64 resultados para Auger electron spectroscopy


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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Novel brominated amorphous hydrogenated carbon (a-C:H:Br) films were produced by the plasma polymerization of acetylene-bromoform mixtures. The main parameter of interest was the degree of bromination, which depends on the partial pressure of bromoform in the plasma feed, expressed as a percentage of the total pressure, R-B. When bromoform is present in the feed, deposition rates of up to about 110 nm min(-1) may be obtained. The structure and composition of the films were characterized by Transmission Infrared Reflection Absorption Spectroscopy (IRRAS) and X-ray Photo-electron Spectroscopy (XPS). The latter revealed that films with atomic ratios Br:C of up to 0.58 may be produced. Surface contact angles, measured using goniometry, could be increased from similar to 63 degrees (for an unbrominated film) to similar to 90 degrees for R-B of 60 to 80%. Film surface roughness, measured using a profilometer, does not depend strongly on R-B. Optical properties the refractive index, n, absorption coefficient, alpha(E), where E is the photon energy, and the optical gap, E-g, were determined from film thicknesses and data obtained by Transmission Ultraviolet-Visible Near Infrared Spectroscopy (UVS). Control of n was possible via selection of R-B. The measured optical gap increases with increasing F-BC, the atomic ratio of Br to C in the film, and semi-empirical modeling accounts for this tendency. A typical hardness of the brominated films, determined via nano-indentation, was similar to 0.5 GPa. (C), 2013 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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Small-angle X-ray scattering (SAXS) and electron paramagnetic resonance (EPR) have been carried out to investigate the structure of the self-aggregates of two phenothiazine drugs, chlorpromazine (CPZ) and trifluoperazine (TFP), in aqueous solution. In the SAXS studies, drug solutions of 20 and 60 mM, at pH 4.0 and 7.0, were investigated and the best data fittings were achieved assuming several different particle form factors with a homogeneous electron density distribution in respect to the water environment. Because of the limitation of scattering intensity in the q range above 0.15 angstrom(-1), precise determination of the aggregate shape was not possible and all of the tested models for ellipsoids, cylinders, or parallelepipeds fitted the experimental data equally well. The SAXS data allows inferring, however, that CPZ molecules might self-assemble in a basis set of an orthorhombic cell, remaining as nanocrystallites in solution. Such nanocrystals are composed of a small number of unit cells (up to 10, in c-direction), with CPZ aggregation numbers of 60-80. EPR spectra of 5- and 16-doxyl stearic acids bound to the aggregates were analyzed through simulation, and the dynamic and magnetic parameters were obtained. The phenothiazine concentration in EPR experiments was in the range of 5-60 mM. Critical aggregation concentration of TFP is lower than that for CPZ, consistent with a higher hydrophobicity of TFP. At acidic pH 4.0 a significant residual motion of the nitroxide relative to the aggregate is observed, and the EPR spectra and corresponding parameters are similar to those reported for aqueous surfactant micelles. However, at pH 6.5 a significant motional restriction is observed, and the nitroxide rotational correlation times correlate very well with those estimated for the whole aggregated particle from SAXS data. This implies that the aggregate is densely packed at this pH and that the nitroxide is tightly bound to it producing a strongly immobilized EPR spectrum. Besides that, at pH 6.5 the differences in motional restriction observed between 5- and 16-DSA are small, which is different from that observed for aqueous surfactant micelles.

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This study assessed alterations on bovine enamel after excessive bleaching. Coronal portions of bovine teeth (n = 30) were sectioned and divided into three groups (n = 10 per group). The coronal parts were further cut incisocervically into two halves. While one half received no bleaching (control), the other half was subjected to either one (group 1), three (group 2), or five bleaching sessions (group 3) with 35% hydrogen peroxide. The enamel surfaces were then analyzed using scanning electron microscopy and energy dispersive x-ray spectroscopy (EDS). Fxcessive bleaching affected the surface morphology and chemistry of the bovine enamel. EDS analysis showed the highest decrease in calcium ion percentages in groups 2 and 3 when compared to their nonbleached halves. Oxygen and phosphorus percentages were comparable on both the control and bleached enamel, regardless of the number of bleaching sessions. Consecutive bleaching sessions with 35% hydrogen peroxide may lead to morphologic and specific elemental changes when performed in a short period of time. Calcium ion percentages may decrease when this bleaching agent is used for more than one session. Int J Prosthodontics 2010;23:29-32.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Photoacoustic spectroscopy was used to determine the critical distance for electron transfer from porphyrin to quinone molecules randomly dispersed in a polymeric matrix. An enhancement of the porphyrin signal was observed as the quinone concentration was increased. The data was analyzed according to the Perrin model [1] and it was found that the electron transfer occurred if the prophyrin-quinone distance was less than 33 Angstrom. To confirm the validity of the method, the fluorescence quenching was also measured for the samples. In this case, the same critical distance was obtained.

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

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Polymer light-emitting devices (PLEDs) with poly(2-methoxy-5-hexyloxy)-p-phenylenevinylene (OC1OC6-PPV) as the emissive layer were studied with an electron injection layer of ionomers consisting of copolymers of styrene and methylmethacrylate (PS/PMMA) with 3, 6 and 8 mol% degree of sulfonation. The ionomers were able to form very thin films over the emissive layer, with less than 30 nm. Additionally, the presence of ion pairs of ionomer suppresses the tendency toward dewetting of the thin film of ionomer (similar to 10 nm) which can cause malfunction of the device. The effect of the ionomers was investigated as a function of the ion content. The devices performance, characterized by their current density and luminance intensity versus voltage, showed a remarkable increase with the ionomer layer up to 6 mol% of ionic groups, decreasing after that for the 8 mol% ionomer device. The study of the impedance spectroscopy in the frequency range from 0.1 to 10(6) Hz showed that the injection phenomena dominate over the transport in the electroluminescent polymer bulk. (c) 2006 Elsevier B.V. All rights reserved.

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The versatility of sensor arrays made from nanostructured Langmuir-Blodgett (LB) and layer-by-layer (LBL) films is demonstrated in two ways. First, different combinations of sensing units are employed to distinguish the basic tastes, viz. sweet, sour, bitter, and salty tastes, produced, respectively, by small concentrations (down to 0.01 g/mol) of sucrose, HCl, quinine, and NaCl solutions. The sensing units are comprised of LB and/or LBL films from semiconducting polymers, a ruthenium complex, and sulfonated lignin. Then, sensor arrays were used to identify wines from different sources, with the high distinguishing ability being demonstrated in principal component analysis (PCA) plots. Particularly important was the fact that the sensing ability does not depend on specific interactions between analytes and the film materials, but a judicious choice of materials is, nevertheless, required for the materials to respond differently to a given sample. It is also shown that the interaction with the analyte may affect the morphology of the nanostructured films, as indicated with scanning electron microscopy. For instance, in wine analysis these changes are not irreversible and the original film morphology is retrieved if the sensing unit is washed with copious amounts of water, thus allowing the sensor unit to be reused.

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The zircon mineral is widely studied in geochronology. In the case of the fission track method (FTM), the age is determined by the density of fission tracks at the zircon surface, which can be observed with an optical microscope after an appropriate chemical treatment (etching). The etching must be isotropic at the zircon grain surface to be used in the FTM, which leads those zircon grains whose etching is anisotropic to be discarded. The only reason for this discarding is the nonuniform morphology of the surface grain seen by optical microscopy, that is, no further physicochemical analysis is performed. In this work, combining micro-Raman and scanning electron microscopy (SEM) to study the etching anisotropy, it was shown that zircon grains that present at least one area at the surface where the density of fission track is uniform can be used in the FTM. The micro-Raman showed characteristic spectra of the standard zircon sample either from the areas where there are tracks or from where there are not. The only difference found was in the Raman bandwidths, which were broader for the areas with higher density of fission tracks. This suggests simply a decrease in the relative percentage of the crystalline/amorphous phases at these areas. The SEM/energy dispersive spectrometry (EDX) showed that there were no significant differences in the principal chemical composition at the areas with and without fission tracks. Copyright (c) 2008 John Wiley & Sons, Ltd.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Structural and textural studies of a CuO/TiO2 System modified by cerium oxide were conducted using Raman spectroscopy, transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and N-2 absorption (BET specific surface area). The introduction of a minor amount of CeO2 (Ce0.09Ti0.82O1.91CU0.09 sample) resulted in a material with the maximum surface area value. The results of Raman spectroscopy revealed the presence of only two crystalline phases, TiO2 anatase and CeO2 cerianite, with well-dispersed copper species. TEM micrographs showed a trend toward smaller TiO2 crystallites when the cerium oxide content was increased. The XPS analysis indicated the rise of a second peak in Ti 2p spectra with the increasing amount of CeO2 located at higher binding energies than that due to the Till in a tetragonal symmetry. The CuO/TiO2 system modified by CeO2 displayed a superior performance for methanol dehydrogenation than the copper catalyst supported only on TiO2 or CeO2.