334 resultados para Dynamic Mechanical Thermal Analysis


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Pós-graduação em Engenharia Mecânica - FEG

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The Polymeric Precursor Method has proved suitable for synthesizing reactive powders using low temperatures of calcination, especially when compared with conventional methods. However, during the thermal decomposition of the polymeric precursor the combustion event can be releases an additional heat that raises the temperature of the sample in several tens of degrees Celsius above the set temperature of the oven. This event may be detrimental to some material types, such as the titanium dioxide semiconductor. This ceramic material has a phase transition at around 600 ° C, which involves the irreversible structural rearrangement, characterized by the phase transition from anatase to rutile TiO2 phase. The control of the calcination step then becomes very important because the efficiency of the photocatalyst is dependent on the amount of anatase phase in the material. Furthermore, use of dopant in the material aims to improve various properties, such as increasing the absorption of radiation and in the time of the excited state, shifting of the absorption edge to the visible region, and increasing of the thermal stability of anatase. In this work, samples of titanium dioxide were synthesized by the Polymeric Precursor Method in order to investigate the effect of Fe (III) doping on the calcination stages. Thermal analysis has demonstrated that the Fe (III) insertion at 1 mol% anticipates the organic decomposition, reducing the combustion event in the final calcination. Furthermore, FTIR-PAS, XRD and SEM results showed that organic matter amount was reduced in the Fe (III)-doped TiO2 sample, which reduced the rutile phase amount and increased the reactivity and crystallinity of the powder samples.

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The urban residues put in landfill of the city of Sa˜o Carlos-SP, Brazil, in 2004 represent 58.7 % of decomposed organic material. The aim of this research was to characterize samples of urban solid waste and its organic extracts targeting the use of this residue without damaging the environment. The curves were obtained in a nitrogen atmosphere, a heating rate of 20 C min-1 , the temperature of 30–600 C. In the original sample after humidity loss, an event occured concerning the water constitution in the TG curve with an endothermic peak in the DTA curve. There was a presence of inorganic residue in the ashes. The organic matter present in the USR sample disposed in the landfill is constituted by several polarity, organics compounds from the degradation of lignin, cellulose, lipids, and other materials which thermal stabilities are distinct. The hexane extract features in its constitution two fatty acids, stearic and triacontano´ic, which are nonpolar compounds originating from bacteria present in the residue. The acids groups in extract hexane also were evidenced by X-ray diffraction and FTIR.

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The potential of clear Ga2S3-GeS2-CsCl based sulfide glasses transparent up to 11.5 μm to be used as new optical material for multispectral applications has been investigated. The addition of large amount of chlorine ions – above 40 mol.% of CsCl – into the chalcogenide vitreous network in order to produce colorless glasses results in a drastic increase of their water contamination. We report for the first time, to the best of our knowledge, the purification of cesium chloride CsCl by dynamic distillations under vacuum in order to reduce water and hydroxyl group contamination before complete melting of the glass. Besides, sulfur purification by dynamic and static distillations was also performed in the implemented method. The obtained glasses were then characterized by UV-visible and infrared (FTIR) spectroscopies, by electron probe microanalysis (EPMA), thermal analysis (DSC), and their refractive indices in the visible and near infrared ranges were also measured. A large improvement of the glass transmission spectrum has been achieved with an estimated reduction of about 45 times of the OH and H2O content and 60 times of the SH content. The glass thermal molding ability and chemical durability with and without protective coating have been tested to probe their potential for fabrication of complex optics.

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The influence of both thermal treatment and laser irradiation on the structural and optical properties of films in the Sb 2 O 3 –Sb 2 S 3 system was investigated. The films were prepared by RF-sputtering using glass compositions as raw materials. Irreversible photodarkening effect was observed after exposure the films to a 458nm solid state laser. It is shown, for the first time, the use of holographic technique to measure “in situ”, simultaneously and independently, the phase and amplitude modulations in glassy films. The films were also photo-crystallized and analysed “in situ” using a laser coupled to a micro-Raman equipment. Results showed that Sb 2 S 3 crystalline phase was obtained after irradiation. The effect of thermal annealing on the structure of the films was carried out. Different from the result obtained by irradiation, thermal annealing induces the crystallization of the Sb 2 O 3 phase. Photo and thermal induced effects on films were studied using UV–Vis and Raman spectroscopy, atomic force microscopy (AFM), thermal analysis (DSC), X-ray diffraction, scanning electron microscopy (MEV) and energy-dispersive X-ray spectroscopy (EDX).

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Thermogravimetric analysis is one of the most common instrumental techniques used for the characterization of pastes, mortars and concretes based on both calcium hydroxide and Portland cement. Important information about pozzolanic materials can be assessed concerning calcium hydroxide consumption and the formation of new hydrated products. Nevertheless, in some cases, problems associated with the overlapped decomposition processes for hydrates make the analysis of obtained data difficult. In this paper, the use of high-resolution thermogravimetric analysis, a powerful technique that allows separating decomposition processes in analysis of hydrated binders, was performed for spent FCC catalyst-Portland cement pastes. These pastes were monitored for 1, 4, 8 h and 1, 2, 3, 7 and 28 curing days. In order to study the influence of the pozzolanic material (spent FCC catalyst), Portland cement replacements of 5, 15 and 30 % by mass were carried out. The presence of spent FCC catalyst in blended pastes modified the amount and the nature of the formed hydrates, mainly ettringite and stratlingite.

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Solid state chelates of general formula H-2[M(EDTA)] . nH2O, where M is Co, Ni, Cu or Zn, and EDTA is ethylenediaminetetraacetate, were prepared. Thermogravimetry-derivative thermogravimetry (TG-DTG), differential thermal analysis (DTA) and complexometry were used to characterize and to study the thermal stability and thermal decomposition of these compounds.