de rayons X : EXAFS, XANES et XMCD. La thèse aura pour but d'étudier expérimentalement ces phénomènes en couches continues sur ces empilements à jonction tunnel avec aimantation perpendiculaire. Plus précisément, le travail de thèse permettra de comprendre les mesures magnétiques (effectuées à l'institut Néel notamment par magnétométrie SQUID et HALL à basse température) grâce à une batterie de mesures structurales (diffraction aux rayons X, rasant, figures de pôles, réflectivité, absorption X …). Notamment, l'influence des paramètres de dépôt (types de couches, épaisseurs, recuits) du matériau sont étudiées via la collaboration entre les différents groupes de recherche précédemment cités. Cette thématique s'inscrit d'une part dans le cadre de travaux menés à Spintec et dédiés à la recherche de nouveaux matériaux à forte valeur ajoutée industrielle (sur le stockage d'information à ultrahaute densité sur media discrets par exemple). Elle s'inscrit d'autre part dans le renforcement de liens entre recherches fondamentales (laboratoire propre du CNRS comme l'institut Néel) et appliquées (CEA), avec un recours aux solides compétences en caractérisations structurales et magnétiques de l'Institut Néel. / In the domain of thin film (thickness ~ Å) combining a magnetic metal (Fe, Co, Ni) and a non-magnetic (largely metal or insulator), remarkable physical properties (magnetization, transport) require fine structural characterization. In particular, include the case of tunnel junctions (metal / insulator / metal) with perpendicular magnetization which are being studied in the laboratory Spintec (UMR8191 (CEA / CNRS / UJF). These nanomaterials are deposited by physical (sputtering) in this laboratory. These nanostructures are probed by X-ray diffraction in the Neel Institute (UPR 2940) via collaboration between Spintec and a team of the Institute (Surface, Interfaces and Nanostructures Department MCFP, Condensed Matter Materials and Functions). These reflectivity measurements X are the preferred sensor of choice in the context of this thesis. Other routes are also used: using means such as synchrotron radiation absorption spectroscopy X-ray: EXAFS, XANES and XMCD. The thesis will aim to study these phenomena experimentally in continuous layers on the tunnel junction stacks with perpendicular magnetization. Specifically, the thesis will include the magnetic measurements (performed at the Institut Néel SQUID magnetometry including HALL and low temperature) through a battery of structural. This theme is part of a share in the context of work carried Spintec and dedicated to research of new materials with high added value industries (information storage on ultra-high density of discrete media for example). It registers on the other hand in strengthening links between basic research (CNRS own laboratories as Neel Institute) and applied (ECA), with strong skills in use of structural and magnetic characterization of the Institute Neel.

Les céramiques transparentes élaborées par cristallisation complète du verre constituent une nouvelle famille de matériaux de qualité photonique en compétition avec la technologie des monocristaux pour les applications optiques. Cette approche verrière offre des avantages considérables par rapport aux monocristaux et aux céramiques polycristallines frittées : un coût réduit, la possibilité d’une production à grande échelle, une large gamme de compositions chimiques accessibles, une mise en forme plus souple et un taux de dopage élevé. Dans le cadre de ce travail, nous avons synthétisé des céramiques polycristallines transparentes de Sr3Al2O6 et Sr3Ga2O6 (structures cubiques) par cristallisation complète du verre de même composition. Les verres d'aluminate de strontium (75SrO-25Al2O3) et de gallate de strontium (75SrO-25Ga2O3) sont élaborés par lévitation aérodynamique couplée à un dispositif de chauffage laser. La transparence de la céramique de Sr3Al2O6 obtenue s’explique par son isotropie optique, ses joints de grains très fins et sa structure totalement dense (non poreuse). Nous avons également développé une nouvelle famille de céramiques transparentes Sr1+x/2Al2+xSi2-xO8 (0<x≤0.4) obtenues par cristallisation complète et congruente du verre. La transmission exceptionnelle de plus de 90% dans la gamme visible et proche infrarouge est expliquée grâce à des études microstructurales et structurales. Cette transparence qui atteint la limite théorique est associée à une biréfringence quasi nulle, des joints de grains très fins et une porosité nulle. Les études par RMN prouvent l'existence d'un désordre chimique qui est à l'origine de la valeur pratiquement nulle de la biréfringence calculée par DFT. Ces matériaux céramiques polycristallins évolutifs et hautement transparents sont des candidats prometteurs pour une large gamme d'applications optiques et photoniques dans les gammes IR et visible. Cette étude a donc conduit à de nouvelles céramiques transparentes, avec des valeurs de transmission jamais atteintes jusqu’à présent pour des oxydes. Elle propose également une nouvelle approche pour l'obtention de céramiques transparentes dans le cas de matériaux anisotropes : introduire un désordre chimique contrôlé au sein du matériau afin d’induire une isotropie optique. Ce concept ouvre la voie à de nouvelles compositions, étendant ainsi le domaine des céramiques transparentes et de leurs applications. / Transparent polycrystalline ceramics elaborated by full crystallization from glass are an emerging class of photonicquality materials competing with single crystal technology, especially for optical applications. This approach provides considerable advantages over single crystals and polycrystalline sintered ceramics represented by cost effectiveness, large scale production, wide range of accessible chemical compositions, easy shaping and high doping level hosting structure. In this work, we show the preparation of transparent cubic Sr3Al2O6 and Sr3Ga2O6 polycrystalline ceramics by full crystallization from the parent strontium aluminate (75SrO-25Al2O3) and strontium gallate (75SrO-25Ga2O3) glasses elaborated by aerodynamic levitation coupled to laser heating system. The transparency of the obtained Sr3Al2O6 ceramics is explained by their optical isotropy, thin grain boundaries and highly dense (non-porous) microstructure. We also show a series of novel Sr1+x/2Al2+xSi2-xO8 (0<x≤0.4) oxide compositions leading to highly transparent and readily scalable polycrystalline ceramics to be obtained by full congruent glass crystallization. The outstanding transparency exceeding 90% in the visible and near IR range is explained through different microstructural and structural (average and local) studies. This transparency, reaching the theoretical limit, is associated to the almost null birefringence, thin grain boundaries and non-porosity. NMR experiments prove the existence of chemical disorder which is at the origin of the relatively zero birefringence value calculated by DFT computations. These scalable and highly transparent polycrystalline ceramic materials are promising candidates for a wide range of optical and photonic applications in the IR and visible ranges. This study besides revealing new ceramic compositions with previously unreported transmission values for micro-scale polycrystalline materials, proposes a new approach for obtaining transparent ceramics in anisotropic materials. This approach consists in inducing a controlled chemical disorder within the material in order to induce optical isotropy. It is anticipated that this proposed concept will open the way to different composition candidates to be elaborated as transparent polycrystalline ceramics, thus extending the ceramic technology domain and its applications.

In this work, our initial efforts have been directed to study the behavior of the magnetization as a function of temperature, calculated according to the approximate method of the anisotropy constants and the resolution of a Hamiltonian (that includes the crystal field) as exemplified for the DyAl2 compound. Furthermore, we investigated the magneto-thermal characteristics of some members of the RX2 series (R: rare earth, X: Al, Ni), including spin reorientation (SR), by using a model Hamiltonian, that consists of localized magnetic moments interacting via exchange and crystal field interaction, in the molecular-field approximation. We studied how the SR depends on the direction of the application of magnetic field, the intensity of this field and temperature. For the magnetic calculations, the problem of self-consistency was solved by using a computational routine developed in the Fortran 90 programming language. We emphasize that special attention was directed to the crystal field, because of its high relevance to the anisotropic characteristics of the RX2 studied compounds. Thus, in our attempts to study the peculiarities of the rare earth elements, due to crystal field effects, we have not only considered the intensity change, but the direction change of the applied field. In the cases of both Er+3 and Tb+3 compounds, we obtained second-order or continuous magnetization behavior along the polar angle axis. We stressed that the crystal field terms plays an important role in the first order spin reorientation for Dy+3 and Ho+3 compounds. First, it can be revealed by the discontinuity in the Cartesian components of the magnetization vector as a function of the polar angle. Second, the discontinuity is of great importance in the calculation of latent heat associated to the spin reorientation in the case where the first order transitions were observed. Finally, we were able to separate the first and second order contributions of the anisotropic magnetic entropy change, which is the main result of this work. / Neste trabalho, nossos esforços iniciais foram direcionados a estudar o comportamento da magnetização em função da temperatura, calculado segundo o método aproximativo das constantes de anisotropia e da resolução de um hamiltoniano (que inclui o campo cristalino) como exemplificado para o composto DyAl2. Além disto, investigamos as características magneto-térmicas de alguns integrantes da série RX2 (R: Terra rara; X: Al, Ni), incluindo a reorientação de spin (RS), usando um hamiltoniano modelo que consiste de momentos magnéticos localizados interagentes via interações de troca e de campo cristalino, na aproximação do campo molecular. Estudamos como a RS depende da direção de aplicação do campo magnético, da sua intensidade e da temperatura. Para os cálculos magnéticos, o problema da auto consistência foi solucionado utilizando uma rotina, computacional desenvolvida na linguagem computacional Fortran 90. Ressaltamos que, uma atenção especial foi direcionada ao campo cristalino, por conta da sua alta relevância sobre as características anisotrópicas dos compostos RX2 estudados. Portanto, em nossas tentativas para estudar as peculiaridades dos elementos terras raras, devido aos efeitos do campo cristalino, não consideramos somente a mudança na intensidade, mas a variação na direção do campo aplicado. No caso dos compostos Er+3 e Tb+3, obteve-se um comportamento da magnetização de segunda ordem ou contínuo face à mudança do ângulo polar. Salientamos que os termos de campo cristalino desempenham um papel fundamental na reorientação de spin de primeira ordem para Dy+3 e Ho+3. Primeiro, tal transição pode ser revelada por uma descontinuidade nas componentes cartesianas do vetor de magnetização em função do ângulo polar. Segundo, a descontinuidade é de grande importância para o cálculo do calor latente associado à reorientação spin nos casos em que foram observadas as transições de primeira ordem. Finalmente, foi possível separar as contribuições de primeira e segunda ordem da variação de entropia magnética anisotrópica, o qual é o principal resultado deste trabalho.

As interessantes propriedades eletrônicas, mecânicas e óticas dos materiais orgânicos conjugados fizeram emergir diversas aplicações tecnológicas e comerciais em dispositivos baseados nesses materiais, tais como sensores, memórias, células solares e diodos emissores de luz poliméricos (LEDs). Neste sentido, o tema central desta tese é o estudo das propriedades elétricas e morfológicas e os mecanismos de transporte eletrônico de cargas no PEDOT:PSS, uma blenda polimérica que consiste de um policátion condutivo, o poli(3,4- etilenodioxitiofeno) (PEDOT) e do poliânion poli(estirenosulfonado) (PSS). PEDOT:PSS é amplamente usado como material de eletrodo em aplicações na área de eletrônica plástica, como mencionado anteriormente. Apesar da condutividade elétrica dos filmes finos de PEDOT:PSS possa variar várias ordens de grandeza, dependendo do método pela qual é processado e transformado em filme fino, as razões para este comportamento é essencialmente desconhecido. Esta tese descreve um estudo detalhado do transporte eletrônico de cargas anisotrópico e sua correlação com a morfologia, as condições e as dimensões da separação de fase entre os dois materiais, PEDOT e PSS. Antes de abordar as propriedades do PEDOT:PSS, uma camada de filme fino inorgânica usada para aumentar o tempo de vida de dispositivos orgânicos é descrita no Capítulo 2. Um importante mecanismo de degradação em LEDs poliméricos é a fotooxidação da camada ativa. Assim, isolar a camada ativa da água, oxigênio e luz, torna-se crucial para o aumento do tempo de vida. Um sistema de deposição química a partir da fase de vapor estimulada por plasma (PECVD) é usado para depositar filmes finos de nitreto de carbono em baixas temperaturas, menores que 100 °C, sobre PLEDs com a intenção de aumentar o tempo de vida destes dipositivos e diminuir a fotodegradação do poli[2-metoxi-5- (2-etil-hexiloxi)-p-fenileno vinileno] (MEH-PPV) em ambiente atmosférico. O filme fino de nitreto de carbono possui as características de um material que pode bloquear a umidade e que tem espessura e flexibilidade adequados para a nova geração de PLEDs flexíveis. As características dos filmes finos de nitreto de carbono e MEH-PPV foram investigadas usando-se técnicas de espectroscopia ótica, com particular ênfase no processo de degradação do MEHPPV sob iluminação. Os resultados mostraram que o filme fino de nitreto de carbono protege o filme polimérico e diminui consideravelmente a fotooxidação. Para avaliar o efeito do encapsulamento em dispositivos reais, LEDs poliméricos foram fabricados e pelas curvas de corrente-tensão um aumento no tempo de vida é confirmado quando a camada de nitreto de carbono é presente. O tempo de vida desejado, maior que 10.000 horas, para aplicações comerciais não foi atingido, entretanto, o encapsulamento pode ser melhorado otimizando as propriedades da camada de nitreto de carbono e combinando-as com camadas de outros materiais orgânicos e inorgânicos. Os capítulos seguintes deste trabalho aborda os estudos realizados com o PEDOT:PSS, uma vez que é amplamente usado em eletrônica orgânica, mas relativamente tem recebido pouca atenção com respeito ao transporte eletrônico de cargas, bem como sua correlação com a morfologia. No Capítulo 3, experimentos com microscopia de varredura por sonda (SPM, Scanning Probe Microscopy) e medidas de condutividade macroscópica são utilizados para estudar e obter um modelo 3D morfológico completo que explica, qualitativamente, a condutividade anisotrópica observada nos filmes finos de PEDOT:PSS depositados pela técnica de spin coating. Imagens topográficas de microscopia de varredura por tunelamento (STM) e imagens da seção transversal observadas com o microscópio de forca atômica (X-AFM) revelaram que o filme fino polimérico é organizado em camadas horizontais de partículas planas ricas em PEDOT, separadas por lamelas quasi-contínuas de PSS. Na direção vertical, lamelas horizontais do isolante PSS reduzem a condutividade e impõe o transporte eletrônico a ser realizado por saltos em sítios vizinhos próximos (nn-H, nearest-neighbor hopping) nas lamellas de PSS. Na direção lateral, o transporte eletrônico via saltos 3D em sítios a longas distâncias (3D-VRH, variable range hopping) ocorre entre as ilhas ricas em PEDOT que são separadas por barreiras muito mais finas de PSS, causando um aumento da condutividade nesta direção. Esta discussão é estendida ao Capítulo 4 com uma descrição quantitativa do transporte eletrônico de cargas predominantes. Particularmente, é demonstrado que o transporte de cargas via saltos 3D em sítios a longas distâncias ocorre entre ilhas ricas em PEDOT e não entre segmentos isolados de PEDOT ou dopantes na direção lateral, enquanto que na direção vertical o transporte de cargas via saltos em sítios vizinhos próximos ocorre dentro das lamelas do quasi-isolante PSS. Em algumas aplicações, faz-se necessário usar PEDOT:PSS com alta condutividade elétrica. Isso pode ser feito adicionando-se sorbitol à solução aquosa de PEDOT:PSS. Após um tratamento térmico, e dependendo da quantidade de sorbitol adicionado, a condutividade aumenta várias ordens de grandeza e as causas e consequências de tal comportamento foram investigadas neste trabalho. O Capítulo 5 investiga as várias propriedades tecnológicas do PEDOT:PSS altamente condutivo tratado com sorbitol, tais como a própria condutividade, os efeitos dos tratamentos térmicos e exposição à umidade. É observado que o aumento da condutividade elétrica, devido à adição de sorbitol na solução aquosa, é acompanhado por uma melhoria na estabilidade da condutividade elétrica em condições atmosféricas. Surpreendentemente, a condutividade elétrica do PEDOT:PSS, sem tratamento com sorbitol (~ 10-3 S/cm), aumenta mais de uma ordem de grandeza sob ambiente úmido de 30-35 % umidade relativa. Este efeito é atribuido a uma contribuição iônica à condutividade total. Análise Temogravimetrica (TGA), espectrometria de massa com sonda de inserção direta (DIP-MS) e análise calorimétrica diferencialmodulada (MDSC) foram usadas como técnicas adicionais para o entendimento dos estudos deste Capítulo. No Capítulo 6, microscopia de varredura por sonda-Kelvin (SKPM) foi empregada para medir o potencial de superfície dos filmes finos de PEDOT:PSS tratados com diferentes concentrações de sorbitol. Mostra-se que a mudança no potencial de superfície é consistente com uma redução de PSS na superfície do filme fino. Para estudar o transporte eletrônico nos filmes finos de PEDOT:PSS altamente condutivos tratados com sorbitol, o Capítulo 7 usa medidas de temperatura e campo elétrico em função da conduvitidade correlacionados com analises morfológicas realizadas por STM. É observado que o transporte eletrônico por saltos, na direção lateral, muda de 3D-VRH para 1D-VRH quando o PEDOT:PSS é tratado com sorbitol. Esta transição é explicada por uma auto-organização das ilhas ricas em PEDOT em agregados 1D, devido ao tratamento com sorbitol, tornando-se alinhadas em domínios micrométricos, como observado pelas imagens de STM. / Employing the unique mechanical, electronic, and optical properties of the conjugated organic and polymer materials several technological and commercial applications have been developed, such as sensors, memories, solar cells and light-emitting diodes (LEDs). In this respect, the central theme of this thesis is the electrical conductivity and mechanisms of charge transport in PEDOT:PSS, a polymer blend that consists of a conducting poly(3,4-ethylenedioxythiophene) polycation (PEDOT) and a poly(styrenesulfonate) polyanion (PSS). PEDOT:PSS is omnipresent as electrode material in plastic electronics applications mentioned above. Although the conductivity of PEDOT:PSS can vary by several orders of magnitude, depending on the method by which it is processed into a thin film, the reason for this behavior is essentially unknown. This thesis describes a detailed study of the anisotropic charge transport of PEDOT:PSS and its correlation with the morphology, the shape, and the dimension of the phase separation between the two components, PEDOT and PSS. Before addressing the properties of PEDOT:PSS, a new barrier layer is described in Chapter 2 that enhances the lifetime of organic devices. An important degradation mechanism in polymer LEDs is photo-oxidation of the active layer. Hence, isolating the active layer from water and oxygen is crucial to the lifetime. Plasma-enhanced chemical vapor deposition (PECVD) is used to deposit a thin layer of carbon nitride at low deposition temperatures, below 100 °C, on a polymer LED that uses poly[2-methoxy-5-(2´-ethylhexyloxy)-1,4- phenylene vinylene] (MEH-PPV) as active layer. A thin layer of carbon nitride acts as barrier for humidity, but is still sufficiently bendable to be used in flexible polymer LEDs. The characteristics of carbon nitride and MEH-PPV films have been investigated using optical spectroscopy, with particular emphasis on the degradation process of MEH-PPV under illumination. The measurements show that the carbon nitride coating indeed protects the polymer film and diminishes the photo-oxidation considerably. To study the effect of the encapsulation in real devices, polymer LEDs were made and their current-voltage characteristics confirm the enhanced lifetime in the presence of a carbon nitride barrier layer. However, the target, a lifetime of more than 10,000 hours for commercial applications, was not achieved. The remaining chapters of this thesis describe the investigations of PEDOT:PSS. PEDOT:PSS is widely used in organic electronics. So far, relatively little attention has, been paid to the mechanisms of charge transport in this material and the correlation of those properties to the morphology. In Chapter 3, scanning probe microscopy (SPM) and macroscopic conductivity measurements are used to obtain a full 3D morphological model that explains, qualitatively, the observed anisotropic conductivity of spin coated PEDOT:PSS thin films. Topographic scanning probe microscopy (STM) and cross-sectional atomic force microscopy images (X-AFM) reveal that the thin film is organized in horizontal layers of flattened PEDOT-rich particles that are separated by quasi-continuous PSS lamella. In the vertical direction, the horizontal PSS insulator lamellas lead to a reduced conductivity and impose nearest-neighbor hopping (nn-H) transport. In the lateral direction, 3D variable-range hopping (3D-VRH) transport takes place between PEDOT-rich clusters which are separated by much thinner barriers, leading to an enhanced conductivity in this direction. This discussion is extended in Chapter 4, where a quantitative description of the length scales of the predominant transport is obtained. Particularly, it is demonstrated that the hopping process takes place between PEDOT-rich islands and not between single PEDOT segments or dopants in the lateral direction, whilst in the vertical direction the current limiting hopping transport occurs between dilute states inside the quasi-insulating PSS lamellas. By a post-treatment it is possible to modify PEDOT:PSS to raise its conductivity, by orders of magnitude. Typically, the addition of sorbitol to the aqueous dispersion of PEDOT:PSS that is used to deposit thin films via spin coating leads to an enhancement of the conductivity after thermal annealing. The causes and consequences of such behavior were investigated in detail. Chapter 5 describes the various properties of the highly conductive sorbitol-treated PEDOT:PSS, such as the conductivity itself, and the effects of thermal annealing and exposure to moisture. It is found that the conductivity enhancement upon addition of sorbitol is accompanied by a better environmental stability. Surprisingly, the electrical conductivity of PEDOT:PSS thin films without sorbitol treatment is increased by more than one order of magnitude in an environment with more than 30-35 % relative humidity. This effect is attributed to an ionic contribution to the overall conductivity. Thermal gravimetric analysis (TGA), direct insert probe-mass spectrometry (DIP-MS) and modulation differential scanning calorimetry (MDSC) were used as additional tools to demonstrate that, after thermal treatment, the concentration of sorbitol in the final PEDOT:PSS layer is negligibly small. In Chapter 6, scanning Kelvin probe microscopy (SKPM) is employed to measure the surface potential and work function of this PEDOT:PSS films that were deposited from water with different sorbitol concentrations. It is shown that work function of PEDOT:PSS is reduced with increasing sorbitol concentration. This shift can be explained by and is in agreement with- a reduction in the surface enrichment with PSS of the film. To study the charge transport properties of the highly conductive sorbitoltreated PEDOT:PSS films, temperature dependent and electric field dependent measurements are correlated with morphological analysis by STM in Chapter 7. It is found that by sorbitol treatment the hopping transport changes from 3DVRH to 1D-VRH. This transition is explained by a sorbitol-induced selforganization of the PEDOT-rich grains into 1D aggregates that are aligned within micrometer sized domains, as observed in STM images.

Plútons graníticos (Patrimônio Santo Antônio, São Domingos, Ouro Verde e Santa Rita) alojados na porção nordeste da Suíte Intrusiva Cunhaporanga (c. 620-590 Ma) intrudiram metassedimentos pelíticos e carbonáticos de baixo grau metamórfico do Grupo Itaiacoca. Os plútons são isótropos, de coloração cinza a rósea e composição monzo- a sienogranítica, predominando granitóides porfiríticos grossos e, secundariamente, tipos inequigranulares a equigranulares. A cartografia regional mostrou que a foliação das rochas metassedimentares encaixantes mergulha dominantemente para NE e contém uma lineação (interseção, mineral) de direção NNW-SSE. A trama metamórfica das encaixantes assume progressivamente a direção NE-SW conforme se aproxima da zona de cisalhamento transcorrente de Itapirapuã, onde quartzo-milonitos verticalizados exibem uma cinemática sinistral. A trama dos plútons foi estudada pela técnica da anisotropia de suscetibilidade magnética (ASM). Foram amostradas 40 estações (300 espécimes) no granito porfírítico Patrimônio Santo Antônio, 7 estações (48 espécimes) no granito equigranular fino de São Domingos, 9 estações (67 espécimes) no granito inequigranular de Ouro Verde e 14 estações (92 espécimes) no granito porfiritico foliado de Santa Rita. A suscetibilidade magnética média (k) do granito Patrimônio Santo Antônio é da ordem de 23,29 x \'10 POT.-3\' SI, enquanto nos granitos Santa Rita (k = 11,85 mSI), São Domingos (k = 7,43 mSI) e Ouro Verde (k = 7,46 mSI) são menores. Por outro lado, a anisotropia magnética (P = \'k IND.max\'/\'k IND.min\', onde \'k IND.max\' > \'k IND.int\' > \'k IND.min\') é menor em Patrimônio Santo Antônio (P = 1,09 ± 0,04) do que no São Domingos (P = 1,21 ± 0,09), Ouro Verde (P = 1,19 ± 0,07) e Santa Rita (P = 1,23 ± 0,11). Estudos termomagnéticos e de magnetização remanente isotermal mostraram que as propriedades magnéticas dos granitoides são dominadas pela magnetita (pobre em Ti) e, secundariamente, Ti-hematita. Sulfetos de Fe (pirita, calcopirita) ocorrem como acessórios. Os óxidos de Fe estão frequentemente associados à titanita, biotita e anfibólio e suas microestruturas são tipicamente magmáticas, exceto no granito Santa Rita onde a microestrutura apresenta evidência de recristalização pós-magmática. A foliação magnética dos maciços graníticos mergulha suave a moderadamente e, no plúton Patrimônio Santo Antônio, exibe um padrão tipicamente dômico. A lineação magnética subhorizontal orienta-se na direção NNW-SSE paralelamente ao eixo do dobramento regional das rochas metassedimentares encaixantes. Esta característica indica que os granitos são sin-tectônicos a um evento deformacional cujo controle está aparentemente relacionado ao funcionamento das grandes transcorrências regionais de direção NE-SW. A ocorrência de domos graníticos (Patrimônio Santo Antônio) e elipsóides magnéticos dominantemente prolatos (São Domingos) sugerem que a trama NNW teria sido formada por uma tectônica que combina transcorrência e extensão. Uma idade concordante U-Pb (SHRIMP) em zircão de 589 ± 6 Ma, atribuída à cristalização do plúton Patrimônio Santo Antônio, indica que a deformação que afetou o granito no estado magmático bem como suas encaixantes ocorreu nos estágios finais da formação da Suíte Intrusiva Cunhaporanga. / Granite plutons located on the northeast of Cunhaporanga Intrusive Suite (Patrimônio Santo Antônio, Ouro Verde, São Domingos and Santa Rita) are emplaced into low grade metasedimentary rocks (Itaiacoca Group) of the Apiaí Domain (Ribeira Belt). Most of these plutons are isotropic with pinkish to grey colors and their compositions vary from monzogranite to sienogranite. They are usually porphyritic and locally inequigranular and equigranular. Regional mapping revealed that the foliation of the metasedimentary host rocks dips mainly to NE while the lineation (intersection, mineral) strikes in the NNW-SSE direction. The host rocks metamorphic fabric rotates progressively to become parallel to the NE-trending Itapirapuã transcurrent shear zone. Kinematic markers such as elongated quartz grains and mica-fish from quartz-milonites indicate the Itapirapuã shear records a sinistral movement. The fabric of the plutons was studied by anisotropy of magnetic susceptibility (AMS) technique. Forty sites (300 specimens) were sampled at the Patrimônio Santo Antônio granite, 7 sites (48 specimens) at São Domingos, 9 sites (67 specimens) at Ouro Verde and 14 sites (92 specimens) at Santa Rita granite. The mean of magnetic susceptibility (k) is higher in Patrimônio Santo Antônio granite (k = 23,29 x \'10 POT.-3\' SI) and lower in the granites of Santa Rita (k = 11,85 mSI), São Domingos (k = 7,43 mSI) and Ouro Verde (k = 7,46 mSI). In contrast the magnetic anisotropy (P) is lower in the Patrimônio Santo Antônio granite (P = 1,09 ± 0,04) and higher in the granites São Domingos (P = 1,21 ± 0,09), Ouro Verde (P = 1,19 ± 0,07) and Santa Rita (P = 1,23 ± 0,11). Thermomagnetic and Isothermal Remanent Magnetization (IRM) studies show that Ti-poor magnetite is the principal carrier of rock magnetic properties but that includes minor contributions of Ti-hematite. Iron oxides are frequently associated with titanite, biotite and amphibole. Microstructures are typically magmatic, except for Santa Rita granite which shows post-magmatic recrystallized microstructures. The magnetic foliation of granitic plutons dips smooth to moderately and for the Patrimônio Santo Antônio body it exhibits a typical dome pattern. The subhorizontal magnetic lineation strikes NNW-SSE parallel to regional folding axe of the metasedimentary rocks. This feature shows that the granites are syntectonic to a deformation event apparently connected to NE-trending transcurrent shears. The occurrence of a foliation dome in the Patrimônio Santo Antônio pluton and prolate magnetic ellipsoids in São Domingos pluton suggest that the NNW-trending structures includes, besides a strike-slip shear fabric, a component of extension that probably assisted the emplacement of the plutons. A U-Pb (SHRIMP) determination in the Patrimônio Santo Antônio zircons have produced a concordia age of 589 ± 6 Ma attributed to the crystallization of the granite. These results indicate that in the latest stages of the development of the Cunhaporanga Intrusive Suite the Apiaí Domain was submitted to a regional strain field recording transcurrent simple shear and extension.

A trama de magmas graníticos alojados na crosta intermediária e superior pode-se originar pela ação de forças de corpo (ascensionais, convectivas) e/ou tectônicas. Diferentes mecanismos podem concorrer para a formação de tramas, embora a interação entre a deformação magmática e a tectônica regional seja um dos mecanismos fundamentais, notadamente nos granitos alojados em faixas orogênicas. No Domínio Apiaí da Faixa Ribeira (SP - PR), os batólitos graníticos alongados têm sido historicamente classificados como sintectônicos, ou seja, colocados durante o desenvolvimento de um arco magmático continental neoproterozóico. Os plútons menores, de forma circular a ovalada, geralmente discordantes e com típica coloração avermelhada, são considerados pós-tectônicos ou alojados após a colisão continental entre os diferentes blocos litosféricos que formaram a Faixa Ribeira. Essa classificação esquemática tem sido baseada em geoquímica e geocronologia dos granitos. Este trabalho identificou e mapeou a trama interna dos plútons sin-tectônicos (Ribeirão Branco) e pós-tectônicos (Capão Bonito e Sguário) utilizando a anisotropia de suscetibilidade magnética (ASM), de forma a inserí-los propriamente nos modelos de classificação tectônica, cujas premissas básicas são de natureza estrutural. Os granitos porfiríticos (Ribeirão Branco e Itaóca) possuem uma elevada suscetibilidade magnética (k 10-2 SI), a qual é menor (k 5 x 10-3 SI) nos granitos vermelhos (Capão Bonito e Sguário). A suscetibilidade dos granitos porfiríticos é proveniente de óxidos ferromagnéticos, notadamente magnetita pobre em Ti, que encontra-se frequentemente associada com titanita, biotita e anfibólio. Nos granitos vermelhos a suscetibilidade é gerada por magnetita, variavelmente oxidada (maghemita) e Ti-hematita (hemo-ilmenita), havendo também significativa contribuição da fração paramagnética (biotita cloritizada) à suscetibilidade total nas rochas, quando k < 10-3 SI. O grau de anisotropia magnética (P) tanto nos granitos porfiríticos como nos vermelhos é variável, porém tipicamente maior nos porfiríticos (P = 1,14, dp. 0,08), se comparado aos vermelhos (P = 1,07, dp. 0,05). A maior anisotropia de suscetibilidade no plúton Ribeirão Branco é atribuída a uma incipiente foliação detectada em vários setores do granito, que contrasta com a microestrutura aparentemente isótropa dos granitos vermelhos. O estudo da trama de silicatos no granito porfirítico Itaóca e no granito Capão Bonito mostrou que os eixos principais de anisotropia de suscetibilidade magnética e da orientação preferencial de forma (OPF) de feldspato e de biotita, são correspondentes, porém, comumente oblíquos. Essa obliquidade entre eixos é atribuída às características físicas próprias (forma, tamanho e anisotropia) dos minerais marcadores da trama. O estudo combinado da ASM e da OPF revelou ainda que P tende a crescer com a intensidade da orientação preferencial de silicatos, o que permitiu identificar os domínios de maior deformação magmática e correlacioná-los com a estrutura regional. A trama magnética do granito Ribeirão Branco organiza-se em coerência com uma tectônica regional transcorrente sinistral. Na margem ocidental deste granito, contudo, a orientação da trama é diferente do restante do maciço, tendo sido aparentemente afetada pela intrusão do granito Sguário. A trama magnética do Ribeirão Branco contrasta com a do plúton Itaóca, este último exibindo um padrão concêntrico que antecedeu ao desenvolvimento da deformação transcorrente regional. Zircões do Itaóca forneceram uma idade U-Pb (SHRIMP) concordante de 623 ± 10 Ma, atribuída à cristalização deste plúton. Dados da literatura indicam que o granito Capão Bonito é aproximadamente 15 Ma mais jovem que os batólitos de granito porfirítico. O Capão Bonito, entretanto, apresenta uma trama muito bem organizada, típica de intrusões sin-tectônicas, destacando-se excelente alinhamento da lineação magnética. No granito Sguário, o arranjo da trama é tipicamente helicoidal e, junto com a estrutura do Capão Bonito, podem ter sido organizadas em resposta a uma deformação transcorrente E-W destral. Este evento tardio estaria associado à reativação da zona de cisalhamento Ribeira, que afetou a borda sul do granito Itaóca e que contém uma componente extensional. A deformação transtensiva E-W, que favoreceu a injeção dos granitos vermelhos no Domínio Apiaí, sucederia a um evento tectonomagmático principal, que teria sido responsável pela colocação e deformação dos batólitos de granito porfirítico. A intrusão dos grandes corpos graníticos ocorreu em torno de 615 Ma e foi relacionada à convergência crustal e estiramento subparalelo à Faixa Ribeira, com a deformação localizada notadamente nas estruturas transcorrentes de direção NE-SW. / The fabric of granitic magmas emplaced in the middle and upper crustal levels can be caused by the stress action during the ascension and convection of plutons and/or tectonic strain. Several mechanisms can contribute for the previous thing, nevertheless the interaction between the distortions and tectonic is the domineering one, principally in granites located in orogenic belts. In the Apiaí domain of the Ribeira belt (SP-PR) the elongated granitic batholiths have been historically classified like syn-tectonic and them was emplaced during the development of a neoproterozoic continental magmatic arch. Small Plutons with subcircular to oval forms generally discordant with regard to the disposition of the regional structures and that in turn possess feldspars of reddish typical colour, had been considered pos-tectonic, and therefore, emplaced after the collision that joined the different litho-tectonic units that constitute the Ribeira orogenic belt. This schematic classification of these granites relicts on geochemistry and geochronology data. In this study was identified and recorded in map the internal fabric of the syn-tectonic Ribeirão Branco granite and of the pos-tectonic Capão Bonito and Sguário granites using the anisotropy of magnetic susceptibility (AMS) with the aim of inserting them appropriately in the models of tectonic classification whose basic premises are of structural nature. The porphyritic Ribeirão Branco and Itaóca granites have a high magnetic susceptibility (k = 10-2 SI), which is minor than (k = 5 x 10-3 SI) in the red granites (Capão Bonito, Sguário). In the first ones the poor Ti magnetite is the main source of susceptibility, commonly associated to titanite, biotite and amphibole. In the red granites, the susceptibility is provided by magnetite variability rusty (maghemite) and Ti - hematite (hemo-ilmenite), in addition to the significant contribution of biotite altered by hydrothermal processes. The grade of anisotropy rise (P) in the porphyritic granites (P = 1,14 SD. 0,08) and this is bigger than in the red ones (P = 1,07, SD. 0,05). In the Ribeirão Branco pluton, the high value of P is attributed to an incipient foliation detected in several sectors, which contrasts with the microstructure seemingly isotropic of the red granites. The study of the fabrics of silicates in the porphyritic granites Ribeirão Branco and Itaóca revealed that the orientations of the main axes of AMS and of shape preferred orientation (SPO) of feldspar and mafic silicates (biotite + amphibole) are congruent, nevertheless some obliquities occur. Those obliquities are attributed to the influence of the proper characteristics (form, size, anisotropy) of the marker minerals of the respective sub fabrics. In the same way, the above-mentioned study of silicates fabric demonstrated that P tends to grow up with the intensity of the SPO of silicates, which allowed to identify domains with major magmatic distortion into de granitic bodies and to correlate them with the regional structure. In general, the magnetic fabric of the Ribeirão Branco granite is organized coherently with the tectonic regional sinestral strike-slip shear zones; nevertheless, in the western sector the orientation of the magnetic fabric was likely modified by the accommodation of the Sguário granite. In the Itaóca granite, the organization of the magnetic fabric is different if compared with fabrics of the previous pluton. In Itaóca granite was recorded a fabric with a concentric organization in 623 ± 10Ma. (MSWD 0,31), according to the concordant U-Pb (SHRIMP) age in zircons obtained for the crystallization of the granite, that seems to be occurred before the strain related with the activation of the regional strike-slip shear zones. Geochronology data of the literature indicates that the Capão Bonito granite is approximately 15 Ma. younger than the batholiths of porphyritic granite. The Capão Bonito granite has an organized fabric typical of syn-tectonic intrusions that has an excellent alignment of the magnetic lineation. In the granite Sguário, the fabric has a spiral organization, in the same way as recorded in Capão Bonito, like response to a strain associated with to a small strike-slip shear zone with W-E direction. This event would be related to the reactivation of the Ribeira strike-slip shear zone, which affected the south sector of the Itaóca granite, with the participation of an extensional component. The W-E transtensive deformation that favoured the injection of the red granites in the Apiaí Domain likely was subsequent to a main tetonomagmatic event and this should have been the responsible by the emplacement and strain in the porphyritic granites. The intrusion of the big granitic bodies ~ 615 Ma. and could be it related to the convergence between crustal blocks and to the consequent stretching sub parallel of the Ribeira belt, in which the distortion was located remarkably in the strike-slip shear zones with NE-SW direction.

Ce mémoire traite de synthèse de textures volumiques anisotropes à partir d’une observation 2D unique. Nous présentons différentes variantes d’algorithmes non paramétriques et multi-échelles. Leur principale particularité réside dans le fait que le processus de synthèse 3D s’appuie sur l’échantillonnage d’une seule image 2D d’entrée, en garantissant la cohérence selon les différentes vues de la texture 3D. Deux catégories d’approches sont abordées, toutes deux multi-échelles et basées sur une hypothèse markovienne. La première catégorie regroupe un ensemble d’algorithmes dits de recherche de voisinages fixes, adaptés d’algorithmes existants de synthèses de textures volumiques à partir de sources 2D multiples. Le principe consiste, à partir d’une initialisation aléatoire, à modifier les voxels un par un, de façon déterministe, en s’assurant que les configurations locales de niveaux de gris sur des tranches orthogonales contenant le voxel sont semblables à des configurations présentes sur l’image d’entrée. La deuxième catégorie relève d’une approche probabiliste originale dont l’objectif est de reproduire, sur le volume texturé, les interactions entre pixels estimées sur l’image d’entrée. L’estimation est réalisée de façon non paramétrique par fenêtrage de Parzen. L’optimisation est gérée voxel par voxel, par un algorithme déterministe de type ICM. Différentes variantes sont proposées, relatives aux stratégies de gestion simultanée des tranches orthogonales contenant le voxel. Ces différentes méthodes sont d’abord mises en œuvre pour la synthèse d’un jeu de textures structurées, de régularité et d’anisotropie variées. Une analyse comparée et une étude de sensibilité sont menées, mettant en évidence les atouts et faiblesses des différentes approches. Enfin, elles sont appliquées à la simulation de textures volumiques de matériaux composites carbonés, à partir de clichés obtenus à l’échelle nanométrique par microscopie électronique à transmission. Le schéma expérimental proposé permet d’évaluer quantitativement et de façon objective les performances des différentes méthodes. / This thesis deals with the synthesis of anisotropic volumetric textures from a single 2D observation. We present variants of non parametric and multi-scale algorithms. Their main specificity lies in the fact that the 3D synthesis process relies on the sampling of a single 2D input sample, ensuring consistency in the different views of the 3D texture. Two types of approaches are investigated, both multi-scale and based on markovian hypothesis. The first category brings together a set of algorithms based on fixed-neighbourhood search, adapted from existing algorithms of texture synthesis from multiple 2D sources. The principle is that, starting from a random initialisation, the 3D texture is modified, voxel by voxel, in a deterministic manner, ensuring that the grey level local configurations on orthogonal slices containing the voxel are similar to configurations of the input image. The second category points out an original probabilistic approach which aims at reproducing in the textured volume the interactions between pixels learned in the input image. The learning is done by non-parametric Parzen windowing. Optimization is handled voxel by voxel by a deterministic ICM type algorithm. Several variants are proposed regarding the strategies used for the simultaneous handling of the orthogonal slices containing the voxel. These synthesis methods are first implemented on a set of structured textures of varied regularity and anisotropy. A comparative study and a sensitivity analysis are carried out, highlighting the strengths and the weaknesses of the different algorithms. Finally, they are applied to the simulation of volumetric textures of carbon composite materials, on nanometric scale snapshots obtained by transmission electron microscopy. The proposed experimental benchmark allows to evaluate quantitatively and objectively the performances of the different methods.

In the present thesis, magnetization reversal in both out-of-plane and in-plane magnetized thin lms and in devices fabricated out of those lms are explored. Pt/Co/Pt stacks with ultrathin Co layer were in-estimated initially for understanding their magnetic properties in this thesis. These perpendicular magnetized systems are good candidates for magnetic hard disc drives due to their large anisotropy, which may allow miniaturization of magnetic data storage devices. The spin Hall e ect mediated current-induced magnetization reversal in patterned Pt/Co/Pt devices were extensively investigated. Investigation of the magnetization reversal by means of a current instead of a magnetic eld is necessary to explore the possibilities of solid state magnetic memory devices. This is the primary motivation behind the investigation of current-induced magnetization reversal in Pt/Co/Pt system, in this thesis. Another important proposal for magnetic data storage is the race track memory, where the domain walls separating magnetic domains (in in-plane or out-of-plane magnetized materials) are moved by using a current. This involves a great deal of understanding of the domain wall motion in Nano-conduits under applied magnetics ends, and currents and also its interaction with engineered geometrical features. In this thesis work, magnetic led-driven domain wall pinning and deepening experiments on in-plane magnetized nanowires of perm alloy were performed to un-distend this interaction and the e act of domain wall chirality. In chapter 1, a general introduction to di errant data storage technologies and the current progress in the leg of spintronic is presented. This will highlight a perspective of this thesis work with respect to the present day research in spintronic and magnetization reversal studies. In chapter 2, a basic background of magnetism using the micromag-netic framework is illustrated. A brief introduction to magnetic domain walls is also presented. The Landau-Lifshitz-Gilbert dynamical equation is discussed and some case studies applied to a single domain particle with uniaxial anisotropy under the effect of spin-orbit torque are illu trated. The basics of spin-orbit coupling leading to spin Hall e ect is also explain In chapter 3, most of the essential experimental tools along with their basic working principles are described. Extensive e orts have been in-vested in designing and building the experimental tools. These include custom designs of a sputter deposition system, an ultra-high vacuum chamber for pulsed laser ablation, a magneto-optic Kerr e ect magne-tometer, a Kerr imaging system and a magneto-transport setup. All of these experimental setups have been automated, details of which are brie y discussed in this chapter. The Kerr imaging system was designed to measure hysteresis loops, observe domain wall motion and to measure domain wall velocity under applied magnetic elds and electric current. The magneto-transport setup was used for studying the domain wall pinning and depinning experiments in permalloy nanowires. In chapter 4, the optimization process for obtaining perpendicular mag-netic anisotropy in Pt/Co/Pt lms is described. The spin reorientation transition with varying thickness of Co (from 1.5 nm down to 0.35 nm) was studied. The magnetization easy axis direction changes from in-plane to out-of-plane as the thickness of Co is reduced. The dependence of Curie temperatures of ultrathin Co lms, with thickness as low as 0.35 nm, on the underlayer Pt thickness and its crystallinity was studied in detail. The e act of Ta but err layer on the texture of the Pt lm, and on the Curie temperature of the Pt/Co/Pt system was evaluated. To gain further insight of the role of the bottom Pt/Co and the top Co/Pt interfaces, ultrathin Cu lbs were inserted at the respective interfaces, and the anisotropy and magnetization reversal behaviour of these lbs were investigated. In chapter 5, studies on current-induced magnetization reversal in mi-corn sized wires of Pt/Co/Pt trilete is presented. The spin Hall e act assisted spin-orbit torque was used to reversibly switch the magnetization of these devices with and without the help of an external magnetic led. Since both the top and bottom layers are Pt, any contribution from Rashia e act towards spin-orbit torque could be ignored. By preparing devices with unequal top and bottom Pt thicknesses, a net spin-orbit torque could be applied to the magnetization of the Co layer. The thickness gradient/induced anisotropy in the Co layer was utilized to experimentally investigate current-induced deterministic switching. Sin-gel domain simulations with spin-orbit torque were also carried out to understand the mechanism of deterministic switching of magnetization in Pt/Co/Pt devices. This study is expected to have made sign cant contributions and to open up the possibilities of further investigation in the studies of spin-orbit torque in Pt/Co/Pt systems for solid state magnetic memory devices. In chapter 6, magnetic led-induced reversal in systems with in-plane magnetic anisotropy is presented. Here the e act of the width of a Nanos-trip on the anisotropy of a soft magnetic material like perm alloy was in-estimated. By introducing a nucleation pad to one end of the perm alloy nanowire, a single domain wall was generated at the junction with apple-cation of a proper magnetic led sequence. This domain wall could be in-jested into the nanowire by a magnetic led and pinned at a geometrical constriction inside the nanowire. The statistics of domain wall pinning and deepening processes indicated two di errant types of domain walls involved in the reversal process. With the assistance of micro magnetic simulations the domain walls were ident end as vortex walls of di errant chirality’s. Thus the interaction of domain walls with a Nano constriction and its dependence on the chirality of domain walls are understood. In chapter 7, a brief summary of the results obtained during the course of investigations is presented. An outlook presented at the end will help the readers of this thesis to understand the important research problems in this area and their potential future aspects.

Magnetostrictive materials belong to an important class of smart magnetic materials which have potential applications as ultrasonic transducers, sensors, actuators, delay lines, energy harvesting devices etc. Although, magnetostrictive property is exhibited by almost all ferro and ferrimagnetic materials, the R-Fe type (R represents rare earth elements) intermetallic compounds display maximum promise owing to the large magnetostriction exhibited by them at ambient temperature. Among the several R-Fe type compounds, Tb-Fe and Sm-Fe alloys are found to exhibit maximum room temperature positive and negative magnetostriction respectively. Recently, Fe-Ga based alloys have gained significant interest as newly emerging magnetostrictive material due to a good combination of magnetic and mechanical properties. These magnetostrictive materials in thin film form are of interests for several researchers both from fundamental and applied perspectives. Currently, many researchers are exploring the possibility of using magnetostrictive thin films in micro- and nano-electromechanical systems (MEMS and NEMS). Three material systems viz. Fe-Ga, Tb-Fe and Sm-Fe in thin film form have been chosen for our investigations. DC magnetron sputtering and e-beam evaporation techniques were used for deposition of these thin films on Si (100) substrates. Several aspects such as evolution of microstructure, film surface morphology, structure and change in film composition with different processing conditions were investigated in detail, as the existing literature could not provide a clear insight. Further, detailed magnetic characterizations of these films were carried out and established a process-structure-property correlation. The thesis is divided into seven chapters. The first chapter presents a brief introduction of magnetostrictive phenomena and the physics behind its origin. A brief history of evolution of magnetostrictive materials with superior properties is also brought out. Introduction to the material systems considered for the present study has also been presented. Discussions on various aspects like crystal structures, magnetic properties, and phase diagrams of these material systems are also included in this chapter. Magnetostriction in thin films and its importance in current technological applications are discussed in short. Further, a summary of existing literature on thin films of these materials has been narrated to highlight the perspective of the work done in subsequent chapters. In addition to this, a clear picture of the grey area for further investigations has been provided. Formulation of detailed scope of work for this study is also provided in this chapter. Details of different experimental techniques used in this study for deposition and characterization of these films are given in chapter 2. In the third chapter of the thesis a detailed study on the structural, microstructural and magnetic properties of Fe-Ga films deposited using dc magnetron sputtering technique are presented. The effect of sputtering parameters such as (i) Ar pressure, (ii) sputtering power, (iii) substrate temperature and (iv) deposition time/film thickness on the magnetic properties of the films are discussed in detail. All the films are found to be polycrystalline in nature with A2 type structure as evidenced from grazing incidence X-ray diffraction (GIXRD) and transmission electron microscope (TEM) studies. Surface morphology of the films are found to be affected with processing conditions considerably. Thermomagnetic behaviour of the films studied using a Superconducting Quantum Interference Device (SQUID) magnetometer under zero field cooled (ZFC) and field cooled (FC) conditions are also presented. The sputtering parameters are also found to influence the magnetic properties of the films through modifications in microstructure, surface morphology and film compositions. Irrespective of the sputtering parameters, room temperature (RT) deposited Fe-Ga films are found to exhibit large magnetic coercively and large saturation magnetic field as compared to the bulk alloy of similar compositions which are not desirable for micromagnetic device applications. A significant improvement in the magnetic properties of the films was obtained in the films deposited at higher substrate temperatures and is correlated with modifications in grain size and film surface roughness. These films are also found to exhibit better magnetostriction than the RT deposited films. Further, the magnetic properties of Fe-Ga films as a function of film thickness in the range 2 – 480 nm are also presented. The nature of variation of coercively with film thickness was correlated with grain size effect and explained successfully with the help of random anisotropy model. In the fourth chapter, studies on the microstructural and magnetic properties of Tb-Fe films were presented. It was reported earlier that TbxFe100-x films exhibit in-plane magnetic anisotropy for the films with x > 42 at.% of Tb and out-of-plane anisotropy for the composition 28 < x < 42. Presence of these anisotropies is technologically important for different applications. We have studied the magnetic properties of Tb-Fe films in these two composition range. TbxFe100-x films with 54  x  59 were prepared using dc magnetron sputtering technique under varying Ar pressure and sputtering power and the details about microstructural and magnetic properties are presented in this chapter. All the films are found to be amorphous in nature. While the composition of the film is found to remain constant with sputtering power, the Fe concentration in the film is found to be depleted with increase in Ar pressure. Magnetic properties are found to change from superparamagnetic to ferromagnetic behaviour with increase in sputtering power. Curie temperature of the films are found to be low (below RT) and is explained based on sperimagnetic ordering of magnetic sub-lattices. The perpendicular magnetic anisotropy (PMA) or out-of-plane anisotropy behaviour of Tb-Fe films were not studied in detail as a function of film thickness. We have successfully prepared TbxFe100-x films with 29  x  40 using e-beam evaporation technique using alloy target composition of TbFe in order to study the PMA behaviour as a function of film thickness. The thickness of the films was varied from 50 to 800 nm. All the films are found to be amorphous and columnar growth structure with fine channels of voids are observed from the TEM studies. Detailed magnetization and thermomagnetic measurements were carried out using SQUID magnetometer at different temperatures. The out-of-plane magnetic coercivity of the films was found to increase with film thickness and then decreases with further increase in thickness. Maximum coercivity of ~ 20 kOe has been obtained for the 400 nm thick film. Magnetic domain patterns were studied using magnetic force microscopy (MFM) technique and the observed magnetic properties are correlated with domain pattern and microstructures. Although there are several reports on device applications of Sm-Fe thin films which exhibit negative magnetostriction, a comprehensive study on the effect of different process parameters on the magnetic properties and its correlation with structure and microstructure is still elusive. Hence, Sm-Fe films were deposited on Si (100) substrate using dc magnetron sputtering technique under varying Ar pressure and sputtering power. Effect of these parameters on the microstructural and magnetic properties of the films was studied in detail and is presented in chapter 5. The curie temperature of the films was found to increase with increase in sputtering power and Ar pressure. This was attributed to increase in film thickness and size of islands (atomic clusters). Coercivity as low as 30 Oe has been achieved in the film deposited at 15 mTorr Ar pressure. The Curie temperature for the films deposited at higher Ar pressure (10 and 15 mTorr) are found to be above RT. Maximum saturation magnetostriction of ~ - 390 -strains has been achieved in the film deposited at 15 mTorr Ar pressure. Rapid thermal processing (RTP) experiments were also carried out to increase the magnetic ordering in the films deposited at low Ar pressure (5 mTorr) by imparting structural ordering. Large improvement in magnetization and Curie temperature of the film was observed after RTA. However, this could be attributed to the formation of nano-crystalline Fe phase as evidenced from the TEM studies and thermomagnetic measurements. An overall summary of the experimental results has been presented in chapter 6. The scope of work for further study in future has also been highlighted in chapter 7.

L’imagerie par résonance magnétique de diffusion (l’IRMd) est actuellement la seule technique non-invasive pour étudier l’architecture tridimensionnelle des fibres myocardiques du cœur humain à la fois ex vivo et in vivo. Cependant, il est difficile de savoir comment les caractéristiques de diffusion calculées à partir des images de diffusion reflètent les propriétés des microstructures du myocarde à cause de l’absence de la vérité-terrain sans parler de l’influence de divers facteurs tels que la résolution spatiale, le bruit et les artéfacts. L'objectif principal de cette thèse est donc de développer des simulateurs de l’IRM de diffusion basés sur des modèles réalistes afin de simuler, en intégrant différentes modalités d'imagerie, les images pondérées en diffusion des fibres myocardiques à la fois ex vivo et in vivo, et de proposer un outil générique permettant d’évaluer la qualité de l’imagerie et les algorithmes de traitement d’images. Pour atteindre cet objectif, le présent travail se focalise sur quatre parties principales. La première partie concerne la formulation de la théorie de simulation IRMd pour la génération d’images de diffusion et pour les applications sur les modèles simples de fibres cardiaques chez l’homme, et essaie de comprendre la relation sous-jacente entre les propriétés mesurées de la diffusion et les caractéristiques à la fois physiques et structurelles des fibres cardiaques. La seconde partie porte sur la simulation des images de résonance magnétique de diffusion à différentes échelles en s’appuyant sur des données du cœur humain issues de l'imagerie par lumière polarisée. En comparant les propriétés de diffusion à différentes échelles, la relation entre la variation de la microstructure et les propriétés de diffusion observée à l'échelle macroscopique est étudiée. La troisième partie consacre à l’analyse de l'influence des paramètres d'imagerie sur les propriétés de diffusion en utilisant une théorie de simulation améliorée. La dernière partie a pour objectif de modéliser la structure des fibres cardiaques in vivo et de simuler les images de diffusion correspondantes en combinant la structure des fibres cardiaques et le mouvement cardiaque connu a priori. Les simulateurs proposés nous fournissent un outil générique pour générer des images de diffusion simulées qui peuvent être utilisées pour évaluer les algorithmes de traitement d’images, pour optimiser le choix des paramètres d’IRM pour les fibres cardiaque aussi bien ex vivo que in vivo, et pour étudier la relation entre la structure de fibres microscopique et les propriétés de diffusion macroscopiques. / Diffusion magnetic resonance imaging (dMRI) appears currently as the unique imaging modality to investigate noninvasively both ex vivo and in vivo three-dimensional fiber architectures of the human heart. However, it is difficult to know how well the diffusion characteristics calculated from diffusion images reflect the microstructure properties of the myocardium since there is no ground-truth information available and add to that the influence of various factors such as spatial resolution, noise and artifacts, etc. The main objective of this thesis is then to develop realistic model-based dMRI simulators to simulate diffusion-weighted images for both ex vivo and in vivo cardiac fibers by integrating different imaging modalities, and propose a generic tool for the evaluation of imaging quality and image processing algorithms. To achieve this, the present work focuses on four parts. The first part concerns the formulation of basic dMRI simulation theory for diffusion image generation and subsequent applications on simple cardiac fiber models, and tries to elucidate the underlying relationship between the measured diffusion anisotropic properties and the cardiac fiber characteristics, including both physical and structural ones. The second part addresses the simulation of diffusion magnetic resonance images at multiple scales based on the polarized light imaging data of the human heart. Through both qualitative and quantitative comparison between diffusion properties at different simulation scales, the relationship between the microstructure variation and the diffusion properties observed at macroscopic scales is investigated. The third part deals with studying the influence of imaging parameters on diffusion image properties by means of the improved simulation theory. The last part puts the emphasis on the modeling of in vivo cardiac fiber structures and the simulation of the corresponding diffusion images by combining the cardiac fiber structure and the a priori known heart motion. The proposed simulators provide us a generic tool for generating the simulated diffusion images that can be used for evaluating image processing algorithms, optimizing the choice of MRI parameters in both ex vivo and in vivo cardiac fiber imaging, and investigating the relationship between microscopic fiber structure and macroscopic diffusion properties.