Gesunder humaner Knochen unterliegt einem permanenten Umbau, um sich den mechanischen Anforderungen anzupassen, Mikrofrakturen zu reparieren und das Mineraliengleichgewicht zu erhalten. Dieser Umbauprozess wird durch Osteoblasten- und Osteoklastenaktivität realisiert, den knochenbildenden bzw. knochenresorbierenden Zellen. Gesteuert wird dieser Prozess durch Osteozyten, dessen Netzwerk mechanosensorische Fähigkeiten zugesprochen werden. Bisphosphonate (BP), hemmen die Osteoklastenaktivität und erhöhen somit die Knochenumsatzzeit. Im ersten Teil dieser Arbeit wurden morphologische Eigenschaften der Osteozyten-Lakunen (OL) in humanem Knochen mittels Synchrotron-µCT untersucht. Dabei wurden sowohl gesunde als auch mit BP behandelte Spender verglichen. Anschließend haben wir Synchrotron-Nano-CT in Kombination mit Phasenkontrast angewandt, um unsere Untersuchungen auf die Morphologie des lakuno-kanalikulären Netzwerkes (LKN) und die Gewebeeigenschaften in der Umgebung des LKN auszuweiten. Wir nahmen an, dass der sekundäre Mineralisierungsprozess mittels eines Diffusionsprozesses durch die Grenzfläche der extrazellulären Flüssigkeit im LKN stattfindet, was zu Gradienten der Massendichte in der Umgebung des LKN führen sollte. Unsere Untersuchungen haben gezeigt, dass sowohl in der Umgebung der OL als auch der Kanäle Massendichtegradienten existieren. Daraus schließen wir, dass der Mineralienaustausch zwischen der extrazellulären Flüssigkeit und der mineralisierten Matrix an der gesamten Oberfläche des LKN stattfindet. Wir schätzten, dass die Kapazität, unter Berücksichtigung des gesamten LKN, Mineralien auszutauschen etwa eine Größenordnung höher ist, gegenüber der Annahme, dass der Austausch lediglich an den Grenzflächen der OL stattfindet. Zukünftige Studien sollten nicht nur die peri-LKN Gewebeeigenschaften während der sekundären Mineralisierung untersuchen, sondern auch Schwankungen der Mineralienkonzentration bei hohen Kalziumanforderungen des Körpers berücksichtigen. / Under healthy conditions human bone undergoes permanent remodeling to adjust to mechanical demands, to repair micro-cracks and to maintain mineral homeostasis. This process of remodeling is performed by osteoblasts and osteoclasts: bone-forming and bone-resorbing cells. The activity of osteoclasts and osteoblasts is triggered by osteocytes, the most frequently occurring type of bone cell, via mechanosensation processes. Bisphosphonates (BP) prescribed during treatment for osteoporosis or bone metastasis inhibit osteoclast activity and thus decrease the bone turnover. In this work, the distribution and morphology of osteocyte lacunae of human cortical jaw bone was investigated in 3D, and a comparison between healthy and BP-treated donors was performed using synchrotron radiation (SR) µCT. In a second approach, we used SR nano-CT with phase contrast to investigate the morphology of the canalicular network and the bone tissue properties in the vicinity of the lacuna-canalicular network of human jaw bone, originating from both healthy subjects and patients treated with BPs. We hypothesized that secondary mineralization takes place via a diffusion process through the fluid-matrix interface at both the lacunar and the canalicular surfaces. This should result in mass density gradients with respect to the distance to the pore boundary. Such mass density gradients were indeed observed at both lacunar and canalicular interfaces. We concluded that mineral exchange between extracellular fluid and mineralized matrix occurs at all bone surfaces, including the canaliculi. Our data suggested that the capacity of the pore network to exchange mineral with the bone matrix would increase by one order of magnitude if the canalicular surface is taken into account. However, more studies should be performed, targeting not only the changes of tissue properties during secondary mineralization, but also during fluctuations of mineral concentration in periods of high mineral demand.

Materiais luminescentes contendo íons terras raras (TR3+) dopados nas matrizes de tungstatos [WO4]2- têm se mostrado excelentes candidatos como fósforos. Portanto, neste trabalho os materiais MWO4:TR3+ (M: Ca2+, Sr2+, Ba2+ e TR3+: Eu, Tb) foram preparados pelo método da coprecipitação com concentração de dopantes 0,1, 1,0, 5,0 e 10 % em mol. Este método comparado aos convencionais (cerâmico, combustão etc.), apresenta vantagens por ser um método simples de operação e rápido, baixo custo, preparado a temperatura ambiente, o processo de obtenção ambientalmente é correto e também produzem-se nanopartículas. Na caracterização destes fósforos foram utilizadas as técnicas: espectroscopia de absorção no infravermelho (IV), análise termogravimétrica (TG), difração de raios X - método do pó (DRX), microscopia eletrônica de varredura (MEV) e energia dispersiva de raios X (EDS). Os picos de difração de raios X foram indexados na estrutura tetragonal scheelita. Os fósforos dopados com Eu3+ e Tb3+ apresentaram cristalitos com dimensões nanométricas. Os estados de oxidação dos íons terras raras foram investigados com a espectroscopia de absorção de raios X com radiação Síncrotron (XANES), onde indicaram a presença apenas do estado trivalente para o európio nos materiais \"como preparados\" e calcinados. No entanto, foram detectados os estados trivalente e tetravalente do térbio dopado nas matrizes CaWO4 e BaWO4, calcinados à 500 ºC. As propriedades fotoluminescentes dos compostos foram investigadas com base nas transições intraconfiguracionais 4f6 (Eu3+) e 4f8 (Tb3+). Os espectros de excitação apresentaram bandas largas na região do UV, atribuídas às bandas de transferência de carga LMCT O→W e O→Eu3+. Os espectros de excitação dos fósforos MWO4:Tb3+ apresentaram as bandas de absorção largas atribuídas transferência de carga LMCT O2-(2p)→W6+(5d) sobrepostas às transições 4f8→4f75d e também picos finos oriundos das transições 4f8 do íon Tb3+. Ademais, os seus espectros de emissão exibiram bandas finas características das transições das 5D4→7FJ do íon térbio trivalente. Os valores altos do parâmetro de intensidade experimental (Ω2 ~18 x 10-20 cm2) indicam que o sítio de simetria ocupado pelo íon Eu3+ dopado nas matrizes de tungstatos não apresentam caráter centrossimétrico, uma vez que os altos valores de Ω2 são mais influenciados pelas pequenas mudanças angulares da geometria local do íon terra rara. Os valores de eficiência quântica de emissão η do nível 5D0 dos fósforos MWO4:Eu3+ estão em torno de 30 %, sugerindo que não há variação significativa quando se altera os íons metálicos alcalinos terrosos. As coordenadas CIE (Commission Internationale l\'Eclairage) sugerem emissões multicolores dos sistemas MWO4:Eu3+ X mol-% que podem ser ajustáveis, em função das intensidades de emissão das bandas largas LMCT e dos picos finos das transições 5D0→7F0-4 e da concentração de dopagem (X mol-%) do íon Eu3+. Estes materiais luminescentes exibem cores de emissão vermelha, verde assim como cores intermediárias. / Luminescent materials containing rare earth ions (RE3 +) doped in [WO4]2- tungstate matrices have demonstrated excellent candidates as phosphors. Therefore, in this work the materials MWO4:TR3+ (M: Ca2+, Sr2+, Ba2+ e TR3+: Eu, Tb) were prepared by the coprecipitation method with doping concentration 0.1, 1.0, 5.0 and 10% mol. This method compared to conventional ones (ceramic, combustion, etc.), has advantages because it is a simple operation and fast, low cost, prepared at room temperature, the process of obtaining is environmentally correct and also make up the nanoparticles. The characterization techniques of these phosphors were investigated by infrared absorption spectroscopy (IR), thermogravimetric analysis (TG), X-ray diffraction patterns - powder method (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray (EDS). The tungstate matrices doped with Eu3+ and Tb3+ showed crystallite sizes with nanometer dimensions. The rare earth oxidation states were investigated using absorption spectroscopy X-ray synchrotron radiation (XANES), which indicated the presence of only trivalent europium state materials \"as prepared\" and calcined. However, it was observed the trivalent and tetravalent state of terbium doped in CaWO4 and BaWO4 matrices, calcined at 500 º C. The photoluminescent properties of the compounds were investigated based on 4f6 (Eu3+) and 4f8 (Tb3+) intraconfigurational transitions. The excitation spectra showed broad bands in the UV region, assigned to the bands of charge transfer LMCT O→W e O→Eu3+. The excitation spectra of MWO4Tb3+ phosphors showed the broad absorption bands attributed charge transfer LMCT O2-(2p)→W6+(5d) overlapping with 4f8→4f75d transitions and narrow peaks arising from 4f8 transitions of Tb3+ ion. Moreover, their emission spectra exhibited narrow characteristic bands assigned to the 5D4→7FJ transitions of trivalent terbium ion. The high values of experimental intensity parameters (Ω2 ~ 18 x 10-20 cm2) indicate that the site symmetry occupied by the Eu3+ ion doped in the tungstates matrix not present centrosymmetric character, since high values of Ω2 are more affected by small angular changes of the local geometry around of rare earth ion. The values of emission quantum efficiencies (η) of the 5D0 level MWO4:Eu3+ phosphors were at around 30%, suggesting that there is no significant variation when changing the alkaline earth metal ions. The CIE coordinates (Commission Internationale l\'Eclairage) data suggest multicolored emissions for the MWO4:Eu3+ X mol-% systems can be tuneable, which depending on the emission intensities of the LMCT broad bands and 5D0→7F0-4 narrow peaks and concentration doping (X mol-%) of the Eu3+ ion. These materials exhibit luminescent emissions with red, green and intermediate colors.

Das Ziel dieser Dissertation ist das Schließen der radiometrischen Lücke zwischen der klassischen Radiometrie und der Radiometrie im Bereich weniger und einzelner Photonen. In dieser Arbeit wurden dazu zwei wesentliche Themen bearbeitet. Erstens, die Charakterisierung und Validierung eines neuen radiometrischen Detektorprimärnormals für den Wellenlängenbereich von 400 nm bis 800 nm basierend auf Silizium-Photodioden. Dieses neuartige Primärnormal kann sowohl in der Radiometrie im Bereich weniger Photonen als auch in der klassischen Radiometrie eingesetzt werden, der sogenannte “Predictable Quantum Efficient Detector” (PQED). Der PQED wurde im Rahmen dieser Arbeit charakterisiert und experimentell validiert. Für die Validierung war es nötig, die relativen Unsicherheiten der klassischen Radiometrie und insbesondere der Kryoradiometrie, deutlich zu verringern. Mit der Inbetriebnahme eines neuen Kryoradiometers wurde das Ziel, in den Unsicherheitsbereich von ca. 10E−5 vorzudringen, erreicht. Zweitens, es wurde eine Kalibriermethode für Einzelphotonendetektoren eingesetzt, rückgeführt auf das internationale Einheitensystem, die auf den einzigartigen Eigenschaften von Synchrotronstrahlung basiert. Diese Methode kann benutzt werden um sowohl Freistrahl- als auch fasergekoppelte Einzelphotonendetektoren bei praktisch jeder gewünschten Wellenlänge zu kalibrieren und erreicht im Moment die weltweit geringsten Messunsicherheiten. Mit dem neuen Kryoradiometer, dem PQED und dem auf Synchrotronstrahlung basierenden Kalibrierverfahren sind die erreichbaren Messunsicherheiten in der Radiometrie im Bereich von wenigen Photonen bis zu Strahlungsleistungen im Milliwattbereich deutlich reduziert worden. / This thesis addresses the bridging of the radiometric gap in the transition from classical radiometry to the few and single photon radiometry. In this context, two main tasks were emphasised. First: A new radiometric primary detector standard for wavelengths between 400 nm and 800 nm, suitable for classical and few photon radiometry, the so-called “Predictable Quantum Efficient Detector” (PQED) was characterised and validated. For the validation of the PQED, the relative uncertainties achievable in classical radiometry and, in particular, with cryogenic radiometers had to be reduced to a level of 10E−5 with the commissioning of a new cryogenic radiometer facility. Second: A calibration method for single photon detectors in the visible and NIR has been used which is based on the unique properties of synchrotron radiation. This calibration method allows radiometric single photon detector calibrations with the lowest uncertainties reported so far. This method can be used to calibrate free space and fibre-coupled single photon detectors traceable to the international system of units at practically every desired optical wavelength. With the new cryogenic radiometer, the PQED, and the calibration method based on synchrotron radiation, the uncertainties in radiometry have been significantly reduced in the range from milliwatts of radiant power down to attowatts corresponding to a few photons per second.

In the framework of quantum theory the characteristics of synchrotron radiation (SR) are considered. In order to simplify theoretical description the process of radiation is restricted to single-photon emission. For arbitrary quantum transitions the spectral-angular distributions of SR power are given in exact analytical form. Scalar particles (bosons) and particles with spin $\\hbar/2$ (electrons) are treated separately. Special attention is given to the particular transitions, namely, to the transitions to first excited and ground states. It is shown that the components of linear polarization of radiation from electron switch places due to the orientation of spin when the electron jumps to the ground state. This fact can be considered an analytical proof for the presence of $\\pi$-component of quantum radiation in the plane of motion. The radiation emitted from weakly excited particles is thoroughly analysed. To describe the evolution of the profiles of angular distributions various functions are introduced both for two- and three-level systems. For quantum transitions from the first excited state to the ground state the comparative analysis of radiation from bosons and electrons is performed, which helps to estimate the influence of spin and its direction on the characteristics of radiation. The radiation from unpolarized electron is considered separately. Tracking the behavior of effective angles allows to discover the inconsistency of well-known classical conclusion about the concentration of total (summed over spectrum) ultrarelativistic radiation in the plane of motion. It is shown that the effective angles of quantum radiation tend to finite values and do not vanish in ultrarelativistic region. A brief review of classical theory includes an introduction of the new concept, $n$-part of spectrum. In order to find an adequate classical analogue for the radiation from weakly excited particles, the idea to reduce classical spectrum was developed. It turns out that the characteristics of radiation calculated for reduced classical spectrum stay in good quantitative and qualitative agreement with their quantum analogues, at least for single-harmonic and two-harmonic quantum spectra, and classical theory of a reduced spectrum can be claimed representational in this sense. The evolution of maximum in radiation spectrum is considered in separate chapter. A well-known approximation obtained for critical frequency in the framework of classical theory is invalid when quantum corrections enter the picture. But there appears a possibility to find the conditions for the maximum to shift to the highest harmonic of finite quantum spectrum. It is shown that the shifts occur successively starting with primary harmonic in non-relativistic case, and this result remains valid independently of spin. For a scalar particle there exists a fixed set of numbers, which are the critical values of external field, such that the shift of radiation maximum in the spectrum of boson can only happen when the intensity of external field is greater than certain critical value related to corresponding harmonic. If this condition is not satisfied, the position of maximum remains unchanged. It turns out that the presence of spin perturbs this picture, so that the critical values of field intensity depend on the number of initial level. / Consideramos as características da radiação sincrotron (RS) no âmbito da teoria quântica. Para simplificar a descrição teórica do processo de radiação restringimos à consideração da emissão de único fóton. Para transições quânticas arbitrárias, as distribuições espectrais e angulares da potência da RS são dadas de forma analítica exata. Tratamos separadamente partículas escalares (bósons) e com spin ½ (elétrons). Atenção especial é dada às transições particulares, a saber, as transições ao primeiro estado excitado e estado fundamental. É mostrado que os componentes de polarização linear da radiação de elétron se trocam em relação à orientação de spin quando o elétron passa para o estado fundamental. Este fato pode ser considerado como uma comprovação analítica para a presença de -componente da radiação quântica no plano de movimento. Analisamos minuciosamente a radiação emitida pela partícula fracamente excitada. Várias funções são introduzidas para descrever a evolução dos perfis de distribuições angulares para sistemas de dois e três níveis. Para transições quânticas do primeiro estado excitado ao estado fundamental a análise comparativa da radiação de bósons e elétrons é realizada, e isso ajuda à estimar a influência de spin e sua direção sobre as características da RS. A radiação de elétrons não polarizados é considerada separadamente. Observando o comportamento dos ângulos efetivos, é fácil perceber a inconsistência da conclusão clássica bem conhecida sobre a concentração de radiação ultra-relativista total no plano do movimento. Mostramos que os ângulos efetivos da radiação quântica tendem aos valores finitos e não desaparecem na região ultrarelativista. Uma revisão breve da teoria clássica inclui a introdução do conceito novo, isto é a n-parte do espectro. A fim de encontrar um análogo clássico adequado para a radiação das partículas fracamente excitados, a ideia de reduzir o espectro clássico foi desenvolvida. Constatamos que as características da radiação calculadas para o espectro clássico reduzido permanecem em boa concordância, tanto quantitativa quanto qualitativa, com os seus análogos quânticos, pelo menos no que diz respeito aos espectros quânticos de uma ou duas harmônicas. Neste sentido, a teoria clássica do espectro reduzido pode ser chamada de representativa. A evolução do máximo no espectro da radiação é considerada em capítulo separado. A aproximação, comumente considerada na teoria classica para frequência crítica, é inválida quando as correções quânticas entram em cena. Mas existe uma possibilidade de encontrar as condições para o máximo transferir-se à harmônica maior do espectro quântico. É mostrado que as transferências ocorrem sucessivamente, comecando com a harmônica principal no caso não relativístico, e este resultado permanece válido, independentemente de spin. Para uma partícula escalar existe um conjunto fixo dos valores críticos do campo externo, de tal modo que a transferência do máximo da radiação entre duas harmônicas específicas pode acontecer somente quando a intensidade do campo externo é maior do que o valor crítico associado com essas harmônicas. Se essa condição não for satisfeita, a posição do máximo permanece inalterada. Verificamos que a presença de spin perturba esta condição, no caso do elétron os valores críticos da intensidade do campo dependem de número do nível inicial.

Dans le cadre de ses recherches menées sur la fusion par confinement inertiel, le Commissariat à l’énergie atomique et aux énergies alternatives met en œuvre un spectromètre X large bande étalonné en absolu et résolu en temps, appelé Diagnostic de Mesure du rayonnement X. Ce diagnostic, composé de 20 voies de mesure, permet de mesurer l’émissivité spectrale d’un plasma créé par laser entre 50 eV et 20 keV. Nous avons développé des voies de mesure complémentaires aux voies existantes, afin d’obtenir une redondance et une amélioration de la précision de la mesure. Le principe de ces nouvelles voies de mesure repose sur un concept original permettant d’obtenir des fonctions de transfert spectrales bornées et constantes. Deux voies ont été développées pour les gammes spectrales 2 – 4 keV et 4 – 6 keV, utilisant des miroirs multicouches apériodiques réalisés au Laboratoire Charles Fabry en Cr/Sc et Ni/W/SiC/W, respectivement. Ces miroirs ont ensuite été caractérisés sur synchrotrons puis intégrés dans le spectromètre. Les nouvelles voies ont été utilisées durant des campagnes d’expériences laser-Plasma sur l’installation laser OMEGA à Rochester (États-Unis). Elles ont permis de déterminer la puissance rayonnée directement avec une seule voie de mesure par bande spectrale et avec une meilleure précision qu’avec celles utilisées habituellement. Les résultats, en bon accord avec les voies de mesure classiques, permettent de valider l’utilisation des miroirs multicouches apériodiques pour la spectrométrie X large bande. / Within the framework of the research on inertial confinement fusion, the “Commissariat à l’énergie atomique et aux énergies alternatives” has studied and implemented an absolute calibrated time-Resolved broadband soft x-Ray spectrometer, called “Diagnostic de Mesure du rayonnement X”. This diagnostic, composed of 20 measurement channels, measures the emitted radiant power from a laser created plasma in the range from 50 eV to 20 keV. We have developed additional measurement channels to obtain redundancy and an improvement in measurement accuracy. The principle of these new channels is based on an original concept to obtain spectral bounded flat-Responses. Two channels have been developed for the 2 – 4 keV and 4 – 6 keV spectral ranges, using aperiodic multilayer mirrors made at the “Laboratoire Charles Fabry” with Cr/Sc and Ni/W/SiC/W layers respectively. These mirrors were characterized at synchrotron radiation facilities and integrated into the spectrometer. The two new channels were used during laser-Plasma experimental campaigns at the OMEGA laser facility in Rochester (USA). This allowed us to determine directly the radiant power with only one measurement within a certain spectral band, and with a better precision when compared with using standard channels. The results, in good agreement with the standard measurement channels, allowed us to validate the use of aperiodic multilayer mirrors for X-Ray broadband spectrometry.

Orientador: Pedro de Magalhães Padilha / Banca: Paulo Roberto Ramos / Banca: Lincoln Carlos de Oliveira / Resumo: No presente trabalho foi feito uma análise qualitativa de cálcio, ferro e zinco em spots de proteínas de amostras de tecido hepático de tilápia do Nilo (Oreochromis niloticus) por Fluorescência de Raios-X de Radiação Síncroton, após a separação das proteínas por Eletroforese Bidimensional em Gel de Poliacrilamida (2D-PAGE). Os espectros de fluorescência obtidos indicaram a presença de cálcio, ferro e zinco em doze, seis e oito spots protéicos das amostras de fígado, respectivamente. Os íons metálicos detectados nas amostras estão distribuídas principalmente em proteínas de massa molar menor que 45 kDa e com pI na faixa de 4,5 a 9,0. Além do cálcio, ferro e zinco foram detectados a presença de enxofre e fósforo, elementos não metálicos, que podem ser constituintes da estrutura das proteínas. As concentrações de cálcio, ferro e zinco ligados às proteínas foram determinadas por FAAS após a mineralização ácida dos spots protéicos, encontrando-se concentrações na faixa de 1,08 a 5,80 mg g-1, 2,02 a 8,03 mm g-1 e 1,60 a 8,55 mg g-1, respectivamente / Abstract: An investigation was made into calcium, iron and zinc in protein spots in samples of Nile tilapia (Oreochromis niloticus) liver tissue obtained after protein separation by two-dimensional polyacrylamide gel electrophoresis (2D-PAGE) and subsequent qualitative and quantitative evaluation by synchrotron radiation X-ray fluorescence (SRXRF) and graphite furnace atomic absorption spectrometry (FAAS). An analysis of the fluorescence spectra indicated the presence of calcium, iron and zinc in twelve, six and eight liver protein spots, respectively. The metal ions found were distributed mainly in proteins with a molar mass of less than 40.00 kDa and more than 12.00 kDa, with pI in the range of 4.70 to 9.40. The only exception was a spot presenting protein with a molar mass of 10.10 kDa. In addition to calcium, iron and zinc, sulfur and phosphorus - which are non-metals that may be part of the protein structure, were also detected. After microwave-assisted acid mineralization of the proteins spots, a FAAS estimation of the concentration of calcium, iron and zinc bound to these proteins indicated a range of 1.08 to 5.80 mg g-1, 2.02 to 8.03 mg g-1 e 1.60 to 8.55 mg g-1, respectively / Mestre

Mn5Ge3 suscite de l'intérêt pour des applications dans le domaine de l'électronique de spin car il a une température de Curie élevée (≈300 K) et il peut croître épitaxialement sur des substrats Ge(111) permettant ainsi d'injecter directement dans le semi-conducteur Ge un courant polarisé en spin.Nous avons étudié par photoémission résolue en angle et en spin (ARPES, SARPES), utilisant le rayonnement synchrotron, des films minces de Mn5Ge3(001), obtenus par croissance sur la surface reconstruites Ge(111)-c(2x8).Les résultats ARPES, obtenus dans les plans GALM et GAHK, sont en accord avec des simulations faites sur la base de calculs de structure de bandes faisant appel à la théorie de la fonctionnelle de la densité.Les mesures SARPES faites en plusieurs points du plan GALM sont aussi bien reproduites par ces simulations.D'une façon globale, nos résultats apportent une validation remarquable de la description des propriétés électroniques de Mn5Ge3 par le modèle de bandes. Seule l'intensité spectrale au niveau de Fermi n'est pas bien expliquée par la simulation. Cette différence est attribuée à la nature tridimensionnelle de l'échantillon et à des effets de corrélation. / Mn5Ge3 attracts strong interest for spintronics applications because it has a high Curie-temperature (≈300 K) and it can be grown epitaxially on Ge(111) substrates, permitting direct injection of a spin-polarized current into the Ge semiconductor.Mn5Ge3(001) thin films grown on Ge(111)-c(2x8) reconstructed surface were studied by angle- and spin- resolved photoemission (ARPES, SARPES) using synchrotron radiation. ARPES results, obtained in the GALM and GAHK planes, are in agreement with simulations done with the help of band structure calculations based on the density functional theory, taking into account lifetime broadening and broadening caused by correlation effects.SARPES measurements done at several k-points of the GALM plane are also well acounted for by these simulations.Overall our results provide a remarkable validation of the band structure model for a proper description of the electronic properties of Mn5Ge3. Only the spectral intensity at the Fermi level is not well explained by the simulation. This departure is attributed to the 3D nature of the sample and to correlation effects.

L'interaction d'un plasma avec une impulsion laser-intense suscite de plus en plus d'intérêt du fait des progrès en matière de technologie laser d'outils numériques. La réaction du rayonnement affecte la dynamique des électrons, celle du rayonnement synchrotron, ainsi que celle des ions via le champ de séparation de charge, pour des intensités laser supérieures à 10puissance22 W/CM2. les équations cinétiques régissant le transport de particules à ultra-haute intensité ont été obtenues. La réaction du rayonnement implique la contraction du volum de l'epace des phases des électrons A l'aide de simulations numériques nous avons démontré la forte rétro-action que les effets collectifs induisent sur le rayonnement synchrotron généré par les électons accélérés. L'importance des effets collectifs dépend fortement de la masse des ions et de l'épaisseur du plasma considéré. Ces effets pourraient être vérifiés expérimentalement avec des cibles cryogéniques d'hydrogène. / Résumé en anglais

Les artefacts en céramique ont une longue histoire et ont été récupérés dans presque toutes les régions du monde. La conservation n’est que rarement impactée par le milieu d’enfouissement. Donc, ils sont des matériaux idéaux pour comprendre l'histoire et la culture de homme. Les principales études archéologiques sur les céramiques anciennes concernent la provenance (datation, atelier, commerce), les matières premières (identification, origine), le processus de fabrication et l'utilisation (analyse des résidus de contenu). Mon travail porte plus précisément sur le processus de fabrication. Les principales étapes du processus de fabrication sont: la sélection des matières premières, la préparation, le façonnage, salle de bains, sur deux possibilités. Soit le vase est cuit avant l'étape de décoration, soit la décoration est appliquée sur le vase cru. Pour finir, l'ensemble est cuit. Mon objectif est d'obtenir des informations sur le procédé de fabrication en analysant la structure des céramiques anciennes, et en particulier, la structure des couches décoratives. La structure des céramiques anciennes est une structure complexe en couches avec des hétérogénéités à différentes échelles (mm à nm). Une céramique décorée est généralement composée d'une pâte et d'un revêtement, y compris de la décoration. Le revêtement peut contenir des natures différentes. L'épaisseur peut être variable de mm à nm. La couche décorative peut être une partie ou du tout la revêtement. La couche décorative peut être constitutive d'une phase vitrifiée amorphe et divers cristaux, tels que cristaux colorants, feldspath, quartz, etc., dont la taille varie de plusieurs microns à nanomètre. La description de cette structure nécessite l'analyse à haute résolution (nm) avec grande zone représentative (souvent plusieurs mm3). C’est difficile à réaliser. Dans mon travail, j'ai proposé une autre approche. L'approche est basée sur trois étapes. Premièrement, les analyses rapides (principalement microscopie optique) à faibles résolutions sont effectuées pour analyser et sélectionner la zone nécessitant une analyse à haute résolution. Ensuite, la zone sélectionnée est analysée à haute résolution par des techniques appropriées en tenant compte des informations recherchées. Troisièmement, on essaie de construire la structure de l'objet sur la base des données partielles, et d’en déduire le processus de fabrication. Je vais illustrer cette approche par trois exemples. La première concerne le pigment jaune de la terre sigillée marbrée romaine (chapitre III). Le second concerne le processus de cuisson des poteries attiques (chapitre III). Le troisième concerne les variations de couleur de la décoration bleue des porcelaines Qinghua (chapitre IV). / Ceramic artifacts have a long history and have been discovered worldwide. Their conservations are rarely impacted by the burial sites. Thus, they are ideal materials for understanding the human history and culture. The main archaeological studies concerning ancient ceramics contains provenance (dating, workshop, trade), raw materials (identification, origin), manufacturing process and utilization (analysis of content residues). For my work, I focused on the investigation of the manufacturing process. The main steps of fabrication process of ancient ceramics is composed of selection of raw materials, preparation (leaching, purification, body, glaze or slip, pigments), shaping (the plastic paste is shaped to the lathe or using the molds). Then, there are two possibilities: either the vase is fired before the decoration stage, or the decoration is applied to the raw vase. To finish, the whole is fired. My objective is to obtain information on the manufacturing process by analyzing the structure of ancient ceramics, and in particular the structure of decorative layers. The structure of ancient ceramics is complex with heterogeneities at different scales (mm to nm). A decorated ceramic generally is composed of a body and a coating, which including of the decoration. The coating could contain different natures. The thickness can be variable from mm to nm. The decorative layer can be a part of the coating or the whole coating. The decorative layer can be constituent of an amorphous vitrified phase and diverse crystals, such as colorant crystals, feldspar, quartz, etc., of which the size varies from several microns to nanometer. The description of such structure requires the analysis at high resolution (nm) with large representative zone (often, several mm3). It is difficult to realize. In my work, I proposed an alternative approach. The approach is based on three stages. Firstly, the rapid investigations (principally, optical microscopy) at low resolutions are effected to analyze and select the zone requiring analysis at high resolution. Secondly, the selected zone is analyzed at high resolution by appropriate techniques according to the information sought. Thirdly, I try to construct the structure of the object based on the partially data, and therefore deduce the manufacturing process. I will illustrate this approach through three examples. The first one concerns the yellow pigment of the Roman marbled terra sigillata (Chapter III). The second one is about the firing process of Attic potteries (Chapter III). The third one concerns the color variations of blue decoration of Qinghua porcelains (Chapter IV).

Les centres de rayonnement synchrotron et les Lasers à Électrons Libres (LEL) sont des sources de rayonnement utilisant des Électrons relativistes. Les onduleurs en constituent un élément important : ces instruments qui génèrent un champ magnétique périodique le long de la trajectoire des électrons, guident ces derniers de façon à les faire rayonner ou à rendre l’onde lumineuse émise plus intense. Ce travail porte sur l’étude d’onduleurs de différents types appliqués au Synchrotron SOLEIL, et sur leur possible application sur un LEL. Une première partie du travail porte sur la réalisation pour SOLEIL de deux onduleurs de type APPLE-II. Ce type d’onduleurs permet d’émettre du rayonnement de polarisation variable et les deux onduleurs construits présentent certaines spécificités par rapport à la plupart des onduleurs de ce type. Le premier (HU36) génère un champ magnétique de courte période tout en conservant une valeur crête relativement importante, ce qui lui permet de rayonner sur une large gamme spectrale. Ces caractéristiques entrainent cependant une hystérésis expliquée par la déformation des supports. Les moyens mis en œuvre pour atteindre ces caractéristiques magnétiques et pour réduire l’hystérésis sont présentés. Le deuxième onduleur APPLE-II construit (HU64) présente la double particularité d’être quasipériodique (ou apériodique) afin de réduire la pollution rayonnée aux harmoniques de la longueur d’onde fondamentale, et de permettre l’accès à de la polarisation linéaire inclinée sur une plage de 180° grâce à son châssis étendu. L’optimisation magnétique de sa structure apériodique est détaillée et les difficultés découlant des configurations étendues sont expliquées. Dans un deuxième temps, la réalisation pour SOLEIL d’un troisième onduleur d’un tout autre type est présentée. Il s’agit d’un onduleur hybride sous-vide appelé U20. Des pôles intercalés entre les aimants guident les lignes de champ de façon à augmenter la densité de flux magnétique sur axe, et l’assemblage magnétique ainsi obtenu est installé dans la chambre à vide, ce qui permet de réduire l’entrefer minimum à 5.5 mm et donc, d’accroitre considérablement la valeur crête du champ magnétique généré. Compte-tenu des connaissances acquises pendant la construction des deux onduleurs APPLE-II et de l’onduleur sous-vide, l’étude d’un onduleur combinant ces deux aspects est ensuite proposée. Cet onduleur de tyoe « APPLE-II sous-vide » serait extrêmement polyvalent puisqu’il permettrait l’émission de rayonnement de différentes polarisations sur une large gamme spectrale. L’étude de principe menée ici met en évidence les nombreuses difficultés à surmonter et propose différentes solutions. La dernière partie du travail porte sur l’étude de l’interaction qui s’opère dans le cas d’un LEL au sein de l’onduleur entre les électrons et l’onde lumineuse, conduisant à l’amplification de cette dernière. Des expériences menées en configuration SASE et en mode injecté sur le SPARC (Italie, Frascati) sont rapportées, puis des calculs sont réalisés dans le cadre du projet LUNEX5, pour évaluer l’efficacité de cette interaction dans un onduleur apériodique, et dans l’onduleur APPLE-II sous-vide envisagé précédemment. / Storage rings and Free Electron Lasers (FEL) are relativistic electron based radiation sources, in which an important element is a device called undulator. This apparatus generates a periodic magnetic field along the electron trajectory, guiding the particles in such a way that they lose energy to the benefit of the radiation. This work deals with the study of several undulators of different types, and also their application on FEL sources. A first part of the work is dedicated to the construction of two APPLE-II type undulators for SOLEIL. Undulators of this type are able to emit radiation of variable polarization states, and the two studied devices present some special characteristics with respect to most of APPLE-II undulators. The first one (HU36) generates a short period high value magnetic field, leading to radiation emitted on a large spectral range. These parameters brought about a hysteresis explained by the deformation of the magnet supports, which was reduced. The second APPLE-II undulator (HU64) is characterized by two particularities: its field is quasi-periodic (or aperiodic) in order to reduce the pollution emitted at harmonics of the fundamental wavelength, and it is based on a special frame enabling radiation of tilted linear polarization on the full range of 180°. The optimization of the aperiodic structure is detailed and the difficulties brought about by the extended frame are explained. The third undulator built for SOLEIL is a hybrid in-vacuum one. Ferromagnetic poles guide the magnetic flux lines in order to increase the on-axis flux density, and the magnetic part of the undulator is included inside the vacuum chamber, which leads to a higher value of the generated field. Starting from the knowledge of both APPLE-II and in-vacuum undulators, the study of a device combining both characteristics is then proposed. Such an in-vacuum APPLE-II undulator would consist in a very performant and flexible apparatus because it could emit radiation of variable polarization on a large spectral range. The study points out the technical difficulties and suggests some solutions. The last part of the work deals with the study of the interaction realized in a FEL between electrons and radiation, resulting in the amplification of the light. Experiments performed in both SASE and injected configurations at the FEL SPARC (Italy, Frascati) are reported. Then calculations are made in the case of the FEL French project LUNEX5 to estimate the interaction efficiency when realized inside a quasi-periodic undulator and also through the previously studied in-vacuum APPLE-II one.