Synthesis and characterization of Li2ZnTi3O8 spinel using the modified polymeric precursor method

In this work we report the synthesis procedure, crystallographic, structural and magnetic properties of the Li2ZnTi3O8 spinel obtained using a modified polymeric precursor method. This synthesis method generates very reactive and property-controlled nanoparticles. The samples were characterized using X-ray powder diffraction (XRD) associated to the Rietveld refinement method, thermogravimetric analysis (TG), specific surface area, scanning electron microscopy (SEM) and magnetic susceptibility measurements.The phase formation temperature of the lithium zinc titanate spinel was observed to decrease due to the homogeneity and highly controlled nanometric particle size. (C) 2003 Elsevier B.V. All rights reserved.

Characterization of ZnO-degraded varistors used in high-tension devices

The effects of the degradation process on the structural, microstructural and electrical properties of ZnO-based varistors were analyzed. Rietveld refinement showed that the BiO2-x phase is affected by the degradation process. Besides the changes in the spinel phase, the degradation process also affects the lattice microstrain in the ZnO phase. Scanning electron microscopy analysis showed electrode-melting failure, while wavelength dispersive X-ray spectroscopy qualitative analysis showed deficiency of oxygen species at the grain boundaries in the degraded samples. Atomic force microscopy using electrostatic mode force illustrated a decrease in the charge density at the grain boundaries of the degraded sample. Transmission electron microscopy showed submicrometric spinel grains embedded in a ZnO matrix, but their average grain size is smaller in the degraded sample than in the standard one. Long pulses appeared to be more harmful for the varistors' properties than short ones, causing higher leakage current values. The electrical characteristics of the degraded sample are partially restored after heat treatment in an oxygen-rich atmosphere. (C) 2006 Elsevier Ltd. All rights reserved.

The nature of the photo luminescence in amorphized PZT

The polymeric precursor method was used to synthesize lead zirconate titanate powder (PZT). The crystalline powder was then amorphized by a high-energy ball milling process during 120h. A strong photoluminescence emission was observed at room temperature for the amorphized PZT powder. The powders were characterized by XRD and the percentage of amorphous phase was calculated through Rietveld refinement. The microstructure for both phases was investigated by TEM. The optical gap was calculated through the Wood and Tauc method using the UV-Vis. data. Quantum mechanical calculations were carried out to give an interpretation of the photoluminescence in terms of electronic structure. (C) 2004 Elsevier B.V. All rights reserved.

Photoluminescence of crystalline and disordered BTO : Mn powder: Experimental and theoretical modeling

Disordered and crystalline Mn-doped BaTiO3 (BTO:Mn) powders were synthesized by the polymeric precursor method. After heat treatment, the nature of visible photoluminescence (PL) at room temperature in amorphous BTO:Mn was discussed, considering results of experimental and theoretical studies. X-ray diffraction (XRD), PL, and UV-vis were used to characterize this material. Rietveld refinement of the BTO:Mn from XRD data was used to built two models, which represent the crystalline BTO:Mn (BTO:Mn,) and disordered BTO:Mn (BTO:Mn-d) structures. Theses models were analyzed by the periodic ab initio quantum mechanical calculations using the CRYSTAL98 package within the framework of density functional theory at the B3LYP level. The experimental and theoretical results indicated that PL is related with the degree of disorder in the BTO:Mn powders and also suggests the presence of localized states in the disordered structure. (c) 2006 Elsevier B.V. All rights reserved.

Importance of oxygen atmosphere to recover the ZnO-based varistors properties

A methodology to recover the non-ohmic properties of ZnO based varistors after degradation with long and short duration pulses was proposed in this work. The basic idea consists in submitt the degraded ceramics at different temperatures and oxygen flows. Thermal treatment at 900 degrees C for 2 h with oxygen flow of 15 l/h allowed to obtain better non-linear coefficient (alpha= 52.5) compared to the standard sample. Rietveld refinement showed that with the thermal treatment, the oxygen species and the beta-Bi2O3 phase, lost in the degradation process, are recovered in the grain boundary.

Effect of PbO excess on the formation of lead magnesium niobate perovskite by the columbite method

The effect of lead excess on the pyrochlore-type formation in Pb(Mg1/3Nb2/3)O-3 (PMN) powders has been investigated. The polymeric precursor method was used in the synthesis of the columbite in association to the partial oxalate method to synthesize the PMN powder samples. Structure refinement of the columbite precursor and PMN powders was carried out using the Rietveld method. The quantitative phase analysis showed that the amount of perovskite phase is not affected by PbO excess, but a great excess drives the pyrochlore-type formation so that 3 wt.% of PbO causes the predominance of Mg-containing pyrochlore phase. Using the refined data obtained from the Rietveld refinement, the compositional fluctuation in the perovskite phase was calculated from Nb/Mg ratio values and Pb occupation factor. Mg inclusion occurs concomitant with Ph one into PMN perovskite phase and this effect is directed by PbO excess during powder synthesis. (C) 2003 Elsevier B.V. All rights reserved.

Composition and electronic structure of Zn7-xMxSb2O12 (M = Ni and Co) spinel compounds

The relation between the composition and electronic structure of the perfectly inverse spinel compound Zn7-xMxSb2O12 (M = Ni and Co) has been studied by powder X-ray diffraction and X-ray photoelectron spectroscopy. Changes in the site occupancy are associated with shifts in the core levels as observed in the core level spectral analyses. The configuration of the density of states in the valence band due to the Co and Ni states can be observed in the valence band spectra. (C) 2004 Elsevier B.V. All rights reserved.

Low-temperature synthesis of single-phase Co7Sb2O12

Polycrystalline Co7Sb2O12 compounds have been synthesized by a chemical route, which is based on a modified polymeric precursor method. In order to study the physical properties of the samples, X-ray diffraction (XRD), thermal analyses (TG and DSC), infrared spectroscopy (IR), specific surface area (BET), and magnetization measurements were performed on these materials. Characterization through XRD revealed that the samples are single-phase after a heat-treatment at 1100degreesC for 2h, while the X-ray patterns of the samples heat-treated at lower temperatures revealed the presence of additional Bragg reflections belonging to the Co6Sb2O6 phase. These data were analyzed by means of Rietveld refinement and further analyze showed that Co7Sb2O12 displays an inverse spinel crystalline structure. In this structure, the Co2+ ions occupy the eight tetrahedral positions, and the sixteen octahedral positions are randomly occupied by the Sb5+ and Co2+ ions. IR studies disclosed two strong absorption bands, v(1) and v(2), in the expected spectral range for a spinel-type binary oxide with space group Fd3m. Exploratory studies concerning the magnetic properties indicated that this sample presents a spin-glass transition at T-f similar to 64 K. (C) 2004 Elsevier B.V. All rights reserved.

The influence of cation segregation on the methanol decomposition on nanostructured SnO2

Here we describe a new route to synthesize ultrafine rare earth doped and undoped tin oxide particles for catalytic applications. The catalytic behavior observed in SnO2 samples suggests the control of the catalytic activity and the selectivity of the products by the segregation of a layer of a rare earth compound with the increase of the heat-treatment temperature. The ultrafine particles were characterized by means of BET, XPS, TEM, XRD and Rietveld refinement. It was demonstrated that the effects of the dopant on the methanol decomposition reaction and on the H-2 selectivity were correlated with the segregation of a rare earth layer on the tin oxide samples. (C) 2002 Published by Elsevier B.V. B.V.

Effect of partial preferential orientation and distortions in octahedral clusters on the photoluminescence properties of FeWO4 nanocrystals

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

Structure, microstructure and dielectric properties of 100-x(Bi0.5Na0.5)TiO3-x[SrTiO3] composites ceramics

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

Influence of the morphology and microstructure on the photocatalytic properties of titanium oxide films obtained by sparking anodization in H3PO4

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

A new processing method of CaZn2(OH)(6)center dot 2H(2)O powders: Photoluminescence and growth mechanism

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Structural and microstructural characterization of SrBi2(Ta0.5Nb0.48W0.02)(2)O-9 powders

SrBi2(Ta0.5Nb0.48W0.02)(2)O-9 powders (SBTN-W) were prepared by the polymeric precursor method. The influence of annealing temperature on the phase formation and specific surface area was evaluated. TG/DTA associated with X-ray diffraction (XRD) analyses showed the formation of perovskite phase at around 500-600 degrees C. An orthorhombic structure with A21am space group was identified by Rietveld refinement. BET analysis revealed that the specific surface area reduces with increasing thermal annealing. SEM micrographies showed grains in an almost-spherical morphology with the presence of agglomerates. (C) 2006 Elsevier B.V. All rights reserved.

Cluster Coordination and Photoluminescence Properties of alpha-Ag2WO4 Microcrystals

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)