254 resultados para chemically modified silica gel


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70SiO(2)-30HfO(2) mol% planar waveguides, doped with Er3+ with concentrations ranging from 0.3 to 2 mol% were prepared by sol-gel route, using dip-coating deposition on vitreous-SiO2 substrates. Infrared-to-visible upconversion emission, upon excitation at 980 nm, has been observed for all the samples. The upconversion results in green, red and blue emissions. The investigation of the upconversion dynamic as a function of the Er3+ concentration and excitation power, show that processes such as excited state absorption and energy transfer upconversion are effective. (C) 2003 Elsevier B.V. All rights reserved.

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The sols produced by admixture of ZrOCl2 acidified solutions to hot H2SO4 aqueous solutions were studied to clarify the effects of Cl- and SO42- ions on the kinetic stability of nanoparticles and to obtain some new evidence concerning the mechanism of a thermoreversible sol-gel transition observed in this system. The study of suspensions prepared with different molar ratios R-S = [Zr]/[SO42-] and R-Cl = [Zr]/[Cl-] revealed domains of composition of formation of thermoreversible gels, thermostable sols, and powder precipitation. The effects of R-S and R-Cl on the structural features of nanoparticles and on the particle solution interface were systematically analyzed for samples of thermoreversible and thermostable sol domains. Small-angle X-ray scattering measurements revealed the presence of small fractal aggregates in all samples of thermoreversible domains, while compact packing aggregates of primary particles are present in the thermostable sol. Extended X-ray absorption fine structure and elemental chemical analysis revealed that irrespective of the nominal value of R-S and R-Cl all studied samples of the thermoreversible domain are constituted by a well-defined compound possessing an inner core made of hydroxyl and oxo groups bridging together zirconium atoms surrounded on the surface by complexing sulfate ligands. zeta potentials of powders extracted by freeze-drying from the thermoreversible gel revealed a point of surface charge inversion attributed to the specific adsorption of SO42- ion. Thermoreversible gel formation is rationalized by considering the effect of the specific adsorption on the electrical double-layer repulsion together with the temperature dependency of the physical chemical properties of ions in solution.

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The sols prepared by mixing a ZrOCl2 acidified solution to a hot H2SO4 aqueous solutions were studied in order to clarify the mechanism of thermoreversible sol-gel transition observed in this system. The viscoelastic properties of these suspensions were analyzed during the sol-gel transition by dynamic rheological measurements and quasi-elastic light scattering. The rheological properties were correlated to mass fractal and nearly linear growth models, and percolation theory. The results evidence that the thermoreversible sol-gel transition in this system is due to the formation of a network of physically linked aggregates having fractal structure. The decrease of the SO42- contents in the initial solution leads to the decrease of the fractal dimensionality from 2.3 to 1.8, indicating a change of the kinetic mechanism of aggregate growth. Near the gel point these samples have the typical scaling expected from percolation theory. (C) 2004 Elsevier B.V. All rights reserved.

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Aware of the difficulties in applying sol-gel technology on the preparation of thin films suitable for optical devices, the present paper reports on the preparation of crack-free erbium- and ytterbium-doped silica: hafnia thick films onto silica on silicon. The film was obtained using a dispersion of silica-hafnia nanoparticles into a binder solution, spin-coating, regular thermal process and rapid thermal process. The used methodology has allowed a significant increase of the film thickness. Based on the presented results good optical-quality films with the required thickness for a fiber matching single mode waveguide were obtained using the erbium- and ytterbium-activated sol-gel silica:hafnia system. The prepared film supports two transversal electric modes at 1550 nm and the difference between the transversal electric mode and the transversal magnetic mode is very small, indicating low birefringence. Photoluminescence of the I-4(13/2) -> I-4(15/2) transition of erbium ions shows a broad band centered at 1.53 mu m with full width at a half maximum of 28 nm. Up-conversion emission was carried out under different pump laser powers, and just one transition at red region was observed. (c) 2006 Elsevier B.V. All rights reserved.

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In order to improve the chemical resistance of zirconium fluoride glass a protective transparent SnO2 layer was deposited by the solgel dip-coating process in the presence of Tiron (R) as particle surface modifier agent. After water immersion for different periods of time, both coated and non-coated fluoride glasses were analyzed by scanning electron microscopy, mass loss evaluation, infrared spectroscopy and X-ray photoelectron spectroscopy. In contrast to the effects occurring for non-coated glass, where the surface undergoes a rapid selective dissolution of the most soluble species, the results for the SnO2-coated glass showed that the filling of the film nanopores by dissolved glass material results in a hermetic barrier protecting the glass surface. The selective glass dissolution was confirmed by liquid chromatography measurements of the etching solution after each exposure time. (c) 2006 Elsevier B.V. All rights reserved.

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Pt-modified SnO2 electrodes were prepared onto titanium substrates in the form of thin films of similar to2 mum at different temperatures in the range from 200 to 400degreesC. Surface morphology was examined by scanning electron microscopy (SEM). It was found that Pt-SnO2 sol-gel layers are significantly rough and have a low porosity. X-ray diffraction (XRD) studies showed that the films consist of Pt nanoparticles with average size varying from about 5 to 10 nm, depending on the preparation temperature, and amorphous tin oxide. X-ray photoelectron spectroscopy (XPS) was employed to determine the superficial composition of the electrodes and demonstrated the presence of Sn4+ in all the samples. XPS spectra of the Pt 4f electrons showed the presence of Pt in the zero-valence state as well as in ionic forms. The general electrochemical behavior was characterized by cyclic voltammetry in 1 mol l(-1) HClO4 and the electrocatalytic activity towards the oxidation of formaldehyde was investigated by potential sweeps and chronoamperometry. The results obtained show that the Pt-SnO2/Ti system exhibits a significant catalytic activity for the oxidation of formaldehyde, with an onset potential below 0.1 V. (C) 2004 Elsevier Ltd. All rights reserved.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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

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In this paper an unprecedent thermo-reversible sol-gel transition for titania nanoparticles dispersed in a solution of p-toluene sulfonic acid (PTSH) in isopropanol is reported. The sol formed by the thermo-hydrolysis at 60 degrees C of titanium tetraisopropoxide (Ti((OPr)-Pr-i)(4)) reversibly changes into a turbid gel upon cooling to room temperature. Turbidimetric measurements performed for samples containing different nominal acidity ratios (A = [PTSH]/[Ti]) have evidenced that the gel transformation temperature increases from 20 to 35 degrees C as the [PTSH]/[Ti] ratio increases from 0.2 to 2.0. SAXS results indicate that the thermo-reversible gelation is associated to a reversible aggregation of a monodisperse set of titania nanoparticles with average gyration radius of approximate to 2 nm. From the different PTSH species evidenced by Raman spectroscopy and TG/DTA of dried gels we proposed that the then-no-reversible gelation in this systems is induced by the formation of a supramolecular network, in which the protonated surface of nanoparticles is interconnected through cooperative hydrogen bonds between -SO3 groups of p-toluene sulfonic acid. (C) 2009 Elsevier Ltd. All rights reserved.

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Erbium activated SiO2 -HfO2 planar waveguides, doped with Er3+ concentrations ranging from 0.01 to 4 mol%, were prepared by sol-gel method. The films were deposited on v-SiO2 and silica-on-silicon substrates using dip-coating technique. The waveguides show high densification degree, effective intermingling of the two film components, and uniform surface morphology. The waveguide deposited on silica-on-silicon substrates shows one single propagation mode at 1.5μm, with a confinement coefficient of 0.81 and an attenuation coefficient of 0.8 dB/cm at 632.8nm. Emission in the C-telecommunication band was observed at room temperature for all the samples upon continuouswave excitation at 980 nm or 514.5 nm. The shape of the emission band corresponding to the 4I13/2 → 4I15/2 transition is found to be almost independent both on erbium content and excitation wavelength, with a FWHM between 44 and 48 nm. The 4I13/2 level decay curves presented a single-exponential profile, with a lifetime ranging between 1.1 - 6.6 ms, depending on the erbium concentration. Infrared to visible upconversion luminescence upon continuous-wave excitation at 980 nm was observed for all the samples. Channel waveguide in rib configuration was obtained by etching the active film in order to have a well confined mode at 1.5 μm.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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