881 resultados para powder diffraction


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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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PTCR barium titanate has been prepared following two different powder preparation techniques: the solid-state reaction route and co-precipitation route for the comparison of results. The co-precipitation route produces better PTCR characteristics with low room temperature resistivity and better reproducibility of prepared samples. The effects of different concentrations of additives like donors, acceptors and excess titanium have been optimized to get good quality PTCR samples. (C) 2002 Elsevier B.V. B.V. All rights reserved.

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Results of differential scanning calometry (DSC), x-ray diffraction (XRD), and F-19 nuclear magnetic resonance (NMR) of InF3-based glasses, treated at different temperatures, ranging from glass transition temperature (T-g) to crystallization temperature (T-c), are reported. The main features of the experimental results are as follows. DSC analysis emphasizes several steps in the crystallization process. Heat treatment at temperatures above T-g enhances the nucleation of the first growing phases but has little influence on the following ones. XRD results show that several crystalline phases are formed, with solid state transitions when heated above 680 K, the F-19 NMR results show that the spin-lattice relaxation, for the glass samples heat treated above 638 K, is described by two time constants. For samples treated below this temperature a single time constant T-1 was observed. Measurements of the F-19 spin-lattice relaxation time (T-1), as a function of temperature,made possible the identification of the mobile fluoride ions. The activation energy, for the ionic motion, in samples treated at crystallization temperature was found to be 0.18 +/- 0.01 eV. (C) 1998 American Institute of Physics.

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SrBi2Ta2O9 ferroelectric thick films were prepared by electrophoretic deposition (EPD). For that, ceramic powders were prepared by chemical method in order to obtain compounds with chemical homogeneity. The polymeric precursor method was used for the synthesis of the SrBi2Ta2O9 powder. The crystallographic structure of the powder was examined by X-ray diffraction, and the surface area was determined by single point BET adsorption. The 0.03 vol% suspension was formed by dispersing the powder in water using two different polymers as dispersants: an ester polyphosphate (C213) and an ammonium polyacrilate (Darvan 821-A). The influence of the different dispersants on the powder surface properties were investigated by zeta potential measurements. The films were deposited on platinum-coated alumina and Pt/Ti/SiO2/Si substrates by electrophoretic deposition using a 4 mA constant current, for 10 min, with two parallel electrodes placed at a separation distance of 3 min in the suspension. Several cycles of deposition-drying of the deposit was carried out until the desired thickness was obtained. After thermal treatment at temperatures ranging from 700 to 1000degreesC, the films were characterized by X-ray diffraction and scanning electron microscopy.

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

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In this work, initial crystallographic studies of human haemoglobin (Hb) crystallized in isoionic and oxygen-free PEG solution are presented. Under these conditions, functional measurements of the O-2-linked binding of water molecules and release of protons have evidenced that Hb assumes an unforeseen new allosteric conformation. The determination of the high-resolution structure of the crystal of human deoxy-Hb fully stripped of anions may provide a structural explanation for the role of anions in the allosteric properties of Hb and, particularly, for the influence of chloride on the Bohr effect, the mechanism by which Hb oxygen affinity is regulated by pH. X-ray diffraction data were collected to 1.87 Angstrom resolution using a synchrotron-radiation source. Crystals belong to the space group P2(1)2(1)2 and preliminary analysis revealed the presence of one tetramer in the asymmetric unit. The structure is currently being refined using maximum-likelihood protocols.

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The aim of this work is to report on the luminescence properties of BaZnSiO4 activated by Eu3+ and Mn2+ ions. Doped and undoped powder samples were prepared by solid-state reaction starting from oxides and carbonates or Ba2SiO4:Eu3+ and Zn2SiO4:Mn2+ precursors. X-ray diffraction powder data, IR vibrational, and UV-vis luminescence spectroscopies were carried out. Results showed that doped and undoped samples from both types of precursors have the same structure and crystallize with a superstructure of hexagonal kalsilite. Vibrational spectroscopy has confirmed the formation of a silicate group, which outlines differences between products and silicate precursors. The observed luminescence assigned to Eu3+ and Mn2+ transitions covered most parts of the visible spectrum, an important requirement for phosphors in fluorescent low-pressure mercury vapor lamps.

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Gallium-doped zinc oxide (ZnO:Ga 1, 2 3, 4 and 5 at%) samples were prepared in powder form by modifying the Pechini method. The formation of zinc gallate (ZnGa2O4) With the spinel crystal structure was observed even in ZnO:Ga 1 at% by X-ray diffraction. The presence of ZnGa2O4 in ZnO:Ga samples was also evidenced by luminescence spectroscopy through its blue emission at 430 nm, assigned to charge transfer between Ga3+ at regular octahedral symmetry and its surrounding O2- ions. The amount of ZnGa2O4 increases as the dopant concentration increases, as observed by the quantitative phase analysis by the Rietveld method. (C) 2006 Elsevier B.V. All rights reserved.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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SrMoO4 doped with rare earth are still scarce nowadays and have attracted great attention due to their applications as scintillating materials in electro-optical like solid-state lasers and optical fibers, for instance. In this work Sr1-xEuxMoO4 powders, where x = 0.01; 0.03 and 0.05, were synthesized by Complex Polymerization (CP) Method. The structural and optical properties of the SrMoO4:Eu3+ were analyzed by powder X-ray diffraction patterns, Fourier Transform Infra-Red (FTIR), Raman Spectroscopy, and through Photoluminescent Measurements (PL). Only a crystalline scheelite-type phase was obtained when the powders were heat-treated at 800 A degrees C for 2 h, 2 theta = 27.8A degrees (100% peak). The excitation spectra of the SrMoO4:Eu3+ (lambda(Em.) = 614 nm) presented the characteristic band of the Eu3 + 5L6 transition at 394 nm and a broad band at around 288 nm ascribed to the charge-transfer from the O (2p) state to the Mo (4d) one in the SrMoO4 matrix. The emission spectra of the SrMoO4:Eu3+ powders (lambda(Exc.) = 394 and 288 nm) show the group of sharp emission bands among 523-554 nm and 578-699 nm, assigned to the D-5(1)-> F-7(0,1and 2) and D-5(0)-> F-7(0,1,2,3 and 4), respectively. The band related to the D-5(0)-> F-7(0) transition indicates the presence of Eu3+ site without inversion center. This hypothesis is strengthened by the fact that the band referent to the D-5(0)-> F-7(2) transition is the most intense in the emission spectra.

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Moisture equilibrium data of persimmon pulp powders with 50% maltodextrin (dry basis) obtained with different drying methods were determined at 20, 30, 40 and 50 degrees C. The spray-dryer gave a dry product with a higher adsorption capacity than the other methods. The vacuum- and freeze-dried products had the same adsorption capacity. The highest isosteric heat of sorption was observed for powders produced by spray-drying. The isokinetic temperature (T(B)) calculated for persimmon pulp powder obtained by vacuum-, spray- and freeze-drying were 541.4 K, 616.3 K, 513.2 K, respectively. The sorption process was spontaneous and enthalpy controlled.

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Nanostructured KSr2Nb5O15 oxide was synthesized by the polymeric precursor method, a chemical synthesis route based on the Pechini's method. The X-ray diffraction (XRD) pattern of the calcined powder at 1150 degreesC were performed in the angular range 5 less than or equal to 20 less than or equal to 120degrees with a 0.02degrees step and a fixed counting time of 30 s. The XRD data were analyzed by the Rietveld refinements using the FullProf software. The results C showed a tetragonal system with the tetragonal tungsten bronze structure (TTB) type (a = 12.4585 (2) Angstrom and c = 3.9423 (6) Angstrom, V = 611,90 (2) Angstrom). In this work, the sites occupancy by the K+ and Sr2+ cations on the TTB type structure were determined. The thermal parameters (B) were analyzed. (C) 2004 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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Hybrid reflections (HRs) involving substrate and layer planes (SL type) [Morelhao et al., Appl. Phys. Len. 73 (15), 2194 (1998)] observed in Chemical Beam Epitaxy (CBE) grown InGaP/GaAs(001) structures were used as a three-dimensional probe to analyze structural properties of epitaxial layers. A set of (002) rocking curves (omega-scan) measured for each 15 degrees in the azimuthal plane was arranged in a pole diagram in phi for two samples with different layer thicknesses (#A -58 nm and #B - 370 nm) and this allowed us to infer the azimuthal epilayer homogeneity in both samples. Also, it was shown the occurrence of (1 (1) over bar3) HR detected even in the thinner layer sample. Mappings of the HR diffraction condition (omega:phi) allowed to observe the crystal truncation rod through the elongation of HR shape along the substrate secondary reflection streak which can indicate in-plane match of layer/substrate lattice parameters. (C) 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim