978 resultados para POLYMERIC PRECURSOR METHOD


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In this work, we report on the magnetic properties of nickel nanoparticles (NP) in a SiO(2)-C thin film matrix, prepared by a polymeric precursor method, with Ni content x in the 0-10 wt% range. Microstructural analyses of the films showed that the Ni NP are homogenously distributed in the SiO(2)-C matrix and have spherical shape with average diameter of similar to 10 nm. The magnetic properties reveal features of superparamagnetism with blocking temperatures T (B) similar to 10 K. The average diameter of the Ni NP, estimated from magnetization measurements, was found to be similar to 4 nm for the x = 3 wt% Ni sample, in excellent agreement with X-ray diffraction data. M versus H hysteresis loops indicated that the Ni NP are free from a surrounding oxide layer. We have also observed that coercivity (H (C)) develops appreciably below T (B), and follows the H (C) ae [1 - (T/T (B))(0.5)] relationship, a feature expected for randomly oriented and non-interacting nanoparticles. The extrapolation of H (C) to 0 K indicates that coercivity decreases with increasing x, suggesting that dipolar interactions may be relevant in films with x > 3 wt% Ni.

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The synthesis of Y(0.9)Er(0.1)Al(3)(BO(3))(4) crystalline powders and vitreous thin films were studied. Precursor solutions were obtained using a modified polymeric precursor method using D-sorbitol as complexant agent. The chemical reactions were described. Y(0.)9Er(0.1)Al(3)(BO(3))(4) composition presents good thermal stability with regard to crystallization. The Y(0.9)Er(0.1)Al(3)(BO(3))(4) crystallized phase can be obtained at 1,150 degrees C, in agreement with other authors. Crack- and porosity-free films were obtained with very small grain size and low RMS roughness. The films thickness revealed to be linearly dependent on precursor solution viscosity, being the value of 25 mPa s useful to prepare high-quality amorphous multi-layers (up to similar to 800 nm) at 740 degrees C during 2 h onto silica substrates by spin coating with a gyrset technology.

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A carbon-supported binary Pt(3)Sn catalyst has been prepared using a modified polymeric precursor method under controlled synthesis conditions This material was characterized using X-ray diffraction (XRD). and the results indicate that 23% (of a possible 25%) of Sn is alloyed with Pt, forming a dominant Pt(3)Sn phase. Transmission election microscopy (TEM) shows good dispersion of the electrocatalyst and small particle sizes (3 6 nm +/- 1 nm) The polarization curves for a direct ethanol fuel cell using Pt(3)Sn/C as the anode demonstrated Improved performance compared to that of a PtSn/C E-TEK. especially in the intrinsic resistance-controlled and mass transfer regions. This behavior is probably associated with the Pt(3)Sn phase. The maximum power density for the Pt(3)Sn/C electrocatalyst (58 mW cm(-2)) is nearly twice that of a PtSn/C E-TEK electrocatalyst (33 mW cm(-2)) This behavior is attributed to the presence of a mixed Pt(9)Sn and Pt(3)Sn alloy phase in the commercial catalysts (C) 2009 Elsevier B V All rights reserved

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This paper presents a study of the electrocatalysis of ethanol oxidation reactions in an acidic medium on Pt-CeO(2)/C (20 wt.% of Pt-CeO(2) on carbon XC-72R), prepared in different mass ratios by the polymeric precursor method. The mass ratios between Pt and CeO(2) (3:1, 2:1, 1:1, 1:2, 1:3) were confirmed by Energy Dispersive X-ray Analysis (EDAX). X-ray diffraction (XRD) structural characterization data shows that the Pt-CeO(2)/C catalysts are composed of nanosized polycrystalline non-alloyed deposits, from which reflections corresponding to the fcc (Pt) and fluorite (CeO(2)) structures were clearly observed. The mean crystallite sizes calculated from XRD data revealed that, independent of the mass ratio, a value close to 3 nm was obtained for the CeO(2) particles. For Pt, the mean crystallite sizes were dependent on the ratio of this metal in the catalysts. Low platinum ratios resulted in small crystallites. and high Pt proportions resulted in larger crystallites. The size distributions of the catalysts particles, determined by XRD, were confirmed by Transmission Electron Microscope (TEM) imaging. Cyclic voltammetry and chronoamperometic experiments were used to evaluate the electrocatalytic performance of the different materials. In all cases, except Pt-CeO(2)/C 1:1, the Pt-Ceo(2)/C catalysts exhibited improved performance when compared with Pt/C. The best result was obtained for the Pt-CeO(2)/C 1:3 catalyst, which gave better results than the Pt-Ru/C (Etek) catalyst. (C) 2009 Elsevier B.V. All rights reserved.

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

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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SrBi4Ti4O15 (SBTi) thin films were obtained by the polymeric precursor method and crystallized in a domestic microwave oven. For comparison, films were also crystallized in a conventional furnace at 700 degrees C for 2 h. Structural and morphological characterization of the SBTi thin films was investigated by X-ray diffraction (XRD) and atomic force microscopy (AFM), respectively. Using platinum coated silicon substrates configuration, ferroelectric properties of the films were determined with remanent\polarization P-r and a coercive field E-c of 5.1 mu C/cm(2) and 135 kV/cm for the film thermally treated in the microwave oven and 5.4 mu C/cm(2) and 85 kV/cm for the film thermally treated in conventional furnace, respectively. The films thermally treated in the conventional furnace exhibited excellent fatigue-free characteristics up to 10(10) switching cycles indicating that SBTi thin films can be a promise material for use in non-volatile memories. (C) 2007 Elsevier B.V. All rights reserved.

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

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This work reports dielectric measurements performed on Pb(Zr0.53Ti0.47)O3 (PZT) thin films prepared by a polymeric precursor method. The -E curves obtained for the PZT film measured at 100 kHz, under a small ac 0.2 kV/cm signal-test and a dc scan featured a typical butterfly curve. However, the -E curves obtained for PZT film under a dc scan, with a scan rate of 0.003 V/s, shows a pronounced asymmetry. The absence of a symmetric secondary peak in -E curves could be an indication of essentially 180 domain switching.

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Nickel nanoparticles into silica-carbon matrix composites were prepared by using the polymeric precursor method. The effects of the polyester type and the time of pyrolysis on the mesoporosity and nickel particle dispersion into non-aqueous amorphous silica-carbon matrix were investigated by thermogravimetric analysis, adsorption/desorption isotherms and TEM. A well-dispersed metallic phase could be only obtained by using ethylene glycol. Weightier polyesters affected the pyrolysis process due to a combination of more amounts of carbonaceous residues and delaying of pyrolysis process. The post-pyrolyzed composites were successfully cleaned at 200 degrees C for I h in oxygen atmosphere leading to an increase in the surface area and without the occurrence of carbon combustion or nickel nanoparticles oxidation. The matrix composites presented predominantly mesoporous with pore size well defined in 38 angstrom, mainly when tetraethylene glycol was used as polymerizing agent. (C) 2007 Elsevier B.V. All rights reserved.

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Thin films of potassium niobate were deposited on (100) Si substrates by the polymeric precursor method (Pechini method). Annealing in static air was performed at 600degrees C for 20 h. The obtained films were characterized by X-ray diffraction and atomic force microscopy (AFM). Electrical characterization of the films pointed to ferroelectricity via hysteresis loop. The dielectric constant, dissipation factor and resistance were measured in frequency region from 10 Hz to 10 MHz. At 1 MHz, the dielectric constant was 158 and the dissipation factor was 0.11. (C) 2004 Elsevier B.V. All rights reserved.

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Nanocrystalline Al(2)O(3)powders have been synthesized by the polymeric precursor method. A study of the evolution of crystalline phases of obtained powders was accomplished through X-ray diffraction, micro-Raman spectroscopy and refinement of the structures through the Rietveld method. The results obtained allow the identification of three steps on the gamma-Al2O3 to alpha-Al2O3 phase transition. The single-phase alpha-Al2O3 Powder was obtained after heat-treatment at 1050 degrees C for 2 h. A study of the morphology of the particles was accomplished through measures of crystallite size, specific surface area and transmission electronic microscopy. The particle size is closely related to gamma-Al2O3 to alpha-Al2O3 phase transition. (c) 2007 Elsevier B.V. All rights reserved.

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Thin films of lithium niobate were deposited on (100) silicon by the polymeric precursor method (Pechini method). Annealing in static air was performed at 500degreesC for 3 h. The films obtained were characterized by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. Electrical characterization of the films pointed to ferroelectricity via hysteresis loop. The dielectric constant, dissipation factor and resistance were measured in the frequency region from 10 Hz to 10 MHz. At 1 MHz, the dielectric constant was 46 and the dissipation factor was 0.043. (C) 2002 Elsevier B.V. B.V. All rights reserved.

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Al2O3 and Al2-x Cr (x) O-3 (x = 0.01, 0.02 and 0.04) powders have been synthesized by the polymeric precursors method. A study of the structural evolution of crystalline phases corresponding to the obtained powders was accomplished through X-Ray Diffraction and UV-vis spectroscopy (reflectance spectra and CIEL* a*b* color data). The obtained results allow to identify the gamma-Al2O3 to alpha-Al2O3 phase transition. The single-phase alpha-Al2O3 powder was obtained after heat treatment at 1050 degrees C for 2 h. The results show that the green to red color transition and ruby luminescence lines observed for the powders of Al2-x Cr (x) O-3 are related to the gamma to alpha-Al2O3 phase transition and the temperature and time range for such transition depends on the chromium content.

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Lanthanum-modified bismuth titanate, Bi4-xLaxTi3O12 (BLT), with x ranging from 0 to 0.75 was grown on Pt/Ti/SiO2/Si substrates using a polymeric precursor solution and spin-coating method. The dielectric constant of highly doped bismuth titanate was equal to 148 while dielectric losses remained low (tan delta = 0.0018), and the films showed well-saturated polarization-electric field curves (2P(r) = 40.6 muC/cm(2) and V-c = 0.99 V). The leakage current densities improve for the lanthanum-doped system. For five-layered BLT films with x = 0.75, a charge storage density of 35 fC/mum(2) and a thickness of 320 nm were found. (C) 2004 Elsevier B.V. All rights reserved.