982 resultados para Microwave assisted
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In this work, zinc oxide powders were synthesized by microwave-assisted hydrothermal method in basic medium. These powders were analyzed by X-ray diffraction (XRD), Field-emisson gum scanning electron microscopy (FEG-SEM), Ultraviolet-visible (UV-vis) absorption spectroscopy and photoluminescence (PL) measurements. XRD pattern confirmed that the pure ZnO phases were obtained after MH processing performed at 130°C/ 1h. FEG-SEM micrographs reveals that these nanostructures are made up of ZnO plates. UV-vis results were employed to determine the optical band gap these materials. Also, it showed existence of photoluminescence (PL) in the different zinc powders. An orange PL emission when excited by 350 nm wavelength at room temperature was observad in the different powders.
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Crystalline terbium-doped indium hydroxide structures were prepared by a rapid and efficient Microwave-Assisted Hydrothermal (MAH) method. Nanostructures were obtained at a low temperature. FE-SEM images confirm that these samples are composed of 3D nanostructures. XRD, optical diffuse reflectance and photoluminescence (PL) measurements were used to characterize the products. Emission spectra of terbium-doped indium hydroxide (In(OH)3:xTb 3+) samples under excitation (350.7 nm) presented broad band emission referent to the indium hydroxide matrix and 5D4 → 7F6, 5D4 → 7F 5, 5D4 → 7F4, and 5D4 → 7F3 terbium transitions at 495, 550, 590 and 627 nm, respectively. Relative intensities of the Tb 3+ emissions increased as the concentration of this ion increased from 0, 1, 2, 4 and 8 mol%, of Tb3+, but the luminescence is drastically quenched for the In(OH)3 matrix. © 2012 Elsevier B.V. All rights reserved.
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In this article, we report the development of an efficient and rapid microwave assisted solvothermal (MAS) method to prepare wurtzite ZnS nanoparticles at 413 K using different precursors. The materials obtained were analyzed by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (MET) ultraviolet-visible (UV-vis) and photoluminescence (PL) measurements. The structure, surface chemical composition and optical properties were investigated as a function of the precursor. In addition, effects as well as merits of microwave heating on the processing and characteristics of ZnS nanoparticles obtained are reported. The possible formation mechanism and optical properties of these nanoparticles were also reported. © 2012 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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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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A shift of the photoluminescence (PL) emission was observed in ZnS prepared by microwave assisted solvothermal method with the increase of the time in microwave. In this work we reported a study of the optical behavior linking with the structural disorder according to XRD and FEG-TEM results. The reduction of intrinsic defects in the lattice is responsible for the decrease of electronic levels in the band gap changing the PL profile. This effect was confirmed by electronic structure calculations.
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In the work presented here, Ce0.97Cu0.03O2 nanoparticles were synthesized by a microwave-assisted hydrothermal method under different synthesis temperatures. The obtained nanoparticles were tested as catalysts in preferential oxidation of CO to obtain CO-free H2 (PROX reaction). The samples were characterized by X-ray diffraction, transmission electron microscopy (TEM), electron paramagnetic resonance spectroscopy (EPR) and temperature-programmed reduction (TPR). X-ray diffraction measurements detected the presence of pure cubic CeO2 for all synthesized samples. TEM images of the Ce0.97Cu0.03O2 nanoparticles revealed that samples synthesized at 80°C are composed mainly of nanospheres with an average size of 20 nm. The formation of some nanorods with an average diameter of 8 nm and 40 nm in length, and the size reduction of the nanoparticles from 20 to approximately 15 nm is observed with increasing synthesis temperature. EPR spectra indicated that copper is found well dispersed in sample synthesized at 160°C, located predominant in surface sites of ceria. For samples synthesized at 80 and 120°C, the species are less dispersed than in the other one, resulting in the formation of Cu2+−Cu2+ dimmers at the surface of ceria. TPR profiles presented two reduction peaks, one below 400°C attributed to the reduction of different copper species and a second peak around 800°C attributed to the reduction of Ce4+→ Ce3+ species located in the volume of the nanoparticles. The peak related to the reduction of copper species shifts to lower temperatures with increasing synthesis temperature, i.e., the sample synthesized at 160°C is more easily reduced than the ones synthesized at 120 and 80°C. The nanoparticles showed active as catalysts for the CO-PROX reaction. The microwave-assisted method revealed efficient for the synthesis of Ce0.97Cu0.03O2 nanoparticles with copper species selective for the CO-PROX reaction, which reaches CO conversions up to 92% for the sample synthesized at 160°C.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
Microwave-assisted hydrothermal synthesis of NiO-Ce1-XEuxO2-δ powders for fuel cell catalytic anodes
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CeO2-based materials doped with rare earth (TR +3) can be used as alternative to traditional NiO-YSZ anodes in solid oxide fuel cells as they have higher ionic conductivity and lower ohmic losses compared to YSZ. Moreover, they allow fuel cell operation at lower temperatures (500-800°C). In the anode composition, the concentration of NiO acting as catalyst in YSZ provides high electrical conductivity and high electrochemical activity of reactions, promoting internal reform in the cell. In this work, NiO - Ce1-xEuxO2-δ compounds (x = 0.1, 0.2 and 0.3) have been synthesized by microwave-assisted hydrothermal method. The materials were characterized by TG, XRD, TPR and SEM-FEG techniques. The refinement of data obtained by X-ray diffraction showed the presence of ceria doped with europium crystallized in a cubic phase with fluorite structure, in addition to the presence of NiO. The microwave-assisted hydrothermal method showed significant reduction in the average particle size and good mass control of phase compositions compared to other chemical synthesis techniques.
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In the present work, we report the synthesis and characterization of NaNbO3 particles obtained by microwave-assisted hydrothermal method from Nb2O5 and NaOH. The synthesis was made at different periods at 180 °C and 300W. The crystallization of NaNbO3 structures produced Na2Nb2O6.H2O in the intermediate phase with fiber-like morphology, and this is associated with the synthesis time. Pure orthorhombic NaNbO3 with cube-like morphology originates after synthesizing for 240 minutes. To verify the remnant polarization of particles, films were obtained by electrophoresis process and sintered at 800°C for 10 minutes in a microwave furnace. The films characterization indicated that films of niobate with fiber-like morphology present remaining polarization, and the morphology of cubes did not show remaining polarization. Considering these results, it can be concluded that the morphology implemented ferroelectric property of NaNbO3.
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A pretreatment with microwave irradiation was applied to enhance enzyme hydrolysis of corn straw and rice husk immersed in water, aqueous glycerol or alkaline glycerol. Native and pretreated solids underwent enzyme hydrolysis using the extract obtained from the fermentation of Myceliophthora heterothallica, comparing its efficiency with that of the commercial cellulose cocktail Celluclast (R). The highest saccharification yields, for both corn straw and rice husk, were attained when biomass was pretreated in alkaline glycerol, method that has not been previously reported in literature. Moreover, FTIR, TG and SEM analysis revealed a more significant modification in the structure of corn straw subjected to this pretreatment.Highest global yields were attained with the crude enzyme extract, which might be the result of its content in a great variety of hydrolytic enzymes, as revealed zymogram analysis. Moreover, its hydrolysis efficiency can be improved by its supplementation with commercial beta-glucosidase.
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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In this work we studied the synthesis of BSCCO-2212 superconducting phase associating a quite similar method developed by Pechini with the microwave-assisted hydrothermal method. To study the influence of the microwaves on the properties of BSCCO system, we synthesized two samples by such method. For one sample we used carbonates and for the other one we used nitrates as chemical reagents. We also produced a reference sample just using carbonates by Pechini's method to compare their morphological and superconducting properties. The structural properties of the samples were analyzed by scanning electron microscopy and X-ray diffraction. The Bi-2212 phase is predominant in all samples and despites the nitrates-like sample has a broader distribution of grain size in comparison with the reference sample, its magnetic behaviour is closer to that presented by the reference one.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)