Structural Refinement and Photoluminescence Properties of MnWO4 Nanorods Obtained by Microwave-Hydrothermal Synthesis

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

Structural refinement and photoluminescence properties of irregular cube-like (Ca-1_Cu-x(x))TiO3 microcrystals synthesized by the microwave-hydrothermal method

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Effect of microwave disinfection on physical and mechanical properties of acrylic resins

This study evaluated the effect of microwave energy on the hardness, impact strength and flexural strength of the Clássico, Onda-Cryl and QC-20 acrylic resins. Aluminum die were embedded in metallic or plastic flasks with type III dental stone, in accordance with the traditional packing technique. A mixing powder/liquid ratio was used according to the manufacturer's instructions. After polymerization in water batch at 74°C for 9 h, boiling water for 20 min or microwave energy at 900 W for 10 min, the specimens were deflasked after flask cooling at room temperature, and submitted to finishing. Specimens non-disinfected and disinfected by microwave irradiation were submitted to hardness, impact and flexural strength tests. Each specimen was immersed in distilled water and disinfected in a microwave oven calibrated to 650 W for 3 min. Knoop hardness test was performed with 25 g load for 10 s, impact test was carried out using the Charpy system with 40 kpcm, and 3-point bending test with a crosshead speed of 0.5 mm/min until fracture. Data were submitted to statistical analysis by ANOVA and Tukey's test (α=0.05). Disinfection by microwave energy decreased the hardness of Clássico and Onda-Cryl acrylic resins, but no effect was observed on the impact and flexural strength of all tested resins.

Structural refinement and photoluminescence properties of cube-like (Ca 1-xCu x)TiO 3 crystals synthesized by the microwave-hydrothermal method

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.

CdMoO 4 synthesized by a microwave-assisted hydrothermal method and their photoluminescence and photocatality properties

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.

Electronic structure and magnetic properties of FeWO 4 nanocrystals synthesized by the microwave-hydrothermal method

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.

Nanostructured Composites Based on Carbon Nanotubes and Epoxy Resin for Use as Radar Absorbing Materials

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Titanate nanotubes produced from microwave-assisted hydrothermal synthesis: Photocatalytic and structural properties

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Structural, optical, and magnetic properties of NiMoO4 nanorods prepared by microwave sintering

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.

Structural Refinement and Photoluminescence Properties of MnWO4 Nanorods Obtained by Microwave-Hydrothermal Synthesis

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.

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.

Sintering and Microwave Properties of Zirconium Tin Titanate Doped with Select Oxides

Zirconium tin titanate (ZST) is often used as a dielectric resonator for the fabrication of microwave devices. Pure compositions do not sinter easily by solid state sintering; therefore, sintering ZST requires sintering aids capable of creating defects that could improve diffusion processes and/or promote liquid phase sintering. The mechanisms by which the additives influence the microstructure and, consequently, the ZSTs dielectric properties are not very clear. The effects of ZnO, Bi2O3, and La2O3, on the stoichiometry and dielectric properties of ZST sintered at different temperatures were investigated in this study.

Laboratory study on the optical properties of absorbing atmospheric aerosols and field applications

The interaction between aerosols and sun light plays an important role in the radiative balance of Earth’s atmosphere. This interaction is obtained by measuring the removal (extinction), redistribution (scattering), and transformation into heat (absorption) of light by the aerosols; i.e. their optical properties. Knowledge of these properties is crucial for our understanding of the atmospheric system. rn Light absorption by aerosols is a major contributor to the direct and indirect effects on our climate system, and an accurate and sensitive measurement method is crucial to further our understanding. A homebuilt photoacoustic sensor (PAS), measuring at a 532nm wavelength, was fully characterized and its functionality validated for measurements of absorbing aerosols. The optical absorption cross-sections of absorbing polystyrene latex spheres, to be used as a standard for aerosol absorption measurements, were measured and compared to literature values. Additionally, a calibration method using absorbing aerosol of known complex refractive index was presented.rn A new approach to retrieve the effective broadband refractive indices (mbroad,eff) of aerosol particles by a white light aerosol spectrometer (WELAS) optical particle counter (OPC) was achieved. Using a tandem differential mobility analyzer (DMA)-OPC system, the nbroad,eff are obtained for both laboratory and field applications. This method was tested in the laboratory using substances with a wide range of optical properties and it was used in ambient measurements to retrieve the nbroad,eff of biomass burning aerosols in a nationwide burning event in Israel. The retrieved effective broadband refractive indices for laboratory generated scattering aerosols were: ammonium sulfate (AS), glutaric acid (GA), and sodium chloride, all within 4% of literature values. For absorbing substances, nigrosine and various mixtures of nigrosine with AS and GA were measured, as well as a lightly absorbing substance, Suwannee river fulvic acid (SRFA). For the ambient measurements, the calibration curves generated from this method were to follow the optical evolution of biomass burning (BB) aerosols. A decrease in the overall aerosol absorption and scattering for aged aerosols during the day after the fires compared to the smoldering phase of the fires was found. rn The connection between light extinction of aerosols, their chemical composition and hygroscopicity for particles with different degrees of absorption was studied. The extinction cross-section (σext) at 532nm for different mobility diameters was measured at 80% and 90% relative humidity (RH), and at an RH<10%. The ratio of the humidified aerosols to the dry ones, fRHext(%RH,Dry), is presented. For purely scattering aerosols, fRHext(%RH,Dry) is inversely proportional with size; this dependence was suppressed for lightly absorbing ones. In addition, the validity of the mixing rules for water soluble absorbing aerosols is explored. The difference between the derived and calculated real parts of the complex RIs were less than 5.3% for all substances, wavelengths, and RHs. The obtained imaginary parts for the retrieved and calculated RIs were in good agreement with each other, and well within the measurement errors of retrieval from pulsed CRD spectroscopy measurements. Finally, a core-shell structure model is also used to explore the differences between the models, for substances with low growth factors, under these hydration conditions. It was found that at 80% RH and for size parameters less than 2.5, there is less than a 5 % difference between the extinction efficiencies calculated with both models. This difference is within measurement errors; hence, there is no significant difference between the models in this case. However, for greater size parameters the difference can be up to 10%. For 90% RH the differences below a size parameter of 2.5 were up to 7%.rn Finally, the fully characterized PAS together with a cavity ring down spectrometer (CRD), were used to study the optical properties of soot and secondary organic aerosol (SOA) during the SOOT-11 project in the AIDA chamber in Karlsruhe, Germany. The fresh fractal-like soot particles were allowed to coagulate for 28 hours before stepwise coating them with SOA. The single scattering albedo for fresh fractal-like soot was measured to be 0.2 (±0.03), and after allowing the soot to coagulate for 28 hours and coating it with SOA, it increased to 0.71(±0.01). An absorption enhancement of the coated soot of up to 1.71 (±0.03) times from the non-coated coagulated soot was directly measured with the PAS. Monodisperse measurements of SOA and soot coated with SOA were performed to derive the complex refractive index (m) of both aerosols. A complex refractive index of m = 1.471(±0.008) + i0.0(±0.002) for the SOA-αO3 was retrieved. For the compact coagulated soot a preliminary complex refractive index of m = 2.04(+0.21/-0.14) + i0.34(+0.18/-0.06) with 10nm(+4/-6) coating thickness was retrieved.rn These detail properties can be use by modelers to decrease uncertainties in assessing climatic impacts of the different species and to improve weather forecasting.rn