Cette thèse traite de l'étude de films ultra minces de Fe par réflectivité magnétique résonante de rayons X mous (SXRMR). La technique de SXRMR associe les effets magnéto-optiques aux propriétés de diffusions des rayons X, ce qui permet sonder les propriétés magnétiques avec une résolution spatiale en profondeur. Un profil magnétique résolu en profondeur est donc dérivé des expériences, permettant d'étudier les effets des interfaces sur l'homogénéité des propriétés magnétiques. Dans un premier temps nous présentons l'étude d'un film mince de Fe sur un substrat vicinal d'Ag(116) recouvert par quinze monocouches d'Au. Cette étude révèle que l'aimantation est augmentée de 20 à 30$\%$ dans les deux à trois monocouches proches des interfaces d'Au et d'Ag, quelque soit la température et l'épaisseur de la couche de Fe. Nous avons également mis en évidence une inhomogénéité de la composante hors du plan à basse température pour des échantillons ayant un axe de facile perpendiculaire aux marches : la composante de l'aimantation hors du plan est de plus en plus grande lorsqu'on se rapproche du substrat vicinal d'Ag. Dans un deuxième temps, nous présentons l'étude d'un film mince de six monocouches de Fe sur du Cu(100) et recouvert par une couche d'Au. En utilisant une approche originale de contrainte sur les paramètres magnétiques, nous avons pû mettre en évidence que la dépendance de l'aimantation en fonction de la température n'était pas la même selon la position de la monocouches dans le film mince de Fe, comme prédit théoriquement par Sandratski. / This thesis deals about depth resolved magnetic profile of ultrathin Fe layers studied by soft X-ray Resonant Magnetic Reflectivity (SXRMR). This SXRMR technique combines magneto-optic effects to X-ray scattering allowing to be sensitive to magnetic properties as well as to be depth resolved. For each experiments, the depth resolved magnetic profile found allows to study interfaces effect on the homogeneity of magnetic properties. First, we present the study of a thin film of Fe grown on a vicinal substrate of Ag(116) and covered by fifteen monolayers of Au. This study reveal that the magnetization is enhanced of 20 to 30$\%$ int the two to three monolayers near both interfaces, whatever the temperature and the Fe thickness are. We have also discover an inhomogeneity of the magnetic out of plane component at low temperature for sample where the magnetization easy axis is perpendicular to the steps : the magnetic out of plane component is more and more important when we go strait to the vicinal substrate of Ag. Second, we show the study of a thin film of six monolayers of Fe grown on a Cu(100) substrate and covered by a Au layer. Using a new way of strain on magnetic parameter we have highlighted that the temperature dependance of the magnetization is not the same depending ont the position of the monolayer inside the Fe thin film as predicted by the theory of Sandratski.

La caractérisation des contraintes internes présentes dans les matériaux de structure ou fonctionnels est primordiale pour une optimisation de leurs propriétés et de leur tenue en service. Ce travail de thèse est une contribution au développement d'une technique de microscopie par diffraction des rayons X, appelée "Differential Aperture X-ray Microscopy", (DAXM, permettant la caractérisation 3D et non-destructive de la microstructure de matériaux cristallins et des contraintes internes présentes dans le matériau. Cette technique est basée sur l'utilisation du rayonnement synchrotron; nous avons utilisé la ligne CRG BM32 du synchrotron européen ESRF. Le faisceau de rayons incident est polychromatique (5-25keV) et fortement focalisé (section sub-micrométrique). En raison la pénétration du faisceau dans le matériau, qui est typiquement de quelques dizaines de microns, l'image de diffraction collectée est une superposition des diagrammes de Laue de tous les cristaux situés sur le trajet du faisceau incident. La DAXM utilise, en supplément de la microdiffraction Laue "classique", un masque mobile (ici un fin fil de tungstène) qui absorbe une partie des faisceaux diffractés. L'analyse de l'évolution des niveaux de gris des pixels de l'image en fonction de la position du masque permet non seulement de reconstruire la microstructure du matériau en profondeur mais aussi d'accéder à la distribution 3D des déformations élastiques (et des contraintes associées). L'un des avantages de la DAXM est sa résolution spatiale, de l'ordre du micromètre, qui permet d'envisager l'analyse des concentrations de contraintes dans les matériaux polycristallins, dans le cadre des approches micromécaniques expérimentales.Le travail mené dans cette thèse avait pour but d'améliorer le dispositif expérimental existant,de mettre en place la formulation théorique du problème, et de développer les outils numériques permettant le traitement des données.Du point de vue expérimental, nous avons notamment développé une machine d'essai mécanique in-situ (flexion 4-points) adaptée à la ligne BM32, et nous proposons un masque multi-fil qui devrait permettre de réduire significativement la durée de l'acquisition des données.Nous avons établi les équations de triangulation reliant la position des pixels du détecteur,la position du fil, et la profondeur de la source le long du faisceau incident. On montre ainsi que la reconstruction 3D nécessite une procédure de dérivation des niveaux de gris; nous nous sommes limités dans ce travail à une dérivation par différence finie d'ordre 1, qui reste sensible au bruit d'image. Ces équations font apparaître la nécessité de déterminer la géométrie du montage avec grande précision. On propose pour cela l'utilisation de la fluorescence de l'échantillon. On adjoint aux équations géométriques une description mathématique simplifiée de l'atténuation du faisceau par l'échantillon, prenant en compte un coefficient d'absorption unique. Le modèle de calibration est testé sur plusieurs matériaux, avec de très bons résultats.La capacité de la DAXM à reconstruire une microstructure est testée sur des échantillons modèles pour lesquels la géométrie 3D de la microstructure est parfaitement connue : empilement de fin fils de GaN sur un substrat, et plan de macle dans un polycristal d'acier inoxydable (316L). On montre que la résolution de la DAXM est variable d'un pixel à l'autre du détecteur; la microstructure peut cependant être reconstruite avec une précision de l'ordre du micromètre.La DAXM est ensuite testée sur un échantillon d'UO2 implanté d'ions Kr, créant une couche de surface d'épaisseur micrométrique fortement déformée (collaboration CEA-Cadarache). On observe que la méthode de reconstruction proposée produit d'importants artefacts, qui sont dus à la transmission variable des faisceaux diffractés dans le masque. Nous mettons en place la formulation permettant de prendre en compte cet effet. / The characterization of the internal stresses present in structural or functional materials is essential for an optimization of their properties and their durability in service. This thesis work is a contribution to the development of the so-called '' Differential Aperture X-ray Microscopy'' (DAXM) technique, allowing 3D and non-destructive characterization of the microstructure of crystalline materials and internal stresses. This technique makes use of synchrotron radiation; we used the beamline CRG BM32 of the European synchrotron ESRF. The polychromatic and highly focused incident beam penetrates the sample, and the collected diffraction image is a superimposition of the Laue diagrams of all the crystals located along the path of the incident beam. The DAXM uses, in addition to the "conventional" Laue microdiffraction technique, a moving mask that absorbs part of the diffracted beams. The analysis of the evolution of the gray levels of the image pixels as a function of the position of the mask makes it possible not only to reconstruct the microstructure of the material at depth but also to access the 3D distribution of the elastic deformations (and associated stress). One of the advantages of the DAXM is its spatial resolution, of the order of a micrometer, which makes it possible to envisage the analysis of stress concentrations in polycrystalline materials, within the framework of experimental micromechanical approaches.The work carried out in this thesis was aimed at improving the existing experimental system,to put in place the theoretical formulation of the problem, and to develop the numerical tools allowing the processing of the data.From an experimental point of view, we have developed an in-situ mechanical test device (4-point bending) adapted to BM32, and we propose a multi-wire mask to significantly reduce the data acquisition time.We have established the geometric equations of the problem. It is thus shown that the 3D reconstruction requires a gray scale derivation procedure. This work is limited to the use of a finite difference derivation method of order 1, which remains sensitive to image noise. These equations show the need to determine the geometry of the setup with great precision. For this purpose, the use of the fluorescence of the sample is proposed, coupled with a simplified description of the beam attenuation by the sample taking into account only a single absorption coefficient. The calibration model is tested on several materials, with very good results.The capacity of the DAXM to reconstruct a microstructure is tested on model samples for which the 3D geometry of the microstructure is perfectly known: a stack of GaN wires on a substrate, and a twin plane in a stainless steel polycrystal. It is shown that the resolution of the DAXM is variable from one pixel to the other of the detector; the microstructure can however be reconstructed with an accuracy of the order of one micrometer.The DAXM is then tested on a sample of UO2 implanted by Kr ions, creating a highly deformed surface layer with micrometric thickness (collaboration with CEA-Cadarache). It is found that the proposed reconstruction method is affected by the variable transmission of the diffracted beams in the mask. We propose a formulation that takes this effect into account.

Abstract Experimental synchrotron radiation induced electron- and ion spectroscopies together with electron-ion and ion-ion coincidence techniques as well as electron energy loss spectroscopy have been used to study the electronic properties of several vapor phase samples. In this thesis studies of the electronic structure and fragmentation of Sb4 clusters, photo- and Auger electron spectroscopy of atomic Si and Pb as well as ultra high resolution VUV absorption of vapor phase KF molecules have been performed. The instrumentation and techniques used in the studies, especially the electron energy loss apparatus and the newly built ultra high resolution FINEST beamline branch, are presented.

La spintronique multifonctionnelle est une nouvelle direction d'avancement pour aller au-delà des limites de l'électronique moderne. Il vise à développer des dispositifs qui seraient sensibles à plus d’un stimulus et/ou ont un signal multi-réponse. Dans cette thèse, nous explorons cette voie multifonctionnelle émergente en combinant l’électronique de spin et les systèmes organiques pour ouvrir la voie vers des dispositifs polyvalents. Nous étudions la formation d'une spinterface dans le système Co/manganèse-phthalocyanine. Nous proposons l'introduction de multifonctionnalités intrinsèques en utilisant des matériaux à transition de spin. Nous développons une nouvelle approche de fonctionnalisation pour ajuster leurs propriétés vers des applications. Nous proposons un contrôle fonctionnel externe sur une spinterface en utilisant un substrat multiferroïque. Dans le cadre de cette thèse, un insert polyvalent à température variable a été développé à la ligne de lumière DEIMOS du synchrotron SOLEIL. Nous démontrons comment il peut être utilisé pour sonder des atomes actifs dans n'importe quel dispositif électronique. / Multifunctional spintronics is a new direction of advancement beyond the limits of modern electronics. By combining elementary charge of an electron and its spin, it aims to develop devices which would be sensitive to more than one stimuli and/or have multiresponse signal. In this thesis, we explore the multifunctional potential emerging while combining spin electronic and organic systems to pave the way towards multipurpose devices. First, we study formation of a ferromagnetic/organic spinterface in Co/manganese-phthalocyanine system. We propose introduction of intrinsic multifunctionality by using spin crossover materials. We develop a novel functionalization approach for tuning their properties towards device applications. We propose an external functional control over any hybrid spinterface by using multiferroic substrate. In the framework of this thesis, a Versatile Variable Temperature Insert was developed at the DEIMOS beamline of the SOLEIL synchrotron. We demonstrate how it can be used to probe active atoms in any microelectronic device.

Orientadores: José Antenor Pomilio, Giancarlo Tosin / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Elétrica e de Computação / Made available in DSpace on 2018-08-27T01:27:04Z (GMT). No. of bitstreams: 1 Baader_JohannEduardo_M.pdf: 5709999 bytes, checksum: b70a7b9c4f9062486fb33d399ad88653 (MD5) Previous issue date: 2015 / Resumo: Desde 1997 o Brasil tem acesso à tecnologia de radiação síncrotron com a inauguração do Laboratório Nacional de Luz Síncrotron (LNLS), localizado na cidade de Campinas, SP. Batizada de UVX, a fonte de luz síncrotron brasileira foi um marco no desenvolvimento científico e tecnológico do país, permitindo pesquisas nas mais diversas áreas do conhecimento, como nanotecnologia, biotecnologia, fármacos, agricultura, energias alternativas, dentre outros. Em 2009 o LNLS iniciou o projeto e a construção de uma nova fonte de luz síncrotron brasileira. Nomeada Sirius, está sendo desenvolvida para ser uma das mais avançadas do mundo na geração de luz síncroton. O alto desempenho deste tipo de máquina depende fortemente da qualidade dos campos magnéticos criados pelos inúmeros magnetos que compõem a rede magnética, o que exigem uma técnica de caracterização rápida, acurada e precisa. O Grupo de Magnetos, responsável pelo projeto, construção e caracterização dos magnetos tanto da fonte UVX como da nova fonte, utiliza um sistema de medição conhecido como Técnica de Bobina Girante. Devido às especificações do projeto Sirius, foi necessário o aprimoramento da bancada de caracterização, objetivo este consolidado principalmente através da análise minuciosa das principais fontes de erro do sistema. Um modelo numérico desenvolvido para estudar algumas classes de erros da técnica deu suporte para diversas correções na bancada, o que permitiu alcançar níveis de precisão comparáveis com os sistemas de caracterização de outros laboratórios. Paralelamente, foi construída a bancada de um sistema protótipo de medição magnético, nomeado Técnica de Minibobina Girante, apresentando uma série de vantagens em relação às limitações da bancada oficial. Algumas das melhorias realizadas nesta bancada durante o seu desenvolvimento foram baseadas nos resultados advindos do modelo numérico das fontes de erros / Abstract: Since 1997 Brazil has access to synchrotron radiation technology with the inauguration of the Brazilian Synchrotron Light Source (LNLS), located in Campinas, Brazil. The source of Brazilian synchrotron light known as UVX was a milestone in scientific and technological development of the country, enabling research in several areas of knowledge such as nanotechnology, biotechnology, pharmaceuticals, agriculture, alternative energy etc. In 2009 LNLS initiated the project and the construction of a new source of Brazilian synchrotron light, named Sirius. It is being developed to be one of the most advanced in the world in the generation of synchrotron light. The high performance of this type of machine depends strongly on the quality of the magnetic fields created by magnets that compose the lattice, which demand a fast, accurate and precise characterization technique. The Magnets Group, responsible for the design, construction and characterization of both the magnetic UVX sources as new sources, uses a measuring system known as Rotating Coil System. Due to the specifications of the Sirius design, an improved characterization bench was necessary. This goal was achieved mainly through a careful analysis of the main sources of error in the system. A numerical model to study some classes of errors in the technique provided support for various fixes in the bench, which allowed us to achieve comparable levels of accuracy along with the characteristics of the systems from other laboratories. At the same time, another bench was built as a prototype system for magnetic measurements known as Small Rotating Coil System, presenting a series of advantages over the constraints of the main bench. Some of the improvements made on this bench during its development were based on the results derived from the numerical model of error sources / Mestrado / Energia Eletrica / Mestre em Engenharia Elétrica

Bi-annual report on the activities at the ROssendorf BeamLine (ROBL) at the ESRF in Grenoble. The report contains selected contributions on actual research topics, a list of all scheduled experiments, and short experimental reports.

The paper describes the Rossendorf Beamline (ROBL) built by the Forschungszentrum Rossendorf at the ESRF. ROBL comprises two different and independently operating experimental stations: a radiochemistry laboratory for X-ray absorption spectroscopy of non-sealed radioactive samples and a general purpose materials research station for X-ray diffraction and reflectometry mainly of thin films and interfaces modified by ion beam techniques. The radiochemistry set-up is worldwide an unique installation at a modern synchrotron radiation source.

The presented work reports on the solidification studies in two alloy systems: the niobium bearing γ-TiAl, relevant for the automotive and aero-engine applications, and aluminium rich Raney-Ni, precursor alloys for catalyses used in the chemical industry. The time-resolved observations of equilibrium liquid-solid phase transformations, as well as non-equilibrium solidification from the undercooled melt, are performed by combination of in situ structural studies using high-energy X-rays at a synchrotron source and the electromagnetic levitation technique. Containerless processing assured the contamination-free environment leading to high undercooling levels even at moderate cooling rates. For the critical part of the Ti-Al-Nb phase diagram an equilibrium involving the liquid phase is deduced from the phase transformations gathered on heating periods of levitation experiment. New experimental data on the partial liquidus and solidus surfaces are delivered as well as the information on the nature of the reactions along the univariant lines. These data provide a valuable contribution to the reassessment of the thermodynamic description. The primary phase selection as function of undercooling is studied in ternary Ti-Al-Nb alloys. The metastable formation of the cubic β phase within the primary solidification region of the hexagonal α phase is observed with increasing melt undercooling. Furthermore, the microstructure evolution of the β solidifying Ti-46Al-8Nb alloy discloses the transition to the thermal growth mode for ∆T>200−250 K, accompanied by complete solute trapping. Supplemented with the data on the solidification velocity determined as function of melt undercooling, this results are discussed within the local non-equilibrium model of the free dendrite growth. The in situ observations of the non-equilibrium solidification of the binary Al-Ni system give insight into multiple phase transformation sequence. The achieved undercooling levels up to 320 K for the aluminium alloys containing 18–31.5 at.% Ni did not alter the primary phase selection. However, during further cooling of L+Al3Ni2 semisolid samples the peritectic formation of a metastable decagonal quasicrystalline phase is observed providing a critical undercooling below the peritectic temperature of Al3Ni phase is reached. On further cooling the metastable phase subsequently transforms into the equilibrium Al3Ni. A similar solidification pathways are expected for the Raney-Ni alloys produced by gas atomisation, where the associated high cooling rates allowed to retain the metastable phase at room temperature.

京都大学 / 0048 / 新制・課程博士 / 博士(工学) / 甲第19709号 / 工博第4164号 / 新制||工||1642(附属図書館) / 32745 / 京都大学大学院工学研究科材料工学専攻 / (主査)教授 辻 伸泰, 教授 乾 晴行, 教授 安田 秀幸 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DFAM

京都大学 / 0048 / 新制・課程博士 / 博士(人間・環境学) / 甲第21432号 / 人博第870号 / 2018||人博||870(吉田南総合図書館) / 京都大学大学院人間・環境学研究科相関環境学専攻 / (主査)教授 内本 喜晴, 教授 田部 勢津久, 教授 吉田 鉄平 / 学位規則第4条第1項該当 / Doctor of Human and Environmental Studies / Kyoto University / DFAM