989 resultados para Microwave-hydrothermal methods


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In this work, (Ca 1-xCu x)TiO 3 crystals with (x = 0, 0.01 and 0.02), labeled as CTO, CCTO1 and CCTO2, were synthesized by the microwave-hydrothermal method at 140°C for 32 min. XRD patterns (Fig. 1), Rietveld refinement and FT-Raman spectroscopy indicated that these crystals present orthorhombic structure Pbnm. Micro-Raman and XANES spectra suggested that the substitution of Ca by Cu in A-site promoted a displacement of the [TiO6]-[TiO6] clusters adjacent from its symmetric center, which leads distortions on the [CaO 12] clusters neighboring and consequently cause the strains into the CaTiO3 lattice. FE-SEM images showed that these crystals have an irregular shape as cube like probably indicating an Ostwald-ripening and self-assemble as dominant mechanisms to crystals growth. The powders presented an intense PL blue-emission.

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This communication reports that FeWO 4 nanocrystals were successfully synthesized by the microwave-hydrothermal method at 443 K for 1 h. The structure and shape of these nanocrystals were characterized by X-ray diffraction, Rietveld refinement, and transmission electron microscopy. The experimental results and first principles calculations were combined to explain the electronic structure and magnetic properties. Experimental data were obtained by magnetization measurements for different applied magnetic fields. Theoretical calculations revealed that magnetic properties of FeWO 4 nanocrystals can be assigned to two magnetic orderings with parallel or antiparallel spins in adjacent chains. These factors are crucial to understanding of competition between ferro- and antiferromagnetic behavior. © 2012 Elsevier Inc.

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Cystalline ceria (CeO2) nanoparticles have been synthesized by a simple and fast microwave-assisted hydrothermal (MAH) under NaOH, KOH, and NH4OH mineralizers added to a cerium ammonium nitrate aqueous solution. The products were characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier transformed-IR and Raman spectroscopies. Rietveld refinement reveals a cubic structure with a space group Fm3m while infrared data showed few traces of nitrates. Field emission scanning microcopy (FEG-SEM) revealed a homogeneous size distribution of nanometric CeO2 nanoparticles. The MAH process in KOH and NaOH showed most effective to dehydrate the adsorbed water and decrease the hydrogen bonding effect leaving a weakly agglomerated powder of hydrated ceria. TEM micrographs of CeO2 synthesized under MAH conditions reveal particles well-dispersed and homogeneously distributed. The MAH enabled cerium oxide to be synthesized at 100 °C for 8 min. © 2012 Elsevier B.V. All rights reserved.

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Titanium dioxide nanocrystals are an important commercial product used primarily in white pigments and abrasives, however, more recently the anatase form of TiO2 has become a major component in electrochemical and photoelectrochemical devices. An important property of titanium dioxide nanocrystals for electrical applications is the degree of crystallinity. Numerous preparation methods exist for the production of highly crystalline TiO2 particles. The majority of these processes require long reaction times, high pressures and temperatures (450–1400 °C). Recently, hydrothermal treatment of colloidal TiO2 suspensions has been shown to produce quality crystalline products at low temperatures (<250 °C). In this paper we extend this idea utilising a direct microwave heating source. A comparison between convection and microwave hydrothermal treatment of colloidal TiO2 is presented. The resulting highly crystalline TiO2 colloids were characterised using Raman spectroscopy, XRD, TEM, and electron diffraction. The results show that the microwave treatment of colloidal TiO2 gives comparable increases in crystallinity with respect to normal hydrothermal treatments while requiring significantly less time and energy than the hydrothermal convection treatment.

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

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Cerium carbonate hydroxide (orthorhombic Ce(OH)CO3) hexagonal-shaped microplates were synthesized by a simple and fast microwave-hydrothermal method at 150 degrees C for 30 min. Cerium nitrate, urea and cetyltrimethylammonium bromide were used as precursors. Ceria (cubic CeO2) rhombus-shape was obtained by a thermal decomposition oxidation process at 500 degrees C for 1 h using as- synthesized Ce(OH)CO3. The products were characterized by X-ray powder diffraction, field-emission scanning electron microscopy, thermogravimetric analysis and Fourier transformed infrared spectroscopy. The use of microwave-hydrothermal method allowed to obtain cerium compounds at low temperature and shorter time compared to other synthesis methods. (C) 2008 Elsevier B.V. All rights reserved.

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The nanocomposites of xTiO(2)+(1-x)Ni0.53Cu0.12Zn0.35Fe2O4 (where 0 <= x >= 1) were prepared using microwave hydrothermal (M H) method at 165 degrees C/45 min. The as-synthesized powders were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM) and Fourier transform infrared spectroscopy (FTIR). The particle size of the powder varies from 18 to 35 nm. The as prepared powders were densified at 500 degrees C/30 min using microwave sintering method. The sintered composites were characterized by XRD and scanning electron microscopy (SEM). The bulk densities of the present composites were increasing with the addition of TiO2. The grain sizes of all the composite vary between 65 nm and 90 nm. The addition of TiO2 to ferrite increased the dielectric properties (epsilon' and epsilon `') also the resonant frequency of all the composites was found to be greater than 1 GHz. The imaginary part of permeability mu `' was found to increase with an increase of TiO2.

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The synthesis of hexagonal barium ferrite (BaFe12O19) was studied under hydrothermal conditions by a method in which a significant amount of ferrous chloride was introduced along side ferric chloride among the starting materials. Though all of the Fe2+ ions in the starting material were converted to Fe3+ ions in the final product, Fe2+ was confirmed to participate differently from the Fe3+ used in the conventional method in the mechanism of forming barium ferrite. Indeed the efficiency of the synthesis and the quality of the product and the lack of impurities such as Fe2O3 and BaFe2O4 were improved when Fe2+ was included. However, the amount of ferrous ions that could be included to obtain the desired product was limited with an optimum ratio of 2:8 for FeCl2/FeCl3 when only 2h of reaction time were needed. It was also found that the role of trivalent Fe3+ could be successfully replaced by Al3+. Up to 50% of their on could be replaced by Al3+ in the reactants to produce Al- doped products. It was also found that the ratio of Fe2+/M3+ could be increased in the presence of Al3+ to produce high quality barium ferrite.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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In this work, we report on the synthesis of SrMoO4 powders by co-precipitation method and processed in a microwave-hydrothermal at 413 K for 5 h. These powders were analyzed by X-ray diffraction (XRD), Fourier transform Raman (FT-Raman), ultraviolet-visible (UV-vis) absorption spectroscopy and photoluminescence (PL). XRD analyses revealed that the SrMoO4 powders are free of secondary phases and crystallize in a tetragonal structure. FT-Raman investigations showed the presence of Raman-active vibration modes correspondent for this molybdate. UV-vis technique was employed to determine the optical band gap of this material. SrMoO4 powders exhibit an intense PL emission at room temperature with maximum peak at 540 nm (green region) when excited by 488 nm wavelength of an argon ion laser. (C) 2007 Elsevier B.V. All rights reserved.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)