Voltage-composition profile and synchrotron X-ray structural analysis of low and high temperature LixCoO2 host material

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

Reaction pathway to the synthesis of anatase via the chemical modification of titanium isopropoxide with acetic acid

Anatase nanoparticles were obtained through a modified sol-gel route from titanium isopropoxide modified with acetic acid in order to control hydrolysis and condensation reactions. The modification of Ti(O(i)Pr)(4) with acetic acid reduces the availability of groups that hydrolyze and condense easily through the formation of a stable complex whose structure was determined to be Ti(OCOCH(3))(O(i)Pr)(2) by means of FTIR and (13)C NMR. The presence of this complex was confirmed with FTIR in the early stages of the process. A doublet in 1542 and 1440 cm(-1) stands for the asymmetric and symmetric stretching vibrations of the carboxylic group coordinated to Ti as a bidentate ligand. The gap of 102 cm(-1) between these signals suggests that acetate acts preferentially as a bidentate rather than as a bridging ligand between two titanium atoms. The use of acetic acid as modifier allows the control of both the degree of condensation and oligomerization of the precursor and leads to the preferential crystallization of TiO(2) in the anatase phase. A possible reaction pathway toward the formation of anatase is proposed on the basis of the intermediate species present in a 1:1 Ti(O(i)Pr)(4):CH(3)COOH molar system in which esterification reactions that introduce H(2)O into the reaction mixture were seen to be negligible. The Rietveld refinement and TEM analysis revealed that the powder is composed of isotropic anatase nanocrystallites.

Aspects of solid state formation and properties of Sn(0.9)Ti(0.1)O(2) system doped with CoO and Nb(2)O(5)

The effect of calcination temperature during the formation of the solid solution Sn(0.9)Ti(0.1)O(2) doped with 1.00 mol % CoO and 0.05 mol % Nb(2)O(5) is presented. The structural characteristics of this system were studied using X-ray diffraction, and the changes in phase formation were analyzed using the Rietveld method. With an increase in calcination temperature, there is increasing miscibility of Ti into the (Ti,Sn)O(2) phase and near 1000 degrees C, and the remaining TiO(2) (anatase) was transformed into the rutile phase. The sintering process, monitored using dilatometry, suggests two mass transport mechanisms, one activated close to 900 degrees C associated with the presence of TiO(2) (anatase) and the second mechanism, occurring between 1200 and 1300 degrees C, is attributed to a faster grain boundary diffusion caused by oxygen vacancies. (C) 2008 International Centre for Diffraction Data.

Rietveld analysis of mechanically activated BaCO(3)-TiO(2) system

BaTiO(3) powders were prepared through mechanical activation chemistry and analyzed by Rietveld refinement with X-ray diffraction data. Raw BaCO(3) and TiO(2) powders were dry milled for 5 and 20 h and then calcinated for 2 and 4 h at 800 degrees C. The milling process was found to have broken up the BaCO(3) and TiO(2) crystals into smaller crystals and formed only small amounts ( 1.5 wt%) of BaTiO(3). Subsequence calcinations for 2 and 4 h at 800 degrees C successfully produced large amounts (>97.7 wt%) of BaTiO(3) crystals. The calcination process also generated microstrains and crystallite-size anisotropy in BaTiO(3). An increase in the calcination time from 2 to 4 h increased the BaTiO(3) weight percentage and the crystal lite-shape anisotropy, but decreased the tetragonal distortion anisotropic microstrains in BaTiO(3) crystals. (C) 2008 International Centre for Diffraction Data.

Powder X-ray characterization of lithium thiazoildine-4-carboxylate

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

Investigação da Interface Metal-Porcelana da Liga Ni-Cr-Mo Soldada a LASER

The interface formed between the metal and the porcelain of a LASER welded Ni-Cr-Mo alloy was studied. The characterization was carried out through optical microscopy, scanning electron microscopy, X-ray dispersive spectroscopy-EDS and mechanical testing by three-point flexion test-TPE in the region LASER welded with and without the porcelain. The porcelain adhesion with the alloy alone is possible after the oxidation of the metallic surface and subsequent application of an adhesive called opaco. The applied porcelain, on the base metal and fusion zone presented some distinct behaviors. After the TPF test the base metal presented fractures while that in the fusion zone was completely gone. One noticed that the region submitted to the LASER welding showed less porcelain adhesion than the region of the base metal due to the microestructural refinement of the fusion zone. These results can be evidenced by the EDS of the studied regions. The TPF had demonstrated that the Ni-Cr-Mo alloy submitted to the LASER welding, undergone significant alterations in its mechanical properties after the application of the porcelain.

Biodegradation of oil refinery residues using mixed-culture of microorganisms isolated from a landfarming

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

Síntese hidrotermal assistida por micro-ondas como metodologia sintética eficiente para obtenção da rede metalorgânica [ZN(BDC)(H2O)2]n

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Influência do método de síntese na obtenção de pós de Na2TiSiO5

Este trabalho apresenta um estudo sistemático sobre a síntese e caracterização de pós de Na2TiSiO5. Foram estudadas as propriedades estruturais e morfológicas dos pós por intermédio de difração de raios X, espectroscopia Raman e microscopia eletrônica de varredura. As amostras foram produzidas por meio de duas rotas sintéticas distintas baseadas em métodos tipo Pechini e submetidas a diferentes tratamentos térmicos. Medidas de espectroscopia Raman nas resinas poliméricas foram feitas visando verificar a influência das diferentes rotas utilizadas na síntese dos pós. Com os dados de difração de raios X foi feito um estudo da evolução das fases cristalográficas. A estrutura cristalina das amostras foi analisada por meio de refinamento Rietveld. Por fim, a morfologia dos compostos de Na2TiSiO5 foi examinada por microscopia eletrônica de varredura. Os resultados obtidos mostraram que é possível melhorar a qualidade das amostras de Na2TiSiO5 alterando-se a rota sintética utlizada.

Caracterização estrutural da cerâmica Ti x(Sm0,2Ce0,8)1-xO 2-delta pelo método de Rietveld

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

Estudo do mecanismo de corrosão por pites em água do mar de aços inoxidáveis supermartensíticos microligados com Nb e Ti

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Mechanically activating formation of layered structured bismuth titanate

Bismuth titanatc-Bi(4)Ti(3)O(12) (BIT) with wide application in the electronic industry as capacitors, memory devices and sensors is the simplest compound in the Aurivillius family, which consists of (Bi(2)O(2))(2+) sheets alternating with (Bi(2)T(i)3O(10))(2-) perovskite-like layers. The synthesis of more resistive BIT ceramics would be preferable advance in obtaining of well-densified ceramic with small grains randomly oriented to limit the conductivity along the (Bi(2)O(2))(2+) layers. Having in mind that the conventional ceramic route for the synthesis can lead to non-stoichiometry in composition, in consequence of the undesirable loss in bismuth content through volatilization of Bi(2)O(3) at elevated temperature, our efforts were addressed to preparation of BIT by mechanical activation the constituent oxides. The nucleation and phase formation of BIT, crystal structure, microstructure, powder particle size and specific surface area were followed by XRD, Rietveld refinement analysis, thermal analysis, scanning electron microscopy (SEM) and the BET specific surface area measurements. (c) 2005 Elsevier B.V. All rights reserved.

Purification, partial characterization and preliminary X-ray diffraction analysis of a mannose-specific lectin from Cymbosema roseum seeds

A lectin from Cymbosema roseum seeds (CRL) was purified, characterized and crystallized. The best crystals grew in a month and were obtained by the vapour-diffusion method using a precipitant solution consisting of 0.1 M Tris-HCl pH 7.8, 8% (w/v) PEG 3350 and 0.2 M proline at a constant temperature of 293 K. A data set was collected to 1.77 angstrom resolution at a synchrotron-radiation source. CRL crystals are orthorhombic, belonging to space group P2(1)2(1)2(1). Crystallographic refinement and full amino-acid sequence determination are in progress.

Effect of processing route on the phase formation and properties of Bi4Ti3O12 ceramics

Our efforts were directed to the preparation of bismuth titanate-Bi4Ti3O12 (BIT) by two procedures: mechanically assisted synthesis and polymeric precursor method to display a variety of their advantages. To follow the nucleation and phase formation of BIT, XRD and Rietveld refinement analysis were used and it was shown that Bi4Ti3O12 ceramic can been successfully prepared from nano-sized powders obtained by both methods. The ferroelectric properties were determined and the loops from BIT obtained by polymeric precursor method were not fully saturated with a remnant polarization of 20 mu C/cm(2) and coercitive field of 1500 kV/cm. BIT obtained from powders prepared by mechanically assisted synthesis shows a remnant polarization of 0.65 mu C/cm(2) and coercitive field of 1050 kV/cm. The grain morphology may be the factor causing the observed differences. (C) 2005 Published by Elsevier Ltd and Techna Group S.r.l.

Correlation of reactivity with structural factors in a series of Fe(II) substituted cobalt ferrites

A series of powdered cobalt ferrites, CoxFe3-xO4 with 0.66 <= x< 1.00 containing different amounts of Fe-II, were synthesized by a mild procedure, and their Fe and Co site occupancies and structural characteristics were explored using X-ray anomalous scattering and the Rietveld refinement method. The dissolution kinetics, measured in 0.1 M oxalic acid aqueous solution at 70 degrees C, indicate in all cases the operation of a contracting volume rate law. The specific rates increased with the Fell content following approximately a second-order polynomial expression. This result suggests that the transfer of Fe-III controls the dissolution rate, and that the leaching of a first layer of ions Co-II and Fe-II leaves exposed a surface enriched in slower dissolving octahedral Fe-III ions. Within this model, inner vicinal lattice Fe-II accelerates the rate of Fe-III transfer via internal electron hopping. A chain mechanism, involving successive electron transfers, fits the data very well. (C) 2006 Elsevier B.V. All rights reserved.