Chemical and structural characterization of V2O5/TiO2 catalysts

A series of V2O5/TiO2 samples was synthesized by sol-gel and impregnation methods with different contents of vanadia. These samples were characterized by x-ray diffraction (XRD), Raman spectroscopy, x-ray photoelectron spectroscopy (XPS), and electronic paramagnetic resonance (EPR). XRD detected rutile as the predominant phase for pure TiO2 prepared by the sol-gel method. The structure changed to anatase when the vanadia loading was increased. Also, anatase was the predominant phase for samples obtained by the impregnation method. Raman measurements identified two species of surface vanadium: monomeric vanadyl (V4+) and polymeric vanadates (V5+). XPS results indicated that Ti ions were in octahedral position surrounded by oxygen ions. The V/Ti atomic ratios showed that V ions were highly dispersed on the vanadia/titania surface obtained by the sol-gel method. EPR analysis detected three V4+ ion types: two of them were located in axially symmetric sites substituting for Ti4+ ions in the rutile structure, and the third one was characterized by magnetically interacting V4+ ions in the form of pairs or clusters. A partial oxidation of V4+ to V5+ was evident from EPR analysis for materials with higher concentrations of vanadium. (C) 2001 American Vacuum Society.

V(2)O(5)/TiO(2) catalytic xerogels raman and EPR studies

Raman spectroscopy and Electron Paramagnetic Resonance (EPR) studies were performed on a series of V(2)O(5)/TiO(2) catalysts prepared by a modified sol-gel method in order to identify the vanadium species. Two species of surface vanadium were identified by Raman measurements, monomeric vanadyls and polymeric vanadates. Monomeric vanadyls are characterized by a narrow Raman band at 1030 cm(-1) and polymeric vanadates by two broad bands in the region from 900 to 960 cm(-1) and 770 to 850 cm(-1). The Raman spectra do not exhibit characteristic peaks of crystalline V(2)O(5). These results are in agreement with those of X-ray Diffractometry (XRD) and Fourier Transform Infrared (FT-IR) previously reported (C.B. Rodella et al., J. Sol-Gel Sci. Techn., submitted). At least three families of V(4+) ions were identified by EPR investigations. The analysis of the EPR spectra suggests that isolated V(4+) ions are located in sites with octahedral symmetry substituting for Ti(4+) ions in the rutile structure. Magnetically interacting V(4+) ions are also present as pairs or clusters giving rise to a broad and structureless EPR line. At higher concentration of V(2)O(5), a partial oxidation of V(4+) to V(5+) is apparent from the EPR results.

Síntese e caracterização da cerâmica PZT dopada com íons bário

Pós de titanato zirconato de chumbo (PZT) puros e dopados com bário foram obtidos pelo método de precursores poliméricos, conformados uniaxialmente, na forma de cilindros, utilizando 15 MPa, e prensados isostaticamente à 210MPa. Com o objetivo de estudar o comportamento de sinterização os compactos foram divididos em dois lotes. Sendo um sinterizado em um forno acoplado a um dilatômetro até a temperatura de 1300 °C e o outro sinterizado em forno tipo mufla, em sistema fechado, na temperatura de 1100 °C por 4 horas. Verificou-se que a adição do íon bário influencia na cinética de sinterização, na densificação final, na microestrutura e nas propriedades elétricas da cerâmica. A adição de bário aumenta a concentração da fase tetragonal no PZT, em função da substituição do chumbo por bário na rede perovskita. As amostras dopadas com concentrações maiores que 5,0 mol % em bário apresentaram segregação de PbO no contorno de grão, inibindo seu crescimento.

Contribution of structural order-disorder to the room-temperature photoluminescence of lead zirconate titanate powders

Intense and broad visible photoluminescent (PL) band was observed at room temperature in structurally disordered PbZr0.53Ti0.47O3 powders. The lead zirconate titanate PbZr0.53Ti0.47O3 powders prepared by the polymeric precursor method and heat treated at different temperatures were structurally characterized at long range by means of X-ray diffraction. The PL was measured at room temperature samples heat treated at different temperatures. Experimental measurements and quantum-mechanical calculations showed that the high structural order and the high structural disorder in PbZr0.53Ti0.47O3 lattice are not favorable to the intense PL emission. Only samples containing simultaneous structural order and disorder in their lattice present the intense visible PL emission at room temperature. (C) 2007 Published by Elsevier B.V.

Effect of annealing time on morphological characteristics of Ba(Zr,Ti)O-3 thin films

Ba(Zr0.50Ti0.50)O-3 thin films were prepared by the polymeric precursor method using the annealing low temperature of 300 degrees C for 8, 16, 24, 48, 96 and 192 It in a furnace tube with oxygen atmosphere. The X-ray diffraction patterns revealed that the film annealed for 192 h presented some crystallographic planes (1 0 0), (1 1 0) and (2 0 0) in its crystalline lattice. Fourier transformed infrared presented the formation of metal-oxygen stretching at around 756 cm(-1). The atomic force microscopy analysis presented the growth of granules in the Ba(Zr0.50Ti0.50)O-3 films annealed from 8 to 96 h. The crystalline film annealed for 192 h already presents grains in its perovskite structure. It evidenced a reduction in the thickness of the thin films with the increase of the annealing time. (C) 2006 Elsevier B.V. All rights reserved.

Temperature dependence of dielectric properties for Ba(Zr0.25Ti0.75)O-3 thin films obtained from the soft chemical method

Ba(Zr0.25Ti0.75)O-3(BZT) thin films prepared by the polymeric precursor method (PPM) were annealed at 500, 600, and 700 degrees C for 4h. All films crystallized in the perovskite structure present a crack-free microstructure. Dielectric properties of the BZT thin films were investigated as a function of frequency and applied voltage. The dielectric constant of the films were 36, 152 and 145 at 1 kHz, while the dielectric loss were 0.08, 0.08, and 0.12 at 1 MHz. (c) 2007 Elsevier B.V. All rights reserved.

Domestic microwave oven adapted for fast heat treatment of Ba0.5Sr0.5(Ti0.8Sn0.2)O-3 powders

In this work, BSTSn powders prepared by the polymeric precursor method were heat treated in a domestic microwave oven (MW) using a SiC susceptor to absorb the microwave energy and transfer the heat to the powder. The main advantage of MW is to reduce the thermal treatment time for phase crystallization. The powders were heat treated at 300 degrees C for 20 h in conventional oven, 300 degrees C for 10 min, 20 min, and 30 min in MW and at 500 degrees C for 1 min in MW. After thermal treatment, the photoluminescent properties of powders at room temperature were analyzed. (c) 2007 Published by Elsevier B.V.

Surface equilibrium angle for anisotropic grain growth in SnO2 systems

Usually, the kinetic models used in the study of sintered ceramic are performed by means of indirect physical tests, such as, results obtained from data of linear shrinkage and mass loss. This fact is justified by the difficulty in the determinations of intrinsic parameters of ceramic materials along every sintering process. In this way, the technique of atomic force microscopy (AFM) was used in order to determine the importance and the evolution of the dihedral angle in the sintering of 0.5 mol% MnO2-doped tin dioxide obtained by the polymeric precursor method.

Obtenção de filmes finos de TiO2 nanoestruturado pelo método dos precursores poliméricos

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

An efficient microwave-assisted hydrothermal synthesis of BaZrO3 microcrystals: growth mechanism and photoluminescence emissions

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Multi-functional properties of CaCu3Ti4O12 thin films

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

External polyacrylate-coating as alternative material for preparation of photopolymerized sol-gel monolithic column

Photopolymerized sol-gel monolithic columns for use in capillary electrochromatography were prepared in 125 mu m i.d. polyacrylate-coated fused-silica capillaries. The polyacrylate-coating, unlike the polyimide one, is transparent to the radiation used (approximate to 370 nm), and thus, no coating removal is necessary. This is a very important particularity since intrinsic capillary column characteristics, such as flexibility and mechanical resistance, are unchanged. A mixture containing metacryloxypropyltrimethoxysilane (MPTMS) as the polymeric precursor, hydrochloric acid as the catalyst, toluene as the porogen and bis(2,4,6-trimethylbenzoyl)-phenylphosphine oxide (Irgacure 819) as the photoinitiator was irradiated at 370 nm for 20 min inside the capillaries to prepare the columns through sol-gel approach. The versatility and viability of the use of polyacrilate as a new capillary external coating were shown through preparation of two columns under different conditions, which were tested in electrochromatography for separation of standard mixture containing thiourea (marker compound), propylbenzene, phenanthrene and pyrene. (C) 2008 Elsevier B.V. All rights reserved.

Optimization of photo-polymerized sol gel monolithic stationary phases prepared in polyacrylate-coated fused-silica capillaries for capillary electrochromatography

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Óxido de zinco dopado com gálio preparado pelo método Pechini

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

Síntese do anodo cerâmico La1-xSr xCr0,5Mn0,5O3 pela técnica dos precursores poliméricos

Compostos da família La1-xSr xCr0,5Mn0,5O3 são apontados como potenciais anodos cerâmicos de células a combustível de óxidos sólidos. A utilização de anodos cerâmicos tem como objetivo eliminar os problemas de depósito de carbono na superfície do níquel e a baixa resistência a ciclos de redução/oxidação observados no compósito cerâmica-metal à base de zircônia estabilizada e níquel, que é o material anódico mais usado nestas células. Neste estudo são apresentados os resultados da síntese pela técnica dos precursores poliméricos e da caracterização de compostos com x = 0,5, estequiométrico e com 5% de deficiência catiônica no sítio A da estrutura perovskita La1-xSr xCr0,5Mn0,5O3 e (La1-xSr x)0,95Cr0,5Mn0,5O3, respectivamente. Os resultados evidenciam que o composto estudado possui altos valores de condutividade elétrica e baixa reatividade com eletrólitos à base de zircônia.