96 resultados para proton trititanate, ammonium ions, Raman spectroscopy, transmission electron microscopy, adsorption


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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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The phase transition from the non-polar a-phase to the polar beta-phase of poly(vinylidene fluoride) (PVDF) has been investigated using micro-Raman spectroscopy, which is advantageous because it is a nondestructive technique. Films of alpha-PVDF were subjected to stretching under controlled rates at 80 degrees C, while the transition to P-PVDF was monitored by the decrease in the Raman band at 794 cm(-1) characteristic of the a-phase, along with the concomitant increase in the 839 cm-1 band characteristic of the P-phase. The alpha ->beta transition in our PVDF samples could be achieved even for the sample stretched to twice (2 X -stretched) the initial length and it did not depend on the stretching rate in the range between 2.0 and 7.0 mm/min. These conclusions were corroborated by differential scanning calorimetry (DSC) and X-ray diffraction experiments for PVDF samples processed under the same conditions as in the Raman scattering measurements. Poling with negative corona discharge was found to affect the a-PVDF morphology, improving the Raman bands related to this crystalline phase. This effect is minimized for films stretched to higher ratios. Significantly, corona-induced effects could not be observed with the other experimental techniques, i.e., X-ray diffraction and infrared spectroscopy.

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Vitreous samples were prepared in the (100 2 x) NaPO3-x WO3 (0 <= x <= 70) glass forming system using conventional melting-quenching methods. The structural evolution of the vitreous network was monitored as a function of composition by thermal analysis, Raman spectroscopy and high resolution one- and two-dimensional P-31 solid state NMR. Addition of WO3 to the NaPO3 glass melt leads to a pronounced increase in the glass transition temperatures, suggesting a significant increase in network connectivity. At the same time Raman spectra indicate that up to about 30 mol% WO3 the tungsten atoms are linked to some non-bridging oxygen atoms (W-O- or W=O bonded species), suggesting that the network modifier sodium oxide is shared to some extent between both network formers. W-O- W bond formation occurs only at WO3 contents exceeding 30 mol%. P-31 magic angle spinning (MAS)-NMR spectra, supported by two-dimensional J-resolved spectroscopy, allow a clear distinction between species having two, one, and zero P-O-P linkages. The possible formation of some anionic tungsten sites suggested from the Raman data implies an average increase in the degree of polymerization for the phosphorus species, which would result in diminished P-31/Na-23 interactions. This prediction is indeed confirmed by P-31{Na-23} and Na-23{P-31} rotational echo double resonance (REDOR) NMR results, which indicate that successive addition of WO3 to NaPO3 glass significantly diminishes the strength of phosphorus-sodium dipole-dipole couplings.

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Blends possessing the elastomeric properties of natural rubber (NR) and the conducting properties of conducting polymer (polyaniline, PANI) were obtained, which are promising for further application in deformation sensors. Blends containing 20% (v/v) of PANI in 80% of NR latex were fabricated by casting in the form of free-standing films and treated either with HCl or with corona discharge, which lead PANI to its conducting state (doping process). Characterization was carried out by Raman spectroscopy, d.c. conductivity and thermogravimetric analysis. Evidence for chemical interaction between PANI and NR was observed, which allowed the conclusion that the NR latex itself is able partially to induce both the primary doping of PANI (by protonation) and the secondary doping of PANI (by changing the chain conformation). Further improvement in the primary doping could be obtained for the blends either by corona discharge or by exposing them to HCl the electrical conductivity reached in the blends was dependent on the doping conditions used, as observed by Raman scattering. Copyright (C) 2003 John Wiley Sons, Ltd.

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We have studied the phase transition behavior of Pb0.76Ca0.24TiO3 thin films using Raman scattering and dielectric measurement techniques. We also have studied the leakage current conduction mechanism as a function of temperature for these thin films on platinized silicon substrates. A Pb0.76Ca0.24TiO3 thin film was prepared using a soft chemical process, called the polymeric precursor method. The results showed that the dependence of the dielectric constant upon the frequency does not reveal any relaxor behavior. However, a diffuse character-type phase transition was observed upon transformation from a cubic paraelectric phase to a tetragonal ferroelectric phase. The temperature dependency of Raman scattering spectra was investigated through the ferroelectric phase transition. The soft mode showed a marked dependence on temperature and its disappearance at about 598 K. on the other hand, Raman modes persist above the tetragonal to cubic phase transition temperature, although all optical modes should be Raman inactive above the phase transition temperature. The origin of these modes must be interpreted in terms of a local breakdown of cubic symmetry by some kind of disorder. The lack of a well-defined transition temperature suggested a diffuse-type phase transition. This result corroborate the dielectric constant versus temperature data, which showed a broad ferroelectric phase transition in the thin film. The leakage current density of the PCT24 thin film was studied at elevated temperatures, and the data were well fitted by the Schottky emission model. The Schottky barrier height of the PCT24 thin film was estimated to be 1.49 eV. (C) 2003 American Institute of Physics.

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Ultrafine PbZr0.20Ti0.80O3 was omorphized through high-energy mechanical milling. The structural evolution through the omorphization process was accompanied by various characterization techniques, such as X-ray diffraction, Fourier-transformed IR spectroscopy (FTIR), high-resolution transmission electron microscopy (HR-TEM), and Raman spectroscopy. A strong photoluminescence was measured at room temperature for amorphized PbZr0.20Ti0.80O3, and interpreted by means of high-level quantum mechanical calculations in the density functional theory frame-work. Three periodic models were used to represent the crystalline and amorphized PbZr0.20Ti0.80O3, and they allowed the calculation of electronic properties that are consistent with the experimental data and that explain the appearance of photoluminescence.

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1. We describe the isolation of viable merozoites from erythrocytes infected with Babesia bovis or Babesia bigemina organisms by ammonium chloride lysis.2. Parasite morphology was examined by both light and transmission electron microscopy. Erythrocyte-free parasites maintain their viability and infectivity, retain their antigenicity and are suitable for use in the indirect fluorescent antibody assay.

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A new synthetic route for producing monodispersed and single crystal acicular goethite particles with small particle size and a high axial ratio adequate for use as a high density magnetic recording media precursor is reported. It essentially consists of the hydrolysis of alkaline Fe-III suspensions in the presence of carbonate by a three-step procedure, the formation of ferrihydrite primary particles, the ferrihydrite dissolution and nucleation of goethite, and the growth of the goethite nuclei. Changing the temperature of heating during ageing achieved a separation of the two last stages. X-Ray diffraction, transmission electron microscopy, infrared spectroscopy and surface area data have been used to determine the mechanism responsible for the formation of goethite particles with controlled size and shape. The best conditions to prepare monodispersed goethite particles have been established. The results show that uniform goethite particles of (a) 60 nm length with an axial ratio of 6 and (b) 230 nm length with a high axial ratio of 10, can be obtained by using an [OH]/[Fe] molar ratio of 0.35 in the initial suspensions with carbonate or sodium hydroxide, respectively. The [OH]/[Fe] molar ratio determines the particle size and elongation by controlling the hydrolysis reaction rate, while the carbonate ions promote a constant [OH] in the solution, keeping the pH around 10 during the entire synthesis process. This procedure, associated with the appropriate temperature control, leads, under certain conditions, to highly homogeneous goethite particles with sizes smaller than those obtained using sodium hydroxide with the same [OH]/[Fe] ratio.

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Photoexpansion and photobleaching effects have been observed in amorphous GeS2 + Ga2O3 (GGSO) thin films, when their surfaces were exposed to UV light. The photoinduced changes on the surface of the samples are indications that the structure has been changed as a result of photoexcitation. In this paper, micro-Raman, energy dispersive X-ray analysis (EDX) and backscattering electrons (BSE) microscopy were the techniques used to identify the origin of these effects. Raman spectra revealed that these phenomena are a consequence of the Ge-S bonds' breakdown and the formation of new Ge-O bonds, with an increase of the modes associated with Ge-O-Ge bonds and mixed oxysulphide tetrahedral units (S-Ge-O). The chemical composition measured by EDX and BSE microscopy images indicated that the irradiated area is oxygen rich. So, the present paper provides fundamental insights into the influence of the oxygen within the glass matrix on the considered photoinduced effects. (C) 2010 Elsevier B.V. All rights reserved.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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