Synthesis of wurtzite ZnS nanoparticles using the microwave assisted solvothermal method

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.

TiO2 synthesized by microwave assisted solvothermal method: Experimental and theoretical evaluation

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

Experimental and theoretical studies of photoluminescence in Zns obtained by microwave-assisted solvothermal method

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.

Synthesis and characterization of NaNbO3 mesostructure by a microwave-assisted hydrothermal method

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.

Rapid preparation of (BiO)(2)CO3 nanosheets by microwave-assisted hydrothermal method with promising photocatalytic activity under UV-Vis light

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Synthesis of Bi-based superconductor by microwave-assisted hydrothermal method

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.

Optical characterization of europium-doped indium hydroxide nanocubes obtained by Microwave-Assisted Hydrothermal method

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

Morphology and properties of (Ba, Sr, Ca) titanates synthesized by microwave-assisted hydrothermal method

Ba1-xCaxTiO3, Ba1-xSrxTiO3 and Sr1-xCaxTiO3 (x = 0, 0.25, 0.50, 0.75 and 1) nanoparticles were synthesized using the microwave-assisted hydrothermal method. Samples were prepared for 40 minutes at 140°C under a pressure of 3 MPa using an adapted domestic microwave oven. The samples were characterized by X-Ray diffraction (XRD), scanning electron microscopy (FE-SEM), and Raman, photoluminescence (PL) and ultraviolet-visible (UV-Vis) spectroscopies. XRD data show that ceramic powders have crystalline phases associated with a short-range structural disorder. This structural disorder is confirmed by Raman spectral bands indicating multi-phonon processes and the presence of defects or impurities. Such defects account for a broad band in the photoluminescence spectrum in the green light (460 nm) region for all samples. Gap energy variation, obtained from UV-Vis spectra, suggest a non-uniform band structure of these titanates in accordance with the PL results. The morphology of each sample is changed with doping and varies from a spherical to cubic appearance for energy minimization.

Relationship between Crystal Shape, Photoluminescence, and Local Structure in SrTiO3 Synthesized by Microwave-Assisted Hydrothermal Method

This paper describes the effect of using different titanium precursors on the synthesis and physical properties of SrTiO3 powders obtained by microwave-assisted hydrothermal method. X-ray diffraction measurements, X-ray absorption near-edge structure (XANES) spectroscopy, field emission scanning electron microscopy (FE-SEM), and high-resolution transmission electron microscopy (HRTEM) were carried out to investigate the structural and optical properties of the SrTiO3 spherical and cubelike-shaped particles. The appropriate choice of the titanium precursor allowed the control of morphological and photoluminescence (PL) properties of SrTiO3 compound. The PL emission was more intense in SrTiO3 samples composed of spherelike particles. This behavior was attributed to the existence of a lower amount of defects due to the uniformity of the spherical particles.

Novel SrTi1-xFexO3 nanocubes synthesized by microwave-assisted hydrothermal method

We report herein for the first time a facile synthesis method to obtain SrTi1-xFexO3 nanocubes by means by a microwave-assisted hydrothermal (MAH) method at 140 degrees C. The effect of iron addition on the structural and morphological properties of SrTiO3 was investigated. X-ray diffraction measurements show that all STFO samples present a cubic perovskite structure. X-ray absorption spectroscopy at Fe absorption K-edge measurements revealed that iron ions are in a mixed Fe2+/Fe3+ oxidation state and preferentially occupy the Ti4+-site. UV-visible spectra reveal a reduction in the optical gap (E-gap) of STFO samples as the amount of iron is increased. An analysis of the data obtained by field emission scanning electron microscopy points out that the nanoparticles present a cubic morphology independently of iron content. According to high-resolution transmission electron microscopy results, these nanocubes are formed by a self-assembly process of small primary nanocrystals.

SnO2 nanocrystals synthesized by microwave-assisted hydrothermal method: towards a relationship between structural and optical properties

The exploration of novel synthetic methodologies that control both size and shape of functional nanostructure opens new avenues for the functional application of nanomaterials. Here, we report a new and versatile approach to synthesize SnO2 nanocrystals (rutile-type structure) using microwave-assisted hydrothermal method. Broad peaks in the X-ray diffraction spectra indicate the nanosized nature of the samples which were indexed as a pure cassiterite tetragonal phase. Chemically and physically adsorbed water was estimated by TGA data and FT-Raman spectra to account for a new broad peak around 560 cm(-1) which is related to defective surface modes. In addition, the spherical-like morphology and low dispersed distribution size around 3-5 nm were investigated by HR-TEM and FE-SEM microscopies. Room temperature PL emission presents two broad bands at 438 and 764 nm, indicating the existence of different recombination centers. When the size of the nanospheres decreases, the relative intensity of 513 nm emission increases and the 393 nm one decreases. UV-Visible spectra show substantial changes in the optical absorbance of crystalline SnO2 nanoparticles while the existence of a small tail points out the presence of localized levels inside the forbidden band gap and supplies the necessary condition for the PL emission.

beta-ZnMoO4 microcrystals synthesized by the surfactant-assisted hydrothermal method: Growth process and photoluminescence properties

In this communication, we investigate the effect of different surfactants: cetyltrimethylammonium bromide (CTAB), sodium dodecyl sulfate (SDS) and polyvinylpyrrolidone (PVP-K40) on the growth process of zinc molybdate (beta-ZnMoO4) microcrystals synthesized under hydrothermal conditions at 140 degrees C for 8 h. These microcrystals were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and photoluminescence (PL) measurements. XRD patterns proved that these crystals are monophasic and present a wolframite-type monoclinic structure. FE-SEM images revealed that the surfactants modified the crystal shapes, suggesting the occurrence of distinct crystal growth processes. The CTAB cationic surfactant promotes the hindrance of small nuclei that leads to the formation of rectangle-like crystals, SDS anionic surfactant induces a growth of irregular hexagons with several porous due to considerable size effect of counter-ions on the crystal facets, PVP-K40 non-ionic surfactant allows a reduction in size and thickness of plate-like crystals, while without surfactants have the formation of irregular plate-like crystals. Finally, the PL properties of beta-ZnMoO4 microcrystals were explained by means of different shape/size, surface defects and order-disorder into lattice. (C) 2011 Elsevier B.V. All rights reserved.

A solvent-free matrix application method for matrix-assisted laser desorption/ionization imaging of small molecules

Matrix application continues to be a critical step in sample preparation for matrix-assisted laser desorption/ionization (MALDI) mass spectrometry imaging (MSI). Imaging of small molecules such as drugs and metabolites is particularly problematic because the commonly used washing steps to remove salts are usually omitted as they may also remove the analyte, and analyte spreading is more likely with conventional wet matrix application methods. We have developed a method which uses the application of matrix as a dry, finely divided powder, here referred to as dry matrix application, for the imaging of drug compounds. This appears to offer a complementary method to wet matrix application for the MALDI-MSI of small molecules, with the alternative matrix application techniques producing different ion profiles, and allows the visualization of compounds not observed using wet matrix application methods. We demonstrate its value in imaging clozapine from rat kidney and 4-bromophenyl-1,4-diazabicyclo(3.2.2)nonane-4-carboxylic acid from rat brain. In addition, exposure of the dry matrix coated sample to a saturated moist atmosphere appears to enhance the visualization of a different set of molecules.