Spherical-shaped Y2O3:Eu3+ nanoparticles with intense photoluminescence emission

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Quantitative phase analysis from X-ray diffraction in Y-TZP dental ceramics: A critical evaluation

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

Effects of the addition of ions barium on the structural and electrical properties of PZT ceramic

Lead zirconate titanate, with Zr/Ti ratio of 53/47 was prepared by the polymeric precursor method. It was investigated the barium (II) modification at 0.0, 0.2, 0.4 and 0.6 mol% in substitution to the lead (II) cation in A site of perovskite structure. The powder samples were characterized by XRD and the diffraction patterns were used to Rietveld refinement. The percentages of tetragonal and rhombohedral phases and a systematic study of the effect of barium (II) on the morphology and the dielectric properties of PZT were carried out. The results showed that the tetragonal phase is favored and the ceramic density is improved with the barium (II) insertion. The Curie temperature (Tc) is increased besides the slight reduction of dielectric constant (Kc).

Preparação e caracterização de nanocompósitos de Fe@SiO2, Fe@Fe3O4 e Fe3O4@PNIPAM

Pós-graduação em Química - IQ

Air abrasion before and/or after zirconia sintering: surface characterization, flexural strength, and resin cement bond strength

The purpose of this in vitro study was to evaluate the effect of air-abrasion/zirconia sintering order on the yttria partially stabilized tetragonal zirconia polycrystal (Y-TZP) surface characterization (roughness, morphology, and phase transformation), flexural strength (FS), and shear bond strength (SBS) to a resin cement. Y-TZP specimens were air abraded with 50-μm Al2O3 particles after (AS), before (BS), or before and after zirconia sintering (BAS). For roughness (Ra), 30 block specimens (12×12×3.0 mm; n=10) had their surfaces analyzed by a profilometer. Next, on the air-abraded surfaces of these specimens, composite resin discs (n=30) were bonded with RelyX ARC. The bonded specimens were stored for 24 hours in distilled water at 37°C before shear testing. Failure mode was determined with a stereomicroscope (20×). The surface morphology (n=2) was evaluated by SEM (500×). For the four-point flexural strength test (EMIC DL2000), 39 bar-shaped specimens (20×4.0×1.2 mm; n=13) were air abraded according to the three conditions proposed, and an additional group (nonabraded) was evaluated (n=13). The quantitative analysis of phase transformation (n=1) was completed with Rietveld refinement with X-ray diffraction data. Ra (μm) and SBS (MPa) data were analyzed by one-way analysis of variance (ANOVA) and the Tukey test (α=0.05). Pearson correlation analysis was used to determine if there was a correlation between roughness and SBS. For FS (MPa) data, one-way ANOVA and the Dunnett C-test (α=0.05) were used. The air-abrasion/zirconia sintering order influenced significantly (p<0.001) Ra, SBS, and FS. The BS and AS groups presented the highest (1.3 μm) and the lowest (0.7 μm) Ra. The highest SBS (7.0 MPa) was exhibited by the BAS group, followed by the AS group (5.4 MPa) and finally by the BS group (2.6 MPa). All groups presented 100% adhesive failure. A weak correlation (r=−0.45, p<0.05) was found between roughness and SBS. The air-abrasion/zirconia sintering order provided differences in the surface morphology. The nonabraded (926.8 MPa) and BS (816.3 MPa) groups exhibited statistically similar FS values but lower values than the AS (1249.1 MPa) and BAS (1181.4 MPa) groups, with no significant difference between them. The nonabraded, AS, BS, and BAS groups exhibited, respectively, percentages of monoclinic phase of 0.0 wt%, 12.2 wt%, 0.0 wt%, and 8.6 wt%. The rougher surface provided by the air-abrasion before zirconia sintering may have impaired the bonding with the resin cement. The morphological patterns were consistent with the surface roughness. Considering the short-term SBS and FS, the BAS group exhibited the best performance. Air abrasion, regardless of its performance order, provides tetragonal to monoclinic transformation, while sintering tends to zero the monoclinic phase content.

Effects of time exposure and low power sonochemical treatment on ZnO mesostructures

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

A joint experimental and theoretical study on the electronic structure and photoluminescence properties of Al-2(WO4)(3) powders

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Experimental and theoretical study on the structure, optical properties, and growth of metallic silver nanostructures in Ag3PO4

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

A relationship between structural and electronic order-disorder effects and optical properties in crystalline TiO2 nanomaterials

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

Structural characterization of Li-MN doped powders prepared by Pechini's method

Pechini's method has been successfully used to prepare Li-doped MgNb2O6(MN) at short time and low temperature. It consists in the preparation of metal citrate solution, which is polymerized at 250°C to form a high viscous resin. This resin was burned in a box type furnace at 400°C/2h and ground in a mortar. Successive steps of calcination up to 900°C were used to form a crystalline precursor. SEM, DTA and XRD were used to characterize the powders. MN precursor powders containing from 0.1 to 5.0 mol% of LiNbO3 additive was prepared aiming better dielectric properties and microstructural characteristics of the PMN prepared from columbite route. SEM analysis showed that particles increased by sintering, forming large agglomerates. The surface area is also substantially reduced with the increase in additive amount above 1.0 mol%. In XRD pattern of the precursor material with 5.0 mol% of additive was observed the LiNbO3 phase of trigonal structure. XRD data were used for Rietveld refinement and a decrease in microstrain and pronounced increase in crystallite size with the increase of LiNbO3 were observed. It is in agreement with the particle morphologies observed by SEM analysis.

Modeling the crystallographic structure of Ho(Ni,Co,Mn)O3±δ perovskite-type manganite

Crystallographic and microstructural properties of Ho(Ni,Co,Mn)O3± perovskite-type multiferroic material are reported. Samples were synthesized with a modified polymeric precursor method. The synchrotron X-ray powder diffraction (SXRPD) technique associated to Rietveld refinement method was used to perform structural characterization. The crystallographic structures, as well as microstructural properties, were studied to determine unit cell parameters and volume, angles and atomic positions, crystallite size and strain. X-ray energies below the absorption edges of the transition metals helped to determine the mean preferred atomic occupancy for the substituent atoms. Furthermore, analyzing the degree of distortion of the polyhedra centered at the transitions metal atoms led to understanding the structural model of the synthesized phase. X-ray photoelectron spectroscopy (XPS) was performed to evaluate the valence states of the elements, and the tolerance factor and oxygen content. The obtained results indicated a small decrease distortion in structure, close to the HoMnO3 basis compound. In addition, the substituent atoms showed the same distribution and, on average, preferentially occupied the center of the unit cell.

Estudo da relação de ordem-desordem estrutural em nanopartículas de TiO2

Pós-graduação em Química - IQ

CuO-CeO2 catalysts synthesized in one-step: Characterization and PROX performance

PEM fuel cells seem to be the most affordable and commercially viable hydrogen-based cells, the biggest challenge being to obtain CO-free H-2 (<100 ppm) as the fuel. In this study, the use of CuO-CeO2 catalysts in preferential oxidation of CO to obtain CO-free H-2 (PROX reaction) was investigated. Ce1-xCuxO2 catalysts, with x (mol%) = 0, 0.01, 0.03, 0.05 and 0.10, were synthesized in one-step by the polymeric precursor method, to obtain a very fine dispersion and strong metal-support interaction, to favor active copper species and a preference for the PROX reaction. The results obtained from catalyzed reactions and characterization of the catalysts by XRD, Rietveld refinement, BET surface area, UV-Vis and TPR, suggest that this one-step synthesis method gives rise to catalysts with copper species selective for the PROX reaction, which reaches a maximum rate on Ce0.97Cu0.03O2 catalyst. Copyright (C) 2012, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.

Effect of partial preferential orientation and distortions in octahedral clusters on the photoluminescence properties of FeWO4 nanocrystals

This communication is a report of our initial research to obtain iron tungstate (FeWO4) nanocrystals by the microwave-hydrothermal method at 170 degrees C for 45 min. X-ray diffraction patterns showed that the FeWO4 nanocrystals prepared with polyethylene glycol-200 have a partial preferential orientation in the (011) plane in relation to other nanocrystals prepared with sodium bis(2-ethylhexyl) sulfosuccinate and water. Rietveld refinement data indicates that all nanocrystals are monophasic with wolframite-type monoclinic structures and exhibit different distortions on octahedral [FeO6]/[WO6] clusters. High resolution transmission electron microcopy revealed an oriented attachment mechanism for the growth of aggregated FeWO4 nanocrystals. Finally, we observed that the photoluminescence properties of these nanocrystals are affected by partial preferential orientation in the (011) plane and distortions on [FeO6]/[WO6] clusters.

Cluster Coordination and Photoluminescence Properties of alpha-Ag2WO4 Microcrystals

In this paper, we report our initial research to obtain hexagonal rod-like elongated silver tungstate (alpha-Ag2WO4) microcrystals by different methods [sonochemistry (SC), coprecipitation (CP), and conventional hydrothermal (CH)] and to study their cluster coordination and optical properties. These microcrystals were structurally characterized by X-ray diffraction (XRD), Rietveld refinements, Fourier transform infrared (FT-IR), X-ray absorption near-edge structure (XANES), and extended X-ray absorption fine structure (EXAFS) spectroscopies. The shape and average size of these alpha-Ag2WO4 microcrystals were observed by field-emission scanning electron microscopy (FE-SEM). The optical properties of these microcrystals were investigated by ultraviolet-visible (UV-vis) spectroscopy and photoluminescence (PL) measurements. XRD patterns and Rietveld refinement data confirmed that alpha-Ag2WO4 microcrystals have an orthorhombic structure. FT-IR spectra exhibited four IR-active modes in a range from 250 to 1000 cm(-1). XANES spectra at the W L-3-edge showed distorted octahedral [WO6] clusters in the lattice, while EXAFS analyses confirmed that W atoms are coordinated by six O atoms. FE-SEM images suggest that the alpha-Ag2WO4 microcrystals grow by aggregation and the Ostwald ripening process. PL properties of alpha-Ag2WO4 microcrystals decrease with an increase in the optical band-gap values (3.19-3.23 eV). Finally, we observed that large hexagonal rod-like alpha-Ag2WO4 microcrystals prepared by the SC method exhibited a major PL emission intensity relative to alpha-Ag2WO4 microcrystals prepared by the CP and CH methods.