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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
151

Switchmode Power Supply Miniaturization with Emphasis on Integrated Passive Components on Prefired High Performance Ceramic Substrates

Hoagland, Richard W. 24 August 1999 (has links)
This Dissertation is a study of Switched Mode Power Supply (SMPS) miniaturization and how to effectively use the available technologies to achieve the ultimate goal of a reduced size without loss of functionality while maintaining a cost effective design. This research investigates several methods used to obtain low loss, highly compact power supplies. Within these constraints, the Dissertation investigates the issues of design, materials, and cost in order to design and achieve these miniaturized power supplies. This research addresses high performance ceramic, passive component integration. Three key issues; electrical characterization, thermal analysis and simulation, and material characterization, are examined in this work. Thick film passive components (capacitors and resistors) on AlN have been developed. Also, guidelines for the design implementation and steps necessary to integrate these passive components on prefired alumina (Al2O3) and aluminum nitride (AlN) ceramic surfaces, for power electronic applications, have been generated. The use of aluminum nitride, as a high performance ceramic substrate and the resulting issues concerning compatible inks, have been investigated. Since a sizable amount of heat is generated by power electronic circuits, the integrated components are analyzed with respect to tolerance and degeneration over a range of temperatures and frequencies. Thick film capacitors on the order of 120pF/mm2 with breakdown voltage ratings of 250V have been developed on prefired AlN. Resistors were developed with impedances ranging from 10W to 10MegW. Thermal measurements, of these resistors, show that the thermal conductivity of the aluminum nitride with passivation layer is two to three times that of alumina. Several versions of a typical SMPS boost circuit have been generated using Direct Bond Copper (DBC) on ceramic, Insulated Metal Substrate (IMS), Printed Circuit Boards (PCB), and prefired ceramic thick film technology. The integrated passive components developed are applied on prefired ceramic versions and compared to the DBC, IMS and PCB versions. A small daughter board consisting of the boost circuit control is introduced to further supplement miniaturization and reduce cost. The daughter board uses thick film technology with integrated thick film resistors. The design of the mother board, which houses the power boost section,can be designedand implemented on virtually any type of substrate (PCB, DBC, IMS, or conventional thick film). The fabrication and testing of each version is reported in this work. / Ph. D.
152

Tribopolymerization: Anti-Wear Behavior of New High Temperature Additive Classes

Valentino, Jeffrey Joseph 06 November 2001 (has links)
Advanced ceramic materials have found many new applications in the automotive and other industries. To satisfy demands of higher temperatures and inert surfaces, new lubrication methods for these ceramics need explored and evaluated. This thesis focuses on a boundary lubrication method termed tribopolymerization -- the formation of polymers at the tribological interphase. The research evaluated new high-temperature classes of anti-wear additives. The work involved experiments on steel and alumina material pairs with a pin-on-disk tribometer used to explore the anti-wear capabilities of selected additives in the liquid phase at concentrations of 1% by weight in hexadecane. New additives included aromatic compounds with various pendant groups adding the design functionality necessary for in-situ polymerization. The amino, hydroxyl, acid, and ester functional groups underwent studies across several aromatic molecular compositions while new heterocyclic additives, in particular the readily available lactams, underwent exploratory tests as a new class under the tribopolymerization design approach. In concentrations of 1%, additives showed significant wear reductions of up to 99.9 %. Anti-wear behavior persisted in select cases at concentrations as low as 0.1% by weight. Compounds from two new classes demonstrated anti-wear behavior at 6x the frictional heat generation of standard exploratory conditions. This surprising effect partially filled a void in the effective range of operating conditions between 0.25 m/s, 40 N and 1.0 m/s, 160 N. Earlier work by Tritt found a complete absence of anti-wear behavior for the previous additive classes at the high-speed conditions. In addition, several individual compounds constituent to an A-R-A + B-R'-B condensation polymerization reaction demonstrated significant anti-wear behavior when used alone. In particular, the compound BTDA from DuPont's Kapton® exhibited higher wear reductions than any other new additive. These findings support tribopolymerization as an effective approach to boundary lubricant design. Low wear was often associated with an attached reaction debris layer. This finding is consistent with previous work involving tribopolymerization anti-wear additives with ceramics. Further research into the roles of the debris layer and tribochemistry will help in understanding the complex anti-wear behavior of these new high-temperature additive classes. / Master of Science
153

A synthetic silica-alumina bead catalyst

Jonas, Reginald H. January 1947 (has links)
M.S.
154

Effect of Processing Parameters on Bond Strength and Effective Plasticity in Al2O3-TiB2 Composites

Holt, Susan Marie 24 October 2011 (has links)
Alumina-titanium diboride (Al2O3-TiB2) composites have high temperature, wear, and impact resistance that could be useful in high performance applications. Determining the effect of processing parameters on relative bond strength and effective plasticity may contribute to optimization and predictability of performance in the Al2O3-TiB2 system. Al2O3-TiB2 composites were obtained from a collection of samples that were created during a separate ongoing research program being conducted by Dr. Kathryn V. Logan. The Logan samples were initially formed by hot pressing powders produced using Self-Propagating High Temperature synthesis (SHS) of Al, TiO2, and B2O3 powders or manual mixing (MM) of Al2O3 and TiB2 powders. Samples were then fractured using standard single edge notched beam (SENB) fracture toughness testing. The obtained fractured surfaces were examined using Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Spectroscopy (EDS). Relative amounts of transgranular and intergranular fracture of Al2O3 and TiB2 grains were determined. Transgranular fracture was used as a measure of relative bond strength. Other samples were obtained from the Logan collection to conduct nano-indentation measurements on polished sample surfaces in Al2O3 grains and in TiB2 grains. Indent locations were verified using SEM. Reduced modulus, final displacements, and fracture toughness for indents in Al2O3 grains and in TiB2 grains were determined from nano-indentation curves. Reduced modulus was used as a measure of relative bond strength. Final displacement and fracture toughness were used as measures of relative effective plasticity. Analysis of Variance (ANOVA) using Taguchi arrays was conducted using the powder processing factor (SHS vs. MM) and the predominant microstructure factor (TiB2 grains surrounding Al2O3 grains vs. TiB2 grains distributed amongst Al2O3 grains) when examining the effect of processing parameters on relative bond strength as measured by amount of transgranular fracture. Analysis of Variance (ANOVA) using Taguchi arrays was conducted using the powder processing factor (SHS vs. MM), the predominant microstructure factor (TiB2 grains surrounding Al2O3 grains vs. TiB2 grains distributed amongst Al2O3 grains), and the indented phase factor (Al2O3 vs. TiB2) when examining the effect of processing parameters on relative bond strength as measured by nano-indentation reduced modulus and both measures of relative effective plasticity. Powder processing was significant for the relative bond strength measures, but was not significant for the relative effective plasticity measures. Predominant microstructure was significant for all measures except relative effective plasticity as measured by fracture toughness, for which none of the factors and interactions were significant. The interaction between powder processing and predominant microstructure was significant for most of the relative bond strength measures and for relative effective plasticity as measured by final displacements. Indented phase was significant for the nano-indentation measures except nano-indentation fracture toughness, although the significance for nano-indentation fracture toughness was just below the critical level. The interaction between powder processing and indented phase and the interaction between predominant microstructure and indented phase were only significant for the relative bond strength measure using nano-indentation reduced modulus. The interaction between powder processing, predominant microstructure, and indented phase was significant for the nano-indentation measures except nano-indentation fracture toughness. The optimum level for powder processing was predominantly manual mixing. The optimum level for predominant microstructure was predominantly TiB2 grains surrounding Al2O3 grains. The optimum level for indented phase was predominantly TiB2. / Master of Science
155

Rational synthesis of novel reforming catalysts

Ewbank, Jessica Lee 27 May 2016 (has links)
Biomass gasification offers the chance to produce carbon neutral, renewable fuels. One of the main problems facing the commercialization of biomass gasification technology is the presence of large quantities of methane and carbon dioxide in the biogas. Catalytic reforming of these wastes allows for effective utilization of biomass derived syngas. In most reforming studies, impregnation methods are the primary synthesis technique. Impregnation methods often lead to poor dispersion and are un-reproducible from batch to batch. In the development of a novel catalyst for reforming applications, another preparation method is implemented, controlled adsorption (CA). Ni/Al2O3 and Co/Al2O3 prepared by CA are compared against catalysts that were prepared by a more traditional method, dry impregnation (DI). It is found that controlling the metal deposition provides catalysts with higher dispersion and consequently higher activity for methane dry reforming. NiAl2O4 catalysts prepared by Pechini synthesis were also studied for catalytic conditioning of biomass derived syngas. Physicochemical characterization revealed unique structural properties, indicated a high degree of mobility of nickel in the aluminate structure, and demonstrated the regeneration properties of nickel aluminates under harsh reaction conditions, which will be important at extended reaction times when catalyst regeneration becomes necessary. Fourfold coordinated nickel species are believed to be responsible for high, stable methane dry reforming activity and metallic nickel is believed to be the active site that allows for high, stable conversion during methane dry reforming.
156

Preparação e caracterização de compósitos abrasivos resinoides reforçados com alumina reciclada / Preparation and characterization of resin bonded abrasives composites reinforced with recycled alumina

Golanda, Alexandre Dutra 07 August 2017 (has links)
A iminente escassez de recursos naturais e de fontes energéticas não renováveis são forças motrizes para a adoção de práticas sustentáveis. Dentre os processos industriais que fazem uso intensivo de recursos naturais, estão os que utilizam processos de usinagem baseados em ferramentas abrasivas para desbaste, esmerilhamento, corte, entre outros. A partir deste panorama geral, é possível enxergar a necessidade de estudar os processos de usinagem com ferramentas abrasivas a fim de aumentar a compreensão sobre eles e de torná-los sustentáveis. Sendo assim, o objetivo deste trabalho é avaliar, por meio do comportamento mecânico de compósitos abrasivos resinoides, o potencial de reciclagem de grãos de alumina oriundos de ferramentas abrasivas. No presente trabalho, foi estudada a preparação e caracterização de compósitos abrasivos resinoides reforçados com grãos alumina reciclada e virgem. Uma das aluminas recicladas é oriunda de rebolos e discos de corte resinoides, outra alumina é oriunda de rebolos vitrificados, e a última, composta por alumina branca, é recuperada de rebolos vitrificados refugados ou usados. As amostras de grãos de alumina reciclada e a de grãos de alumina marrom virgem foram caracterizadas por meio das técnicas de fluorescência de raios X (FRX), difratometria de raios X (DRX), microscopias óptica (MO) e eletrônica de varredura (MEV). Corpos de prova de compósitos utilizando os quatro tipos de alumina foram preparados por meio da mistura, prensagem e tratamento térmico de grãos de alumina e resinas fenólicas resol e novolaca. Por fim, os compósitos foram caracterizados por meio das técnicas de calorimetria exploratória diferencial (DSC), módulo elástico por excitação por impulso, impacto Izod, flexão em quatro pontos, análise térmica dinâmico-mecânica (DMTA), dureza por Sand Blasting Penetration (SBP), porosidade pelo método de Arquimedes e microscopias óptica e eletrônica de varredura. Os resultados dos ensaios mecânicos mostraram que os compósitos de alumina reciclada apresentaram depreciação em todas as propriedades estudadas em relação ao compósito de alumina virgem, exceto a resistência ao impacto Izod, no qual todas as amostras apresentaram baixa resistência. A razão desta baixa resistência ao impacto deveu-se à estrutura formada pelo grão de alumina, ligante (resina fenólica) e porosidade, na qual a baixa proporção de resina fenólica (10% m.) foi a responsável pelo resultado. Por outro lado, a causa da depreciação nas propriedades mecânicas apresentadas pelos compósitos de alumina reciclada foi a menor concentração em alumina e a presença de impurezas oriundas da produção das ferramentas abrasivas. Neste caso, o compósito de alumina branca reciclada apresentou melhores resultados das propriedades mecânicas em relação aos compósitos de alumina oriunda de rebolos vitrificados e os de alumina oriunda de rebolos e discos resinoides. Concluindo, o potencial de reciclagem dos grãos de alumina oriundos de ferramentas abrasivas visando o seu reaproveitamento no processo de fabricação destas ferramentas é limitado pela sua pureza, de modo que se no processo de reciclagem dos grãos for aumentada a concentração de alumina haverá possibilidade de seu reaproveitamento. / The imminent scarcity of natural resources and nonrenewable energy sources are driving forces for the adoption of sustainable practices. Among the industrial processes that make intensive use of natural resources, there are those that use machining processes based on abrasive tools for roughing, grinding, cutting, among others. From this general panorama, it is possible to see the need to study the machining processes with abrasive tools in order to increase the understanding about them. Thus, the objective of this work is to evaluate, through the mechanical behavior of resin-bound abrasive composites, the recycling potential of alumina grits from abrasive tools. In the present work, the preparation and characterization of resinoid abrasive composites reinforced with recycled and virgin alumina grits was studied. One of the recycled aluminas comes from resin-bound grinding wheels and thin wheel cut-off discs, another alumina comes from vitrified grinding wheels, and the latter, composed of white alumina, is recovered from scrapped or used glazed grinding wheels. The samples of recycled alumina grits and virgin brown alumina grits were characterized by X-ray fluorescence spectroscopy (XRF), X-ray diffractometry (XRD), optical microscopy (OM) and scanning electron microscopy (SEM). Composite test bodies using the four types of alumina were prepared by mixing, pressing and heat treatment of alumina grits and resol and novolak phenolic resins. Finally, the composites were characterized by differential scanning calorimetry (DSC), impulse excitation elastic modulus, Izod impact, four-point flexing, dynamic-mechanical thermal analysis (DMTA), Sand Blasting Penetration hardness (SBP), porosity by the Archimedes method and optical and scanning electron microscopy. The results of the mechanical tests showed that the recycled alumina composites presented depreciation in all the studied properties in relation to the virgin alumina composite, except the Izod impact resistance, in which all the samples presented low resistance. The reason for this low impact strength was due to the structure formed by the alumina grit, binder (phenolic resin) and porosity, in which the low proportion of phenolic resin (10% m) was responsible for the result. On the other hand, the reason for the depreciation in the mechanical properties presented by the recycled alumina composites was the lower concentration in alumina and the presence of impurities from the production of the abrasive tools. In this case, the recycled white alumina composite presented better mechanical properties in relation to alumina composites from vitrified grinding wheels and those from alumina from grinding wheels and resinoid disks. In conclusion, the recycling potential of the alumina grits from abrasive tools aiming at their reuse in the process of manufacturing these tools is limited by their purity, so that if in the grit recycling process the alumina concentration increases it will make possible its reuse.
157

Estudo da dispersão das propriedades físico-químicas em blocos de alumina marrom obtida por eletrofusão / Study of dispersion of physicochemical properties in brown alumina blocks obtained by electrofusion

Faria, Robersio Marinho de 19 December 2016 (has links)
Tendo em vista a natureza finita dos minerais naturais, torna-se evidente a necessidade de utilizarmos este recurso de maneira estratégica. Desta forma, diversas pesquisas vêm sendo desenvolvidas principalmente nas áreas químicas, metalúrgicas e mineralógicas desde as etapas de extração, beneficiamento, aplicação e reutilização dos resíduos de minérios. Portanto, é extremamente importante a intensificação dos estudos para aumentar o conhecimento quanto às características e propriedades físico-químicas destes minerais, visando melhorar o seu aproveitamento e longevidade das jazidas naturais, como as fontes de bauxita, que é a principal matéria-prima para a produção de óxido de alumínio fundido. Na sua forma cristalina mais comum, denominada coríndon, ou óxido de alumínio ?, sua baixa condutividade elétrica, baixo calor específico, alta condutividade térmica, alto ponto de fusão, elevada dureza e resistência mecânica, o torna adequado para uso em produtos refratários, cerâmicos e abrasivos tais como, lixas, rebolos, ferramentas de corte e de polimento. Na síntese deste produto as principais impurezas que afetam a qualidade dos grãos são Fe, Si, Ca, K, Na e Zr, oriundas da matéria prima bauxita e da carta de mistura, composta por ilmenita, limalha de ferro, carvão vegetal e coque de petróleo. Desta forma, o presente trabalho assumiu o objetivo de estudar a dispersão das propriedades físico-químicas em blocos de alumina fundida marrom obtida em fornos Higgins a arco por eletrofusão, produzidos na Saint-Gobain Abrasivos, unidade de Lorena, SP. Por fim, foram utilizadas técnicas de caracterização físico-químicas de difratometria de raios X (DRX), análises químicas de fluorescência de raios X (FRX), ensaio de dureza Knoop e caracterização microestrutural via (MEV/EDS). Desta forma, foi definido o mapeamento composicional nos blocos de alumina eletrofundida marrom, que servirão como referência técnico-científica para subsidiar ações de melhoria deste produto, em decorrência do avanço do estado da arte deste referido assunto. / The mineral ores are not renewable sources and we need to use it in the best way possible. In this way, a large number of researches are being developed around the world aiming the improvement of current methods of production mainly in chemical, metallurgy, mineralogical from the steps of extraction, processing, application and reuse of waste ore. Therefore, it is extremely important to intensify the studies to increase the knowledge about the characteristics and physicochemical properties of these minerals, in order to improve their utilization and longevity of natural deposits, such as sources of bauxite, which is the main raw material to product aluminum oxide fused. In its most common crystalline form, called corundum or ?-aluminum oxide, its low electrical conductivity, low specific heat, high thermal conductivity, high melting point, high hardness and mechanical strength, making it suitable for use as refractories, ceramics and fine or coarse abrasives. The synthesis of this product major impurities that affect quality of grain is Fe, Si, Ca, K, Na and Zr, derived from the raw material bauxite and the mixture chart consisting of ilmenite, iron filings, charcoal and coke oil. Thus, this shows the dispersion of physicochemical properties of brown fused alumina blocks produced by eletrocfusion at Higgins furnace process in the company Saint Gobain Abrasivos, Lorena- SP. Finally, the samples were physicochemical analyzed by X ray diffraction (XRD), chemical analyses by X ray fluorescence (XRF), hardnes using Knoop method, microstructural characterization by (SEM). The results of this work show a compositional gradient map of the fused alumina block; that shows the main physicochemical differences into the block, to support changes in the alumina production process; and it is also important to improve the actual state of art of this particular theme.
158

Compósitos de alumina com adições de NbC, TaC e TiC para aplicação em ferramentas de corte / Alumina composites with additions of NbC, TaC and TiC for application in cutting tools

Tonello, Karolina Pereira dos Santos 15 March 2013 (has links)
No presente trabalho foram desenvolvidos compósitos à base de alumina, com adição de carbetos de metais de transição, NbC, TaC e TiC, como reforço. Os carbetos, na forma de partículas, foram adicionados em 1,5% em volume à matriz de alumina durante a moagem em attritor. O processamento foi realizado por moagem em attritor, secagem em rotoevaporadora e desaglomeração em peneira. A dinâmica de oxidação dos carbetos e das composições dos compósitos foi estudada para a definição de parâmetros de sinterização e processamento dos compósitos. A cinética de sinterização foi estudada por dilatometria, com taxa de 10°C/min. até 1600°C em atmosfera de ar sintético, e até 1800°C, em atmosfera de argônio, com esta etapa foi possível verificar que o NbC e o TiC dificultaram a sinterização da alumina e que o TaC auxiliou nos processos de retração. Nas amostras que foram sinterizadas em dilatômetro ao ar foram detectadas fases resultantes de fusão congruente nos compósitos Al2O3/NbC e Al2O3/TaC, foram também observadas evidências de formação de líquido no compósito com adição de TaC. Com base nesses resultados foram estudadas duas técnicas de produção das ferramentas de corte: prensagem uniaxial seguida de sinterização sem pressão e sinterização por prensagem a quente. Todas as amostras foram caracterizadas microestruturalmente e quanto às propriedades mecânicas, tendo-se determinado que as amostras produzidas por prensagem a quente possuem microestrutura mais controlada e propriedades mecânicas superiores às produzidas por sinterização sem pressão. Pelos processos estudados foi observado que os carbetos influenciam diferentemente a sinterização da alumina. De maneira geral a presença destas fases nos contornos de grãos promove alterações na microestrutura modificando o tamanho de grãos da alumina. Foi proposta a hipótese de que esse comportamento é afetado pela formação de uma camada superficial resultante da oxidação dos reforços, com isto, de acordo com os diagramas de fase é possível a formação de soluções sólidas entre alumina e Ta2O5 e Nb2O5 além da formação de fase líquida, estes mecanismos alterariam a mobilidade dos contornos de grão da alumina. Para o processamento das ferramentas de corte foi utilizada prensagem a quente, escolhido pelo critério da microestrutura e propriedades mecânicas. Os testes de usinagem foram realizados com ferramentas de corte de geometria quadrada, em peças de ferro fundido cinzento e vermicular. O tempo de vida útil da ferramenta produzida com o compósito Al2O3/ NbC foi 13% superior quando comparado à uma ferramenta cerâmica comercial no teste de usinagem de ferro fundido cinzento. / In the present work alumina based composites with addition of transition metal carbides, NbC, TaC and TiC as reinforcement phase were developed. The carbides, in particulate form, were added in 1.5vol.% on the alumina matrix during attritor milling. The processing was conducted by attritor milling, drying in a rotoevaporator and deagglomeration in sieve. The oxidation dynamics of carbides and composities were studied in order to define the sintering and processing parameter of composites. The sintering kinetics was studied by dilatometry at 10° C/min. up to 1600 ° C in synthetic air atmosphere and up to 1800°C in argon, with this step it was possible to verify that the NbC and TiC hindered the sintering of alumina and the TaC helped in the retraction process. In the sintered by dilatometer in air phases resultant from congruent melting on Al2O3/NbC and Al2O3/TaC composites were detected in the composite with TaC addition was also observed evidence of liquid phase. In the samples sintered in dilatometer in air were detected solid solutions on composites CN and CTa and evidence of liquid formation in the composite with TaC addition. Based on these results two techniques were studied in order to produce cutting tools: uniaxial pressing, followed by pressureless sintering and hot pressing. All samples were characterized by microstructure and mechanical properties, and it was shown that samples produced by hot pressing have more controlled microstructure and mechanical properties superior to those produced by pressureless sintering. With the studied processes it was observed that the carbides influence differently alumina sintering. Generally the presence of these phases at the grain boundary causes changes in the microstructure modifying alumina grain size alumina. The proposed hypothesis is that this behavior would be affected by the formation of a surface layer resulting from oxidation of reinforcements with that, according to the phase diagrams, it is possible to find solid solutions between alumina and Ta2O5 and Nb2O5 and possible formation of liquid phase, which alter the mobility of the grain boundary of alumina. Hot pressing was used for the processing of cutting tools, chosen due to the microstructure and mechanical properties. The machining tests were performed with square geometry cutting tools, in samples of gray cast iron and compacted graphite iron. The tool life of cutting tool produced with Al2O3 / NbC composite was 13% higher when compared to a commercial ceramic cutting tool on machining of gray cast iron.
159

Estudo da influência dos íons Mg2+ e Zr4+ na transição de fase amorfo-gama da alumina. / Effect of Mg2+ and Zr4+ Ions on the stability of amorphous phase transition of gama alumina.

Rosário, Deise Cristina Carvalho do 26 January 2012 (has links)
Alumina é um material amplamente aplicado em diversas áreas. Uma dessas aplicações utiliza a alumina amorfa e a alumina gama, como suporte catalítico devido suas elevadas áreas de superfície específica e defeitos em suas estruturas cristalinas. Porém, problemas com a estabilidade das aluminas metaestáveis em altas temperaturas se tornaram um desafio. Assim a combinação da alumina com alguns óxidos emergiu como uma nova classe de materiais catalíticos com melhor estabilidade quando comparada com a alumina gama ou alumina amorfa convencional. Entretanto, entender como se dá à estabilização das fases através desses aditivos se tornou outro desafio. Assim, este trabalho teve como objetivo avaliar os possíveis efeitos de aditivos nas propriedades termodinâmicas da alumina. Além de sua influência sobre a transição de fases amorfo-gama, ou seja, a influência sobre o balanço energético através da evolução do tamanho de partícula. Para isto foram sintetizadas aluminas com diferentes concentrações de Mg2+ e Zr4+ através do método proposto por Pechini. As amostras foram calcinadas e caracterizadas por Calorimetria Diferencial de Varredura, Análise de Superfície Específica pelo método de Adsorção-Desorção de Gases, Difração de Raios X, Espectrometria de Infravermelho por Transformada de Fourier e Picnometria. Os resultados das análises mostraram um aumento da estabilidade para as amostras dopadas com os aditivos, porém com distintas evoluções de área de superfície específica, evidenciando que o caminho adotado pelo aditivo quando inserido em um material matriz independe de sua concentração. / Alumina is a material applied in several areas. One such application uses the gamma alumina and amorphous alumina as catalyst support. The use of alumina as the catalyst support is because of their high specific surface areas and defects in their crystal structures. However, problems with the stability of metastable aluminas at high temperatures have become a challenge. To solve this problem, we use a combination of some oxides to alumina improves the stability of the material when compared with conventional catalytic aluminas. However, a new challenge, to understand the performance of these oxides in the stabilization of alumina. This work aimed to evaluate the possible effects of additives on the thermodynamic properties of alumina, through its influence on the amorphous-phase transition range. The assessment of influence on the energy balance was made by the evolution of particle size. For this alumina powders were synthesized with different concentrations of Mg2+ and Zr4+ using the method proposed by Pechini. The samples were calcined and characterized by Differential Scanning Calorimetry, Surface Analysis by the method of Specific Adsorption-Desorption of Gases, X-Ray Diffraction, Infrared Spectroscopy Fourier Transform and Picnometry. The analysis results showed an increased stability for the samples doped with additives, but with different evolutions of specific surface area, showing the path taken by the additive when inserted into a matrix material depend on its concentration.
160

Caracterização por ressonância magnética nuclear de Na β\" alumina hidratada / Characterization of Na β alumina by nuclear magnetic resonance

Gobato, Yara Galvão 14 August 1989 (has links)
Neste trabalho, estudamos a dependência com a temperatura dos tempos de relaxação nuclear T1 e T2 do 1H em policristais de Na &#946;\" alumina hidratada, no intervalo de temperatura de 255<T<540K, em 24,5MHz . Três amostras em pó foram selecionadas para medidas de RMN: duas puras e uma dopada com Fe (500ppm em peso). A presença de impurezas magnéticas nessas amostras foi observada através de espectros de Ressonância Paramagnética Eletrônica. Estudamos também a liberação de moléculas de água em função da temperatura pela técnica de TGA (Thermal Gravimetric Analysis). O sinal de RMN observado no intervalo de temperatura de 258<T<423K foi associado a moléculas de água fracamente ligadas enquanto que o sinal observado em temperaturas superiores foi associado a moléculas fortemente ligadas, provavelmente localizadas no plano de condução. Nossos resultados mostram que a hidratação o comportamento em função da temperatura dos tempos de relaxação nuclear são consideravelmente afetados pela presença de impurezas magnéticas / Proton NMR relaxation times T1 and T2 were measured on hydrated polycrystalline Na &#946; alumina in the temperature range 255<T<540K at 24.5MHz In order to get some feeling for the temperature at which water would leave the sample a thermal gravimetric analysis (TGA.) was also performed. Three powder samples, two pure and one iron doped (500ppm nominal), with particle diameters of 150-250micrômetros were selected for NMR measurements. Paramagnetic impurities were detected by EPR studies. Our results suggest that loosely bound water produces the NMR signal at temperatures lower than 423K while more tightly bound water, probably in the conduction planes, is predominant at higher temperatures. The relaxation time measurements show that magnetic impurities affect considerably the temperature dependence

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