132 resultados para characterizations


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One-dimensional nanostructures of KNbO3 have attracted a great interest in the scientific community, mainly because of their promising application as nanoelectromechanical systems (NEMS). However, the synthesis of KNbO3 structures becomes complex due to the natural tendency to form non-stoichiometric potassium niobates. In this context, we report on the crystallization of one-dimensional KNbO3 nanostructures through the reaction between Nb2O5 and KOH under microwave-assisted hydrothermal synthesis (M-H). The use of this synthesis method made possible a very fast synthesis of singlecrystalline powders. Based on SEM, TEM and XRD characterizations, the influence of the synthesis time and the reactants concentration in the structure and morphology of the resultant KNbO3 was established. The conditions that favor the crystallization of nanofingers were determined to be small amounts of Nb2O5 and short reaction times. (C) 2008 Elsevier B.V. All rights reserved.

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There are many advantages to using a microwave as a source of heat in hydrothermal reactions. Because it is a quick and homogeneous way to crystallize ceramic powders, it was used in this work for the production of antiferroelectric sodium mobate (NaNbO3) in a cubic-like form and its intermediary phase, disodium diniobate hydrate (Na2Nb2O6 center dot H2O), with a fiber morphology. The syntheses were carried out by treating niobic acid (Nb2O5 center dot nH(2)O) with NaOH. By changing the reaction time and the concentration of the reactants, particles with different structures and different morphologies could be obtained. The structural evolution of the products of this reaction was elucidated on the basis of the arrangement of the NbO6 octahedral units. Conclusive results were obtained with morphological and structural characterizations through XRD, TEM, MEV, and NMR and Raman spectroscopy. ((C) Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2008).

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Thin films were prepared using glass precursors obtained in the ternary system NaPO(3)-BaF(2)-WO(3) and the binary system NaPO(3)-WO(3) with high concentrations of WO(3) (above 40% molar). Vitreous samples have been used as a target to prepare thin films. Such films were deposited using the electron beam evaporation method onto soda-lime glass substrates. Several structural characterizations were performed by Raman spectroscopy and X-ray Absorption Near Edge Spectroscopy (XANES) at the tungsten L(I) and L(III) absorption edges. XANES investigations showed that tungsten atoms are only sixfold coordinated (octahedral WO(6)) and that these films are free of tungstate tetrahedral units (WO(4)). In addition, Raman spectroscopy allowed identifying a break in the linear phosphate chains as the amount of WO(3) increases and the formation of P-O-W bonds in the films network indicating the intermediary behavior of WO(6) octahedra in the film network. Based on XANES data, we suggested a new attribution of several Raman absorption bands which allowed identifying the presence of W-O and W=O terminal bonds and a progressive apparition of W-O-W bridging bonds for the most WO(3) concentrated samples (above 40% molar) attributed to the formation of WO(6) clusters. (C) 2008 Elsevier B.V. All rights reserved.

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Titanium oxide is a good candidate as new support for hydrotreating (HDT) catalysts, but has the inconvenience of presenting small surface area and poor thermal stability. To overcome these handicaps TiO2-Al2O3 mixed oxides were proposed as catalyst support. Here, the results concerning the preparation, characterization and testing of molybdenum catalyst supported on titania-alumina are presented. The support was prepared by sol-gel route using titanium and aluminum isopropoxides, chelated with acetylacetone (acac) to promote similar hydrolysis ratio for both the alcoxides. The effect of nominal complexing ratios [acac]/[Ti] and of sol aging temperature on the structural features of nanometric particles was analyzed by quasi-elastic light scattering (QELS) and N-2 adsorption isotherm measurements. These characterizations have shown that the addition of acac and the increase of aging temperature favor the full dispersion of primary nanoparticles in mother acid solution. The dried powder presents a monomodal distribution of slit-shaped micropores, formed by irregular packing of platelet primary particles, surface area superior to 200 m(2) g(-1) and mean pore size of about 1 nm. These characteristics of porous texture are preserved after firing at 673 K. The diffraction patterns of sample fired above 973 K show only the presence of anatase crystalline phase. The crystalline structure of the support remained unaltered after molybdenum adsorption, but the surface area and the micropore volume were drastically reduced. (C) 2002 Published by Elsevier B.V. B.V.

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Welding in the dentistry has been used for great part of the specialized dentist-surgeons in the implants area to solve prosthesis supported by implant adaptation problems. The development of new equipments Laser and TIG allowed a larger use of these processes in the prosthesis production. In this work, it was studied welded joints made by Laser and TIG, using commercial purity titanium, cpTi, applied in prosthesis supported by implants. The weld characterizations were carried out by light microscopy, EDS_elementary mapping, microhardness and tensile test. Through metallographic characterization, the weld bead presented a martensitic microstructure in the Laser welding process, originated from shear provoked by deformations in the lattice. This caused structural changes of the transformed area, which determines a fine plate-like morphology. In the weld bead from TIG, besides presenting higher hardness, was observed formation of Widmansttaten structure, which is characteristic of a geometric model, resulted of new phase formation along of the crystallographic plans. The martensitic structure is more refined than Widmansttaten structure, due to the high-speed cooling (10(3)degrees C/s) imposed by the Laser process.

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PbZr0.3Ti0.7O3 (PZT) films were produced by polymeric precursor route and deposited by spin-coater technique on Pt(111)/Ti/SiO2/Si(100) substrates. The films were heat-treated using different furnaces: (a) a conventional furnace, at 700 degrees C; and (b) a domestic microwave oven, at 600 degrees C. The X-ray patterns revealed that both films are single phase and reflections were identified as belongs to the PZT phase. The intensity of these reflections showed a (111), (001) and (100) preferred orientation. Morphological and electrical characterizations showed that all samples present a rather different microstructure and both with high spontaneous polarization.

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Detailed characterizations of the karyotypes of the Brazilian leptodactylid frogs Pleurodema diplolistris, the only species of Pleurodema not studied cytogenetically so far, and Physalaemus nattereri, a species in the Ph. biligonigerus group, are presented. Both karyotypes had 2n = 22 and their chromosomes had a very similar morphology, except for pair 11, which was metacentric in Pl. diplolistris and telocentric in Ph. nattereri. The localization of nucleolar organizer regions (NORs) and heterochromatic bands allowed the differentiation of chromosomes that were morphologically indistinguishable between these species, such as pairs 1, 3 and 10, which showed interstitial C-bands in Ph. nattereri, and pair 8, that had an NOR and an adjacent C-band in Pl. diplolistris. Pair 8 also has NOR-bearing chromosomes in many other Pleurodema species. However, in these species, the NOR is located proximal to the centromere on the short arm, while in Pl. diplolistris it occurred distally on the long arm, a condition that may be considered a derived state. In Ph. nattereri, the NOR occurred on chromosome I 1 and differed from the other species of the Ph. biligonigerus group. In contrast, C-banding revealed a heterochromatic block near the centromere on the short arm of pair 3, a characteristic common to all members of this group of Physalaemus.

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Transparent glasses were synthesized in the NaPO3-BaF2 WO3 tertiary system and several structural characterizations were performed by X-ray absorption spectroscopy (XANES) at the tungsten L-I and L-III absorption edges and by Raman spectroscopy. Special attention was paid to the coordination state of tungsten atoms in the vitreous network.XANES investigations showed that tungsten atoms are only six-fold coordinated (octahedra WO6) and that these glasses are free of tungstate tetrahedra (WO4).In addition, Raman spectroscopy allowed to identify a break in the linear phosphate chains as the amount of WO3 increases and the formation of P-O-W bonds in the vitreous network indicating the modifier behavior of WO6 octahedra in the glass network. Based on XANES data, we suggested a new attribution of several Raman absorption bands which allowed to identify the presence of W-O- and W=O terminal bonds and a progressive apparition of W-O-W bridging bonds for the most WO3 concentrated samples (≥ 30% molar) due to the formation of WO6 clusters. © 2004 Elsevier B.V. All rights reserved.