320 resultados para thermogravimetry and differential thermal analysis
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Strontium stannate titanate Sr(Sn, Ti)O3 is a solid solution between strontium stannate (SrSnO3) and strontium titanate (SrTiO3). In the present study, it was synthesized at low temperature by the polymeric precursor method, derived from the Pechini process. The powders were calcined in oxygen atmosphere in order to eliminate organic matter and to decrease the amount of SrCO3 formed during the synthesis. The powders were annealed at different temperatures to crystallize the samples into perovskites-type structures. All the compositions were studied by thermogravimetry (TG) and differential thermal analysis (DTA), infrared spectroscopy (IR) and X-ray diffraction (XRD). The lattice former, Ti4+ and Sn4+, had a meaningful influence in the mass loss, without changing the profile of the TG curves. On the other hand, DTA curves were strongly modified with the Ti4+:Sn4+ proportion in the system indicating that intermediate compounds may be formed during the synthesis being eliminated at different temperature ranges, while SrCO3 elimination occurs at higher temperature as shown by XRD and IR spectra. © 2013 Akadémiai Kiadó, Budapest, Hungary.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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The basic carbonates of lanthanum with 10%, 20%, 50% and 80% of europium were prepared by precipitation from homogeneous solutions via the hydrolysis of urea, without the addition of an auxiliary anion, at two different temperatures. Elemental analysis, complexometric methods, X-ray diffraction patterns, solid state IR absorption, thermogravimetry/derivative thermogravimetry (TG/DTG) and differential thermal analysis (DTA) were used to characterise the compounds and study their thermal behaviour.
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Starch is one of the most important sources of reserve of carbohydrate in plants and the main source in the human diet due to its abundance in the nature. There no other food ingredient that can be compared with starch in terms of sheer versatility of application in the food industry. Unprocessed native starches are structurally too weak and functionally too restricted for application in today’s advanced food and industrial technologies. The main objective of this study was to compare the thermal behavior of native cassava starch and those treated with hydrogen peroxide, as well as those treated with hydrogen peroxide and ferrous sulfate. The cassava starch was extracted from cassava roots (Manihot esculenta, Crantz) and treated by standardized hydrogen peroxide (H2 O2 ) solutions at 1, 2 and 3% (with or without FeSO4 ). Investigated by using they are thermoanalytical techniques: thermogravimetry - TG, differential thermal analysis – DTA and differential scanning calorimetry - DSC, as well as optical microscopy and X-ray powder diffractometry. The results showed the steps of thermal decomposition, changes in temperatures and in gelatinization enthalpy and small changes in crystallinity of the granules.
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Pequenas partículas de fase peroviskita de BaMnO3 foram preparadas por dois métodos: a rota da coprecipitação convencional (RCC) e o método convencional de microemulsão (MCM). As técnicas instrumentais utilizadas para caracterizar as amostras foram: microscopia eletrônica de varredura (SEM), difratometria de raios X (XRD), termogravimetria (TG) e análise térmica diferencial (DTA). A síntese de materiais em sistemas coloidais auto-organizados tem por objetivo aumentar a homogeneidade de tamanho e forma das partículas. Nos últimos anos aumentou a busca por materiais mais uniformes visando o aperfeiçoamento da microestrutura. A rota de microemulsão é um método alternativo para a síntese de materiais porque permite o controle da relação entre as concentrações de água e do tensoativo, (w), o qual controla o tamanho das gotículas de microemulsão denominadas microreatores. Peroviskita pura obtida de microemulsão forma-se em temperatura menor do que a fase precipitada, e resulta.em partículas com distribuição de tamanho mais adequada, de aproximadamente 0,1 mm de diâmetro comparado com a média de 0,5 mm das partículas coprecipitadas.
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The effect of Cu2+ contents and of firing temperature on sintering and crystallite growth of nanocrystalline SnO2 xerogels was analyzed by thermoanalysis (mass loss (TG), linear shrinkage, and differential thermal analysis (DTA)), X-ray powder diffraction (XRPD), and EXAFS (extended X-ray absorption fine structures) measurements. Samples were prepared by two methods: (a) coprecipitation of a colloidal suspension from aqueous solution containing both Sn(IV) and Cu(II) ions and (b) grafting copper(II) species on the surface of tin pride gel. The thermoanalysis has shown that the shrinkage associated with the mass loss decreases by increasing the amount of copper. The EXAFS measurements carried out at the Cu K edge have evidenced the presence of copper in substitutional solid solution for the dried xerogel prepared with 0.7 mol % of copper, while for higher concentration of doping, copper has been observed also at the external surface of crystallites. The solid solution is metastable and copper migrates toward the surface during firing. The XRPD and DTA results have shown a recrystallization process near 320 degrees C, which leads to crystallite growth. The presence of copper segregated near the crystallite surface controls its growth.
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Aluminium Hydroxides were precipitated from Aluminium Nitrate and Ammonium Hydroxide, at the temperatures 64 degrees C (hot) and 25 degrees C (cold), under the pH conditions 5, 7 and 9. The samples were characterized by X-Ray Diffraction (XRD) and Differential Thermal Analysis (DTA). The hydroxide precipitated at pH 9 and 64 degrees C is built up by pseudoboehmite and a minor share of others apparently amorphous hydroxides. The crystallinity of the hot yielded pseudoboehmite diminishes with the pH. The crystallite size was evaluated as about 40 Angstrom for the best crystallized sample. The cold precipitated product is apparently composed by amorphous or very poorly crystallized hydroxides. Upon heating, the cold precipitated hydroxides, and the low pH and hot precipitated hydroxide, release their structural water before the occurrence, about 430 degrees C, of the transition of the pseudoboehmite to gamma-alumina, and exhibit a shifting (towards low temperature side) and a broadening in the peak of the transition to alpha-alumina, which occurs at 1200 degrees C in the pseudoboehmite pattern. The yielded pseudo-boehmite peptized by HNO3, addition and gelified by evaporation in a critical concentration approximately 0.17 gcm(-3).
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Pós-graduação em Química - IBILCE
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Pós-graduação em Química - IBILCE
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Pós-graduação em Ciência e Tecnologia de Materiais - FC