989 resultados para Microwave-hydrothermal methods


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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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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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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Wurtzite-type Zn1-xMnxO (x = 0, 0.03, 0.05, 0.07) nanostructures were successfully synthesised using a simple microwave-assisted hydrothermal route and their catalytic properties were investigated in the cellulose conversion. The morphology of the nanocatalysts is dopant-dependent. Pure ZnO presented multi-plate morphology with a flower-like shape of nanometric sizes, while the Zn0.97Mn0.03O sample is formed by nanoplates with the presence of spherical nanoparticles; the Zn0.95Mn0.05O and Zn0.93Mn0.07O samples are mainly formed by nanorods with the presence of a small quantity of spherical nanoparticles. The catalyst without Mn did not show any catalytic activity in the cellulose conversion. The Mn doping promoted an increase in the density of weak acid sites which, according to the catalytic results, favoured promotion of the reaction. © 2013 Institute of Chemistry, Slovak Academy of Sciences.

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An efficient microwave-hydrothermal (MAH) method has been developed for the synthesis of highly crystalline Co3O4 spinel nanocubes via β-Co(OH)2 without any surfactant assistance. The structure and surface chemical composition along the growth process are studied. The effects as well as the merits of the MAH method on the processing and characteristics of obtained Co3O4 spinel nanocubes are highlighted. © 2013 The Royal Society of Chemistry.

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ZnO and doped M:ZnO (M = V, Fe and Co) nanostructures were synthesized by microwave hydrothermal synthesis using a low temperature route without addition of any surfactant. The transition metal ions were successfully doped in small amount (3% mol) into ZnO structure. Analysis by X-ray diffraction reveals the formation of ZnO with the hexagonal (wurtzite-type) crystal structure for all the samples. The as-obtained samples showed a similar flower-like morphology except for Fe:ZnO samples, which presented a plate-like morphology. The photocatalytic performance for Rhodamine B (RhB) degradation confirmed that the photoactivity of M:ZnO nanostructures decreased for all dopants in structure, according to their eletronegativity. Photoluminescence spectroscopy was employed to correlate M:ZnO structure with its photocatalytical properties. It was suggested that transition metal ions in ZnO lattice introduce defects that act as trapping or recombination centers for photogenerated electrons and holes, making it impossible for them reach the surface and promote the photocatalytical process.

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Manganese tungstate (MnWO4) nanorods were prepared at room temperature by the co-precipitation method and synthesized after processing in a microwave-hydrothermal (MH) system at 140 degrees C for 6-96 min. These nanorods were structurally characterized by X-ray diffraction (XRD), Rietveld refinements and Fourier transform (FT)-Raman spectroscopy. The growth direction, shape and average size distribution of nanorods were observed by means of transmission electron microscopy (TEM) and high resolution TEM (HR-TEM). The optical properties of the nanorods were investigated by ultraviolet visible (UV-vis) absorption and photoluminescence (PL) measurements. XRD patterns, Rietveld refinement data and FT-Raman spectroscopy indicate that the MnWO4 precipitate is not a single phase structure while the nanorods synthesized by MH processing have a wolframite-type monoclinic structure without deleterious phases. FT-Raman spectra exhibited the presence of 17 Raman-active modes from 50 to 1,000 cm(-1). TEM and HR-TEM micrographs indicated that the nanorods are aggregated due to surface energy by Van der Waals forces and grow along the [100] direction. UV-vis absorption measurements confirmed non-linear values for the optical band gap (from 3.2 to 2.72 eV), which increased as the MH processing time increased. The structural characterizations indicated that the presence of defects in the MnWO4 precipitate promotes a significant contribution to maximum PL emission, while MnWO4 nanorods obtained by MH processing decrease the PL emission due to the reduction of defects in the lattice.

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In this communication, we report the effect of different surfactants [cetyltrimethylammonium bromide (CTAB), sodium dodecyl sulfate (SDS) and sodium bis(2-ethylhexyl)sulfosuccinate (AOT)] on the shape, growth and photoluminescence (PL) behavior of manganese tungstate (MnWO4) crystals synthesized by the microwave-hydrothermal (MH) method at 413 K for 45 min. These crystals were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), ultraviolet-visible (UV-vis) absorption spectroscopy and PL measurements. XRD patterns proved that these crystals have a monoclinic structure. FE-SEM images showed that MnWO4 crystals exhibit different shapes and growth mechanisms depending on the surfactant employed. The CTAB cationic surfactant promotes the hindrance of small nuclei that leads to the formation of flake-like nanocrystals, while SDS and AOT anionic surfactants promote a growth of crystals to plate-like and leaf-like crystals due to considerable size effect of counter-ions (RSO4- and RSO2O-) and an increase in Na+ ion remnants. UV-vis absorption spectroscopy revealed different optical band gap values due to modifications in the shape, surface and crystal size. Finally, the effect of surfactants on the crystal shapes and average crystal size distribution causing changes in the PL behavior of MnWO4 crystals was explained. (C) 2011 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.

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In this work CdMoO 4 nanoparticles were obtained under hydrothermal conditions using microwave radiation (2.45 GHz) (MH) at 100°C for different times. 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 CdMoO 4 phases were obtained. FEG-SEM powders present large-scale and homogeneous particles with microspheres-like morphology. UV-vis results were employed to determine the optical band gap these materials. Also, it showed existence of photoluminescence (PL) emission in the green wavelength range of 540-546 nm. Photocatalytic activity of CdMoO 4 nanocrystals was examined by monitoring the degradation of rhodamine B dye.

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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.