Made available in DSpace on 2014-10-09T12:55:17Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:05:56Z (GMT). No. of bitstreams: 1 12938.pdf: 9953963 bytes, checksum: abe25b7224002370db20a3af3b1f2044 (MD5) / Tese (Doutoramento) / IPEN/T / Escola Politecnica, Universidade de Sao Paulo - POLI/USP

Made available in DSpace on 2014-10-09T12:30:35Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:06:13Z (GMT). No. of bitstreams: 1 11284.pdf: 1048342 bytes, checksum: 7c02b6af9d9ad4a16392929179dce2f7 (MD5) / Dissertacao (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Made available in DSpace on 2014-10-09T12:32:58Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:06:11Z (GMT). No. of bitstreams: 0 / O óxido de alumínio foi um dos primeiros compostos investigados, com vista a detectar e medir a radiação por meio da termoluminescência (TL). Comumente referido como \"alumina\", o óxido de alumínio tem características interessantes para o desenvolvimento de materiais para a dosimetria. Seu número atômico efetivo é intermediário entre o do osso e do tecido mole do corpo. Pode ser transformado em material termoluminescente pela inserção de elementos químicos em sua estrutura cristalina. Além da TL, a alumina pode apresentar luminescência opticamente estimulada (OSL), fenômeno que também pode ser usado para determinar a dose de radiação. Neste estudo, dois métodos foram investigados para inserir íons metálicos na alumina. O primeiro método foi baseado na capacidade de adsorção da alumina e o segundo denominado método da coprecipitação foi baseado na formação simultânea de compostos insolúveis. As amostras obtidas por adsorção de íons Cu2+ e Mn2+ não mostraram resultados satisfatórios. No entanto, as pastilhas de óxido de alumínio impurificado com Tm3+ via coprecipitação mostraram sinais de TL e OSL. Foi verificado também que a alumina eletrofundida disponível comercialmente é um material que apresenta resposta TL e OSL. Este material que contém diversos íons metálicos em sua estrutura foi transformado em pastilhas por sinterização com vidro. As curvas da resposta TL em função da temperatura e da resposta TL e OSL em função da dose foram determinadas. Os resultados obtidos indicam que estudos mais aprofundados das pastilhas desenvolvidas podem melhorar suas características para que sejam aplicadas em dosimetria. / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

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This thesis focuses on a number of aspects governing the transformation of gibbsite, via intermediate phases, to a-alumina. These aspects include the size and morphology of the gibbsite grains, the influence of additions of foreign elements, the effect of a mechanical treatment of the gibbsite prior to calcination, and combinations of these factors. The materials were characterisedb y scanninge lectron microscopy, X-ray diffraction and surfacea rea measurementsF. or someo f the calcined materials an attempt was made to sinter the powders to a dense body to investigate if any of the treatments during calcination had an effect on this process. The literature review covers the current state of understanding of the production of bulk alumina powder by the Bayer process and the phase changes seen on calcination of precursors to the stable a-alumina phase. A detailed description of the phase changes is given and the various routes and conditions necessary for the transformations to occur are considered. The transformations are examined in relation to the morphology of the crystals and the variables controlling the phase transformation route are discussed. Calcination in air showed that the size of the gibbsite grain governs the calcination route taken to reach a-alumina. The standard gibbsites used in this work show a mixed calcination sequence transforming both via the boehmite phase, followed by the y, 8 and 0 phases, and via the x and K phases. The formation of boehmite is attributed to retention of water vapour within the grainDifferences in morphology of the starting materials showed that for the range of materials seen, the morphology of the grain is less important than its size. The super fine material confirmed that a small grain size transforms via the non-boehmite route only, with the other gibbsites taking intermediate routes as for the standard gibbsites. Of the additions made prior to calcination, aluminium fluoride was found to reduce the transformation temperature to a-alumina by approximately 300°C. Other additions had little effect on the transformation temperature although a reduction in grain size was seen with aluminium chloride. It was found that good mixing of the alumina fluoride was essential to obtain reliable and reproducible results. This is due to the small amounts of additive that are needed and the sensitivity of the process to concentration variations. Mineralisation of a range of gibbsites showed that the presence of sodium in the starting material was crucial in reducing the calcination temperature. This led to the conclusion that the sodium and fluoride react to form a liquid phase. The presence of a liquid phase increases the mobility of the aluminium and oxygen atoms resulting in a reduction of the transformation temperature. Fluoride additions to the gibbsites with different morphologies showed that the presence of sodium was the governing factor in reduction of the transformation temperature. Milling of the starting materials showed that there was a small reduction in the transformation temperature between some of the phases. The energy involved in milling leads to activation of the gibbsite. This activation takes the form of a reduction in the grain size and in a reduction of the crystallinity seen in the XRD patternFluoride additions during the calcination of sapphire with a standard gibbsite powder showed preferential grain growth. It was possible to initiate growth of small plate-like crystals on the polished surface of a piece of sapphire parallel to the basal plane. Crystal growth was also seen in scratches on a polished surface perpendicular to the basal plane

No description available.

Materiais nanoestruturados têm atraído grande interesse nos últimos anos. Isso se deve, por um lado, aos recentes avanços na capacidade de investigar, manipular e organizar a matéria em escala nanométrica, que abriram um novo horizonte de possibilidades para a fabricação e o controle da estrutura da matéria ao nível atômico e molecular e, por outro, devido ao extenso potencial de aplicação em biosensores, dispositivos fotônicos, magnéticos e ótico-eletrônicos. Em especial, a demanda por materiais magnéticos com capacidade para gravação em alta densidade é uma área com grande interesse nas novas possibilidades oferecidas pela nanociência e nanotecnologia. Processos que possibilitem a criação de estruturas de nanopartículas nas quais seja possível a otimização das propriedades estruturais (tamanho, forma e distribuição) são de grande interesse científico e tecnológico. Dentre os métodos utilizados para síntese destas estruturas, aqueles que utilizam uma membrana de alumina anódica como molde têm sido considerados como muito interessantes devido às várias vantagens sobre as demais técnicas convencionais (p. e. as litografias por feixe de elétrons, por micro-feixe iônico e AFM), como o grande controle da forma das estruturas, uniformidade, longas áreas de ordenação sobre a amostra, baixo custo e relativa facilidade de fabricação. Neste trabalho, estudou-se a preparação de amostras de alumina nanoporosa a partir do alumínio ultra-puro pelo processo de oxidação anódica. Investigou-se a influência dos dois estágios de anodização no grau de ordenação da amostra e também se verificou a relação entre as condições de anodização, eletrólito e tensão, e as características morfológicas das amostras obtidas. As amostras foram caracterizadas por Microscopia Eletrônica de Varredura (MEV) e Microscopia de Força Atômica (AFM), técnicas que se mostraram poderosas ferramentas para investigação das nanoestruturas obtidas. Além da produção das amostras, foi construído e implementado um arranjo experimental para a fabricação de alumina nanoporosa por oxidação anódica no Laboratório de Física Aplicada - LFA-CDTN. / Nanostructured materials, i.e. materials whose structural elements (thin films, clusters, crystallites or molecules) have at least one dimension in the 1 to 100 nm range, have attracted great interest in recent years because the extensive application potential. The explosion in both scientific and technological interest in these materials over the past decade arises from the remarkable variations in fundamental electrical, optical and magnetic properties that occur as one progresses from an infinitely extended solid to a nanoscale material. As a remarkable example, the demand for magnetic materials capable of recording with high density is an area with great interest among the new possibilities offered by nanoscience and nanotechnology. Processes that enable the preparation of nanoscale materials in which it is possible to optimize the structural properties (size, shape and distributions), aiming to investigate the effects mentioned above, are of great scientific and technological interest. Among the methods used for synthesis of such nanostructures, those using an anodic alumina membrane have been considered as very interesting due to several advantages over other classical techniques (e.g. electron beam and ion beam lithography), such as the large control of structure size, uniformity, long area of ordering on the sample, low cost and relative simplicity of production. In this work, nanoporous alumina was prepared from ultra-pure aluminum by anodic oxidation process in order to be used as templates in the synthesis of magnetic nanostructures. It was investigated the influence of the two stages of anodizing in the degree of ordering of the sample and also investigated the relationship between the conditions of anodizing (electrolyte solution and voltage) and the morphological characteristics of the samples. The samples were characterized by scanning electron microscopy (SEM) and Atomic Force Microscopy (AFM), techniques that have proved powerful tools for investigation of nanostructure materials. Besides the production of the samples, it was implemented the infrastructure and methodology necessary for the production of nanoporous alumina in the LFA/CDTN.

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Made available in DSpace on 2014-10-09T12:44:23Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T13:56:52Z (GMT). No. of bitstreams: 1 06879.pdf: 7295215 bytes, checksum: b1fc7c93971eff30770441f658186e7b (MD5) / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP