Growth mechanism of octahedron-like BaMoO4 microcrystals processed in microwave-hydrothermal: Experimental observations and computational modeling

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Synthesis and structural characterization of Eu(III)-doped Zn7Sb2O12

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

Structural characterization and Curie temperature determination of a sodium strontium niobate ferroelectric nanostructured powder

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

Deriving the magnitude of niobium off-center displacement in ferroelectric niobates from infrared spectroscopy

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Effects of strontium and calcium simultaneous substitution on electrical and structural properties of Pb1-x-y Ca (x) Sr (y) TiO3 thin films

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

Infrared studies of the monoclinic-tetragonal phase transition in Pb(Zr, Ti)O-3 ceramics

Recently, the observation of a new monoclinic phase in the PbZr1-xTixO3 (PZT) system in the vicinity of the morphotropic phase boundary was reported. Investigations of this new phase were reported using different techniques such as high-resolution synchrotron x-ray powder diffraction and Raman spectroscopy. In this work, the monoclinic --> tetragonal phase transition in PbZr0.50Ti0.50O3 ceramics was studied using infrared spectroscopy between 1000 and 400 cm(-1). The four possible nu(1)-stretching modes (Ti-O and Zr-O stretch) in the BO6 octahedron in the ABO(3) structure of PZT in this region were monitored as a function of temperature. The lower-frequency mode nu(1)-(Zr-O) remains practically unaltered, while both intermediate nu(1)-(Ti-O) modes decrease linearly as temperature increases from 89 to 263 K. In contrast, the higher-frequency nu(1)-(Ti-O) and nu(1)-(Zr-O) modes present anomalous behaviour around 178 K. The singularity observed at this mode was associated with the monoclinic --> tetragonal phase transition in PbZr0.50Ti0.50O3 ceramics.

Hydrothermal Microwave: A New Route to Obtain Photoluminescent Crystalline BaTiO3 Nanoparticles

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Synthesis, Characterization, Anisotropic Growth and Photoluminescence of BaWO4

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Magnetic resonance study of the crystallization behavior of InF3-based glasses doped with Cu2+, Mn2+ and Gd3+

The crystallization of fluoroindate glasses doped with Gd3+, Mn2+ and Cu2+ heat treated at different temperatures, ranging from the glass transition temperature (Tg) to the crystallization temperature (Tc), are investigated by electron paramagnetic resonance (EPR) and 19F nuclear magnetic resonance (NMR). The EPR spectra indicate that the Cu2+ ions in the glass are located in axially distorted octahedral sites. In the crystallized glass, the g-values agreed with those reported for Ba2ZnF6, which correspond to Cu2+ in a tetragonal compressed F- octahedron and to Cu2+ on interstitial sites with a square-planar F- co-ordination. The EPR spectra of the Mn2+ doped glasses exhibit a sextet structure due to the Mn2+ hyperfine interaction. These spectra suggest a highly ordered environment for the Mn2+ ions (close to octahedral symmetry) in the glass. The EPR spectra of the recrystallized sample exhibit resonances at the same position, suggesting that the Mn2+ ions are located in sites of highly symmetric crystalline field. The increase of the line intensity of the sextet and the decrease of the background line in the thermal treated samples suggest that the Mn2+ ions move to the highly ordered sites which contribute to the sextet structure. The EPR spectra of the Gd3+ doped glasses exhibit the typical U-spectrum of a s-state ion in a low symmetry site in disordered systems. The EPR of the crystallized glasses, in contrast, have shown a strong resonance in g ≈ 2.0, suggesting Gd3+ ions in environment close to cubic symmetry. The 19F NMR spin-lattice relaxation rates were also strongly influenced by the crystallization process that takes over in samples annealed above Tc. For the glass samples (doped or undoped) the 19F magnetization recoveries were found to be adjusted by an exponential function and the spin-lattice relaxation was characterized by a single relaxation time. In contrast, for the samples treated above Tc, the 19F magnetization-recovery becomes non-exponential. A remarkable feature of our results is that the changes in the Cu2+, Mn2+, Gd3+ EPR spectra and NMR relaxation, are always observed for the samples annealed above Tc. © 2006 Elsevier B.V. All rights reserved.

Structural refinement, growth mechanism, infrared/Raman spectroscopies and photoluminescence properties of PbMoO4 crystals

Lead molybdate (PbMoO4) crystals were synthesized by the co-precipitation method at room temperature and then processed in a conventional hydrothermal (CH) system at low temperature (70 °C for different times). These crystals were structurally characterized by X-ray diffraction (XRD), Rietveld refinement, micro-Raman (MR) and Fourier transformed infrared (FT-IR) spectroscopies. Field emission scanning electron microscopy images were employed to observe the shape and monitor the crystal growth process. The optical properties were investigated by ultraviolet-visible (UV-Vis) absorption and photoluminescence (PL) measurements. XRD patterns and MR spectra indicate that these crystals have a scheelite-type tetragonal structure. Rietveld refinement data possibilities the evaluation of distortions in the tetrahedral [MoO 4] clusters. MR and FT-IR spectra exhibited a high mode ν1(Ag) ascribed to symmetric stretching vibrations as well as a large absorption band with two modes ν3(Eu and Au) related to anti-symmetric stretching vibrations in [MoO 4] clusters. Growth mechanisms were proposed to explain the stages involved for the formation of octahedron-like PbMoO4 crystals. UV-Vis absorption spectra indicate a reduction in optical band gap with an increase in the CH processing time. PL properties of PbMoO4 crystals have been elucidated using a model based on distortions of tetrahedral [MoO4] clusters due to medium-range intrinsic defects and intermediary energy levels (deep and shallow holes) within the band gap. © 2012 Elsevier Ltd. All rights reserved.

Fe K-edge X-ray absorption spectroscopy study of Pb(Fe2/3W 1/3)O3-PbTiO3 multiferroic ceramics

The present paper is a comprehensive study concerning Fe K-edge X-ray absorption spectroscopy (XAS) measurements, which were performed to characterize the local structure of (1 - x)Pb(Fe2/3W1/3)O 3-xPbTiO3 samples as a function of temperature and PbTiO3 content. Results obtained by the fits of extended X-ray absorption fine structure consist with rhombohedral symmetry for Pb(Fe 2/3W1/3)O3 composition at temperatures lower than room temperature. This result is in apparent disagreement with X-ray and neutron diffraction characterization which have been reported. This apparent disagreement is related to the fact that XAS probes the short-range order, whereas X-ray diffraction provides structural information about the average structure. Moreover, as the PbTiO3 content increases, a disorder has been detected at local structure of the FeO6 octahedron. Analysis of X-ray absorption near edge structure spectra did not show modifications in intensity nor energy of transitions. © 2013 American Institute of Physics.

Study of a series of cobalt(II) sulfonamide complexes: Synthesis, spectroscopic characterization, and microbiological evaluation against M. tuberculosis. Crystal structure of [Co(sulfamethoxazole)2(H 2O)2]·H2O

Nowadays, the research for new and better antimicrobial compounds is an important field due to the increase of immunocompromised patients, the use of invasive medical procedures and extensive surgeries, among others, that can affect the incidence of infections. Another big problem associated is the occurrence of drug-resistant microbial strains that impels a ceaseless search for new antimicrobial agents. In this context, a series of heterocyclic- sulfonamide complexes with Co(II) was synthesized and characterized with the aim of obtaining new antimicrobial compounds. The structural characterization was performed using different spectroscopic methods (UV-Vis, IR, and EPR). In spite of the fact that the general stoichiometry for all the complexes was Co(sulfonamide)2·nH2O, the coordination atoms were different depending on the coordinated sulfonamide. The crystal structure of [Co(sulfamethoxazole)2(H2O)2]·H 2O was obtained by X-ray diffraction showing that Co(II) is in a slightly tetragonal distorted octahedron where sulfamethoxazole molecules act as a head-to-tail bridges between two cobalt atoms, forming polymeric chains. Besides, the activity against Mycobacterium tuberculosis, one of the responsible for tuberculosis, and the cytotoxicity on J774A.1 macrophage cells were evaluated. © 2012 Elsevier B.V. All rights reserved.

Dielectric and structural characterization of Pb1-xAxZr0.40Ti0.60O3 (A = Sr, Ca) ferroelectric ceramics

This paper reports the influence of Sr- and Ca-substitution on the structural and ferroelectric properties of Pb1-xSrxZr0.40Ti0.60O3 (PSZT) and Pb1-xCaxZr0.40Ti0.60O3 (PCZT) ceramic systems. The dielectric measurements show that these substitutions cause a diffuse behavior in the dielectric permittivity curves for all samples. According to the X-ray absorption near-edge structure (XANES) spectra collected at Ti K- and LIII-edge, when Pb was replaced by Sr or Ca, a decrease in the local distortion around Ti atoms in the TiO6 octahedron could be observed. The O K-edge XANES spectra also revealed that the hybridization between O 2p and Pb 6sp states decreased as the amount of Sr or Ca atoms increased. Based on these results, it was possible to ascertain that the ferroelectric behavior in PSZT and PCZT samples bears a close correlation to the hybridization weakening between O 2p and Pb 6 sp states. © 2013 by American Scientific Publishers.

Ferroelectric and structural instability of (Pb,Ca)TiO3 thin films prepared in an oxygen atmosphere and deposited on LSCO thin films which act as a buffer layer

Structural, microstructural and ferroelectric properties of Pb0.90Ca0.10TiO3 (PCT10) thin films deposited using La0.50Sr0.50CoO3 (LSCO) thin films which serve only as a buffer layer were compared with properties of the thin films grown using a platinum-coated silicon substrate. LSCO and PCT10 thin films were grown using the chemical solution deposition method and heat-treated in an oxygen atmosphere at 700 °C and 650 °C in a tube oven, respectively. X-ray diffraction (XRD) and Raman spectroscopy results showed that PCT10 thin films deposited directly on a platinum-coated silicon substrate exhibit a strong tetragonal character while thin films with the LSCO buffer layer displayed a smaller tetragonal character. Surface morphology observations by atomic force microscopy (AFM) revealed that PCT10 thin films with a LSCO buffer layer had a smoother surface and smaller grain size compared with thin films grown on a platinum-coated silicon substrate. Additionally, the capacitance versus voltage curves and hysteresis loop measurement indicated that the degree of polarization decreased for PCT10 thin films on a LSCO buffer layer compared with PCT10 thin films deposited directly on a platinum-coated silicon substrate. This phenomenon can be described as the smaller shift off-center of Ti atoms along the c-direction 〈001〉 inside the TiO6 octahedron unit due to the reduction of lattice parameters. Remnant polarization (P r ) values are about 30 μC/cm2 and 12 μC/cm2 for PCT10/Pt and PCT10/LSCO thin films, respectively. Results showed that the LSCO buffer layer strongly influenced the structural, microstructural and ferroelectric properties of PCT10 thin films. © 2013 Elsevier Ltd and Techna Group S.r.l.

Preparação e caracterização de filmes finos do tipo 'Pb IND. 1-x-yCa IND. xSr IND.yTiO IND. 3'

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