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Study on the Growth and Characterization of Epitaxial Cu2O Thin Films by Magnetron SputteringLin, Chaio-Wei, 30 August 2012 (has links)
Cuprous oxide (Cu2O) was first investigated in the 1920s as a semiconductor material with Eg~2.17 eV. It is ideal for applications in solar cells, electrochromic devices, oxygen and humidity sensors because of its high optical absorption coefficient, non-toxic nature, abundant availability and low cost for production. Many groups have tried different ways to grow the cuprous oxide by, for instance, sputtering, CVD, PLD, MBE, and electro-deposition etc. Among them, the sputtering method is probably the most cost-effective and easy to operate.
In this work, the cuprous oxide thin films were grown on R-Al2O3 and (110)-MgO substrates by DC reactive magnetron sputtering. Thin films grown at different temperatures under various oxygen partial pressures were studied by X-ray diffraction (XRD) to test their structural perfections. Samples with the Cu2O on Al2O3(1012) and MgO(110) were studied via measurement of cathodoluminescence(CL) spectroscopy, photoluminescence (PL) spectroscopy, transmission spectroscopy and magneto transport behaviors. The correlation of growth condition and physical properties are discussed.
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The synthesis and phase transformation of tohdite and alumina condensatesPan, Chiennan 17 August 2006 (has links)
Abstract
The present thesis focused on the synthesis and phase transformation of tohdite and alumina via static compression of gels at high temperature-pressures and dynamic laser ablation condensation of metal target under oxygen background gas.
In part I, hydrous Al2O3-TiO2 (78:22 in molar ratio) gel was fired at various PT conditions using a piston-cylinder apparatus and identified by XRD, FTIR, optical microscopy and electron microscopy. Below 675oC, the sample remained amorphous at ambient pressure, yet transformed at 1.5 kbar to Ti-doped tohdite, which is elongated along the crystallographic c-axis, with well-developed (0001) base and {10 0} faces. Tohdite has a significant water/hydroxy content and is therefore susceptible to pore coalescence parallel to the basal layer upon electron dosage. Tohdite also contains Ti4+ up to 3 at.%, which replaces Al3+ in tetrahedral and/or octahedral sites to form superstructures and defect microstructures. In contrast, a higher T-P condition (above 675oC and 8 kbar) caused the formation of more stable Ti-doped corundum, which is hexagonal-rhombohedral crystal form and in epitaxial association with rutile nuclei. Ti-doped tohdite and corundum shed light on a sol-gel route for their occurrence in peraluminous metamorphic rock. The nanoporous and nanodelaminated tohdite may have potential catalytic applications (Part I).
In part II, amorphous Al2O3 nanocondensates were synthesized via very energetic Nd-YAG laser pulse irradiation of oxygen-purged Al target for a very rapid heating/cooling effect. The nanocondensates above a critical diameter of 20 nm were phase separated as
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Study on the Polishing Characteristics of Silicon Wafer for New Type Ultraprecision PolisherHuang, Wei-Hang 25 July 2003 (has links)
In conventional abrasive machining , it must using dresser to dress the surface of polishing disc periodically , in order for polishing disc to maintain its ability of machining , and then ensuring the quality of work piece. It will make polishing disk thin , finally it must losing it ability of machining , and then be replaced by a new disc. For this reason , in the study , an idea of a new type ultraprecision polisher is proposed . Using Sn-Al2O3 composite coating to reach the mirror surface grinding of silicon wafer in the tin bath , and grinding with electroplating continuously . It will ensure the ability of machining of polishing disc .
In the study , first , analyzing the effect of rotational speed rate of wafer and polishing disc on the grinding trajectories type of machining surface . From the result of analysis , find that , when the rotational speed rate is more irregular or it could not divided , the arrangement of grinding trajectories is more complex .
And then , investigating the effect of cathode current density , rotational speed of polishing disc and time of plating on the characteristics of composite coating . In the experiment of composite electroplating , when cathode current density is higher , the size of crystal is smaller , the thickness of coating is thicker , and the quantity of Al2O3 within coating decrease lightly . The increase of the rotational speed of polishing disk could increase the size of crystal , the thickness of coating and the quantity of Al2O3 lightly . The time of plating is longer , the shape of crystal is more obvious , the thickness of coating is thicker and it also increase the quantity of Al2O3 .
Finally , investigating the effect of cathode current density and cationic surfactant PEI on the characteristics of coating and wafer . In practical abrasive machining , the removal rate of wafer increases with cathode current density , and the addition of PEI could increase the quantity of Al2O3 indeed . Besides , under the same machining condition , in the tin bath with PEI , the removal rate is higher than the one in the tin bath without PEI .
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Vliv plazmové aktivace keramických částic na technologii přípravy a vlastnosti pokročilých keramických materiálů / Influence of plasma activation of ceramic particles on ceramic technology and propertiesKlevetová, Tereza January 2019 (has links)
This thesis is focused on the study of the influence of plasma activation of powder ceramic materials on sintered microstructure. In this experiment Diffuse Coplanar Surface Barrier Discharge (DSCBD) device was used for plasma treatment and two materials were chosen to be investigated – Al2O3 (TAI) and ZrO2 doped with 3 mol % Y2O3 (TZ). Two methods of powders dispergation in suspension were used – ultrasound and ball milling. The effect of using of DCSBD on alumina and zirconia powders was investigated by mercury intrusion porosimetry, dilatometry and by evaluation of final relative densities and grain sizes. Generally, was investigated that plasma surface activation of ceramic particles has measurable influence on the final microstructure. In comparison with the non-plasma treated alumina powders, plasma activated powders disperged with ultrasound and ball milling achieved lower values of grain size at comparable relative densities. In case of zirconia powders was observed that plasma treated powders achieve higher relative densities, if ultrasound was used. On the other hand, plasma treated zirconia powders disperged with ball milling achieve lower relative densities compared with non-plasma treated zirconia powders. Final sintering trajectory of plasma treated TZ powders disperged with ultrasound is comparable to the sintering trajectory of non-plasma treated zirconia powders disperged with ball milling and vice versa. Plasma surface treatment is the way of more ecological friendly preparation of suspension and its stabilization than the conventional stabilization methods using chemical additives.
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Synthèse de bio-liquide de seconde génération par hydroliquéfaction catalytique de la lignine / Synthesis of second generation fiofuels by catalytic hydroliquefaction of ligninJoffres, Benoît 15 November 2013 (has links)
Actuellement, la transformation de la biomasse en bio-carburant ou molécules pour l'industrie chimique fait l'objet de nombreuses recherches. La lignine, en tant que coproduit de l'industrie papetière et de l'éthanol cellulosique, est une ressource des plus disponibles qui pourait être utilisée pour la production d'aromatiques ou de composés phénoliques. Cependant, cette macromolécule constituée d'unités propylphénoliques liées par des liaisons éthers nécessite d'être dépolymérisée. Ce travail porte sur la compréhension des mécanismes de liquéfaction par hydroconversion catalytique d'une lignine de paille de blé extraite par un procédé papetier à la soude. Dans un premier temps, nous avons mené une caractérisation poussée de cette lignine à l'aide de diverses techniques qui nous a permis de proposer une structure modèle. Ensuite, nous avons mis en place un mode opératoire de conversion et un protocole de récupération des produits. La réaction est réalisée en réacteur semi-ouvert à 350°C en présence d'H2 (8MPa), d'un solvant donneur d'hydrogène (tétraline) et d'un catalyseur d'hydrotraitement NiMoP/Al2O3 sulfuré. Les produits se répartissent en une phase liquide (liquéfiat), une phase gaz, une lignine résiduelle et des solides non-solubles dans le THF. Un taux de conversion a été défini comme le rendement en produits non-solides et les valeurs maximales atteintes sont de 81% pds après 28h de réaction avec un excellent bilan matière. Les fractions récupérées ont ensuite été caractérisées en détail avec des techniques d'analyse adaptées. Grâce à ce protocole d'analyse, nous avons pu observer que le solvant permet d'éviter la formation de solides et que le catalyseur intervient principalement sur l'hydrodésoxygénation et l'hydrogénation des molécules issues de la dépolymérisation de la charge. Enfin, nous avons suivis la réaction au cours du temps, ce qui nous a permis de présenter une ébauche de schéma réactionnel. Les premières étapes de conversion sont la décarboxylation, l'hydrogénolyse des OH aliphatiques et la rupture des liaisons éthers entre les unités élémentaires de la lignine, qui entraînent sa dépolymérisation. Puis des processus plus lent se produisent comme l'élimination des groupes méthoxy, principalement par déméthylation suivi de déshydroxylation. Ainsi, les principaux produits obtenus sont des composés phénoliques et des composés désoxygénés / Nowadays, the transformation of lignocellulosic biomass is deeply investigated in order to provide biofuels and chemicals. Lignin, a by-product of pulp and bio-ethanol industry, is an available resource which could be used for the production of aromatic and phenolic compounds. However, this macromolecule mainly made of propylphenolic units linked by ether functions needs to be depolymerized. This work focuses on the study of liquefaction mechanisms by catalytic hydroconversion of wheat straw lignin extracted by a soda pulping. In the first part of this study, an in-depth characterization of this lignin was carried out using techniques. A structure of our lignin was proposed as a result. Then, a procedure was developed to perform the catalytic hydroconversion and recover the products. Catalytic experiments were carried out in a semi-batch reactor at 350°C, using H2 (8 MPa), a hydrogen donor solvent (tetralin) and a sulfide NiMoP/Al2O3 catalyst. The recovered products were separated into a liquid phase, gases, a lignin residue and THF insoluble solids. A conversion of 81 wt% of lignin into non-solid products was reached after 28h of reaction with an excellent mass balance. The characterization of the different fractions was carried out using techniques. Thanks to this protocol, we were able to point out the role of the H-donor solvent for preventing solid formation as well as the role of the catalyst for hydrodeoxygenation and hydrogenation of the depolymerized products. Finally, the catalytic hydroconversion of the lignin was carried out with the different residence times, which helps understanding the transformations occurring during the conversion. At the beginning of the reaction, we observed decarboxylation, hydrogenolysis of aliphatic OH and cleavage of ether linkages between the phenolic units of the lignin. Then, we observed elimination of methoxy groups, mainly by demethylation followed by dehydroxylation. Finally, the main products obtained during the reaction were phenolic and deoxygenated compounds such as aromatics, naphthenes and alkanes
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Microstructural, mechanical, and optical characterization of a ZTA (zirconia-toughened alumina) composite after aging / Caracterização microestrutural, mecânica e óptica de um compósito ZTA (alumina reforçada por zircônia) após envelhecimentoLopes, Adolfo Coelho de Oliveira 08 March 2019 (has links)
Aim: To validate a method for the synthesis of a ZTA composite (Al2O3-80%/ Zr2O- 20%) and to characterize the experimental materials topography, optical, and mechanical properties in the as-sintered condition and after a simulated low temperature degradation (LTD) aging protocol compared to a translucent Y-TZP (ZPEX). Material and methods: Experimental ZTA (ZTA ZPEX 80/20) and translucent Y-TZP (ZPEX) green-state disc-shaped specimens were obtained by uniaxial/isostatic ceramic powder pressing technique. Discs were sintered according to a preestablished protocol. After sintering, two-sided polishing was performed with diamond discs and diamond suspensions to 1 m. Thirty specimens of each group underwent an aging protocol in autoclave (20h, 134ºC and 2.2 bar). The specimens were subjected to the following characterization tests, in the as-sintered condition and aged: 1) nanoindentation testing to acquire the materials elastic modulus (E) and hardness (H); 2) interferometry was utilized to characterize topographical parameters (Sa/Sq); 3) X-ray Diffraction (XRD) to assess the tetragonal-monoclinic phase transformation; 4) scanning electron microscopy (SEM) to evaluate the homogeneity of surfaces and distribution of grains; 5) reflectance tests on white and black background to determine the Contrast Ratio (CR) and the Translucency Parameter (TP) by color difference (E) and 6) biaxial flexural strength testing according to ISO 6872:2015. Apparent density was measured using Archimedes principle. Weibull 2-p was used to calculate characteristic stress, Weibull modulus, and probability of survival (reliability) at 300, 500 and 800 MPa. Data were statistically evaluated through Repeated Measures ANOVA following post-hoc comparisons by Tukey test (p<0.05). Results and Conclusion: The proposed method was able to successfully synthetize an aging resistant ZTA ZPEX 80/20 composite, with the elastic modulus being the only decreased property after aging. For such composite, the surface roughness parameters, hardness, optical and mechanical properties were not affected by simulated LTD aging. In contrast, the translucent Y-TZP zirconia presented a significant extent of tetragonal to monoclinic phase transformation compared to ZTA composite after aging, along with significant alterations in all evaluated parameters, except for surface roughness. / Objetivos: Validar um método para a síntese de um compósito ZTA (Al2O3-80%/ Zr2O- 20%) e caracterizar a topografia do material experimental e suas propriedades ópticas e mecânicas, antes e após um protocolo de envelhecimento simulando uma degradação em baixa temperatura (DBT), comparado a uma zircônia Y-TZP translúcida (ZPEX). Material e métodos: Os espécimes experimentais ZTA (ZTA ZPEX 80/20) e Y-TZP translúcido (ZPEX) em forma de disco foram obtidos por técnica de prensagem uniaxial / isostática do pó cerâmico. Os discos foram sinterizados de acordo com um protocolo pré-estabelecido. Após a sinterização, um polimento bilateral foi realizado com discos de diamante e suspensões de diamante de até 1 m. Trinta espécimes de cada grupo foram submetidos a um protocolo de envelhecimento em autoclave (20h, 134ºC e 2,2 bar). Os espécimes foram submetidos aos seguintes testes de caracterização, antes e após envelhecimento: 1) ensaios de nanoindentação para obtenção do módulo de elasticidade dos materiais (E) e dureza (H); 2) a interferometria foi utilizada para caracterizar os parâmetros topográficos (Sa / Sq); 3) difração de raios X (XRD) para avaliar a transformação da fase monoclínica para tetragonal; 4) microscopia eletrônica de varredura (MEV) para avaliar a homogeneidade da superfícies e distribuição dos grãos; 5) testes de refletância em fundo branco e preto para determinar a Relação de Contraste (RC) e o Parâmetro de Translucidez (PT) por diferença de cor (E) e 6) teste de flexão biaxial (TFB), de acordo com a ISO 6872: 2015 . A densidade aparente foi medida usando o princípio de Arquimedes. Weibull 2- p foi utilizada para calcular a resistência característica, módulo de Weibull e a probabilidade de sobrevida (confiabilidade) a 300, 500 e 800 MPa. Os dados foram submetidos à análise de variância medidas repetidas, seguida de comparações múltiplas pelo teste de Tukey (p <0,05). Resultados e Conclusão: O método proposto foi capaz de sintetizar com sucesso um compósito ZTA ZPEX 80/20 resistente ao envelhecimento, sendo o módulo de elasticidade a única propriedade que diminuiu após o envelhecimento. Para tal compósito, os parâmetros de rugosidade superficial, propriedade nanomecânica de dureza, propriedades ópticas e mecânicas não foram afetadas pelo envelhecimento simulado de DBT. Em contraste, a zircônia translúcida Y-TZP apresentou uma extensão significativa da transformação da fase tetragonal para monoclínica em comparação ao composto ZTA após o envelhecimento, juntamente com alterações significativas em todos os parâmetros avaliados, exceto a rugosidade superficial.
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Síntese de gem-dicloroaziridinas empregando KF/Al2O3 / Synthesis of gem-dichloroaziridine employing KF/Al2O3Meirelis, Francine Paulina 31 March 2014 (has links)
Nos últimos anos, questões ambientais têm merecido destaque na mídia nacional e internacional. A química tem uma grande participação nos dias atuais com os inúmeros produtos fundamentais à humanidade. A sua presença pode ser destacada desde diversos combustíveis aos mais complexos medicamentos. As reações de síntese orgânica devem ser guiadas por novas práticas mais sustentáveis. Nesse campo, tem-se o conceito da Green Chemistry ou Química Verde, que consiste na estratégia em desenvolver metodologias e processos que usem e gerem a menor quantidade de materiais tóxicos e/ou inflamáveis ou reaproveitáveis. Com o intuito de contribuir com a Química Verde, estudou-se a síntese de iminas que consistiu da primeira etapa do processo de aminação livre de solventes orgânicos e apresentaram rendimentos superiores a 95,0 %; gem-dicloroaziridinas foram preparadas a partir de inserção de diclorocarbeno em iminas em condições mínimas de solvente orgânico, utilizando como catalisador o KF/Al2O3 e com rendimentos superiores a 98,0%. As gem-dicloroaziridinas foram convertidas em amidas por hidrolise, na ausência de solvente e com rendimentos superiores a 98,0%. Dentro do conceito de Química Verde foram preparadas as seis iminas: N-benzilfenilmetanoimina, N-fenil-furilmetanoimina, N-fenilfenilmetanoimina, N-fenil-(4-metoxifenil)-metanoimina, N-benzil-(4-metoxifenil)metanoimina e N-furfurilfurilmetanoimina; duas gem-dicloroaziridinas: 2,2-dicloro-1,3-difenilaziridina e 1-benzil-2,2-dicloro-3-fenilaziridina e duas amidas: cloro-fenilacetanilida e N-benzil-cloro-fenilacetamida. / For the last years Environmental issues have deserved featured in the National and International media. Chemistry has had great participation on currently days with countless products which are fundamental to humanity. Its presence can be detached from various fuels to the most complex drugs.The organic synthesis reactions should be guided by more sustainable new practices. In this field, the Green Chemistry concept or (Química Verde) strategy which aims to develop methodology and and/or processes which use and generate the minimum quality of toxic inflammable material. With the purpose of contribute to green chemistry, we studied the synthesis of imines which consisted of the first stage of the process of amination, free of organic solvents and have yields higher than 95%; gem-dichloroaziridine were prepared from the imines insertion dichlorocarbene in a minimum of organic solvent conditions, using as catalyst KF/Al2O3 and yields higher than 98%. The gem-dichloroaziridines were converted to amides by hydrolysis in absence of solvent and yields higher than 98.0%. Within the concept of Green Chemistry were prepared six imines: N-benzyl- phenylmethanimine, N-phenyl-2- furylmethanimine, N-phenyl- phenylmethanimine, N-phenyl-(4-methoxyphenyl)methanimine, N-benzyl-(4-methoxyphenyl)metha-nimine,N-(2-furylmethyl)-2-furylmethanimine; two gem-dichloroaziridinas: 2,2-dichloro-1,3-diphenyla-ziridine and 1-benzyl-2,2-dichloro-3-phenylaziridine and two amides: chlorophenylacetanilide and N-benzyl-chloro-phenylacetamide.
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Síntese de potenciais intermediários de princípios ativos, buscando sempre o emprego de técnicas para proteção do meio ambiente / Synthesis of potential intermediaries active, always seeking the use of techniques to protect the environmentLeite, Juliana Aparecida dos Santos 03 December 2012 (has links)
A química verde, que tem a preocupação com o desenvolvimento de tecnologias e processos incapazes de causar poluição, tem sido citada cada vez mais em destaque, pela mídia, como mais uma das iniciativas para prevenção da poluição desenfreada. Neste estudo tem-se buscado a redução ou eliminação de solventes, adaptação dos sistemas reacionais para operação em temperatura ambiente e aumento do rendimento em processos de reações guiados pelos doze princípios da química verde. O objetivo deste trabalho consiste na síntese de intermediários de princípios ativos para uso industrial, através de processos de formação de oximas e oximas éteres. O trabalho foi dividido em duas etapas principais, preparação de oximas e preparação de oximas éteres. Na primeira preparou-se oximas através da reação de aldeídos (benzaldeído, furfuraldeído, salicilaldeído e p-anisaldeído) e cetonas (ciclopentanona, ciclohexanona, metil etil cetona, benzofenona e acetofenona) com cloreto de hidroxilamina, sem a utilização de solventes orgânicos e sem adição de água. Na segunda o objetivo foi preparar oximas éteres (O-butil benzaldeído oxima, O-butil furfuraldeído oxima, N-butoxi-(2-butoxifenil) metanimina, O-butil p-anisaldeído oxima, O-butil ciclohexanona oxima, O-butil ciclopentanona oxima e O-butil metil etil cetona oxima) a partir da alquilação de oximas utilizando um suporte sólido de KF/Al2O3 como catalisador. Todos os compostos foram caracterizados por RMN 13C (apt) e alguns por infravermelho e RMN 1H. / Green chemistry, which is concerned with the development of technologies and processes incapable of causing pollution, has been cited increasingly highlighted, by the media, as another of the initiatives to prevent pollution rampant. This study has sought a reduction or elimination of solvents, reaction to adjust the systems operating at room temperature and yield increase in reactive processes that are guided by the twelve principles of green chemistry. The objective of this work is the synthesis of active intermediates for industrial use, through processes of formation of oximes, oximes ethers. The work was divided into two phases, preparation of oximes and preparation of oximes ethers. In the first was prepared oximes by reaction of aldehydes (benzaldehyde, furfuraldeyde, salicylaldehyde and p-anisaldeyde) and ketones (cyclopentanone, cyclohexanone, methyl ethyl ketone, benzophenone and acetophenone) with hydroxylamine chloride without the use of organic solvents and without adding water. For the second was prepared oximes ethers (O-butyl benzaldheyde oxime, O-butyl furfuraldeyde oxime, N-butoxy-(2-butoxyphenyl) methanimine, O-butyl p-anisaldeyde oxime, O-butyl cyclohexanone oxime, O-butyl cyclopentanone oxime e O-butyl methyl ethyl ketone oxime) from the alkylation of oximes, using a solid support as catalyst KF/Al2O3. All compounds were characterized by 13C NMR (apt) and some infrared and 1H NMR.
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Fibras de Al2O3/GdAlO3 obtidas por fusão a laser para aplicações odontológicas. / Al2O3/GdAlO3 fiber for dental porcelain reinforcement.Medeiros, Igor Studart 16 September 2004 (has links)
O apelo estético da odontologia moderna tem impulsionado a busca por materiais cerâmicos de alto desempenho estético e mecânico. Este trabalho objetivou o desenvolvimento de fibras cerâmicas de alumina/aluminato de gadolínio (Al2O3/GdAlO3) obtidas por meio de fusão a laser (laser heated pedestal growth LHPG) e a sua aplicação como reforço de materiais odontológicos. Os pedestais foram obtidos a partir da mistura dos pós precursores (óxido de gadolínio (Gd2O3) e óxido de alumínio (Al2O3) pré-sinterizados para a obtenção de fibras de Al2O3/GdAlO3 de 0,8 mm de diâmetro médio. Variou-se: a velocidade de puxamento das fibras de 48mm/h a 240mm/h, em pedestais de composição eutética; e em outro grupo a composição dos pedestais (da composição eutética (23 mol% de Gd2O3 e 77 mol% de Al2O3) a 5 % (em peso) de excesso de Al2O3), puxadas com velocidade fixa de 96 mm/h. A melhor condição de obtenção da fibra foi com a velocidade de puxamento de 240mm/h que forneceu fibras com 0,6m de espaçamento médio entre as fases e 1790 MPa de resistência à flexão. Quando as fibras foram aplicadas como reforço de porcelana odontológica houve um aumento da resistência à flexão de 91MPa para 218MPa. Por meio desta metodologia, observou-se que as fibras cerâmica de Al2O3/GdAlO3 apresentaram elevado desempenho mecânico e compatibilidade com porcelanas odontológicas que indicam uma grande potencialidade de uso como reforço estrutural de cerâmicas odontológicas. / The esthetic appeal of modern Dentistry has prompted the search for ceramic materials with high esthetic and mechanical performance. This research aimed at the development of Al2O3/GdAlO3 ceramic fibers, obtained by laser heated pedestal growth (LHPG) and its application as reinforcement of dental materials. Pedestals were obtained from the mixture of precursor powders (Gd2O3 e Al2O3), pre-sintered to form Al2O3/ GdAlO3 fibers with average diameter of 0,8 mm. Variables were: fiber pulling rates (in pedestals of eutectic composition): from 48 mm/h to 240 mm/h; and pedestal composition: from eutectic composition (23 mol% of Gd2O3 and 77 mol% of Al2O3) to 5 wt% of excess Al2O3, pulled at 96 mm/h. The best results were obtained with a pulling rate of 240 mm/h, which originated fibers with average distance between phases of 0.6 m and three-point bending flexural strength of 1790 MPa. When fibers were used as re-enforcement of dental porcelain (Cerabien- Noritake), an increase in flexural strength from 91 MPa to 218 MPa was obtained. The methods employed in this study allowed the observation that Al2O3/GdAlO3 ceramic fibers presented high mechanical performance and compatibility with dental porcelain, indicating a significant potential as re-enforcement of dental ceramics for infrastructure.
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Etude de la passivation de surface du silicium cristallin type P par dépôt de couches atomiques d'alumine pour application aux cellules solaires à haut rendement / P-type crystalline silicon passivation using atomic layer deposition of alumina : application to high efficiency solar cellsPawlik, Matthieu 23 April 2015 (has links)
La diminution du coût ainsi que l'augmentation du rendement des cellules solaires sont devenues les axes principaux de recherche depuis la crise qui a touché le marché du photovoltaïque en 2011. Une des principales stratégies est l’amincissement des cellules solaires dans le but de réduire les coûts des matériaux. Cependant, ceci diminue fortement le rendement de conversion suite à une plus forte influence des défauts structurels et électroniques, présents en surface. Ces défauts peuvent être « passivés » par l’Al2O3 déposé par technique PE-ALD. Ce matériau présente les meilleurs résultats de passivation de surface du silicium cristallin de type p. La couche de passivation nécessite un traitement thermique pour être effective. Ce phénomène se traduit par une augmentation de la durée de vie des porteurs de charge. Cette thèse, encadrée par les deux projets ANR PROTERRA et BIFASOL, ainsi qu’un financement de l’Ecole Centrale de Lille, présente l’optimisation des paramètres de dépôt de la couche de passivation d’Al2O3 ainsi qu’une étude approfondie du phénomène d’activation de la passivation, sur des échantillons avec et sans émetteur. L’analyse de la passivation a été réalisée grâce à des mesures couplées de durée de vie (PCD), électriques (C-V), de potentiel de surface (Sonde de Kelvin) et de spectrométrie (XPS, SIMS). Les sources de la passivation chimique et par effet de champ sont déterminées dans l'empilement Si/SiO2/Al2O3. Le rôle et la dynamique des hydrogènes contenus dans la couche d’alumine sont explicités. L’impact d’une encapsulation par du SiNx ainsi qu’un recuit de diffusion des contacts de 3s à 830°C est étudié / The decrease of solar cell cost as well as the increase in their efficiency are main research topics since the photovoltaic market crisis in 2011. One of the main strategy is to move towards thinner solar cells, in order to decrease raw material consumption. However, the result is a higher impact of surface phenomena on cell characteristics because of a high influence of structure and electronic defects at the surface. These defects can be passivated by Al2O3 coated by PE-ALD (Plasma Enhanced-Atomic Layer Deposition) which has been shown to provide the best surface passivation on p-type silicon. In an as-deposited state, the passivation level of Al2O3 is very low and required an annealing treatment to be "activated". This phenomenon provides an increase of the minority carrier effective lifetime. This thesis founded by the ANR PROTERRA and BIFASOL projects with the financial support of the Ecole Centrale de Lille, focuses on the optimization of the deposition parameters of alumina with a deeper insight on the passivation activation phenomena on samples with and without emitter. The passivation analysis has been performed thanks to coupled lifetime (QSS and micro PCD), surface potential (Kelvin probe), electrical (C-V) and chemical (SIMS, XPS) characterizations. The origin of the chemical and field effect passivation has been determined within the Si/SiO2/Al2O3 stack. The dynamics of the hydrogen contained in bulk alumina is explained. The impact of a SiNx capping layer and a contact alloying anneal at 830°c for 3s is also investigated
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