Caracterização estrutural de géis de sílica de diferentes porosidades preparados a partir da sono-hidrólise do tetraetilortosilicato
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Data
2008-07-31
Autores
Scalari, Juliana Possebon [UNESP]
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Editor
Universidade Estadual Paulista (Unesp)
Resumo
As propriedades estruturais de sonogéis de sílica preparados a partir da sonohidrólise do tetraetilortosilicato (TEOS) foram estudadas em função da porosidade. Sonogéis com diferentes porosidades foram preparados usando diferentes razões molares água/TEOS (R) na etapa de hidrólise do processo. Os valores de R utilizados foram R = 4, 6, 8, 12, e 16. Um dos objetivos foi obter géis com diferentes “porosidades” no estado úmido e estudar o efeito da porosidade nas propriedades estruturais dos sonogéis. Também foi objetivo estudar e comparar técnicas alternativas, como DSC e SAXS, aplicáveis na caracterização estrutural de géis ainda no estado úmido de preparação. Os géis foram estudados em estágios que vão desde o estado saturado (gel úmido) até o estado seco do gel, resultante do processo de secagem supercrítica (aerogel). Os géis úmidos foram estudados por termogravimetria (TG), calorimetria diferencial exploratória (DSC) e espalhamento de raios-X a baixo ângulo (SAXS). Os aerogéis foram estudados por adsorção de nitrogênio e espalhamento de raios-X a baixo ângulo (SAXS). Géis úmidos exibem uma estrutura fractal de massa, num certo domínio do intervalo de distâncias, explorado por valores grandes do módulo q do vetor de espalhamento de raios-X a baixo ângulo. A dimensão fractal de massa D nos géis úmidos é essencialmente igual a 2, aproximadamente independente de R. O tamanho da estrutura fractal de massa dos géis úmidos é limitada a um comprimento característico x, que aumenta de cerca de 3,3 nm para 7,2 nm com o aumento de R de 4 para 16. A “porosidade” dos géis úmidos varia entre cerca de 87% a 91% do volume da amostra, com o aumento de R de 4 para 16. A troca da fase líquida dos géis úmidos por água pura, para os ensaios de DSC, aumenta a dimensão fractal D...
The structural property of silica sonogels prepared from the sonohydrolysis of tetraethoxysilane (TEOS), were studied in function of the porosity. Sonogels with porosities were prepared using different molar ratio water/TEOS (R) in the stage of hydrolysis of process. The values of used R were 4,6,8,12,16. One of the objectives was to obtain gels with different porosities in the wet state and to study the effect of the porosity in the structural properties of the sonogels. It was also objective to study and to compare alternative techniques, like DSC and SAXS, applicable in the structural characterization of gels still in the wet state of preparation. The gels were studied in stages that are going from the saturated state (wet gel) until the dry state of the gel, resulting from the process of drying supercritical (aerogel). The wet gels were studied by termogravimetria (TG), exploratory differential calorimetry (DSC) and small angle X-Ray scattering (SAXS). The aerogels were studied by adsorption of nitrogen and small angle X-Ray scattering (SAXS). Wet gels exhibit a mass fractal structure, in a certain domain of the interval of distances, explored by big values of the module q of the scattering vector from ray-X to low angle. The dimension mass fractal D in the wet gels is essentially equal to 2, approximately independent of R. The size of the fractal mass structure of the wet gels is limited to a characteristic length, that it increases about 3,3 nm for 7,2 nm with the increase of R of 4 for 16. The porosity of the wet gels range about 87% to 91% of the volume of the sample, with the increase of R of 4 for 16. The change of the liquid phase of the wet gels for pure water, for the rehearsals of DSC, increases the dimension fractal D and it reduces the characteristic size ξ. The value of D in the changed gels range... (Complete abstract click electronic access below)
The structural property of silica sonogels prepared from the sonohydrolysis of tetraethoxysilane (TEOS), were studied in function of the porosity. Sonogels with porosities were prepared using different molar ratio water/TEOS (R) in the stage of hydrolysis of process. The values of used R were 4,6,8,12,16. One of the objectives was to obtain gels with different porosities in the wet state and to study the effect of the porosity in the structural properties of the sonogels. It was also objective to study and to compare alternative techniques, like DSC and SAXS, applicable in the structural characterization of gels still in the wet state of preparation. The gels were studied in stages that are going from the saturated state (wet gel) until the dry state of the gel, resulting from the process of drying supercritical (aerogel). The wet gels were studied by termogravimetria (TG), exploratory differential calorimetry (DSC) and small angle X-Ray scattering (SAXS). The aerogels were studied by adsorption of nitrogen and small angle X-Ray scattering (SAXS). Wet gels exhibit a mass fractal structure, in a certain domain of the interval of distances, explored by big values of the module q of the scattering vector from ray-X to low angle. The dimension mass fractal D in the wet gels is essentially equal to 2, approximately independent of R. The size of the fractal mass structure of the wet gels is limited to a characteristic length, that it increases about 3,3 nm for 7,2 nm with the increase of R of 4 for 16. The porosity of the wet gels range about 87% to 91% of the volume of the sample, with the increase of R of 4 for 16. The change of the liquid phase of the wet gels for pure water, for the rehearsals of DSC, increases the dimension fractal D and it reduces the characteristic size ξ. The value of D in the changed gels range... (Complete abstract click electronic access below)
Descrição
Palavras-chave
Fisica, Sonogéis de sílica - Propriedades, Silica sonogels - Structural property
Como citar
SCALARI, Juliana Possebon. Caracterização estrutural de géis de sílica de diferentes porosidades preparados a partir da sono-hidrólise do tetraetilortosilicato. 2008. 75 f. Dissertação (mestrado) - Universidade Estadual Paulista, Instituto de Geociências e Ciências Exatas, 2008.