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Laser welding was investigated as a potential joining technology for alumina ceramic substrates. The objective of this study was to develop a method to preheat the ceramic using a single defocused laser beam prior to welding. Engineering ceramics are employed in a variety of systems and environments due to their unique properties. Joining technologies must be developed to facilitate the manufacture of complex or large ceramic components. Laser welding is advantageous as it forms joints rapidly, and does not introduce intermediate materials to form the bond, which can have deleterious effects. The Laser Machining System (LMS) at Queen’s University was adapted for this study. A defocused far-infrared (FIR) laser beam was positioned to overlay a focused near-infrared (NIR) laser beam; the defocused FIR beam preheated the ceramic substrate and the focused NIR beam formed the weld. A finite element model was developed in COMSOL MultiPhysics to simulate the preheating processes and to develop a preheating protocol. The protocol was implemented using the FIR beam and adjusted to achieve preheating temperatures of 1450, 1525, and 1600degC. Welds were performed on 1 mm thick alumina plates using the preheating protocols and NIR beam powers of 25, 50, and 75 W. Weld speed was held constant throughout the study at 0.5 mm/s. The preheating protocols were successful at achieving near-constant preheating temperatures, with standard deviations below 32 degrees. Partially penetrating welds were formed with the NIR beam at 25 W, and fully penetrating welds at 50 and 75 W. Large pores were present in the 25 W and 50 W welds. Minimal porosity was observed in the welds formed at 75 W. All of the welded plates experienced a transverse fracture that extended perpendicular to weld, and a longitudinal fracture extending parallel to the weld. This study shows that a fixed defocused laser beam can successfully preheat alumina substrates to the high temperatures required for welding; however, non-homogenous cooling results in fracture. Increasing the preheating beam diameter or introducing an auxiliary means to provide a controlled cool-down cycle may mitigate these effects. / Thesis (Master, Mechanical and Materials Engineering) -- Queen's University, 2013-04-29 17:59:57.43

OBJECTIVES: To investigate the effect of different alumina fabrication techniques and sintering temperatures on the biaxial flexural strength. Also, to assess the resulting color of multiple metal salt solutions at different concentrations in monolithic alumina and its effect on the optical properties of the restoration. MATERIAL & METHOD: Forty disk-shape alumina specimens were divided into 4 groups (n=10) based on the fabrication process (slip cast or die press) and sintering temperature (1530°C or 1600°C). Biaxial flexural strength was calculated using universal testing machine at a crosshead speed rate of 0.5 mm/min until failure occurred. For the coloring part of the study, nine elements (Ba, Ce, Cr, Fe, Mn, Nd, Pr, Sm, Zn) were used to form metal-salt coloring solutions at a concentration of 0.1%, 1% and 5% wt. The solutions were then used to infuse 162 pre-sintered porous alumina disks that are either slip-casted (A1000) or die-pressed (CT3000). Color coordinates were recorded in CIE L*a*b* system using spectrophotometer. Color differences relative to the control (ΔE), translucency parameter (TP), contrast ratio (CR) and total transmission were calculated and analyzed using two-way analysis of variance (ANOVA) with Tukey post hoc test at α = 0.05. RESULTS: Slip cast group sintered at 1530°C had the highest flexural strength (479.14 MPa), but there was no significant difference between the four groups neither by fabrication process (p = 0.127) nor by sintering temperature (p = 0.276). Die press specimens colored with Ba at 0.1% and 1% showed significantly higher TP (2.65 and 2.49) and lowest CR (96.15 and 96.30) among the groups. There was a statistically significant effect on TP and CR when changing alumina powder on specimens colored by Ba, Ce, and Zn (p < 0.05). Changing the concentration of the coloring solution caused a significant effect on the optical properties of specimens colored by Ba, Nd, Cr, Mn. ΔE was significantly changed when changing alumina powder and coloring concentration for all elements except Ce, Pr, and Sm. CONCLUSION: Changing fabrication method and sintering temperature did not affect the biaxial flexural strength. However, the fabrication method and metal-salt colorant concentration affected the optical properties of the specimens. / https://hdl.handle.net/2144/35681

Neste trabalho, a formação da fase AlNbO4 no sistema (x Al2O3 + 1-x Nb2O5) foi estudada por técnicas de difração de raios X e microscopia eletrônica. 0; 0,15; 0,5; 2 e 4% m/m de Nb2O5 foram incorporados em Al2O3-α e sinterizados a 1400, 1500 e 1600°C durante 60 min a uma taxa de aquecimento de 2,5°C.min-1. Os sinterizados foram analisados por difração de raios X, tendo o ajuste dos picos de difração e as fases formadas quantificadas pelo Método de Rietveld. Os materiais produzidos também foram analisados por microscopia eletrônica de varredura tendo a composição química de pontos específicos da amostra analisada por espectroscopia de raios X por dispersão de energia. Mapas de raios X característicos e perfis de composição química microestrutural também foram analisados por espectroscopia por dispersão de comprimento de onda através de microssonda eletrônica. Detalhes da microestrutura foram escolhidos para uma investigação mais aprofundada e removidos da microestrutura original por meio de feixe de íons localizados e analisados por microscopia eletrônica de transmissão de alta resolução. Os resultados mostraram que uma fase de origem não identificada se formou a partir da adição de 0,15% m/m de Nb2O5 em Al2O3-α e que a fase estável do sistema, AlNbO4 foi verificada por difração de raios X a partir de 0,5% m/m de Nb2O5 Também se verificou que todo o Nb2O5 foi consumido durante a sinterização das amostras. Os ajustes dos picos de difração pelo Método de Rietveld permitiram concluir que não existem distorções significativas na rede cristalina da Al2O3-α e que nenhum vestígio de solubilidade do Nb na Al2O3-α foi observado. O AlNbO4 pôde ser quantificado pelo Método de Rietveld apenas para as amostras contendo 2 e 4% m/m de Nb2O5, excluindo-se do refinamento os picos da fase de origem não identificada. As análises por microscopia eletrônica de varredura mostram que com o aumento do teor de Nb2O5 incorporado há um aumento de fase intergranular no sinterizado. Mostra, também, que o Nb2O5 atua como agente de sinterização da Al2O3-α favorecendo o aumento de seus grãos e de sua densificação. A análise por microscopia eletrônica de transmissão de alta resolução mostrou que a região de interesse e a região de interface possuem orientações cristalográficas distintas. O padrão de difração de elétrons desta região mostrou que a mesma possui estrutura monocristalina e está associada à fase AlNbO4. Mostrou, ainda, que esta região monocristalina está em uma matriz com orientação distinta e que nesta orientação puderam ser verificadas distâncias interplanares correspondentes às distâncias interplanares dos picos de origem não identificada. / In this work, the AlNbO4 phase formation in the system (x Al2O3 + 1-x Nb2O5) was studied by X-ray diffraction and electron microscopy techniques. 0; 0.15; 0.5; 2 and 4 Nb2O5 wt% were added in α-Al2O3 and sintered at 1400, 1500 and 1600°C for 60 min using a heating rate of 2.5°C.min-1. The sintered samples were analyzed by X-ray diffraction, with the adjustment of the diffraction peaks and the formed phases quantified by Rietveld Method. The samples were also analyzed by scanning electron microscopy and the chemical composition of specific points of the sample analyzed by energy dispersive X-ray spectroscopy. Characteristic X-ray maps and microstructural chemical composition profiles were analyzed by wavelength dispersion spectroscopy through an electron microprobe. Details of the microstructure were chosen for further investigation and removed from the original microstructure by focused ion beam system and analyzed by high resolution transmission electron microscopy. The results showed that an unidentified phase was formed when 0.15 Nb2O5 wt% were added in α-Al2O3 and that the stable phase of the system, AlNbO4 was verified by X-ray diffraction after the addition of 0.5 Nb2O5 wt% It was also found that all Nb2O5 was consumed during the sintering of the samples. Adjustments of the diffraction peaks by Rietveld Method allowed to conclude that no significant distortions in the α-Al2O3 crystalline lattice were observed and that no trace of Nb solubility in α-Al2O3 was verified. AlNbO4 could be quantified by Rietveld Method only for samples containing 2 and 4 Nb2O5 wt%, after excluding the peaks of the unidentified phase. The scanning electron microscopy analysis shows that the increase of the incorporated Nb2O5 content increases the intergranular phase in the sintered samples. It also shows that Nb2O5 acts as a sintering agent for α-Al2O3 favoring the increase of its grains and its densification. High resolution transmission electron microscopy showed that the interest region and the interface region have different crystallographic orientations. The electron diffraction pattern of this region showed a monocrystalline structure and it was associated to the AlNbO4 phase. It also showed that the monocrystalline region is in a different orientation matrix and in this orientation, interplanar distances corresponding to the interplanar distances of the unidentified peaks could be verified.

Made available in DSpace on 2014-06-12T17:38:40Z (GMT). No. of bitstreams: 2 arquivo4087_1.pdf: 3717955 bytes, checksum: c558abb160a867b5f16716ff3c05269c (MD5) license.txt: 1748 bytes, checksum: 8a4605be74aa9ea9d79846c1fba20a33 (MD5) Previous issue date: 2011 / Faculdade de Amparo à Ciência e Tecnologia do Estado de Pernambuco / O petróleo bruto é uma substância altamente corrosiva, por isso, provoca rápida degradação das superfícies metálicas com as quais tem contato direto, como no caso de tanques de armazenamento e transporte desse material. Dessa forma, uma alternativa para solucionar esse problema é utilizar um tipo de revestimentos inerte a essa corrosão. Materiais cerâmicos geralmente apresentam essa característica e podem ser uma opção de material para esse revestimento. Esse estudo é de suma importância, pois com a abertura da refinaria de petróleo no estado de Pernambuco, a necessidade de armazenar e transportar petróleo cru irá crescer e com isso serão necessárias formas de transporte e armazenamento que sejam resistentes a corrosão provocada por esse petróleo. Nesse sentido é importante investigar novos materiais cerâmicos de alto desempenho que sejam inertes a corrosão e que possam ser utilizados como revestimentos para tanques. Neste contexto, o trabalho destina-se ao processamento e caracterização de compósitos cerâmicos, através da produção de peças com matriz metálica, e posterior análise de viabilidade na aplicação, por processos adequados, em tanques e tubulações em escala laboratorial, revestidas com as cerâmicas Al2O3-ZrO2 variando entre 5 a 20% (em peso) de ZrO2, com aditivos de óxido de terra rara CeO2 e a avaliação do desempenho em condições reais de petróleo cru oriundo de diferentes poços de petróleo do nordeste. O objetivo deste trabalho é estudar materiais intrinsecamente suscetíveis à fratura devido a sua pouca deformação plástica e destina-se ao desenvolvimento e caracterização de compósitos cerâmicos alumina-zircônia-céria compatíveis ao problema em questão. As cerâmicas foram produzidas por reação em estado sólido e sinterizadas de maneira direta (1200ºC à 1400ºC) num intervalo de até 24hrs e produzidas por processo; de moagem, termo-mecânico, e tratamentos térmicos em proporções adequadas. A caracterização estrutural e microestrutural foi realizada por método de difração de raio-X (DRX) e microscopia eletrônica de varredura (MEV). As propriedades mecânicas foram avaliadas por ensaios de densidade e dureza Vickers (HV). Na fase final foi avaliado o desempenho do revestimento em petróleo cru. Os resultados das propriedades mecânicas encontradas em 0,20 de ZrO2 se mostram superiores aos outros analisados, mostrando-se mais adequados a aplicação em questão

Orientador: Elidiane Cipriano Rangel / Banca: José Humberto Dias da Silva / Banca: Adriana de Oliveira Delgado Silva / Resumo: Filmes de alumina foram depositados a partir de um nova metodologia de deposição a plasma, utilizando o pó de acetilacetonato de alumínio (AAA) como precursor. Em trabalho prévio do grupo, foi demonstrada a viabilidade do sputterring do AAA em plasma de argônio para deposição de filmes finos. Os bons resultados obtidos estimularam o desenvolvimento do presente trabalho, visando a aperfeiçoamento da metodologia de deposição. Para isso, primeiramente foram investigados os efeitos da alteração da composição química da atmosfera do plasma, por meio da incorporação de diferentes proporções de oxigênio (02%) ao argônio, tornando o processo em sputtering reativo. As deposições foram realizadas espalhando-se o pó do AAA no eletrodo inferior de uma sistema de plasma acoplado capacitivamente. Argônio, oxigênio ou mistura de ambos foram admitidos até a pressão de 11,0 Pa. O plasma foi gerado pela aplicação de sinal de radiofrequêcia (13,56 MHz, 150 W) ao eletrodo contendo o pó, mantendo-se o eletrodo superior, também utilizando como porta-amostras, aterrado. O tempo de deposição foi de 90 minutos. Investigou-se o efeito da O2%, variada de 0 a 100% nas propriedades dos filmes. Na etapa subsequente, filmes foram depositada por sputtering reativo utilizando-se a condição considerada ótima na última etapa do trabalho (02% = 25%) e mantendo-se as condições de pressão, potência e tempo de tratamento constantes. Todavia, ao invés de aterrar o porta-amostras, pulsos retangulares negativos (600 V, 2 kHz, 1-100% de ciclo dos trabalho) foram aplicados, promovendo bombardeamento iônico durante a deposição por sputtering reativo. O efeito de ciclo de trabalho dos pulsos nas propriedades dos filmes foi avaliado. Na última etapa do trabalho, filmes foram depositadas pelo sputtering reativo a partir de atmosferas contendo 25% de O2 e 75% de Ar e em condições mais... (Resumo completo, clicar acesso eletrônio abaixo) / Abstract: Alumina films were deposited by a new plasma deposition method using aluminum acetylacetonate (AAA) powder as precursor. In a previous study by our group, the feasibility of AAA sputtering in argon plasmas for thin films deposition was demonstrated. The good results stimulated the development of this work, aiming at the improvement of the deposition methodology. For this, the effects of modification in the chemical composition of the plasma atmosphere were first investigated, through the use of different oxygen to argon proportions (O2%), making the process a reactive sputtering. The deposition were performed by spreading the AAA powder on the lower electrode of a capacitively coupled plasma system. Argon, oxygen or a mixture of both were admitted up to a pressure of 11.0 Pa. Application of radiofrequency power (13.56 MHz, 150 W) to the powder covered electrode generated the plasma, keeping the upper electrode, also used as a sample holder, grounded. Deposition times of 90 minutes were used. The effects of varying the oxygen proportion from 0 to 100% on the film properties were studied. In the subsequent stage, films were deposited by reactive sputtering using the condition considered best in the stage of the work (O2%=25%) and keeping the pressures, power and treatment time constant. Instead of grounding the sample holder, however, negative rectangular pulses (600 V, 2 KHz, 1-100% duty cycle) were appliedm promoting ion bombardment during the deposition by reactive sputerring. The influence of the pulse duty cycle on the properties of the films was evaluated. In the last study stage, films were deposited by reactive sputtering from atmspheres containing 25% O2 and 75% Ar and with more energetic conditions than those used in previous cycles. For such, a first samples set was prepared by resistive heating of the sample holder (410ºC) in a lower plasma pressure (4,0 Pa) than that previously used... (Complete abstract electronic access below) / Mestre

In this work cis-inositol, epi-inositol and myo-inositol carbonate were successfully synthesised and used for coordination studies. The preparation of cis-inositol was achieved by reduction of tetrahydroxybenzoquinone via hydrogenation with palladium hydroxide as the catalyst and was purified by chromatographic separation using Dowex resin. The synthesis of epi-inositol was achieved by the nitric acid oxidation of myo-inositol to form epi-inosose which was subsequently reduced by hydrogenation using palladium hydroxide as the catalyst. myo-Inositol was converted into its mono-orthoformate derivative and the equatorial hydroxy group was then protected as a tertiary-butyldimethylsilyl ether. The carbonate group was introduced onto this protected inositol and then the protecting groups were removed by acid hydrolysis. The coordination characteristics of four inositols, viz cis-inositol, epi-inositol, myo-inositol and myo-inositol carbonate with calcium, aluminium, gallium, lanthanum and samarium ions have been investigated. Interactions of the aluminate anion with epi-inositol and myo-inositol in deuterated sodium hydroxide were also investigated. Three methods were used in the study of complexation behaviour of these systems. namely, [superscript]13C NMR spectroscopy, HPLC and ion exchange chromatography. [superscript]13C NMR spectroscopy was found to be most useful for determining possible complexation behaviour of the inositols. Chemical shift changes of the resonance signals in the [superscript]13C NMR spectra on sequential addition of cations to solutions of the inositols at near neutral pH, have led to determination of possible coordination sites of the inositols. In general, large induced chemical shift changes have been interpreted to signify strong cation-inositol interaction at specific hydroxy groups. / Triaxial sites of the inositols have shown a preference to coordinate small ions with ionic size of at least 60 pin, smaller ions than this displayed very weak interactions. Likewise large ions (90-100 pm) imparted weak interactions on triaxial sites of the inositols. These large ions coordinated well with the axial-equatorial-axial sites of the inositols although it was observed that calcium ions appeared to form a 2:1 ligand:cation complex with cis-inositol at the triaxial site despite being a large cation (100 pm). The detection of complex formation by HPLC showed a possible formation of very stable complexes of epi-inositol complexes with calcium ions. However, a change of refractive index of the solution on sequential addition of the cation may have caused an interference in the results such that direct interpretation was not possible. Ion exchange chromatography provided the quickest guide on how strongly the inositols interact with a particular cation. However, determination of complex stoichiometry and or structure was not possible using this technique.

The AAO membrane with nanopore arrays were fabricated by anodizing highly pure aluminum foils (99.9995%) in electrolyte. Ordered array have been obtained under optimized anodizing condition, and pore diameter can be controlled by different anodic voltage and electrolyte. After we got such an ordered arrangement porous alumina array, the following analysis of the material optical properties were characterized. Photoluminescence measurements showed a strong PL peak in blue. The PL peak was 420nm excited by He-Cd laser. From the transmittance spectra, the results showed that material was transparent above 400nm. The XRD spectra of AAO without and with annealing, both showed the diffraction peaks of (311)¡B(400)¡B(440), corresponding to the £^-Al2O3 phase appear. High ordered anodic porous alumina with holes interval 65nm was prepared in mixture solution of H3PO4 and H2SO4 under high temperature and high concentration. Through the use of porous anodic alumina masks, nanopore arrays were fabricated on Si¡BGaAs substrates by reactive ion etching. Also, metal nanodot arrays were formed through the AAO mask by evaporation. Thin AAO slabs also enhance the light extraction from the QDs, and control the PL emission wavelength.