119 resultados para complex polymerization method

em Repositório Institucional UNESP - Universidade Estadual Paulista "Julio de Mesquita Filho"


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The BaMoO4 nanopowders were prepared by the Complex Polymerization Method (CPM). The structure properties of the BaMoO4 powders were characterized by FTIR transmittance spectra, X-ray diffraction (XRD), Raman spectra, photoluminescence spectra (PL) and high-resolution scanning electron microscopy (HR-SEM). The XRD, FTIR and Raman data showed that BaMoO4 at 300 degrees C was disordered. At 400 degrees C and higher temperature, BaMoO4 crystalline scheelite-type phases could be identified, without the presence of additional phases, according to the XRD, FTIR and Raman data. The calculated average crystallite sizes, calculated by XRD, around 40 nm, showed the tendency to increase with the temperature. The crystallite sizes, obtained by HR-SEM, were around of 40-50 nm. The sample that presented the highest intensity of the red emission band was the one heat treated at 400 degrees C for 2 h, and the sample that displayed the 'highest intensity of the green emission band was the one heat treated at 700 degrees C for 2 h. The CPM was shown to be a low cost route for the production of BaMoO4 nanopowders, with the advantages of lower temperature, smaller time and reduced cost. The optical properties observed for BaMoO4 nanopowders suggested that this material is a highly promising candidate for photoluminescent applications. (C) 2005 Elsevier B.V. All rights reserved.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Purpose: This study evaluated the influence of polymerization cycle and thickness of maxillary complete denture bases on the porosity of acrylic resin. Materials and Methods: Two heat-activated denture base resins - one conventional (Clássico) and one designed for microwave polymerization (Onda-Cryl) - were used. Four groups were established, according to polymerization cycles: A (Onda-Cryl, short microwave cycle), B (Onda-Cryl, long microwave cycle), C (Onda-Cryl, manufacturing microwave cycle), and T (Clássico, water bath). Porosity was evaluated for different thicknesses (2.0, 3.5, and 5.0 mm; thicknesses I, II, and III, respectively) by measurement of the specimen volume before and after its immersion in water. The percent porosity data were submitted to Kruskal-Wallis for comparison among the groups. Results: The Kruskal-Wallis test detected that the combinations of the different cycles and thicknesses showed significant differences, and the mean ranks of percent porosity showed differences only in the thinnest (2.0 mm) microwave-polymerized specimens (A = 53.55, B = 40.80, and C = 90.70). Thickness did not affect the results for cycle T (I = 96.15, II = 70.20, and III = 82.70), because porosity values were similar in the three thicknesses. Conclusions: Microwave polymerization cycles and the specimen thickness of acrylic resin influenced porosity. Porosity differences were not observed in the polymerized resin bases in the water bath cycle for any thickness. © 2007 by The American College of Prosthodontists.

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The present paper describes the synthesis, characterization, structural refinement and optical absorption behavior of lead tungstate (PbWO(4)) powders obtained by the complex polymerization method heat treated at different temperatures for 2h in air atmosphere. PbWO(4) powders were characterized by X-ray diffraction (XRD), Rietveld refinement, Fourier transform Raman (FT-Raman) spectroscopy and ultraviolet visible (UV-vis) absorption spectroscopy measurements. XRD, Rietveld refinement and FT-Raman revealed that PbWO(4) powders are free of secondary phases and crystallizes in a tetragonal structure. The UV-vis absorption spectroscopy measurements suggest the presence of intermediary energy levels into the band gap of structurally disordered powders. (C) 2008 Elsevier B.V. All rights reserved.

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In this work Ba0.99Eu0.01MoO4 (BEMO) powders were prepared by the first time by the Complex Polymerization Method. The structural and optical properties of the BEMO powders were characterized by Fourier Transform Infra-Red (FTIR), X-ray Diffraction (XRD), Raman Spectra, High-Resolution Scanning Electron Microscopy (HR-SEM) and Photoluminescent Measurements. XRD show a crystalline scheelite-type phase after the heat treatment at temperatures greater than 400 degrees C. The ionic radius of Eu3+ (0.109 nm) is lower than the Ba2+ (0.149 nm) one. This difference is responsible for the decrease in the lattice parameters of the BEMO compared to the pure BaMoO4 matrix. This little difference in the lattice parameters show that Eu3+ is expected to occupy the Ba2+ site at different temperatures, stayed the tetragonal (S-4) symmetry characteristic of scheelite-type crystalline structures of BaMoO4. The emission spectra of the samples, when excited at 394 nm, presented the D-5(1)-> F-7(0, 1 and 2) and D-5(0)-> F-7(0, 1, 2, 3 and 4) Eu3+ transitions at 523, 533, 554, 578, 589, 614, 652 and 699 nm, respectively. The emission spectra of the powders heat-treated at 800 and 900 degrees C showed a marked increase in its intensities compared to the materials heat-treated from 400 to 700 C. The decay times for the sample were evaluated and all of them presented the average value of 0.61 ms. Eu3+ luminescence decay time follows one exponential curve indicating the presence of only one type of Eu3+ symmetry site.

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Crystalline molybdate thin films were prepared by the complex polymerization method. The AMoO(4) (A = Ca, Sr, Ba) films were deposited onto Si wafers by the spinning technique. The Mo-O bond in the AMoO(4) structure was confirmed by FTIR spectra. X-ray diffraction revealed the presence of crystalline scheelite-type phase. The mass, size, and basicity of A(2+) cations was found to be dependent on the intrinsic characteristics of the materials. The grain size increased in the following order: CaMoO4 < SrMoO4 < BaMoO4. The emission band wavelength was detected at around 576 nm. Our findings suggest that the material's morphology and photoluminescence were both affected by the variations in cations (Ca, Sr, or Ba) and in the thermal treatment.

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SrMoO4 doped with rare earth are still scarce nowadays and have attracted great attention due to their applications as scintillating materials in electro-optical like solid-state lasers and optical fibers, for instance. In this work Sr1-xEuxMoO4 powders, where x = 0.01; 0.03 and 0.05, were synthesized by Complex Polymerization (CP) Method. The structural and optical properties of the SrMoO4:Eu3+ were analyzed by powder X-ray diffraction patterns, Fourier Transform Infra-Red (FTIR), Raman Spectroscopy, and through Photoluminescent Measurements (PL). Only a crystalline scheelite-type phase was obtained when the powders were heat-treated at 800 A degrees C for 2 h, 2 theta = 27.8A degrees (100% peak). The excitation spectra of the SrMoO4:Eu3+ (lambda(Em.) = 614 nm) presented the characteristic band of the Eu3 + 5L6 transition at 394 nm and a broad band at around 288 nm ascribed to the charge-transfer from the O (2p) state to the Mo (4d) one in the SrMoO4 matrix. The emission spectra of the SrMoO4:Eu3+ powders (lambda(Exc.) = 394 and 288 nm) show the group of sharp emission bands among 523-554 nm and 578-699 nm, assigned to the D-5(1)-> F-7(0,1and 2) and D-5(0)-> F-7(0,1,2,3 and 4), respectively. The band related to the D-5(0)-> F-7(0) transition indicates the presence of Eu3+ site without inversion center. This hypothesis is strengthened by the fact that the band referent to the D-5(0)-> F-7(2) transition is the most intense in the emission spectra.

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The study of the photoluminescent properties affected by order and disorder of the BaMoO4 powders is the principal objective in this work. BaMoO4 compounds were prepared using soft chemical process called Complex Polymerization Method. In this work, different deagglomeration types and different heating rates were used to promote different disorder degrees. Scheelite type phase (BaMoO4) was determined by X-ray Diffraction (XRD), Fourier Transformed Infra-Red (FTIR) and Raman spectroscopy after heat treating the sample at 400 degrees C. The room temperature luminescence spectra revealed an intense single-emission band in the visible region. Based on XRD and Raman data it was observed that the transition between the completely disordered structure to completely ordered structure is a good condition for photoluminescence (PL) emission. The best PL emission is obtained when the material possesses short range disorder, i.e., is periodically ordered (XRD), but some disorder as measured by Raman spectroscopy. The excellent optical properties observed for disordered BaMoO4 suggested that this material is a highly promising candidate for optical applications.

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CaMoO4 (CMO) disordered and ordered thin films were prepared by the complex polymerization method (CPM). The films were annealed at different temperatures and time in a conventional resistive furnace (RF) and in a microwave (MW) oven. The microstructure and surface morphology of the structure were monitored by atomic force microscopy (AFM) and high-resolution scanning electron microscopy (HRSEM). Order and disorder were characterized by X-ray diffraction (XRD) and optical reflectance. A strong photoluminescence (PL) emission was observed in the disordered thin films and was attributed to complex cluster vacancies. The experimental results were compared with density functional and Hartree-Fock calculations. (C) 2008 Elsevier B.V. All rights reserved.

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