ZnO architectures synthesized by a microwave-assisted hydrothermal method and their photoluminescence properties

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Determination of free glycerol in biodiesel at a platinum oxide surface using potential cycling technique

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Y2O3:Eu3+ (5 mol%) with Ag nanoparticles prepared by citrate precursor

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

Óxido de zinco dopado com gálio preparado pelo método Pechini

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

Influência do oxalato de amônio na formação do precursor columbita obtido pelo método Pechini

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

Método sol-gel modificado para obtenção de alumina nanoencapsulada com terras raras

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

Luminescent properties and lattice defects correlation on zinc oxide

The ZnO luminescent properties are strongly influenced by the preparation method and they are principally related to electronic and crystalline structures. This work reports about the correlation among luminescence properties of ZnO, obtained from zinc hydroxycarbonate, and crystalline lattice defects, microstrain, as function of thermal treatment. The crystallite size increase and the qualitative microstrain, obtained by Williamson-Hall plots, decrease as function of temperature. The evolution of electronic defects is analyzed by luminescence spectroscopy based on energy of the electronic transitions. From excitation spectrum, it is verified two bands around 377 nm and 405 nm attributed to the transitions between valence-conduction bands and valence band to interstitial zinc level, respectively. The emission spectra of sample treated at 600 degreesC shows large band at 670 nm. However, the green emission around 530 nm is observed for samples treated at 900 degreesC. The intensities of excitation and emission bands are associated with the increase of the electronic defects that depend on the strain lattice decrease. The lowest strain lattice results on the best green luminescent properties of zinc oxide. (C) 2001 Elsevier B.V. Ltd. All rights reserved.

Development of metal - SiO2 nanocomposites in a single-step process by the polymerizable complex method

This work presents the synthesis and characterization of SiO2:metal (Ni, Co, Ag, and Fe) nanocomposites processed by the polymerizable complex method. The polymeric precursor solutions obtained were characterized by means of FT-Raman and C-13 NMR spectroscopy. The results show the formation of a hybrid polymer with carbon and silicon in the macromolecule chain and the transition metal cation arrested within this polymeric chain. The nanocomposites are formed during the controlled polymeric precursor pyrolysis. The reduction of the metal cation is promoted by the CO/CO2 atmosphere resulting from the pyrolysis of the organic material. Microstructural characterization, performed by TEM and X-ray diffraction (XRD), showed that the nanocomposites are formed by metal nanoparticles embedded in a amorphous matrix formed by SiO2 and carbon. In the SiO2:Fe system, Fe3C was also detected by XRD.

Synthesis and characterization of PLZT (9/65/35) by the Pechini method and partial oxalate

ZrTiO4 (ZT), obtained by the Pechini method, was used as precursor for obtaining PLZT (lead lanthanum zirconium titanate). An aqueous solution of oxalic acid was prepared with particles of ZT, Pb(NO3)(2) and La2O3. After the PbC2O4 and La2O3 precipitate on ZT particles, the materials were calcined and X-ray diffraction (XRD) showed the cubic phase of PLZT. This material was sintered, in two steps, and a density of about 8.0 g/cm(3) was obtained. After the second sintering the XRD pattern showed the occurrence of tetragonal and rhombohedral phases. This was caused by a stoichiometric deviation and the material showed a high optical transparency. (C) 1998 Elsevier B.V. B.V. All rights reserved.

Development and testing of anode-supported solid oxide fuel cells with slurry-coated electrolyte and cathode

A laboratory setup was designed and put into operation for the development of solid oxide fuel cells (SOFCs). The whole project consisted of the preparation of the component materials: anode, cathode and electrolyte, and the buildup of a hydrogen leaking-free sample chamber with platinum leads and current collectors for measuring the electrochemical properties of single SOFCs. Several anode-supported single SOFCs of the type (ZrO(2):Y(2)O(3)+NiO) thick anode/(ZrO(2):Y(2)O(3)) thin electrolyte/(La(0.65)Sr(0.35)MnO(3)+ZrO(2):Y(2)O(3)) thin cathode have been prepared and tested at 700 and 800 degrees C after in situ H(2) anode reduction. The main results show that the slurry-coating method resulted in single-cells with good reproducibility and reasonable performance, suggesting that this method can be considered for fabrication of SOFCs. (c) 2005 Elsevier B.V. All rights reserved.

Indium tin oxide films prepared via wet chemical route

In this work, indium tin oxide (ITO) films were prepared using a wet chemical route, the Pechini method. This consists of a polyesterification reaction between an alpha-hydroxicarboxylate complex (indium citrate and tin citrate) with a polyalcohol (ethylene glycol) followed by a post annealing at 500 degrees C. A 10 at.% of doping of Sn4+ ions into an In2O3 matrix was successfully achieved through this method. In order to characterize the structure, the morphology as well as the optical and electrical properties of the produced ITO films, they were analyzed using different experimental techniques. The obtained films are highly transparent, exhibiting transmittance of about 85% at 550 nm. They are crystalline with a preferred orientation of [222]. Microscopy discloses that the films are composed of grains of 30 nm average size and 0.63 nm RMS roughness. The films' measured resistivity, mobility and charge carrier concentration were 5.8 x 10(-3) Omega cm, 2.9 cm(2)/V s and -3.5 x 10(20)/cm(3), respectively. While the low mobility value can be related to the small grain size, the charge carrier concentration value can be explained in terms of the high oxygen concentration level resulting from the thermal treatment process performed in air. The experimental conditions are being refined to improve the electrical characteristics of the films while good optical, chemical, structural and morphological qualities already achieved are maintained. (C) 2007 Elsevier B.V. All rights reserved.

Sol-gel prepared Pt-modified oxide layers: Synthesis, characterization, and electrocatalytic activity

Thin films of pure RuO2 and IrO2 and mixed Ru0.5Ir0.5O2 oxide modified with Pt particles were prepared by a sol-gel method in the form of thin films of similar to 2 mu m thickness on Ti substrates. Surface morphology of these Pt- modified oxides was examined by scanning electron microscopy and was found to exhibit a significant influence of the chemical composition of the oxide matrix. Element mapping showed homogeneous distribution of the metals. X- ray diffraction and X- ray photoelectron spectroscopy analyses showed that these films consist of metallic Pt particles dispersed in an oxide matrix. Cyclic voltammetry in acid solutions showed that the sol- gel prepared layers have relatively high Pt surface areas. The electrocatalytic activity of these materials toward the anodic oxidation of formaldehyde and methanol was compared in terms of onset potential and current density and was found to follow the sequence: Pt- Ru0.5Ir0.5O2/ Ti > Pt- RuO2/ Ti > Pt- IrO2/ Ti.

Effect of ceria content on the sintering of ZrO2 based ceramics synthesized from a polymeric precursor

Zirconia-ceria powders with ceria concentration varying from 0 to 12 mol% were synthesized using a polymeric precursor route based on the Pechini process. Powder characteristics were evaluated with regard to the crystallite size, BET surface area, phase distribution, nitrogen adsorption/desorption behavior, and agglomeration state. Sintering was studied considering the shrinkage rate, densification, grain size, and phase evolution. It was demonstrated that the synthesis method is effective to prepare nanosized powders of tetragonal zirconia single-phase. Sinterability mainly depended on the agglomeration state of powders and the monoclinic phase content, fully tetragonal zirconia ceramic, with grain size of 2.4 mu m, was obtained after addition of at least 9 mol% ceria and sintering at 1500 degrees C for 4 h. (C) 2000 Elsevier B.V. Ltd. All rights reserved.

SAXS study of formation and growth of tin oxide nanoparticles in the presence of complexing ligands

The effect of acetylacetone (acac) complexing ligand on the formation and growth of tin oxide-based nanoparticles during thermohydrolysis at 70 degreesC of a tin precursor SnCl4-n(acac)(n) (0 less than or equal to n less than or equal to 2) solution was analyzed by in situ small-angle X-ray scattering. A. transparent and stable sol was obtained after 2 h of thermohydrolysis at 70 degreesC, allowing the quantitative determination of the particle volume distribution function and its variation with the reaction time. The number of colloidal particles for equivalent thermohydrolysis temperature and time decreases as the [acac]/[Sn] ratio in initial solution increases from 0.5 to 6. Instead, the amount of soluble species remaining in solution increases for increasing [acac]/[Sn] ratio within the same range. This indicates that increasing amounts of Sn-acetylacetone complexes partially prevent the hydrolysis and consequent formation of colloidal particles. The N-2 adsorption isotherm characterization of freeze-dried powders demonstrates that the average pore size is approximately equal to the average size (approximate to9 Angstrom) of the colloidal primary particles in the sol, and that the porosity and surface area (approximate to200 m(2) g(-1)) are independent of the acac content in the initial solution.

Anisotropic growth of oxide nanocrystals: Insights into the rutile TiO2 phase

In this work, we report the synthesis of titanium oxide nanocrystals, especially the rutile TiO2 phase with nanorod morphology, by a method based on peroxotitanium complex decomposition. The results indicate that the anisotropic morphology reported for rutile TiO2 nanocrystals is related to the oriented attachment process. Despite the predominance of rutile nanocrystals at longer treatment times, the nanocrystals were obtained also in the anatase type, according to the degradation time adopted. XANES results evidenced the absence of structural correlation between the peroxytitanium complex and phase evolution, and the coexistence of the two phases strongly suggests a correlation of the oriented attachment mechanism and the rutile phase stabilization.