889 resultados para Solid state synthesis


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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 dos Materiais - FEIS

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Oxidation states of transition metal cations in spinels-type oxides are sometimes extremely difficult to determine by conventional spectroscopic methods. One of the most complex cases occurs when there are different cations, each one with several possible oxidation states, as in the case of the magnetoresistant Mn(2-x)V(1+x)O4 (x=0, 1/3 and 1) spinel-type family. In this contribution we describe the determination of the oxidation state of manganese and vanadium in Mn(2-x)V(1+x)O4 (x=0, 1/3,1) spinel-type compounds by analyzing XANES and high-resolution K beta X-ray fluorescence spectra. The ionic models found are Mn22+V4+O4, Mn5/32+V4/33.5+O4 and Mn2+V23+O4. Combination of the present results with previous data provided a reliable cation distribution model. For these spinels, single magnetic electron paramagnetic resonance (EPR) lines are observed at 480 K showing the interaction among the different magnetic ions. The analysis of the EPR parameters show that g-values and relative intensities are highly influenced by the concentration and the high-spin state of Mn2+. EPR broadening linewidth is explained in terms of the bottleneck effect, which is due to the presence of the fast relaxing V3+ ion instead of the weak Mn2+ (S state) coupled to the lattice. The EPR results, at high temperature, are well explained assuming the oxidation states of the magnetic ions obtained by the other spectroscopic techniques. (c) 2013 Elsevier Inc. All rights reserved.

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The study of ceramic materials is constantly evolving, especially in research related to advanced ceramics. Once these have many applications, this paper relates to synthesis by solid state reaction of calcium copper titanate (CCTO) ceramic material means doping with strontium. The powders were characterized using thermal analysis techniques such as TG (thermogravimetry), DTA (differencial thermal analysis), dilatometry, X-ray diffraction (XRD) and scanning electron microscopy (SEM). The compositions have submitted weight loss at around 6% with respect to carbonates used, and was attributed a temperature of 950° C to perform the calcination according to thermogravimetric analysis. After the process of calcination and milling, the particles presented approximately spherical shapes and high percentages of substitution Ca2+ with Sr2+ was evident by the presence of necks between to particles due to the milling calcination. Analyses with Energy Dispersive Spectroscopy (EDS) showed stoichiometries in different samples very similar to the theoretical stoichiometry