122 f. / Submitted by Ana Hilda Fonseca (anahilda@ufba.br) on 2013-03-22T17:20:17Z No. of bitstreams: 1 Tese corrigida final.pdf: 1322795 bytes, checksum: a277616fb5634d49040e3b569eae8dd2 (MD5) / Approved for entry into archive by Ana Hilda Fonseca(anahilda@ufba.br) on 2013-06-05T17:38:45Z (GMT) No. of bitstreams: 1 Tese corrigida final.pdf: 1322795 bytes, checksum: a277616fb5634d49040e3b569eae8dd2 (MD5) / Made available in DSpace on 2013-06-05T17:38:45Z (GMT). No. of bitstreams: 1 Tese corrigida final.pdf: 1322795 bytes, checksum: a277616fb5634d49040e3b569eae8dd2 (MD5) Previous issue date: 2012 / CAPES / No presente trabalho, desenvolveu-se um método alternativo para determinação de cobre, ferro, níquel e zinco, usando a espectrometria de fluorescência de raios-X com energia dispersiva (EDXRF), em amostras de etanol combustível e cachaça, após procedimento de pré-concentração. O procedimento consistiu na retenção dos analitos em papel cromatográfico de troca iônica, suporte sólido que se mostrou apropriado para medições diretas por EDXRF. Algumas variáveis foram otimizadas e os melhores resultados obtidos foram: vazão de amostragem de 2,0 mL min-1, pH entre 5,0 e 7,5 e volume de amostragem de 10 mL. No procedimento, com auxílio de uma bomba peristáltica, alíquotas da solução padrão ou amostra foram passadas em papel cromatográfico de troca catiônica, que foi cortado em círculos com 13 mm de diâmetro e adaptados em suporte para filtração. Após a secagem dos papéis cromatográficos, foram realizadas medições diretas no papel empregando espectrômetro de fluorescência de raios-x de energia dispersiva. As curvas de calibração apresentaram resposta linear no intervalo de 0,050 a 1,50 μg mL-1 dos analitos. As repetibilidades, expressas em termos de RSD das soluções-padrão contendo 0,25 μg mL-1 de Cu, Fe, Ni e Zn, calculadas a partir de 15 determinações consecutivas, foram de 2,5, 2,8, 3,0 e 2,7%; e 3,1, 2,9, 2,8 e 2,7%, para matrizes com 96% e 50% de etanol, respectivamente. Obteve-se limites de quantificação (LQ) iguais a 43, 50, 50 e 40; e 47, 54, 59 e 45 μg mL-1, para matrizes com 96% e 50% de etanol, respectivamente. O procedimento foi verificado através de testes de recuperação, adicionando-se 100 μg L-1 de cada metal nas diferentes amostras, com resultados entre 92 e 99%. Os resultados obtidos pelo método proposto foram comparados com os resultados obtidos por um método comparativo usando ICP OES, após digestão das amostras, não apresentando diferenças significativas, com um nível de confiança de 95%. O método proposto é simples e não exigiu que as amostras fossem submetidas a qualquer pré-tratamento drástico ou demorado. / Salvador

The thesis deals with composting and ways of handling biodegradable waste and biodegradable municipal waste. It explains the terms related to composting and processing of BW and BMW and clarifies the difference between humus and primary organic matter and its composition. Furthermore, the thesis covers qualitative and quantitative features of compost, raw material composition of the dump, and factors influencing the process of decomposition itself. The practical part of the thesis describes the quality of the compost from the municipal composting plant Písek. This part also includes a description of the composting plant and a description of the composting process. The main part and the goal of the thesis is to determine the ion-exchange capacity T according to Sandhoff and to suggest the optimal composting technology in the Municipal composting plant Písek.

Made available in DSpace on 2016-06-02T19:56:54Z (GMT). No. of bitstreams: 1 6022.pdf: 1662458 bytes, checksum: 4e6f5f48dc72f84e96a68be96f5ddf02 (MD5) Previous issue date: 2014-03-28 / Financiadora de Estudos e Projetos / Penicillin G acylase (PGA) is the key enzyme for the industrial production of β-lactam antibiotics. Major current PGA demand is attended for producer organisms as Escherichia coli and Bacillus megaterium genetically modified. The enzyme produced by Escherichia coli accumulates in the periplasmic space of the bacteria and it requires cell disruption for recovery, whereas the enzyme from Bacillus megaterium is secreted into the production medium. This study aimed to evaluate the adsorption of PGA expressed by these two recombinant microorganisms in cationic and anionic resins for recovery and purification of the enzyme. For E. coli PGA was evaluated ionic adsorption of the enzyme in Streamline SP XL® cation exchanger resin after cell disruption by sonication. In this step, we assessed the influence of pH and buffer, to reduce the loss of enzyme inactivation and adjust the pH to a value suitable for a subsequent selective adsorption of the enzyme. The buffers evaluated were acetate, citrate, phosphate and carbonate, and the values of pH were adjusted between 4,5 and 11,0. No denaturation of the enzyme was observed in buffers and pHs evaluated. However, it was observed enzyme adsorption in cellular debris at pH values equal or smaller than 5,4, this debris adsorption was more apparent in the presence of acetate buffer. Thus, cell disruption was defined at pH 6.0 to prevent loss PGA in the adsorption of debris and adjustment of pH and salt molarity by dilution in the appropriate buffer to prevent denaturation of the enzyme by local reduction of the pH when uses concentrated acid. The STREAMLINE SP XL® resin showed higher adsorption capacity of PGA at pH 5,0 and the temperature range (4 and 25°C) did not influence it. The Langmuir isotherm represented adequately the experimental data of the enzyme adsorption resin at 4 and 25°C (pH 5,0) with similar values of qm and KL 25,4 U/g 185,2 U/g, respectively. Purification of PGA in a fixed-bed column showed overall recovery of activity around 50% and purification factor of about 9 times. The adsorption capacity of cationic resin in this mode of operation was 10,9 UNIPAB/mlresin. The PGA purification secreted by Bacillus megaterium recombinant, produced in a synthetic medium, was studied by ion adsorption resins and the following pH values: Streamline SP XL ® and IMMOBEAD IB-C435 (cation-exchanger resins, pH 5,0, 5,5 and 6,0); manae-agarose activated with 40 and 80mmoles/g amino groups (cation exchanger resin, pH 6,0, 7,0 and 7,5); STREAMLINE DEAE XL® and STREAMLINE Q XL® (anionic exchange resins, pH 7,5 and 8,5). Equilibrium experiments in cationic resins Streamline SP XL ® (4°C, pH 5,0) and IB-C435 IMMOBEAD (4°C, pH 5,5) allowed estimation of the parameters of the Langmuir model qm = 76,6 and 91,5 U/g KL = 294,7 and 412,3 U/g, respectively. Despite the high adsorptive capacity of these resins, they were not suited to purification of PGA, because their adsorbes PGA and the contaminants. Manae-agarose resins (40 and 80 μmoles/g) were not effective in PGA adsorption. The STREAMLINE anionic exchangers resins not adsorbed significant amount of PGA in pH evaluated, however, this resin performed a adsorption of almost of 50% proteins present in the medium, demonstrating selective for removal contaminating proteins. Adsorption assays in fixed-bed column Streamline Q XL ® (22°C, pH 8,0) showed that the resin is effective in adsorption of contaminating proteins, it is possible to recover approximately 70 % PGA with a purification factor of 4 times and high specific activity of about 25 U/mg. Already on STREAMLINE SP XL® (22ºC, pH 5,0) resin, the total enzyme recovery was 70 %, but with a purification factor of only 1,61 times and specific activity of around 11 U/mg. It was concluded that adsorption in anionic mode is more advantageous, because presents a better performance and avoid the enzyme dilution. The cultivation of recombinant B. megaterium in a high cell density bioreactor using complex medium, allowed to reach PGA volumetric activity of 50 U/mL. After concentration of the enzyme extract by ultrafiltration to 100 U/mL, was evaluated purification of the enzyme on gel filtration resin column using Superdex 200 Prep Grad (22 °C, pH 7,5). This technique allowed high enzyme recovery (>93%), however with a purification factor of 3 times and specific activity of 13 U/mg. / Penicilina G acilase (PGA) é a enzima chave para a produção industrial de antibióticos β-lactâmicos. Grande parte da demanda atual pela enzima é atendida pela sua produção por Escherichia coli e Bacillus megaterium geneticamente modificados. A enzima produzida por Escherichia coli acumula-se no espaço periplasmático da bactéria, requerendo rompimento celular para sua recuperação, enquanto que a enzima produzida por Bacillus megaterium é secretada para o meio de produção. Este trabalho teve como objetivo avaliar a adsorção de PGA produzida por esses dois microrganismos recombinantes em resinas catiônicas e aniônicas para recuperação e purificação da enzima. Para PGA de E. coli avaliou-se a adsorção iônica da enzima na resina de troca catiônica STREAMLINE SP XL® após rompimento celular por sonicação. Nesta etapa, avaliou-se a influência do tampão e do pH, visando reduzir a perda de enzima por inativação e ajustar o pH a um valor apropriado para uma posterior adsorção seletiva da enzima. Os tampões avaliados foram acetato, citrato, fosfato e carbonato, ajustados para valores de pH entre 4,5 e 11,0. Não se observou desnaturação da enzima nos tampões e pHs avaliados. Contudo, observou-se adsorção da enzima nos debris celulares a valores de pH iguais ou menores que 5,4, sendo mais acentuada essa adsorção na presença de tampão acetato. Definiu-se, assim, rompimento celular em pH 6,0 para evitar perda de PGA por adsorção nos debris e ajuste do pH e da molaridade do sal por diluição no próprio tampão da adsorção, para evitar desnaturação da enzima por redução local do pH quando se utiliza ácido concentrado. A resina STREAMLINE SP XL® mostrou maior capacidade de adsorção de PGA em pH 5,0, não sendo influenciada nas temperaturas avaliadas (4 e 25ºC). A isoterma de Langmuir representou adequadamente os dados experimentais de adsorção da enzima nessa resina a 4 e 25ºC (pH 5,0), com valores similares de qm e KL, 25,4 U/g e 185,2 U/g, respectivamente. A purificação de PGA em coluna de leito fixo apresentou recuperação global de atividade em torno de 50% e fator de purificação de aproximadamente 9 vezes. A capacidade de adsorção da resina de troca catiônica nesse modo de operação foi de 10,9 UNIPAB/mLresina. A purificação de PGA secretada por Bacillus megaterium recombinante, produzida em meio sintético, foi estudada por adsorção iônica da enzima nas seguintes resinas e valores de pH: STREAMLINE SP XL® e IMMOBEAD IB-C435 (resinas de troca catiônica, pHs 5,0, 5,5 e 6,0); MANAE-agarose ativada com 40 e 80 μmoles de grupos amino/g (resina de troca catiônica, pHs 6,0, 7,0 e 7,5); STREAMLINE DEAE XL® e STREAMLINE Q XL® (resinas de troca aniônica, pHs 7,5 e 8,5). Ensaios de equilíbrio para as resinas de troca catiônica STREAMLINE SP XL® (4ºC, pH 5,0) e IMMOBEAD IB-C435 (4ºC, pH 5,5) permitiram a estimativa dos parâmetros do modelo de Langmuir: qm = 76,6 e 91,5 U/g e KL= 294,7 e 412,3 U/g, respectivamente. Apesar da alta capacidade adsortiva dessas resinas, as mesmas não foram adequadas à purificação de PGA, pois adsorveram tanto PGA quanto proteínas contaminantes. As resinas MANAE-AGAROSE (40 e 80 μmoles/g) não foram eficazes na adsorção de PGA. As resinas STREAMLINE de troca aniônica não adsorveram quantidade significativa de PGA nos valores de pH avaliados, entretanto, adsorveram quase 50% de proteínas presentes no meio, mostrando-se assim seletiva para retirada das proteínas contaminantes. Ensaios de adsorção em coluna de leito fixo com STREAMLINE Q XL® (22ºC, pH 8,0) mostraram que a resina é eficaz na adsorção de proteínas contaminantes, sendo possível a recuperação de aproximadamente 70% de PGA com um fator de purificação de 4 vezes e alta atividade específica, em torno de 25 U/mg. Já na resina STREAMLINE SP XL® (22ºC, pH 5,0) a recuperação total da enzima foi de 70%, mas com um fator de purificação de apenas 1,61 vezes e atividade específica em torno de 11 U/mg. Assim, conclui-se que a adsorção no modo aniônico é mais vantajosa, pois além de maior purificação, não dilui a enzima. O cultivo de B. megaterium recombinante em biorreator com alta densidade celular, utilizando meio complexo, permitiu atingir atividade volumétrica de PGA de 50 U/mL. Após concentração do extrato enzimático por ultrafiltração até 100 U/mL, avaliou-se a purificação da enzima em coluna de gel de filtração utilizando a resina Superdex 200 prep grad (22ºC, pH 7,5). Essa técnica permitiu alta recuperação da enzima (>93%), entretanto com um fator de purificação de 3 vezes e atividade específica de 13 U/mg.

Made available in DSpace on 2016-06-02T19:56:57Z (GMT). No. of bitstreams: 1 6607.pdf: 6190774 bytes, checksum: 3ea1f5345ec9e1a04d7b61ab8fabc3f1 (MD5) Previous issue date: 2015-02-24 / In order to increase accessibility to catalytic sites, several studies currently aimed at reducing the diameter of the particles of zeolites to the nanometer scale. So, the increase in aging temperature caused a reduction in the size of the particle to 40 ° C, higher values for the phenomenon of crystal growth has become prevalent. At temperatures between 50 ° C and above, evidenced the formation of materials with relative crystallinity, even before the hydrothermal treatment step. On aging at 60 ° C for 24 h, according to the XRD patterns and the use of the Scherrer equation was obtained the smaller crystallite sizes of all the syntheses performed, those having dimensions of about 12 nm and particle of 300 nm. Thus, when the synthesis time compared to the literature, there obtained a reduction of 54 h and no more necessary to make the hydrothermal treatment step at 100 ° C. To evaluate the influence of the size of the zeolite crystals, when they apply the basic catalysis, using the commercial and nanometric zeolites synthesized. Both materials modified by ion exchange with ammonium cations and methylammonium, in order to generate catalytic sites with strong basic properties. Due to steric hindrance ion exchange not completely occurred, however the nanometric zeolite showed values of ion exchange higher for all cations used for commercial zeolite, except for the tetramethylammonium cation, where the results were equal. Among all exchangers used cations, zeolites containing methylammonium had better conversions. The catalytic evaluations conducted have shown overall prevalence of catalysts with nanosized front of commercial micrometric zeolite. The greater accessibility and better diffusion of the reactants and products through the pores of zeolites with nanosized crystallites provided better performance in catalytic studies on activity, kinetics, reaction rate, activation energy and TOF. / Com o objetivo de aumentar a acessibilidade aos sítios catalíticos, inúmeras pesquisas são realizadas atualmente visando a redução do diâmetro das partículas das zeólitas para a escala nanométrica. Assim, a fim de aperfeiçoar e reduzir o tempo de síntese da zeólita FAU nanométrica foram empregadas algumas modificações no método reportado na literatura sem a utilização de direcionadores orgânicos. O aumento da temperatura de envelhecimento proporcionou a redução do tamanho das partículas até 40°C, para valores superiores o fenômeno de crescimento tornou-se predominante. Na temperatura de 50°C e superiores, evidenciou-se a formação de materiais com relativa cristalinidade antes mesmo da etapa de tratamento hidrotérmico. No envelhecimento a 60°C por 24 h, de acordo com os difratogramas e com o emprego da equação de Scherrer foram obtidos os menores tamanhos de cristais dentre todas as sínteses realizadas, estes possuindo dimensões em torno de 12 nm. Em uma avaliação catalítica preliminar utilizando todas as zeólitas sintetizadas na forma sódica, na reação modelo de condensação de Knoevenagel, os melhores resultados foram obtidos pela zeólita constituída de cristais de 12 nm e partículas de 300 nm. Desse modo, quando comparado o tempo de síntese com a literatura, atingiu-se uma redução de 54 h, além de não ser mais necessária a etapa de tratamento hidrotérmico a 100°C. Para avaliar a influência do tamanho dos cristais zeolíticos quando estes aplicados à catálise básica, utilizou-se as zeólitas comercial e nanométrica sintetizada no trabalho. Ambos os materiais foram modificados por troca iônica com cátions de amônio e metilamônio, objetivando a geração de sítios catalíticos com propriedades básicas mais fortes. Devido a impedimentos estéricos a troca iônica não ocorreu totalmente, porém, a zeólita com cristais de 12 nm apresentou valores de troca iônica superiores para todos os cátions utilizados em relação a zeólita comercial, exceto para o cátion tetrametilamônio, em que os resultados foram similares. Dentre todos os cátions trocadores utilizados, as zeólitas contendo monometilamônio apresentaram melhores conversões. As avaliações catalíticas realizadas demostraram melhor desempenho dos catalisadores nanométricos frente a zeólita micrométrica comercial. A maior acessibilidade e a melhor difusão dos reagentes e produtos pelos poros da zeólita nanométrica, proporcionaram melhores resultados nos estudos catalíticos referentes a atividade, cinética, velocidade da reação, energia de ativação e TOF.

Le développement des sources supercontinuum a engendré des avancées majeures dans de nombreux domaines tels que la spectroscopie, la métrologie ou encore la biologie avec la tomographie optique cohérente. Récemment, l'arrivée des fibres à cristaux photoniques (FCPs) a permis la fabrication de telles sources avec des lasers impulsionnels de pompe moins puissants. Ainsi, de par leur compatibilité avec les fibres optiques, les lasers impulsionnels réalisés en optique intégrée sur verre semblent une alternative intéressante pour la réalisation d'une source supercontinuum intégrée. Notre travail a donc eu pour objectif l'étude et la réalisation d'un laser impulsionnel déclenché par modulation passive des pertes assez puissant et compatible avec les fibres à cristaux photoniques dans le but de générer un supercontinuum. Nous avons alors conçu et fabriqué ce laser constitué d'un guide d'onde amplificateur réalisé par échange d'ions dans un verre dopé au néodyme et d'une cavité Fabry-Perot fermée par un miroir diélectrique en entrée et sans miroir de sortie ce qui permet un couplage direct avec une fibre optique. L'hybridation de l'absorbant saturable sous la forme d'une couche mince d'acétate de cellulose dopée au BDN sur le guide d'onde a permis la génération d'impulsions ayant une puissance crête de (2,8 ± 0,6) kW. La source supercontinuum réalisé avec une FCP pompée par le laser préalablement étudié présente un spectre allant de 440 nm à 1600 nm. Les perspectives de cette étude portent sur le changement de matériau absorbant saturable pour permettre l'émission d'impulsions plus puissantes, ainsi que sur l'intégration monolithique de la FCP pour réaliser un dispositif encore plus compact. Elles portent aussi sur la réalisation de lasers intégrés à modes bloqués utilisant cette technologie. Nous avons démontré sa faisabilité ainsi que son régime de fonctionnement en soliton dissipatif. Des caractérisations préliminaires ont également été effectuées. / Supercontinuum sources made possible major break through in spectroscopy metrology and biology like the development of optical coherent tomography. Photonics crystal fiber have been useful for supercontinuum generation allowing the use of relatively low peak power pulsed laser sources. Regarding this kind of devices, pulsed lasers made by integrated optics on glass seemed to be a good candidate. The aims of this work were hence to develop and realize Q-switched lasers for photonic crystal fiber pumping. We demonstrated the possibility to realize a supercontinuum source pumped by an integrated Q-switched laser made by ion exchange on Neodymium doped glass. The Fabry-Perot cavity used is closed by a dielectric mirror on one hand and by the waveguide facet on the other side allowing direct coupling with optical fiber. The saturable absorber has been hybridized on the amplifying waveguide to interact with the evanescent wave. (2.8 ± 0.6) kW peak-power pulses have been generated, which coupled in a photonic crystal fiber, generated a 440 nm to 1600 nm large supercontinuum. As a perspective, a mode-locked laser realized with the same technology has been demonstrated. We show that this laser operates in dissipative soliton regime. This laser is then preliminary characterized.

Ce travail s'inscrit dans le contexte du retraitement du combustible irradié dans l'industrie nucléaire. La gestion du combustible usé fait partie des enjeux majeurs de l'industrie nucléaire aujourd'hui. Ses vastes implications sont de nature économique, politique et écologique. Puisque le combustible irradié contient 97 % des matières valorisables, de nombreux pays ont choisi de retraiter le combustible, non tant pour des raisons économiques que pour le besoin de réduire la quantité en déchets radiotoxiques. Le procédé de séparation le plus répandu est connu sous le nom PUREX et consiste à diluer le combustible dans une solution d'acide nitrique afn d'en extraire les matières valorisables, comme notamment l'uranium et le plutonium. Le procédé est soumis à des strictes contrôles qui s'effectuent au présent par prélèvement et analyse manuel des flux radiotoxiques. Il n'existe cependant peu d'outils pour la supervision du procédé en ligne. Ces travaux visent alors à développer un capteur adapté à cet environnement de mesure à la fois acide et ionisant. Les verres borosilicates étant répandus pour leur inertie chimique, nous proposons l'étude d'un capteur optique fondé sur le substrat de verre Borofloat 33 de Schott. Le capteur étudié et réalisé a été fabriqué grâce à deux technologies différentes : l'optique intégrée sur verre par échange d'ions pour la fabrication de fonction de guidage optique, et la microfluidique pour la gestion des flux acides au sein du capteur. L'approche optique permet de répondre aux besoins de polyvalence, de sensibilité et d'immunité au rayonnement électromagnétique. La microfluidique permet, quant à elle, de travailler sur des très faibles volumes d'échantillon, réduisant ainsi la radiotoxicité des flux d'analyse. Le principe de mesure du capteur repose sur l'effet photothermique, induit dans le fluide par absorption optique d'un faisceau laser d'excitation. L'absorption entraîne un changement de l'indice de réfraction du fluide qui est sondé par un interféromètre de Young, intégré sur la puce. Le volume sondé au sein du canal était de (33,5 ± 3,5) pl. Le changement d'indice de réfraction à la limite de détection était de ∆n_min = 1,2 × 10−6 , nous permettant de détecter une concentration minimale de cobalt(II) dans de l'éthanol de c_min = 6 × 10−4 mol/l, équivalent à un coefficient d'absorption de alpha_min = 1,2 × 10−2 cm−1. À la limite de détection du capteur, une quantité de N_min = (20 ± 2) fmol de cobalt(II) peut être détectée. La longueur d'interaction était de li = 14,9 µm et par conséquent l'absorbance minimale détectable égal K_min = (1,56±0,12)×10−5. / This work has been done in the context of fuel reprocessing in the nuclear industry. In fact, the handling of nuclear waste is one of the major issues in the nuclear industry. Its implications reach from economical to political to ecological dimensions. Since used nuclear fuel consists of 97 % of recyclable substances, many countries have chosen to reprocess used fuel, not only for economical reasons but also to limit the quantity of nuclear waste. The most widely employed extraction technique is the PUREX process, where the used fuel is diluted in nitric acid. The recyclable compounds can then be extracted by solvent techniques. Such processes need to be monitored crucially. However, nowadays, the process supervision is carried out by manually sampling the radioactive fluents and analyzing them in external laboratories. Not only prone to potential risks, this approach is little responsive and produces radiotoxic samples that cannot be reintroduced in the nuclear fuel cycle. In this study, we therefore present the development of a microfluidic glass sensor, based on the detection of a photothermal effect induced in the sample fluid. Microfluidics allows fluid handling on a microliter-scale and can therefore significantly reduce the sample volume and thereby the radiotoxcicity of the analyzed fluids. Photothermal spectrometry is well suited for small-scale sample analysis, since its sensitivity does not rely on the length of optical interaction with the analyte. The photothermal effect is a local refractive index variation due to the absorption of photons by the analyte species which are contained in the sample. On the sensor chip, the index refraction change is being sensed by an integrated Young interferometer, made by ion-exchange in glass. The probed volume in the channel was (33.5 ± 3.5) pl. The interferometric system can sense refractive index changes as low as ∆n_min = 1.2 × 10−6 , allowing to detect a minimum concentration of cobalt(II) in ethanol c_min = 6 × 10−4 mol/l, which is equivalent to an absorption coefficient of alpha_min = 1.2 × 10−2 cm−1 . At the detection limit, we could sense an absolute quantity of cobalt(II) of N_min = (20 ± 2) fmol. The interaction length between the excitation light and the sensing zone was li = 14.9 µm leading to a minimum detectable absorbance of K_min = (1.56 ± 0.12) × 10−5 .

Le niveau de sécurité requis dans l'aviation civile a conduit à l'utilisation de plusieurs chaînes séparées de mesures pour une même information. Il est désormais recommandé de les compléter par une chaîne de mesure dissemblable. Ainsi, THALES Avionics développe depuis 2006 un anémomètre laser dont l'injecteur est réalisé en optique intégrée sur verre pour la mesure de la vitesse de l'avion. Ce travail de thèse vise à poursuivre la miniaturisation en hybridant sur une puce de verre la diode laser de pompe qui alimente l'injecteur optique. L'architecture proposée repose sur le verrouillage d'une diode laser à ruban large sur son mode fondamental grâce à une cavité externe planaire. Celle ci est constituée d'un convertisseur modal réalisé par échange d'ions sur verre intégrant un réseau de Bragg à sa sortie monomode. Le travail réalisé dans cette thèse comporte trois étapes principales. Dans un premier temps, un modèle analytique a permis de dimensionner la rétroaction optique à imposer sur la diode. L'échange d'ions sélectivement assisté par champ électrique a permis dans un second temps de réaliser un convertisseur modal adapté à la liaison entre la diode ruban et la fibre optique monomode de récupération. Finalement, le verrouillage modal a été démontré grâce à l'utilisation d'une fibre optique à réseau de Bragg. L'émission spectrale de la diode laser a été stabilisée autour de la longueur d'onde de Bragg sur une largeur spectrale de 0,3 nm tandis que la puissance en sortie de la fibre monomode a atteint 100 mW. Le réseau de Bragg a alors été intégré sur la puce optique et l'émission de la diode laser ruban a également été stabilisée par la rétroaction intégrée. La forte réflexion du réseau a limité la puissance en sortie du dispositif et une émission sur deux modes transverses a été constatée. Les perspectives de cette étude portent, d'une part, sur l'augmentation de la puissance en sortie du dispositif et, d'autre part, sur la réalisation d'un système de pompage monolithique d'un milieu actif placé au sein de la cavité externe. / Objectives of security in civil aviation are reached in multiplying separated measuring chains. The use of dissimilar measuring chains is now encouraged. For this purpose, THALES Avionics has developed an aircraft speed laser anemometer. The suitability of integrated optics on glass for the miniaturisation of the system has been proven in 2006. This thesis aims at pushing ahead with the miniaturisation in hybridising the pump laser diode which supplies the seed laser on a glass platform. The structure consists on locking the fundamental of a Broad Area Laser Diode (BALD) thanks a planar external cavity, composed of a modal converter made by ion exchange on glass and a Bragg grating. First, easy to use conception rules for the BALD's optical feedback are elaborated. Then, the technique of selective field assisted ion exchange is shown to be adapted to the realisation of a modal converter between the BALD and a single mode collecting optical fibre. The realised converter demonstrated the modal locking thanks to the use a fibre Bragg grating. The BALD has been stabilized around the Bragg wavelength with a spectral width of 0.3 nm and stable single mode output power has reached 100 mW. The Bragg grating has then been integrated on the optical chip and the integrated locking of the BALD has been achieved. The output power has been limited by the high reflectivity of the grating. As perspectives, the increase of the output power has been studied and a highly integrated system of intra cavity pumping is proposed.

L'essor des télécommunications sur fibres a conduit depuis quarante ans au développement des composants optiques intégrés. Cependant, en raison de difficultés technologiques, un dispositif n'a pas encore été réalisé de façon satisfaisante : il s'agit de l'isolateur optique, dont la fonction est de propager la lumière dans un seul sens. Ces travaux s'inscrivent dans cette problématique puisqu'ils visent à l'intégration d'un isolateur grâce à la technologie de l'échange d'ions Na+/Ag+ sur verre. La configuration adoptée se compose de trois éléments sur puce : un séparateur de polarisation et deux rotateurs de polarisation à 45 °, l'un réciproque et l'autre non. Le séparateur de polarisation a été réalisé sous la forme d'une jonction Y asymétrique. Après une étude théorique, nous présentons le procédé de fabrication ainsi que les résultats expérimentaux obtenus. Les diaphonies mesurées sont à l'état de l'art, elles dépassent (31,1 ± 0,4) dB et (32,7 ± 0,4) dB en mode TE et TM sur une plage spectrale supérieure à 70 nm. Nous avons mené l'étude du rotateur Faraday en collaboration avec le Laboratoire Télécom Claude Chappe de Saint Etienne pour la partie magnéto-optique. La structure employée est un guide d'onde à enterrage différentiel sur lequel est déposé un matériau magnéto-optique par un procédé sol-gel. Un angle de rotation non-réciproque de 50 ° a été mesuré, validant ainsi l'approche hybride. Un nouveau procédé de fabrication est également présenté pour un rotateur réciproque à évolution de mode adiabatique. Celui-ci consiste en un enterrage sous champ présentant une inhomogénéité transverse. Nous proposons finalement une méthode de fabrication de l'isolateur complet basée sur l'intégration monolithique des différents éléments. / For the past forty years, the growth of fiber telecommunications has led to the development of integrated optical components. However, due to technological issues, a device has not yet been realized: the optical isolator, which propagates light in a single direction. Our work fits into this context. It deals with the integration of an isolator using the Na+/Ag+ ion-exchange technology. The configuration we adopted consists of three elements on chip: a polarization splitter and two 45 ° polarization rotators, one is reciprocal and the other is not. The polarization splitter has been realized in the shape of an asymmetrical Y junction. After a theoretical study, we present the fabrication process and experimental results. State-of-the-art diaphonies of (31.1 ± 0.4) dB and (32.7 ± 0.4) dB have been measured in TE and TM mode over a bandwidth larger than 70 nm. The magneto-optical part of the study has been undertaken in collaboration with the Laboratoire Télécom Claude Chappe (LT2C) from Saint Etienne, France. The Faraday rotator is a selectively buried waveguide on which a magneto-optical material has been deposited using a sol-gel process. A non-reciprocal rotation of 50 ° has been measured, hence validating the hybrid approach. A novel fabrication process is presented for a reciprocal mode-evolution polarization rotator. The process consists in the burring of a waveguide under an electric field presenting a transverse inhomogeneity. We finally propose a fabrication method of the complete optical isolator. It is based on the monolithic integration of the three elements.

Les besoins actuels des systèmes de télécommunications et des capteurs optiques poussent à réaliser des circuits intégrés optiques présentant toujours plus de fonctions sur un même substrat. Atteindre un tel niveau d'intégration est difficile, car les matériaux et les procédés technologiques employés pour implémenter les différentes fonctions optiques ne sont pas toujours compatibles entre eux. Cette thèse s'inscrit dans la problématique de l'intégration des fonctions optiques actives (émission, amplification) et passives (multiplexage, filtrage, etc.) sur substrat passif et reporte la réalisation d'un laser DFB hybride tridimensionnel par échange d'ions sur verre passif et report de plaque d'un verre actif codopé Er3+:Yb3+. Ce laser est constitué d'un guide canal de Bragg, sélectivement enterré dans le substrat passif, et chargé par un guide plan, réalisé dans le verre actif (dopé avec une concentration massique de 2,3% en Er2O3 et 3,6% en Yb2O3). Il est caractérisé par une émission monomode de (420±15) µW à 1534 nm, pour (390±20) mW de puissance de pompe injectée. Ce dispositif ouvre ainsi la voie vers l'intégration de fonctions actives, localisées à la surface du substrat passif, avec des fonctions passives, réalisées en exploitant le volume et la surface du même substrat. / The current needs of optical telecommunications and sensors require developing integrated optical circuits providing different and heterogeneous functions on the same substrate. The main issue is the incompatibility between the manufacturing processes of these optical functions. This work deals with the integration of active (emission, amplification) and passive (multiplexing, filtering, etc.) functions on a passive glass substrate. Its aim is to develop a DFB three-dimensional hybrid laser by ion-exchange in passive glass. This laser is made of a Bragg channel waveguide, selectively buried in the passive glass substrate, loaded by a plane waveguide, defined at the surface of an Er3+:Yb3+ codoped active glass wafer. It emits a (420±15) µW laser signal at 1534 nm for (390±20) mW injected pump power. Hence this device opens the way towards the integration of active functions, located at the surface of the passive glass substrate, with passive ones, spreading at its surface and in its volume.

De nombreux capteurs optiques, tels que les LIDARS, nécessitent des sources laser à la fois puissantes et spectralement fines. Dans ce contexte, l'objectif de ce projet est la réalisation de sources laser impulsionnelles intégrées, dont les caractéristiques spectrale et temporelle atteignent la limite théorique prédite par la théorie de Fourier. Pour ce faire, nous proposons une structure laser de type DFB avec un fonctionnement déclenché. La technologie de l'échange d'ions est retenue pour réaliser des guides d'onde amplificateurs dans un verre phosphate dopé ytterbium. La cavité DFB est ensuite constituée par gravure d'un réseau de Bragg à la surface des guides amplificateurs. Le comportement impulsionnel est obtenu par dépôt, sur la structure précédente, d'une couche mince d'acétate de cellulose dopée avec l'absorbant saturable BDN. Cette structure nous a permis d'obtenir des lasers impulsionnels monomodes longitudinaux dont les caractéristiques spectrales atteignent la limite de Fourier. Une étude en concentration d'absorbant saturable du superstrat montrent une variation de la durée des impulsions de 2,5 ns à 100 ns avec des puissances crêtes respectives de 30 W et 14 W. Nous parvenons donc à des spectres de largeur à mi-hauteur de valeur 9 MHz. Ces résultats ouvrent la voie à la réalisation de sources laser compactes pour les lidars embarqués. / Various optical sensors, such as LIDARs, need laser sources both powerful and narrow-linewidth. In this context, the aim of this project is the realization of integrated pulsed laser sources with a Fourier Transform Limited (FTL) spectrum. To do so, we propose a passively Q-switched DFB laser structure. Ion-exchange technology is used to realize amplifier waveguides on Ytterbium-doped phosphate glass. The DFB cavity is made by dry etching of a Bragg grating on the waveguides surface. The Q-Switched behavior is obtained by depositing a BDN-doped cellulose acetate coating layer, acting as a saturable absorber. This structure allowed us obtaining FTL single-frequency pulsed lasers. When studying the impact of BDN concentration, we observe pulses ranging from 2,5 ns with 40 W peak power, to 100 ns with 14 W peak power. Thus, our device FWHM linewidth goes down to 9 MHz. These results pave the way for the realisation of compact laser sources for embedded lidar systems.