886 resultados para preparation and synthetic applications


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Silica gel with a surface area of 500 m2g-1 and an average pore diameter of 60 angstrom was chemically modified with Ti(IV) oxide using the grafting method. The amount of metal oxide attached to the surface was 1.8.10(-3) mol g-1. The X-ray photoelectron spectra showed that the metal ion species on the surface are Ti(IV) in TiO2 and MTiO3 (M = Ca2+, Sr2+, Ba2+ and Pb2+), i.e. they have the binding energy of Ti2p3/2 = 458.7 eV. The dehydration of the solid at higher temperature increased the O(II)/Ti (O(II) = oxygen bound to titanium atom) ratio, presumably due to a reticulation of the hydrous Ti(IV) oxide on the silica surface at higher temperatures. Migration of Ti(IV) into the silica gel matrix was observed but the specific surface area was not significantly changed.

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This work presents the preparation of SrBi2Nb2O9 (SBN) directly by the combustion synthesis. Strontium nitrate, niobium ammonium oxalate (NH4H2[NbO-(C2O4)(3)].3H(2)O) and bismuth oxide were used as oxidant reactants and urea as fuel. The influence of the fuel was evaluated by the addition of different fuel amounts (50%, 100%, 200% and 300%), 100% being the stoichiometric proportion. The XRD patterns showed that the SBN perovskite crystallized as the majority phase. The as-synthesized stoichiometric powder presented a specific surface area of around 13 m(2)/g and a mean grain size of around 16 nm. Dilatometric measurements showed that the maximum sintering rate occurs at 1275degreesC. The determination of the ferroparaelectric transition showed a Curie temperature (T-c) of 429degreesC. (C) 2002 Elsevier B.V. B.V. All rights reserved.

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Polycrystalline tin oxide thin films were prepared from ethanol solution of SnCl2.H2O (concentrations: 0.05, 0.1, 0.2 and 0.4 mol/dm(3)) at different substrate temperatures ranging from 300 to 450 degreesC. The kinetic deposition processes were studied in terms of various process parameters. The crystal phases, crystalline structure, grain size and surface morphology are revealed in accordance to X-ray diffractometry and scanning electron microscopy (SEM). Texture coefficients (TCs) for (110), (2 0 0), (2 11) and (3 0 1) reflections of the tetragonal SnO2 were calculated. Structural characteristics of deposited films with respect to varying precursor chemistry and substrate temperature are presented and discussed. (C) 2003 Published by Elsevier B.V.

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Various properties of particles can be altered by coating them with a layer of different chemical composition. Yttrium iron garnet (YIG) particles has been coated with silica for control of their sintering, corrosion resistance, and stabilization of magnetic properties. This silica cover was obtained by hydrolysis of tetraethylorthosilicate (TEOS) in 2-propanol. This material was characterized by transmission (TEM) electron microscopy, (XEDS) X-ray energy-dispersive spectrometry, (XPS) X-ray photoemission spectroscopy and (VSM) vibrating sample magnetometry. YIG was heterocoagulated by silica as indicated by TEM micrographies. XPS measurements indicated that only binding energy for silicon and oxygen was found on the silica shell, which confirms that the YIG was covered. The values of the saturation magnetization differ from the heterocoagulated system to well-crystallized YIG.

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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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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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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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PANI-LiNi0.8Co0.2O2 nanocomposite material with improved properties as positive electrode was prepared by a new synthesis method. In a first step, LiNi0.8Co0.2O2 mixed oxide in the form of a fine powder was dispersed in aniline and this suspension was sprayed on the surface of an aqueous solution of HCl and ammonium peroxodisulfate. The resulting PANI-LiNi0.8Co0.2O2 nanocomposite is spontaneously formed by polymerization of the aniline molecules present in the drops together with small particles of the oxide. This method induces the formation of nanocomposites showing a better distribution of the oxide particles in the polymer matrix than that observed in related PANI-LiNi0.8Co0.2O2 microcomposites prepared under ultrasound irradiation to disperse the oxide particles during PANI polymerization. Measurements of electrical conductivity and zeta potential, as well as structural characterization of PANI-LiNi0.8Co0.2O2 nanocomposites, reveal the existence of relatively strong interactions between the conducting polymer and the oxide particles. This feature determines higher values of the electrical conductivity (0.5 S cm(-1)) and of the average operative voltage (3.6 V), as well as of other technological parameters of the nanocomposite when it is used as the positive electrode of rechargeable lithium batteries, in comparison to those of the related microcomposite materials already reported.

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Solid state compounds were prepared of Ln-4-MeO-BP, where Ln is a trivalent lanthanide (except promethium) or yttrium, and 4-MeO-BP is 4-methoxybenzylidenepyruvate. Thermogravimetry-derivative thermogravimetry (TG-DTG), differential scanning calorimetry (DSC) and other methods of analysis have been used to characterize and to study the thermal stability and thermal decomposition of these compounds. © 1993.

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The preparation of spherical Y2O2S and Y2O2S:Eu particles using a solid-gas reaction of monodispersed precursors with elemental sulfur vapor under an argon atmosphere has been investigated. The precursors, undoped and doped yttrium basic carbonates, are synthesized by aging a stock solution containing the respective cation chloride and urea at 82-84 °C. Y2O2S and Y2O2S:Eu were characterized in terms of their composition, crystallinity and morphology by chemical analysis, X-ray powder diffraction (XRD), IR spectroscopy, and scanning electron microscopy (SEM). The Eu-doped oxysulfide was also characterized by atomic absorption spectrophotometry and luminescence spectroscopy. The spherical morphology of oxysulfide products and of basic carbonate precursors suggests a topotatic inter-relationship between both compounds.

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A polymeric precursor solution was employed in preparing SrBi2Nb2O9 (SBN) powder and thin films dip coated onto Si(100) substrate. XRD results show that the SBN perovskite phase forms at temperatures as low as 600°C through an intermediate fluorite phase. This fluorite phase is observed for samples heat-treated at temperatures of 400 and 500°C. After heat treatment at temperatures ranging from 300 to 800°C, thin films were shown to be crack free. Grazing incident angle XRD characterization shows the occurrence of the fluorite intermediate phase for films also. The thickness of films, measured by MEV, was in the order of 80-100 nm.