No description available.

No description available.

No description available.

Three types of polycrystalline aluminum oxide, with varying amounts of impurities, were tempered and then annealed to study the behavior of residual stress relaxation. Results from microprobe analysis, thermal expansion analysis, annealed strength measurements, and scanning electron fractography clearly indicate stress relaxation at annealing temperatures occurred by elastic creep through crack nucleation and growth in regions under tensile stresses. From the scanning electron fractographs, it was found that intergranular glassy phase played an important role in the crack formation and propagation. At elevated temperature, viscous intergranular glassy phase behaved as an adhesive layer and when under tensile stresses caused de-adhesion of grain-boundaries or the formation of cracks. Fine-grained aluminas, with little or no glassy phase, exhibited both sub-critical and critical crack propagation. Since cracks decrease the load-carrying ability of the aluminas, it was concluded that by minimizing the glassy phase, porosity, grain size and residual stresses one can suppress crack formation. / Master of Science

Call number: LD2668 .T4 1986 C64 / Master of Science / Chemical Engineering

Grinding is a critical manufacturing process and is often the only alternative when producing precision components or when machining brittle materials such as ceramics. Characterizing and modeling the surface finish in the grinding process is a difficult task due to the stochastic nature of the size, shape and spatial distribution of abrasive grains that make up the surface of grinding wheels. Since the surface finish obtained in grinding is a direct function of the wheel surface topography, which is conditioned by a single point dressing process, understanding the effects of dressing parameters on the wheel topography is essential. Therefore, the main objectives of this thesis are: 1) to experimentally characterize the three-dimensional surface topography of a conventional grinding wheel including attributes such as the abrasive grain height distribution, grain geometry and spacing parameters and their respective statistical distributions, 2) to determine the effects of single point dressing conditions on the three-dimensional wheel surface topography parameters and their distributions, 3) to model and simulate the three-dimensional wheel surface topography, and 4) to experimentally validate the wheel topography model. In this research, new and existing characterization methods are used to characterize the wheel surface and the individual abrasive grains. The new techniques include the use of X-ray micro-tomography (μCT) to obtain a better understanding of the grinding wheel's internal micro-structure, and a focus variation based optical measurement method and scanning electron microscopy to characterize previously ignored attributes such as the number of sides and aspect ratio of individual grains. A seeded gel (SG) vitrified bond conventional grinding wheel is used in the study. A full factorial design of single point wheel dressing experiments is performed to investigate the effects infeed and lead dressing parameters on the grinding wheel surface topography. A custom wheel indexing apparatus is built to facilitate precision relocation of the grinding wheel surface to enable optical comparison of the pre- and post-dressing wheel surface topography to observe wheel surface generation mechanisms such as macro-fracture and grain dislodgement. Quantitative descriptions of how each dressing parameter affects the wheel surface characteristics are given in terms of the wheel surface roughness amplitude parameters (Sp, Ssk, Sku) and areal and volume parameters (Spk, Sk, Vmp, Vmp, Vvc, Smr1) derived from the bearing area curve. A three-dimensional wheel topography simulation model that takes as input the abrasive grain height distribution and the statistical distributions for the various abrasive grain geometry parameters is developed and experimentally validated. The results of wheel characterization studies show that the actual abrasive grain height distribution in the SG wheel follows a beta distribution. The μCT work shows that the abrasives are polyhedral in shape, as opposed to the spherical or conical shapes commonly assumed in grinding literature. Grain spacing is found to follow a beta distribution while the number of sides of the grain and the grain aspect ratio are found to follow the gamma and the Weibull distribution, respectively. The results of the dressing study show that the lead dressing parameter has the strongest effect on wheel topography. Using statistical distributions for the key parameters (e.g. grain height, number of sides, grain spacing), a stochastic three-dimensional model is developed to simulate the wheel surface topography under different dressing conditions. The resulting model is shown to yield realistic results compared to existing models mainly due the fact that additional abrasive grain geometry parameters and more realistic assumptions of the different grain attributes are used in the model. It is shown that the model follows the overall wheel surface topography trends during dressing but has difficulty in accurately simulating some of the wheel characteristics under specific dressing conditions. The thesis then concludes with a summary of the main findings and possible future research avenues including extending the model to rotary dressing and simulation of wheel-workpiece interaction.

Corundum ou safira (α − Al2O3) é um importante material tecnológico, utilizado em inúmeras aplicações ópticas e eletrônicas e, mais recentemente, como um sensor de radiação para baixas doses e aplicações de curta exposição. Os dosímetros em estudo são provenientes da Landauer Crystal Growth Facility (Stillwater, EUA). Trata-se de fitas multicamadas, onde o material cerâmico Encontra−se aprisionado entre duas camadas de um material polimérico. O processo de recuperação do óxido de alumínio contido nestes sensores, pré − definido, é realizado na empresa SAPRA S⁄A. Este trabalho envolve a caracterização dos materiais que compõem o dosímetro e, principalmente, a caracterização do produto final obtido, verificando se ocorreram mudanças em suas propriedades dosimétricas após passar por todo o processo. Desta maneira, este estudo está voltado para a recuperação do Al2O3 a nível de processo industrial, visando a obtenção de um produto que conserve suas características estruturais e que mantenha suas propriedades dosimétricas / Corundum or sapphire (α − Al2O3) is an important technological material in many optical and electronic applications and, more recently, as a radiation detector. Dosimeters are provided by Landauer Crystal Growth Facility (Stillwater, USA) which consist of a multilayer tape made out mainly of an aluminum oxide layer enfolded by two layers of a polymeric material. The recovering process of the aluminum oxide is undertaken by Sapra S⁄A. This work comprises the characterization of the constituent material of the dosimeter, especially the final product, concerning to the possible change that could occur in the dosimetry properties after the recuperation process of the aluminum oxide. Therefore, this work is looking forward a industrial recovering process which assures a good quality of the final product

"Recently, nanomaterials have been vigorously studied for the development of biosensors. Among them, carbon nanotubes (CNTs) have stimulated enormous interest for constructing biosensors due to their unique physical and chemical properties such as high surface-to-volume ratio, high conductivity, high strength and chemical inertness. Our study is to develop a general design of biosensors based on vertically aligned CNT arrays. Glucose biosensor is selected as the model system to verify the design of biosensors. In the preliminary design, glucose oxidase (GOx) is attached to the walls of the porous alumina membrane by adsorption. Porous highly ordered anodized aluminum oxide (AAO) prepared by two-step anodization are used as templates. Deposited gold on both sides of template surfaces serve as a contact and prevent non-specific adhesion of GOx on the surface. In order to find out optimized thickness of gold coating, the oxidation and reduction (redox) reaction in [Fe(CN)6]3¨C /[Fe(CN)6]4¨C system is monitored by Cyclic Voltammetry (CV). Subsequently, enzymatic redox reaction in glucose solutions is also attempted by CV. We expect protein layers with GOx form a conductive network. However, no obvious enzymatic redox reaction is detected in the voltammogram. To take advantage of the attractive properties of CNTs, the design of enzyme electrodes is modified by attaching CNT onto the sidewalls of AAO template nanopores and then immobilizing GOx to the sidewalls and tips of CNTs. AAO templates provided vertical, parallel, well separated and evenly spacing nanochannels for CNT growth. Cobalt is used as a catalyst to fabricate CNTs. As a result, multi-walled carbon nanotubes (MWCNTs) are fabricated inside the AAO templates by catalytic chemical vapor deposition (CCVD). Characterization of AAO templates and cobalt electrochemical deposition are employed by scanning electron microscope (SEM), and energy dispersive X-ray spectrometry (EDS). Detailed structure and texture of CNTs are examined by transmission electron microscope (TEM). "

Revestimentos de máquinas e equipamentos industriais sofrem desgastes consideráveis por abrasão, impacto e ataque químico, o que torna necessária frequente parada de produção para ações de manutenção. Esta situação motiva o desenvolvimento de materiais de maior resistência a estas solicitações. A adição de óxidos de zircônio e cério em compostos à base de alumina tem demonstrado a capacidade de aumentar as propriedades mecânicas deste tipo de cerâmica, tornando estes materiais promissores candidatos ao uso em maquinário industrial. Neste contexto, o objetivo deste trabalho foi o estudo da influência da adição de diferentes teores, 25, 30 e 35% de zircônia parcialmente estabilizada com 14% de céria (ZPEC) em compósitos à base de alumina. Para obtenção destes compostos, óxido de alumínio, óxido de cério e óxido de zircônio foram misturados em moinho de bolas e conformados por prensagem isostática a frio, seguido de secagem e sinterização entre 1300 e 1600°C. As propriedades físicas, químicas e mecânicas dos materiais após a sinterização foram avaliadas por ensaios porosidade aparente, densidade relativa, retração linear de queima, dureza Vickers, resistência à flexão em 4 pontos e ao choque térmico, e tenacidade à fratura (KIc). Os materiais investigados apresentaram densificação na faixa de 94,3% a 95,75% da densidade teórica para a temperatura de sinterização de 1600°C, e estes valores aumentaram com aumento do teor de ZPEC. Estes compósitos apresentaram uma melhora de 23% na resistência à flexão em comparação coma alumina pura. / Machinery and industrial equipment coatings suffer considerable damage from abrasion, impact and chemical attack, which makes it necessary to stop frequent maintenance actions. This situation motivates the development of materials of greater resistance to these requests. The insertion of zirconium oxide and cerium oxide in alumina-based compound has shown the ability to increase the mechanical properties of this type of technical ceramics. In this context, the objective of this work is the study of the influence of zirconium oxide and cerium oxide content (25 to 35%) in alumina-based composite. For these compounds, aluminum oxide, cerium oxide and zirconium oxide were mixed in ball mill and then, conformed by isostatic pressing. After, passed through a drying process and were the 1300, 1500 and 1600°C sintering. The mechanical properties of the materials after sintering were evaluated by mechanical resistance tests, Vickers hardness, KIc, thermal shock, linear shrinkage and porosity. The investigated materials showed densification in the range of 94.3 % to 95.75% of the theoretical density at sintering temperature of 1600 ° C and these values increased with the increase of ZPEC content. These composites can reach 23% of flexural strength greater than that of pure alumina, and with a tendency to increase this improvement with the percentage increase of ZPEC in alumina.

As restaurações monolíticas de Y-TZP (Zircônia Tetragonal Policristalina estabilizada por Itria) se apresentam como uma alternativa interessante devido a suas elevadas propriedades mecânicas, porém existe a preocupação quanto a Degradação em Baixa Temperatura (DBT). Os compósitos ZTA (Alumina reforçada por Zircônia) tem o potencial de atender a esta demanda, apesar do desafio estético uma vez que a passagem de luz pode ser limitada pela combinação de duas fases cristalinas. O presente trabalho teve como objetivo inovar na criação de um compósito ZTA sintetizado com Y-TZP translúcida, na procura de um material com alta resistência mecânica em relação à alumina, resistente à DBT quando comparada à YTZP e com propriedades ópticas melhoradas em relação ao ZTA sintetizado com Y-TZP convencional. Sessenta corpos de prova (discos de 12 mm de diâmetro por 1 mm de espessura) foram confeccionados e divididos em quatro grupos: zircônia convencional (3YSB-E), zircônia translucida (Zpex), compósito ZTA (Al2O3-70%v ZrO2-30%) sintetizado com 3YSB-E (ZTA-3YSB-E) e outro com zircônia translucida Zpex (ZTA-Zpex). Os corpos de prova foram obtidos mediante prensagem uniaxial e isostática dos pós cerâmicos. Após sinterização, o polimento das duas faces foi realizado com discos e suspensões diamantadas de até 1 m. A caracterização óptica foi realizada mediante testes de refletância sobre fundo branco e preto para determinar a razão de contraste (RC) e o parâmetro de translucidez (PT) mediante a diferença de cor (E). Difração de Raios-X (DRX) e Microscopia Eletrônica de Varredura (MEV) foram realizadas para estudo da microestrutura do material. Análise de variância ANOVA e teste de Tukey com nível global de significância de 5% foram utilizados na análises dos dados de propriedades ópticas. A RC mostrou opacidade significativamente menor para o grupo Zpex (0.77; p=0.0001), o grupo 3YSB-E mostrou valores intermediários (0.84; p=0.0001), sendo que os dois compósitos ZTA apresentaram valores maiores de opacidade (ZTA-3YSB-E = 0.99 e ZTA-Zpex = 1) sem diferença significante entre eles (p=0.7433). Para o PT os compósitos ZTA mostraram um E baixo (ZTA-Zpex = 0.22 e ZTA-3YSB-E = 0.43), sem diferença significante entre os grupos (p=0.5). O grupo 3YSB-E apresentou valores intermediários e significativamente diferentes em relação aos outros grupos (E = 7.11 p<0.0001). Já o grupo Zpex apresentou a menor capacidade de mascaramento com E =10.19 (p<0.0001). A DRX mostrou similaridade das fases cristalinas dos grupos 3YSB-E e ZPEX evidenciando que as mesmas foram preservadas na mistura nos compósitos, sem mostrar alterações da estrutura cristalina. A analise no MEV em até 1.500x de aumento evidenciou pouca alteração morfológica entre as zircônias e entre os ZTAs. As propriedades ópticas do ZTA Zpex não foram estatisticamente diferentes do compósito sintetizado com 3YSB-E, sendo que as Y-TZPs apresentaram menor opacidade. As Y-TZPs mostraram estrutura cristalina regular sem a formação de aglomerados e os compósitos ZTAs apresentaram uma mistura uniforme, mantendo as características da estrutura cristalina tanto da Y-TZP quanto da Al2O3, sem formação de aglomerados nem segregação dos grãos dos compósitos. Novos estudos são necessários para avaliar a resistência a DBT e as propriedades mecânicas destes materiais experimentais. / Monolithic Yttria stabilized Tetragonal Zirconia Polycrystals (Y-TZP) prostheses are considered an interesting treatment alternative due to their high mechanical properties. Nevertheless there is concern about the Low Temperature Degradation (LTD) process. Zirconia-Toughened Alumina (ZTA) composites seem to be capable of meeting this demand, while facing the challenge of being aesthetically suitable, since the passage of light can be limited by the combination of two polycrystalline phases. The present work aimed to innovate in the synthesis of a ZTA composite with a translucent Y-TZP for dental applications, in the search for a material with high mechanical resistance when compared to alumina, resistant to LTD when compared to Y TZP, and with improved optical properties over ZTA synthesized with conventional Y-TZP. Sixty disc shaped specimens with 12 mm diameter and 1 mm thick, were prepared and divided in four groups: a conventional zirconia (3YSB-E), a translucent zirconia (Zpex), a ZTA composite (Al2O3-70%v ZrO2-30%) synthetized with 3YSB-E (ZTA- 3YSB-E), and a ZTA composite synthetized with translucent zirconia (ZTA-Zpex). The specimens were obtained by uniaxial and isostatic pressing of the ceramic powders. After sintering, polishing of both sides was performed with diamond disks and suspensions up to 1 m. The optical characterization was performed by means of reflectance on a white and a black background to determine the contrast ratio (CR) and the translucency parameter (TP) of the experimental groups. XRD and SEM analyses were performed to study the crystalline structure. Analysis of variance ANOVA and Tukey test with a global significance level of 0.05% were used to analyze the data. CR showed significantly lower opacity for Zpex group (0.77, p = 0.0001), 3YSB-E showed intermediate values of opacity (0.84, p = 0.0001), and both ZTA composites presented higher opacity (ZTA-3YSB-E = 0.99 and ZTA-Zpex = 1) with no statistically significant difference between them (p = 0.7433). The TP showed a low E for ZTA composites (ZTA-Zpex = 0.22 and ZTA-3YSB-E = 0.43), with no statistically difference between the groups (p = 0.5). The 3YSB-E group presented intermediate and significantly different values of TP relative to the other groups (E = 7.11 p <0.0001). The Zpex group presented the lowest masking ability with E = 10.19, also significantly different from the other groups (p <0.0001). The XRD showed similarity of the crystalline phases of 3YSB-E and ZPEX, structure that were preserved in the blends in ZTA composites, without showing changes in the crystalline structure of the materials. SEM analysis (up to 1.500 x) showed low morphologic alteration between Y-TZP and ZTA composites. Optical properties of ZTA-Zpex showed no statistical difference when compared with ZTA-3YSB-E, whereas Y-TZP groups showed less opacity than other groups. The experimental Y-TZPs showed a regular crystalline structure without the formation of agglomerates, and the ZTA composites presented a uniform mixture of the phases, maintaining the characteristics of the polycrystalline structure of both Y-TZPs and Al2O3, without the formation of agglomerates or segregation of the grains in the composites. Future tests evaluating the resistance to LTD and mechanical properties of these experimental materials are warranted.