953 resultados para evaporation crystallization
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Glasses with compositions (1-x)ZrF4-xLnF(3), 0.2 less than or equal to x less than or equal to 0.4 and Ln = La or La, Eu have been synthesized and investigated using differential scanning calorimetry, X-ray diffraction, Raman scattering and Eu3+ optical spectroscopy. Single-phase polycrystalline lanthanum fluorozirconates with Zr/Ln ratio equal to 1, 2 and 3 have been investigated using the same techniques for comparison. The crystalline phases LnZrF(7), LnZr(2)F(11), LT-LnZr(3)F(15) (orthorhombic) and HT-LnZr(3)F(15) (trigonal) have been characterized in the recrystallized glasses and in samples spontaneously crystallized from the melt. Another phase has also been observed but remains undefined, the Raman scattering spectra of the vitreous samples are related to the vibration modes of [ZrF6] isolated octahedra, and of [ZrF7] and [ZrF8] structural units with bridging fluorine ions. The Eu3+ fluorescence data are related to a predominant local environment of the lanthanide ions in the glasses similar to that of the lanthanide in LnZrF(7).
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Fluoride glasses have been extensively studied due to their high transparency in the infrared wavelength. The crystallization kinetics of these systems has been studied using DTA and DSC techniques. Most of the experimental data is frequently investigated in terms of the Johnson-Mehl-Avrami (JMA) model in order to obtain kinetic parameters.In this work, DSC technique has been used to study the crystallization of fluorozirconate glass under non-isothermal conditions. It was found that JMA model was not fit to be applied directly to these systems, therefore, the method proposed by Malek has been applied and the Sestak-Berggren (SB) model seems to be adequate to describe the crystallization process.
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A myotoxic phospholipase A(2), bothropstoxin II, which exhibits low hydrolytic activity, was crystallized and X-ray diffraction data were collected to a resolution of 2.2 Angstrom. Preliminary analysis reveals the presence of three molecules in the asymmetric unit. Copyright (C) 1996 Elsevier B.V. Ltd.
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Carboxyhaemoglobin-II isolated from the pacu (Piaractus mesopotamicus) has been crystallized and X-ray diffraction data were collected to 2.0 Angstrom resolution using synchrotron radiation. Crystals were characterized as belonging to the space group I23; preliminary structural analysis reveals the presence of one dimer in the asymmetric unit.
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SnO2 varistors doped with CoO, Cr2O3 and Nb2O5 were prepared by evaporation and decomposition of suspensions. The composition of the varistors was optimized to improve electrical properties, such as nonlinearity, leakage current and electrical stability. The best results were achieved with the following composition: 99.15% SnO2 +0.75% CoO+0.05% Cr2O3 +0.05% Nb2O5. Samples showed high density, reaching 99.5% of the theoretical density, as well as an homogeneous microstructure. The nonlinear coefficient was higher than 30 in the current range from 10(-7) to 10(-2) A/cm(2). The leakage current was 0.86 mu A/cm(2). These samples showed high stability of electrical parameters when they were exposed to high current of 27 mA/cm(2) for different time periods up to 30 min. (c) 2005 Elsevier Ltd. All rights reserved.
Crystallization and preliminary X-ray diffraction analysis of a lectin from Canavalia maritima seeds
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Tuberculosis remains the leading cause of mortality arising from a bacterial pathogen ( Mycobacterium tuberculosis). There is an urgent need for the development of new antimycobacterial agents. The aromatic amino-acid pathway is essential for the survival of this pathogen and represents a target for structure-based drug design. Accordingly, the M. tuberculosis prephenate dehydratase has been cloned, expressed, purified and crystallized by the hanging-drop vapour-diffusion method using PEG 400 as a precipitant. The crystal belongs to the orthorhombic space group I222 or I2(1)2(1)2(1), with unit-cell parameters a = 98.26, b = 133.22, c = 225.01 angstrom, and contains four molecules in the asymmetric unit. A complete data set was collected to 3.2 angstrom resolution using a synchrotron-radiation source.
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The hspA gene (XAC1151) from Xanthomonas axonopodis pv. citri encodes a protein of 158 amino acids that belongs to the small heat-shock protein ( sHSP) family of proteins. These proteins function as molecular chaperones by preventing protein aggregation. The protein was crystallized using the sitting-drop vapour-diffusion method in the presence of ammonium phosphate. X-ray diffraction data were collected to 1.65 angstrom resolution using a synchrotron-radiation source. The crystal belongs to the rhombohedral space group R3, with unit-cell parameters a = b = 128.7, c = 55.3 angstrom. The crystal structure was solved by molecular-replacement methods. Structure refinement is in progress.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
CRYSTALLIZATION PROCESS AND CHEMICAL DISORDER IN FLASH EVAPORATED AMORPHOUS GALLIUM ANTIMONIDE FILMS
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Both narrow and broad photoluminescence bands were observed in Ga1-XAsX films prepared by flash evaporation of polycrystalline GaAs containing native C impurities. The observed narrow crystalline-like bands are similar to band-to-band and C acceptor impurity emissions in crystalline GaAs. The narrow bands are evidence that the As excess favors the PL active GaAs crystallite formation in films deposited onto silicon (10 0) substrate, even when the As excess is very large (X = 0.84). This favoring is not observed in twin samples grown on silica glass substrates nor on Ga rich samples, indicating the important role of the combined effect of the As excess and Si substrate in the GaAs crystallite formation. The broad amorphous-like bands were observed in Ga rich and in moderately As rich samples. The photoluminescence emission is compared with the microstructure of the material as determined from the micro-Raman, absorption edge and reflectance measurements. The volume fraction of the crystallites formed is small and PL emission indicates that the crystallite electronic quality is much better than the ones formed heat treating films grown on silica glass substrates. (C) 2004 Elsevier B.V. All rights reserved.
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Pure and lanthanum-doped Bi4Ti3O12 thin films were deposited on Pt/Ti/SiO2/Si substrate using a polymeric precursor solution. The spin-coated films were specular and crack-free and crystalline after annealing at 700 degreesC for 2 h. Crystallinity and morphological evaluation were examined by X-ray diffraction (XRD), scanning electron microscopy (SEM), and atomic force microscopy (AFM). Multilayered films obtained using the intermediate-crystalline layer route present a dense microstructure with spherical grains. Films obtained using the intermediate-amorphous layer, present elongated grains around 250 nm in size. The dielectric and ferroelectric properties of the lanthanum-doped Bi4Ti3O12 films are strongly affected by the crystallization route. The hysteresis loops are fully saturated with a remnant polarization and drive voltage of the films, heat-treated by the intermediate-crystalline (P-r = 20.2 muC/cm(2) and V = 1.35 V) and for the film heat-treated by amorphous route (P-r = 22.4 muC/cm(2) and V = 2.99 V). (C) 2004 Elsevier B.V. All rights reserved.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Zhaoermiatoxin, an Arg49 phospholipase A(2) homologue from Zhaoermia mangshanensis (formerly Trimeresurus mangshanensis, Ermia mangshanensis) venom is a novel member of the PLA(2)-homologue family that possesses an arginine residue at position 49, probably arising from a secondary Lys49 -> Arg substitution that does not alter the catalytic inactivity towards phospholipids. Like other Lys49 PLA(2) homologues, zhaoermiatoxin induces oedema and strong myonecrosis without detectable PLA(2) catalytic activity. A single crystal with maximum dimensions of 0.2 x 0.2 x 0.5 mm was used for X-ray diffraction data collection to a resolution of 2.05 angstrom using synchrotron radiation and the diffraction pattern was indexed in the hexagonal space group P6(4), with unit-cell parameters a = 72.9, b = 72.9, c = 93.9 angstrom.