Šiame darbe sprendžiama struktūrinių intarpų kiekio safyro gardelėje temperatūrinės priklausomybės problema. Darbo apimtis 38 lapai. Darbą sudaro įvadas, dvi dalys, išvados, naudotos literatūros sąrašas ir priedai. Darbe pateikiami 23 paveikslai. Įvade trumpai pateikiama, kodėl pasirinkta ši darbo tema, iškeliama darbo problema, tikslai, uždaviniai ir metodai. Pirmoje dalyje pateikiama teorinė medžiaga, kurioje apžvelgiama kietųjų kūnų klasifikacija, medžiagų struktūra, kristalų defektai, struktūros tyrimo metodai, Brego dėsnio panaudojimas defektų tyrimui Antroje dalyje supažindinama su darbo metodika, prietaisais ir priemonėmis kurios naudojamos atliekant tyrimą. Pateikiami tyrimo rezultatai. Panaudojant minkštosios rentgeno spinduliuotės sukeltą vakansijų generavimą, ateityje galima tikėtis naujų prietaisų gamybos technologijų. Prieduose pateikiama kompaktinė plokštelė. / Temperature dependency on structural interspace quantity of sapphire in grating, is surveyed in this work. The size of the work is 38 pages. The paper consists of an introduction, two major parts, conclusions, a list of bibliography, and appendixes. There are 23 pictures enclosed. The theme, problems, aims, goals, and methods are shortly presented in the introductory part. The first part introduces theoretical material that reviews classification of solid-state, composition agent, defects of crystals, composition research methods, Bregg law use researching defects The second part presents methodology of the work, and devices used in the research. It contains the results of the research. In future using vacancies generation evoked by irradiated soft x-rays the development of the new producing technologies can be hoped. Appendixes contain the CD.

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Recently, the evolutions of wireless communication systems are growing rapidly to satisfy the personal communication requirements. Compact, small size, low cost, easy fabrication, and multi-function are the major developing trends among these modern wireless communication devices. In this research, high quality Al2O3 ceramic materials are used as a substrate to fabricate modifiable dual-mode bandpass filters with the advantages of light weight, small size, and high performance. Dual mode cavity and dielectric resonator filters are the mainstay of satellite communications. In this research, a class generation of planar dual mode filters are introduced which significantly offers the advantages of small size, light weight, and low cost. The proposed bandpass filters are first simulated on Al2O3 (er=9.4) substrate for microwave frequency, and the proposed structures consist one square-typed patch, one circle-typed patch, or one meander-typed patch. Each pattern is connected with two 50£[ microstrip line, one for input and another for output. Two 50£[ microstrip lines are connected to the central of the patch with two notches, and the patch will act as the elliptic-function bandpass filters. Before the fabrication of a bandpass filter, IE3D microwave simulation software is used to simulate the designed filters. With a metal mask, the filter patterns are fabricated on the Al2O3 substrate by using evaporation method. It is found that as the length of notches increase, the three of structures band-pass filters reveal better filtering effect, i.e., the smaller insertion loss (S21), and larger return loss (S11), and the perturbation in the patch facilitates coupling between two orthogonal modes within the resonator, i.e., the perturbation size can modify bandwidth and resonator frequency. After the measurement of the fabricated filters, it is found that the measured results will match the simulated results.

Cette thèse se focalise sur les propriétés passivantes octroyées par des couches minces d’Al2O3 déposées par Atomic Layer Deposition (ALD) à partir de TMA et H2O pour les cellules photovoltaïques en silicium ayant des températures de fabrication inférieures à 400 °C. La première partie de ce travail de doctorat vise à identifier les mécanismes de formation des charges électrostatiques négatives présentes dans l’oxyde d’aluminium. Pour ce faire, les effets de l’illumination post-dépôt (à savoir le flux et l’énergie des photons), ainsi que la température du substrat ont été étudiés. Il a été constaté qu’au moins 70 % de ce qu’on appelle généralement les « charges fixes » sont en fait des charges piégées résultant de l’injection d’électrons du substrat de silicium dans l’oxyde d’aluminium. Par la suite, nous avons étudié l’influence des paramètres de dépôt de l’Al2O3 ainsi que l’impact des traitements post-dépôt sur le piégeage des charges et donc sur les performances passivantes qui en résulte au sein d’un empilement Al2O3/a-SiNX:H déposé sur du silicium cristallin de type p. Les liens entre l’épaisseur de l’Al2O3, la qualité et la durabilité de la passivation ont pu être établis. Le meilleur compromis s’est avéré être aux alentours 60 cycles ALD (~ 6 nm), permettant une durée de vie des porteurs de charges minoritaires allant jusqu’à 4500 μs. La deuxième partie de ce travail doctoral porte sur les mécanismes de dégradation de la passivation. La formation de cloques à l’interface c-Si/Al2O3 est le premier mécanisme de dégradation étudié. Grâce à la microscopie acoustique colorée, la dégradation de l’interface Al2O3/c-Si lors de l’épaississement de l’Al2O3 a été confirmée, mais également lors la réduction de sa température de dépôt, c’est-à-dire en augmentant sa teneur en hydrogène. Une dérive thermique pendant l’ALD (TD-ALD) a été utilisée pour résoudre ce problème de cloquage. L’augmentation continue de la température du substrat pendant le dépôt favorise la libération de l’hydrogène à partir de l’interface c-Si/Al2O3. Pour 60 cycles ALD, le TD-ALD a permis d’augmenter la durée de vie des porteurs de charges jusqu’à 5500 μs. Enfin, l’affaiblissement de la passivation par effet de champ résultant des charges positives dans la couche de protection a-SiNX:H a été mis en évidence par simulation numérique. Les propriétés du a-SiNX:H ont été expérimentalement optimisée grâce à une approche par plan d’expérience. Une nouvelle couche mince d’a-SiNX: H contenant 50 % de charges fixes positives en moins a permis d’obtenir une durée de vie des porteurs de charges de 8800 μs pour 60 cycles de TD-ALD, c’est-à-dire une vitesse de recombinaison de surface exceptionnelle basse de 0,8 cm.s-1. / This thesis focuses on the passivation properties provided by thin Al2O3 films grown by atomic layer deposition (ALD) from TMA and H2O for silicon solar cells having process temperatures lower than 400 °C. The first part of this doctoral work aims at identifying the formation mechanisms of negative electrostatic charges in aluminium oxide. Thus, the effects of post-deposition illumination (namely photon flux and photon energy), as well as substrate temperature were investigated. It was found that at least 70 % of what are generally named “fixed charges” are in fact trapped charges resulting from the injection of carriers from the silicon substrate into the aluminium oxide. From this result, we studied the influence of Al2O3 deposition parameters and post-deposition treatments on charge trapping and resulting passivation performances within an Al2O3/a-SiNX:H stack on p-type c-Si. The dependence of passivation performance (and stability) on Al2O3 thickness has been highlighted. Best compromise has been found to be around 60 ALD cycles (~6 nm), providing a lifetime up to 4500 µs. The second part of this PhD deals with the degradation mechanisms of passivation. Blistering at the c-Si/Al2O3 interface is the first studied degradation mechanism. Thanks to coloured picosecond acoustic microscopy, the Al2O3/c-Si adhesion has been confirmed to be reduced by Al2O3 thickening but also by the reduction of its deposition temperature, i.e. an increase of hydrogen content. A thermal drift during ALD (TD-ALD) has been used to solve this blistering issue. Gradual increase of the substrate temperature during the growth favours the release of hydrogen from the wafer/Al2O3 interface. For 60 ALD cycles, TD-ALD increased the lifetime up 5500 µs. Finally, the weakening of the electrostatic passivation arising from the positive charges in a-SiNX:H capping layer has been underlined by finite element simulations. The a-SiNX:H properties have been experimentally tuned thanks to a design of experiment approach. New a-SiNX:H capping containing 50 % less positive fixed charges resulted in a lifetime of 8800 µs for 60 TD-ALD cycles, i.e. an outstanding surface recombination velocity of 0.8 cm.s-1.

RF magnetron sputtering has been employed to deposit n-type epitaxial zinc oxide thin films on p-type silicon substrates to form p-n diode structures. Commonly found on silicon, native SiOx layers, typically of a few nanometer thick, would hinder the epitaxial growth of ZnO. In this thesis work, a crystalline metal oxide layer was introduced as a buffer layer by redox reaction between a metal layer and the native SiO2. Aluminum was first sputtered for 20 seconds (4 nm), 40 seconds (8 nm), 60 seconds (12 nm) to produce three sets of samples. Each set was then annealed in situ at 450¢J for 20 minutes, 40 minutes, 60 minutes, respectively, to generate 9 different fabrication conditions meant to ignite a redox reaction between aluminum and the silicon oxide. All samples were treated for comparison by rapid thermal annealing to 900¢J, intended to improve the crystalline quality of the buffer layer and thus the epitaxial zinc oxide. Means to characterize the samples included (1) cross-sectional TEM (Transmission Electron Microscopy) observations of the interfaces and defects in various regions of the formed material or device structures; (2) x-ray crystallography via £s-2£c and rocking scans in regards to the perfection of the crystal structures and the relative film-substrate orientations; (3) photoluminescence spectroscopy, which showed oxygen deficiency in the ZnO epitaxial thin films as judged by the peaks of near-edge luminescence and mid-gap impurity states. The resulted material structure is a pin diode with a transparent n-ZnO layer sandwiching in the middle an aluminum oxide insulating layer with the p-Si substrate. The electrically insulating aluminum oxide layer serves to increase the minority carrier accumulation effect, extending carriers¡¦ effective life times and hence enhancing the light emission efficiency. Measuring the current-voltage characteristics of the pin device structures provides insights into the interface charges, while high-frequency capacitance-voltage curves helps give a glimpse of the interfaces between ZnO and Al2O3 or AlOx, as well as those between Al2O3 or AlOx and silicon, all concerning the electronic accumulations at each interface. Keywords: sputtering, ZnO, Al2O3 , pin diode.

The present study aims at studying the surface morphology, crystallinity and optical emission property of Mg added ZnO grown by molecular beam epitaxy. Zn1-xMgxO epitaxial films were first grown at a fixed Zn flux of 1¡Ñ10-7 mbar and Mg flux of 4¡Ñ10-10 to 6.2¡Ñ10-9 mbar on sapphire substrates at 400 oC. The corresponding Mg content (x) is in a range of <0.01 to 0.17. Scanning electron microscopy observations indicated that the surface of the films are flat. The orientation relationship between the film and the substrate is: (0001)Zn1-xMgxO¡ü(0001)Al2O3©M[101 ¡Â0] Zn1-xMgxO¡ü[112 ¡Â0] Al2O3. The full width at half maximum (FWHM) of the (0002) reflection in rocking curve measurement is in a range of 3.83 o to 4.81 o. Photoluminescence results showed that the intensities of both the near band-gap emission and the deep level emission increases with increasing Mg content. The former has FWHM values of 0.16-0.21 eV. While the epitaxial films were grown at a high Zn flux of 5¡Ñ10-7 mbar and Mg flux of 2¡Ñ10-9 to 9.6¡Ñ10-9 mbar on sapphire and LiAlO2 substrates at 400 oC, the film surface are at high roughness. The FWHM of (0002) rocking curve is 4.43 o to 5.71 o for films grown on sapphire and is relatively larger of 6.88 o to 8.18 o for films grown on LiAlO2, respectively. These films possess a stronger near band-gap emission and a lower deep level emission as compared to the films grown at a low Zn flux. After annealed at 600 oC in oxygen or nitrogen, the FWHMs of the (0002) rocking curve for most of the epilayers decreased slightly. The photoluminescence results were rather distinct. For samples having low Mg content (x<0.05), the intensity of the near band-gap emission increases 50-200 ¢H after annealed in oxygen. The intensity of the near band-gap emission did not change but that of the deep level emission decreases ~50 ¢H for the film having x=0.16 after annealing in oxygen. The emission characteristics basically do not change after annealed in nitrogen.

In this thesis, n-type ZnO thin films are grown on buffered p-type Si substrates by RF sputtering. The buffer is a pure nanometer-thick Al layer deposited onto a Si substrate that has a native SiOx over-layer. The Al- layer is meant to react with the native oxide and reduce it back to the pure Si formation when the Al-layer is itself oxidized into AlOx. The pin diodes with ZnO grown on AlOx are expected to outperform those with ZnO on SiOx on the aspects of electrical quality and crystallographic orientations. The transmission electron microscopy was employed to study the epitaxial relationship between the ZnO layers and the Si substrates, the crystal structure, and defects at the ZnO-Al or Al-SiOx interfaces. X-ray diffraction studies through £s-2£c, rocking curve, GIXRD and pole-figure scans were also conducted to see the differences between as-deposited and post-annealing treated samples concerning with the ZnO crystallographic orientations and general qualities. Through comparisons of the leakage current and the tunneling behaviors , the electrical measurements can be used to analyze the pin devices.

Nanoscaled-Al2O3 particles reinforced 1050 Aluminum composites by FSP were successfully fabricated in this study. The grain size of 1050 aluminum was obviously refined to about 0.5£gm by friction stir process(FSP), and there was a tendency that grain size decreased with increasing of Al2O3 content, where grain size of 0.84£gm was achieved with 24.7vol% of Al2O3. Nanoscaled-Al2O3 particles reinforced 1050 Al alloy by FSP revealed an excellent strengthening effect and excellent ductileity, Where hardness and UTS of the composite with 24.7vol% nanoscaled-Al2O3 particles were increased up to Hv113 and 310MPa respectively. The tensile result showed a 400% of increase in UTS comparing to the pure Al after FSP.

Made available in DSpace on 2014-12-17T15:41:54Z (GMT). No. of bitstreams: 1 JoaoPCE_DISSERT.pdf: 3180656 bytes, checksum: 4103bde23e39119f96e6397a04b288a2 (MD5) Previous issue date: 2011-02-25 / Conselho Nacional de Desenvolvimento Cient?fico e Tecnol?gico / This study proposes to find a biodiesel through transesterification of rice bran oil with KI/Al2O3 checking the influence of two types of alumina (Amorphous and Crystalline) for conversion into methyl esters. The catalyst was synthesized by the wet impregnation method. Adding 30 mL of 35% KI(aq.) in 10 g of alumina, under stirring at 80 ?C for 3 hours. The reaction conditions used in this study were optimized, with a molar ratio methanol:oil of 15:1, 8 h of reaction time and reflux temperature. The catalyst amount was varied in the range of 1 to 5 % wt. The solid catalysts materials were analyzed by: x-ray diffraction (XRD), thermogravimetry (TG), N2 adsorption/desorption, scanning electron microscopy (SEM) and basicity, for the identification of its structure and composition, verifying the presence of basic sites. The results showed that Al2O3(A) presents an amorphous structure, high surface area and a better catalytic activity, in relation to the catalyst synthesized with Al2O3(C) support that proved to have a more crystalline structure, having as well, a lesser surface area, enabling difficulties for the incorporation of active sites. The obtained biodiesel with 5% wt. KI/Al2O3(A) presented physicochemical properties within the standards specified by the Resolution No 7/2008 ANP and obtained the best reaction yield with 95.2%, according to quantitative measurement from the TG, which showed 96.2% conversion into methyl esters. It was furthermore found that with the increasing amount of the quantity of the catalyst in the reaction, there was also an increase in the ester content obtained. The specific mass and the kinematic viscosity were reduced with the increase of the amount of quantity of the catalyst, indicating an increase in the conversion of triglycerides / Esse estudo prop?e-se a obter um biodiesel a partir da transesterifica??o do ?leo de farelo de arroz com KI/Al2O3 verificando a influ?ncia de dois de tipos de alumina (Amorfa e Cristalina) na convers?o em ?steres met?licos. O catalisador foi sintetizado pelo m?todo de impregna??o via ?mida. Adicionando 30 mL de uma solu??o de 35% KI(aq.) em 10 g de alumina, sob agita??o constante a 80?C por 3h. As condi??es reacionais utilizadas nesse estudo foram otimizadas, como raz?o molar de metanol:?leo de 15:1, tempo reacional de 8hs e temperatura de refluxo. A quantidade de catalisador foi variada na faixa de 1 a 5% wt. Os materiais s?lidos catal?ticos foram analisados por: difra??o de raios-X (DRX), an?lise termogravim?trica (TG/DTG), adsor??o/dessor??o de nitrog?nio, microscopia eletr?nica de varredura (MEV) e teste de basicidade para identifica??o da estrutura e sua composi??o, verificando a presen?a de s?tios b?sicos. Os resultados mostraram que Al2O3(A) apresenta uma estrutura amorfa, alta ?rea superficial e uma melhor atividade catal?tica em rela??o ao catalisador sintetizado com o suporte Al2O3(C) que mostrou-se uma estrutura mais cristalina, menor ?rea superficial, dificultando a incorpora??o dos s?tios ativos. O biodiesel obtido com 5% wt. KI/Al2O3(A) apresentou propriedades f?sico-qu?micas dentro das normas especificadas pela resolu??o N?7/2008 da ANP e o melhor rendimento da rea??o com 95,2%, em conformidade com a medida quantitativa a partir da TG, que exibiu 96,2% de convers?o em ?steres met?licos. Foi verificado que com o aumento da quantidade de catalisador na rea??o, aumenta o teor de ?steres obtidos. A massa espec?fica e a viscosidade cinem?tica foram reduzidas com o aumento da quantidade de catalisador, indicando um aumento na convers?o dos triglicer?deos

Made available in DSpace on 2014-12-17T15:41:58Z (GMT). No. of bitstreams: 1 JulioCTS_DISSERT.pdf: 2360843 bytes, checksum: 9fc8ef936717b3177303c0d0bd2e0718 (MD5) Previous issue date: 2012-04-19 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / It is known that the head office world energetics is leaning in the fossil fuels. However, the world panorama is changing quickly, for linked reasons to three of the humanity's great concerns in that century beginning: environment, global economy and energy. The biodiesel production is based on the transesterifica??o of vegetable oils or animal fats, using catalysts homogeneous or heterogeneous. The process of heterogeneous transesterifica??o presents lower conversions in comparison with the homogeneous, however, it doesn't present corrosion problems and it reduces to the occurrence of parallel reactions as saponification. In this sense, this work has for purpose the synthesis of a heterogeneous catalyst, KNO3/Al2O3, that soon afterwards was used in the reaction of transesterifica??o of the oil of the Helianthus annuus L. (sunflower). The solid materials (it supports and catalyst) they were analyzed by diffraction of ray-X (XRD) and electronic microscope of sweeping (MEV). After the analysis of Al2O3, a structure monophase amorphous tetragonal was verified, with characteristic patterns of that material, what could not be visualized in the difratograma of the catalyst. The biodiesel obtained with 4% wt. of KNO3/Al2O3 it was what obtained a better cinematic viscosity 8,3 mm2/s, comparing with the norms of ANP, and it also presented the best conversion tax in ethyl ?steres, in accordance with the quantitative measure starting from TG, that was of 60%. While the biodiesel with 6% wt. and with 8% wt. of KNO3/Al2O3 it was it that no transesterificou, because it was observed in the analysis termogravim?trica of those two materials, a single thermal event, that it corresponds the decomposition or volatilization of the triglycerides / Sabe-se que a matriz energ?tica mundial est? apoiada nos combust?veis f?sseis. No entanto, o panorama mundial est? mudando rapidamente, por motivos ligados a tr?s das grandes preocupa??es da humanidade nesse in?cio de s?culo: meio ambiente, economia global e energia. A produ??o de biodiesel ? baseada na transesterifica??o de ?leos vegetais ou gorduras animais, utilizando catalisadores homog?neos ou heterog?neos. O processo de transesterifica??o heterog?nea apresenta convers?es mais baixas em compara??o com o homog?neo, por?m, n?o apresenta problemas de corros?o e reduz ? ocorr?ncia de rea??es paralelas como saponifica??o. Neste sentido, este trabalho tem por finalidade a s?ntese de um catalisador heterog?neo, o KNO3/Al2O3, que em seguida foi utilizado na rea??o de transesterifica??o do ?leo da Helianthus annuus L.(girassol). Os materiais s?lidos (suporte e catalisador) foram analisados por difra??o de raios-X (DRX) e microsc?pio eletr?nico de varredura (MEV). Ap?s a an?lise da Al2O3, foi constatada uma estrutura monof?sica tetragonal amorfa, com padr?es caracter?sticos desse material, o que pode ser visualizado no difratograma do catalisador. O biodiesel obtido com 4% m/m de KNO3/Al2O3 foi o que obteve uma melhor viscosidade cinem?tica 8,3 mm2/s, comparando com as normas da ANP, e tamb?m apresentou a melhor taxa de convers?o em ?steres et?licos, em conformidade com a medida quantitativa a partir da TG, que foi de 60%. Enquanto o biodiesel com 6% m/m e com 8% m/m de KNO3/Al2O3 foi o que n?o transesterificou, pois foi observado na an?lise termogravim?trica desses dois materiais, um ?nico evento t?rmico, que corresponde a decomposi??o ou volatiliza??o dos triglicer?deos