Made available in DSpace on 2014-10-09T12:55:21Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:05:58Z (GMT). No. of bitstreams: 0 / Dissertação (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

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Made available in DSpace on 2014-10-09T12:55:21Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:05:58Z (GMT). No. of bitstreams: 0 / A utilização de lasers de estado sólido bombeados por diodos laser tem atraído interesse crescente devido a sua alta eficiência, seu tamanho compacto e com a possibilidade da operação com altas potências-pico. O objetivo deste trabalho foi estudar configurações de cavidades ressonantes laser, que possibilitem a obtenção de pulsos chaveados Q e futura dobra de freqüência, para aplicações em LIDAR (Light Detection and Ranging), utilizando como meio ativo cristais de Nd:YLF crescidos pelo método de Czochralski no Centro de Lasers e Aplicações IPEN USP, com bombeio lateral por diodo laser, com uma, duas, quatro e nove reflexões internas totais do feixe laser na superfície do cristal. Das seis cavidades construídas, três cavidades foram desenvolvidas para operarem com baixo ganho, grande armazenamento de energia e com grande aproveitamento de inversão de população, bombeadas com diodo laser em 806 nm e outras três cavidades foram desenvolvidas para operarem com alta absorção de bombeio e alto ganho, bombeadas com diodo laser emitindo em 797 nm. Das seis cavidades desenvolvidas, as que apresentaram melhor eficiência de conversão óptica, foram as cavidades operando com alto ganho e alta absorção (cavidade quatro a seis), com 29,5% e 20,7% de eficiência de conversão óptica, propiciando a obtenção de pulsos chaveados de 20 ns com potência-pico de 160kW. / Dissertação (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Submitted by Luciana Ferreira (lucgeral@gmail.com) on 2015-10-16T12:51:01Z No. of bitstreams: 2 Tese - Zanine Vargas Fabris - 2015.pdf: 4567493 bytes, checksum: 24146ff0e9bb765933e4a57f07af4a33 (MD5) license_rdf: 23148 bytes, checksum: 9da0b6dfac957114c6a7714714b86306 (MD5) / Approved for entry into archive by Luciana Ferreira (lucgeral@gmail.com) on 2015-10-16T12:52:37Z (GMT) No. of bitstreams: 2 Tese - Zanine Vargas Fabris - 2015.pdf: 4567493 bytes, checksum: 24146ff0e9bb765933e4a57f07af4a33 (MD5) license_rdf: 23148 bytes, checksum: 9da0b6dfac957114c6a7714714b86306 (MD5) / Made available in DSpace on 2015-10-16T12:52:38Z (GMT). No. of bitstreams: 2 Tese - Zanine Vargas Fabris - 2015.pdf: 4567493 bytes, checksum: 24146ff0e9bb765933e4a57f07af4a33 (MD5) license_rdf: 23148 bytes, checksum: 9da0b6dfac957114c6a7714714b86306 (MD5) Previous issue date: 2015-01-22 / Bismuth tellurite, Bi2TeO5, here labeled BTeO has a lot of properties like improper ferroelectricity, photochromic, photorefractive, with two optical axes large optical window and another interesting optical and electrical properties, as recently we discovered, photovoltaic effect. BTeO single crystal growth and processing has two inherent difficulties, high vapor pressure of tellurium oxide close to bismuth tellurite melting point and BTeO cleavage plane parallel to (100) plane. So, BTeO factory good sample for material characterization require singular precautions and depends on researcher experience invariably. Present work is dedicated to detailed study of BTeO single crystals growth parameters in a modified Czochralski method with unpublished concept double crucible system. In our case, we used oxides mix on external crucible with volatile oxide bigger quantity related to internal crucible to create a supersaturated atmosphere used to control crystal growth liquid phase stoichiometry reducing tellurium oxide evaporation. We also highlighted important details about good quality samples production, like crystal cut and polish enclosed in acrylic resin to avoid cleavages during this processes. Finally, we characterized BTeO by optical spectroscopy (optical absorption, Raman scattering and luminescence) and electrical properties (conductivity, photoconductivity and impedance spectroscopy). We measured BTeO photorefractive properties with 633 nm wavelength for the first time and results suggested that material could be photovoltaic, hypothesis tested and confirmed in the present work. / O telurito de bismuto, Bi2TeO5, aqui nomeado BTeO é um material ferroelétrico impróprio, fotocrômico, fotorrefrativo, opticamente biaxial, com ampla janela óptica, entre outras várias características interessantes quanto às propriedades elétricas e ópticas, como por exemplo, apresentar propriedades fotovoltaicas, como descoberto neste trabalho. O crescimento e processamento de monocristais de BTeO possui duas dificuldades inerentes, a alta pressão de vapor do óxido de telúrio à temperatura de fusão do telurito de bismuto e a presença de um plano de clivagem acentuado em sua estrutura, paralelo ao plano (100). Assim sendo, a obtenção de boas amostras para caracterização do material exige uma série de cuidados específicos, além de depender invariavelmente da experiência do responsável pela manipulação do objeto de estudo. Este trabalho é dedicado ao estudo minucioso dos diversos parâmetros vinculados ao crescimento de monocristais de BTeO a partir de um método de Czochralski modificado com sistema de duplo cadinho cujo conceito é inédito. Em nosso caso, utilizamos uma mistura de óxidos no cadinho externo com quantidade maior do óxido volátil em relação ao cadinho interno a fim de formar uma atmosfera supersaturada do mesmo e, pela formação desta atmosfera, controlar a estequiometria da fase líquida de crescimento, reduzindo os efeitos de evaporação na mesma. Além disso, também destacamos uma série de detalhes importantes para a obtenção de amostras de boa qualidade, como a realização de cortes e polimento do cristal embutido em resina acrílica para minimizar a probabilidade de clivagens durante tais processos. Finalmente, uma série de caracterizações foi realizada tanto por espectroscopia óptica (absorção óptica, espalhamento Raman e luminescência) quanto das propriedades elétricas do material (condutividade, fotocondutividade e espectroscopia de impedância). Medidas das propriedades fotorrefrativas do material foram realizadas pela primeira vez com comprimento de onda de 633 nm e os resultados sugeriram que o material poderia ser fotovoltaico, hipótese testada e comprovada neste trabalho.

Thesis: Ph. D., Massachusetts Institute of Technology, Department of Materials Science and Engineering, 1977 / Vita. / Includes bibliographical references. / by Edward Paul Martin, Jr. / Ph. D. / Ph. D. Massachusetts Institute of Technology, Department of Materials Science and Engineering

This work presents the Czochralski growth dynamics as time-varying delay based model, applied to the growth of La3Ga5.5Ta0.5O14 (LGT) piezoelectric crystals. The growth of high-quality large-diameter oxides by Czochralski technique requires the theoretical understanding and optimization of all relevant process parameters, growth conditions, and melts chemistry. Presently, proportional-integral- derivative (PID) type controllers are widely accepted for constant-diameter crystal growth by Czochralski. Such control systems, however, do not account for aspects such as the transportation delay of the heat from crucible wall to the crystal solidification front, heat radiated from the crucible wall above the melt surface, and varying melt level. During crystal growth, these time delays play a dominant role, and pose a significant challenge to the control design. In this study, a time varying linear delay model was applied to the identification of nonlinearities of the growth dynamics. Initial results reveled the benefits of this model with actual growth results. These results were used to develop a long-range model predictive control system design. Two different control techniques using long range prediction are studied for the comparative study. Development and testing of the new control system on real time growth system are discussed in detail. The results are promising and suggest future work in this direction. Other discussion about the problems during the crystal growth, optimization of crystal growth parameters are also studied along with the control system design.

No description available.

L’optique non linéaire qui convertit la gamme de fréquences des sources lasers vers l’ultraviolet, le visible, l’infrarouge ou le térahertz par exemple, joue un rôle crucial pour la médicine, l’industrie, les applications militaires, la recherche etc. L’accord de phase par biréfringence (BPM) ou le quasi-accord de phase (QPM) à partir de processus non linéaires quadratiques, peuvent être utilisés pour la conversion de fréquence dans le domaine de transparence de cristaux non linéaires. Dans ce travail de thèse, un cristal uniaxe de La3Ga5.5Nb0.5O14 (LGN) a été élaboré en utilisant une méthode de Czochralski, puis il a été étudié pour le BPM. Nous avons aussi validé la théorie du QPM angulaire (AQPM), qui correspond à la généralisation du QPM à n’importe quel angle par rapport au vecteur du réseau. Pour cela, nous avons étudié un cristal biaxe de Rb: KTiOPO4 à domaines ferroélectriques alternés périodiquement (PPRKTP) usiné en forme de sphère. Tous ces résultats constituent une base fiable for les études avenir consacrées à la conception de dispositifs pour la conversion de fréquence. / Nonlinear optics converting the frequency range of laser sources to ultraviolet, visible, infrared or terahertz ranges for example, plays a crucial role in medicine, industry, military applications, research and so on. Birefringence phase-matching (BPM) or quasi-phase-matching (QPM) from quadratic nonlinear processes, can be used for frequency conversion in the transparency range of nonlinear crystals. In this PhD work, a La3Ga5.5Nb0.5O14 (LGN) uniaxial crystal was grown using a Czochralski method and then studied for BPM. We also validated the theory of angular-QPM (AQPM), corresponding to a generalization of QPM achieved at any angle with respect to the grating vector. For that purpose, we studied a periodically-poled large-aperture Rb:KTiOPO4 (PPRKTP) biaxial crystal cut a sphere. All the results provide a reliable basis for further studies devoted to the design of frequency conversion devices.

Les cellules photovoltaïques à base de silicium cristallin représentent plus de 90% du marché photovoltaïque mondial. Des architectures de cellules à haut rendement de conversion sont actuellement développées. Pour atteindre leurs performances maximales, ces architectures nécessitent néanmoins une amélioration des propriétés électriques des substrats de silicium cristallin. Les objectifs de cette thèse sont d’identifier les défauts limitant les propriétés électriques de ces substrats, de comprendre les mécanismes menant à leur formation et de proposer des moyens permettant leur neutralisation. Les matériaux étudiés sont des plaquettes de silicium Czochralski de type n, généralement utilisé pour les applications à haut rendement. Le four de tirage Czochralski a d’abord été modélisé afin de comprendre comment le passé thermique subi par le lingot de silicium lors de la cristallisation affecte la génération des défauts. Ces travaux ont été confirmés via des confrontations avec des données expérimentales, en utilisant une méthode originale développée dans le cadre de ce travail. Nous avons ensuite étudié l’influence du budget thermique lié aux procédés de fabrication des cellules sur la population de défauts. Nous avons ainsi pu montrer que la nature des défauts limitant les propriétés électriques du silicium était grandement modifiée selon le procédé de fabrication de cellules utilisé. Nous avons en outre mis en évidence une dégradation inattendue des propriétés électriques du silicium Czochralski de type n sous illumination, liée à la formation d’un défaut volumique inconnu. Les conditions de formation et de suppression de ce défaut ont été étudiées en profondeur. Enfin, les principaux défauts limitant les propriétés électriques du silicium ayant été identifiés et les mécanismes menant à leur formation compris, nous proposons dans un dernier chapitre des nouvelles techniques de caractérisation permettant de détecter les plaquettes défectueuses en début de ligne de production de cellules photovoltaïques, et ce à une cadence industrielle. / Photovoltaic solar cells based on crystalline silicon represent more than 90% of the worldwide photovoltaic market. High efficiency solar cell architectures are currently being developed. In order to allow their maximal performances to be reached, the electronic properties of their crystalline silicon substrate must however be enhanced. The goals of the present work are to identify the defects limiting the electronic properties of the substrate, to understand the mechanisms leading to their formation and to propose routes for their neutralization. The studied materials are n-type Czochralski silicon wafers, usually used as substrates for high efficiency photovoltaic applications. The Czochralski puller was first modeled in order to understand how the thermal history experienced by the silicon ingot during crystallization affects the defects generation. This study were validated through the comparison with experimental data using an original method developed in the frame of this work. We then studied the influence of the thermal budget associated to solar cell fabrication processes on the defects population. We thus showed that the nature of lifetime-limiting defects was completely changed depending on the solar cell fabrication process. Besides, we evidenced an unexpected degradation of the electronic properties of n-type Czochralski silicon under illumination, related to the formation of an unknown bulk defect. The formation and deactivation features of this defect were extensively studied. Finally, the main limiting defects being identified and the mechanisms resulting in their formation understood, we propose in a last chapter new characterization techniques for the detection of defective wafers at the beginning of production lines at an industrial throughput.

Nous avons caractérisé différents cristaux piézoélectriques de Langatate La3Ga5.5Ta0.5O14 (LGT), de différentes couleurs afin d’évaluer l’influence des défauts sur la qualité de dispositifs du domaine Temps-Fréquence (résonateurs acoustiques).Nous avons étudié la composition de ces cristaux dont les variations autour de la composition stoechiométrique sont surtout dues à l’évaporation du Ga2O au cours de la croissance compensée par un excès de Ga2O3 dans le mélange initial. Pour déterminer cette composition, la technique ICP-AES, précédée par une mise en solution par fusion alcaline, est la plus fiable.La présence d’impuretés chimiques, telles que les éléments métalliques ou les terres rares, liée à la pureté des oxydes de base, au frittage de la charge dans un creuset alumine… est étudiée. Nous expliquons ainsi la nature des centres colorés qui évolue selon l’atmosphère de tirage ou lors d’un recuit particulier.C’est ainsi que nous avons déterminé certaines propriétés de LGT permettant l’obtention de dispositifs comme les résonateurs à ondes de volume dont le produit Q.f est supérieur à celui des résonateurs à quartz. Pour cela, nous montrons notamment qu’il est nécessaire que :- la composition du cristal soit la plus proche possible de la stoechiométrie,- la résistivité électrique soit la plus grande possible,- l’étude spectroscopique ne révèle aucune absorption dans le domaine du visible.Dans ces conditions, le facteur de qualité Q d’une résonance à 10 MHz peut être de 1.44 million au point d’inversion de la courbe fréquence-température (1.35 pour le quartz) mais qu’il diminue notablement pour atteindre 0.35 million si nous pratiquons un recuit sous air à 1000°C pendant 48 h. / We have characterized Langatate piezoelectric crystals La3Ga5.5Ta0.5O14 (LGT), differently colored in order to evaluate the defects influence on the quality of Bulk Acoustic Waves resonators for the Time and Frequency domain.We have analyzed the composition of crystals whose variations around stoichiometric composition are mainly due to the evaporation of the Ga2O during growth compensated by adding an excess of Ga2O3 in the initial mixture. Among different techniques, the ICP-AES spectrometry, preceded by a dissolution by alkaline fusion seems to be the most accurate technique to determine the composition.The inevitable presence of chemical impurities, such as metallic elements, rare earth… linked to the purities of the raw materials, to the sintering of the load in an alumina crucible… is also studied. We try to explain in particular the nature of the color centers that evolve according to the growth atmosphere or during a particular annealing.So, we conclude by a list of necessary properties to obtain BAW resonators exhibiting a Q.f product higher than quartz. For this, we establish that it is necessary that:- the crystal composition is as close as possible to the stoichiometric composition,- the electrical resistivity is the highest possible,- the spectroscopic study does not reveal any absorption band in the visible domain.In these conditions, we were able to highlight that the quality factor of a 10 MHz resonance is of 1.44 million at the inversion temperature of the frequency-temperature curve (1.35 for the quartz crystal in the same conditions), but that this one decreases significantly to reach 0.35 million if we perform an annealing under air at 1000 °C during 48 hours.