243 resultados para Thermogravimetric analysys
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Thin solid films of bis benzimidazo perylene (AzoPTCD) were fabricated using physical vapor deposition (PVD) technique. Thermal stability and integrity of the AzoPTCD PVD films during the fabrication (similar to 400 degrees C at 10(-6) Torr) were monitored by Raman scattering. Complementary thermogravimetric results showed that thermal degradation of AzoPTCD occurs at 675 degrees C. The growth of the PVD films was established through UV-vis absorption spectroscopy, and the surface morphology was surveyed by atomic force microscopy (AFM) as a function of the mass thickness. The AzoPTCD molecular organization in these PVD films was determined using the selection rules of infrared absorption spectroscopy (transmission and reflection-absorption modes). Despite the molecular packing, X-ray diffraction revealed that the PVD films are amorphous. Theoretical calculations (density functional theory, B3LYP) were used to assign the vibrational modes in the infrared and Raman spectra. Metallic nanostructures, able to sustain localized surface plasmons (LSP) were used to achieve surface-enhanced resonance Raman scattering (SERRS) and surface-enhanced fluorescence (SEF).
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Organic-inorganic hybrid materials based on the assembly between inorganic 2D host structure and polymer have received considerable attention in the last few years. This emerging class of materials presents several applications according to their structural and functional properties. Particularly, among others, layered double hydroxides (LDHs) provide the opportunity of preparing new organically modified 2D nanocomposites. Pyrrole carboxylic acid derivatives, namely 4-(lH-pyrrol-1-yl)benzoate, 3-(pyrrol-i-yl)-propanoate,7-(pyrrol-1-yl)-heptanoate, and aniline carboxylic acid derivative, namely 3-aminobenzoic acid, have been intercalated in LDHs of intralamellar composition Zn2Al(OH)(6). The LDHs were synthesized by the co-precipitation method at constant pH followed by hydrothermal treatment for 72 h. The materials were characterized by powder X-ray diffraction patterns (PXRD), transmission electron microscopy (TEM) thermogravimetric analysis (TGA), and electron spin resonance (ESR). The basal spacing found by the PXRD technique gives evidence of the formation of bilayers of the intercalated anions. ESR spectra present a typical signal with a superhyperfine structure with 6 + 1 lines (g = 2.005 +/- 0.0004), which is assigned to the interaction between a carboxylate radical from the guest molecules and a nearby aluminium nucleus (I = 5/2) from the host structure. Additionally, the ESR data suggest that the monomers are connected to each other in limited number after thermal treatment. (c) 2007 Elsevier Ltd. All rights reserved.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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The characteristics of log smoldering after an Amazonian deforestation fire are described. The experiment was carried out in 2001 at the Caiabi farm, near the city of Alta Floresta, state of Mato Grosso, Brazil, as part of a set of tests that have been performed in the same area since 1997. A 200 x 200m(2) test area was slashed in the beginning of June and burned on 20 August. The area contained 507 logs with diameter at breast height (DBH) higher than 10 cm, per hectare. In the day following the main burn 59 logs were found to remain smoldering, a number that corresponds to 2.9% of the total in the area. We chose 11 of the 59 logs to have their smoldering process monitored. Their diameter, moisture content and CHN dry biomass composition after the plot burn and before smoldering were determined. Other parameters such as temperature distribution while smoldering, porosity, density and mass volatilized during thermogravimetric test were also determined. Average smoldering speeds were in the range from 0.8 to 1.5 cm h(-1) for logs that smoldered without transition to the flaming regime. The average speed increased to 2.1 cm h(-1) for those logs that oscillated between smoldering and flaming. The speeds were lower overnight as compared to values determined during daytime for the same log. Higher log moisture contents were found to produce decreased speeds. Micro-porous biomass was not observed in the set of the 11 selected logs. Smoldering was observed to occur at substantial intensity in crossing of logs, with no longitudinal propagation. (C) 2003 Elsevier Ltd. All rights reserved.
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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A composite of cellulose extracted from bagasse with Nb2O5 center dot nH(2)O in three different proportions (16.67, 37.5 and 50.0 wt%) was prepared using the co-precipitation method. The materials were characterized by X-ray diffractometry (XRD), Fourier transform infra-red spectroscopy (FTIR), thermogravimetric analysis (TG/DTG), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). TG data obtained show that the presence of inorganic material influenced slightly the stability of the hybrid material. The precipitation of 16.67 wt.% of oxide was sufficient to inhibit the combustion peaks present in the DSC curve of cellulose. This work will help find new applications for these materials. Published by Elsevier Ltd.
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Este trabalho apresenta um método de produção para a obtenção de cinza de casca de arroz (CCA) de elevada reatividade a partir de um processo de combustão não controlado. São detalhados os processos de obtenção da CCA, assim como sua atividade pozolânica. Pela Análise Termogravimétrica (TGA), foi possível quantificar o consumo de portlandita por parte da CCA, ou seja, a reação pozolânica. Adicionalmente, foram preparadas argamassas com diferentes porcentagens de CCA (5%, 10% e 15%) com o objetivo de comprovar sua influência nas propriedades mecânicas. Os resultados obtidos mostram que a CCA em estudo apresenta elevada reatividade, podendo ser utilizada como uma fonte alternativa da sílica ativa (SA).
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Octakis(cyanopropyldimethylsiloxy)octasilsesquioxane was prepared and characterized by C-13, Si-29 NMR (MAS), SEM, FF-IR, XRD and thermogravimetric techniques. The four groups alpha, beta, gamma, kappa (to the terminal silicon atom), associated with an acrylonitrile, were clearly seen in the C-13 NMR (alpha-CH2 at 17.9; P-CH2 at 31.3; gamma-CH, at 50.4; K-C N at 59.0 ppm). The Si-29 NMR spectrum of the final product, exhibits only Q type silicon signal, ascribed to Q(4) (-118.0 ppm). The presence of acrylonittile substituted for octameric cube confers a relative change phase and thermal stability to the material. With regard to the applications for this new material, it was intended, in this case, to react with Na-2[Fe(CN)(5)NH3] by chemical substitution. This composite was incorporated into a carbon paste electrode and the electrochemical studies were performed by cyclic voltammetry. The cyclic voltammogram of the modified graphite paste electrode, showed one redox couples with formal potential (E-1/2(ox)) = 0.24 V versus SCE. (c) 2006 Elsevier B.V. All rights reserved.
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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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Cellulose nanowhiskers were prepared by sulfuric acid hydrolysis from coconut husk fibers which had previously been submitted to a delignification process. The effects of preparation conditions on the thermal and morphological behavior of the nanocrystals were investigated. Cellulose nanowhisker suspensions were characterized by Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), thermogravimetric analysis (TGA) and X-ray diffraction. Results showed that it was possible to obtain ultrathin cellulose nanowhiskers with diameters as low as 5 nm and aspect ratio of up to 60. A possible correlation between preparation conditions and particle size was not observed. Higher residual lignin content was found to increase thermal stability indicating that by controlling reaction conditions one can tailor the thermal properties of the nanowhiskers. Published by Elsevier Ltd.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)