957 resultados para Sol-gel growth


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SiO2@Gd2MoO6:EU3+ core-shell phosphors were prepared by the sol-gel process. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectra (EDS), transmission electron microscopy ITEM), photoluminescence (PL) spectra as well as kinetic decays were used to characterize the resulting SiO2@Gd2MoO6:Eu3+ core-shell phosphors. The XRD results demonstrate that the Gd2MoO6:Eu3+ layers on the SiO2 spheres begin to crystallize after annealing at 600 degrees C and the crystallinity increases with raising the annealing temperature. The obtained core-shell phosphors have a near perfect spherical shape with narrow size distribution (average size ca. 600 nm), are not agglomerated, and have a smooth surface. The thickness of the Gd2MoO6:Eu3+ shells on the SiO2 cores could be easily tailored by varying the number of deposition cycles (50 nm for four deposition cycles). The Eu3+ shows a strong PL luminescence (dominated by D-5(0)-F-7(2) red emission at 613 nm) under the excitation of 307 nm UV light.

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Sol-gel derived TiO2/SiO2/ormosil hybrid planar waveguides have been deposited on soda-lime glass slides and silicon substrates, films were heat treated at 150 degreesC for 2 h or dried at room temperature. Different amounts of water were added to sols to study their impacts on microstructures and optical properties of films. The samples were characterized by m-line spectroscopy, Fourier transform infrared spectroscopy (FT-IR), UV/VIS/NIR spectrophotometer (UV-vis), atomic force microscopy (AFM), thermal analysis instrument and scattering-detection method. The refractive index was found to have the largest value at the molar ratio H2O/OR = 1 in sol (OR means -OCH3, -OC2H5 and -OC4H9 in the sol), whereas the thickest film appears at H2O/OR = 1/2. The rms surface roughness of all the films is lower than 1.1 nm, and increases with the increase of water content in sol. Higher water content leads to higher attenuation of film. (C) 2004 Elsevier B.V. All rights reserved.

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The development of efficient anti-corrosion and environmentally friendly coating systems are needed for the replacement of the highly toxic Cr-based conversion coatings for corrosion protection of aluminum alloys. In this study, we demonstrate that the direct application of ceramic cerium-based sol-gel coatings to AA7075-T6 substrates produces high-performance anti-corrosion layers. Electrochemical experiments and analyses of the microstructure demonstrate that the protective layers are very efficient for the passivation of the alloy surfaces operating as both passive and active barrier for corrosion protection.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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The evaluation of free carrier concentration based on Drude's theory can be performed by the use of optical transmittance in the range 800-2000 nm (near infrared) for Sb-doped SnO2 thin films. In this article, we estimate the free carrier concentration for these films, which are deposited via sol-gel dip-coating. At approximately 900 mn, there is a separation among transmittance curves of doped and undoped samples. The plasma resonance phenomena approach leads to free carrier concentration of about 5 x 1020 cm(-3). The increase in the Sb concentration increases the film conductivity; however, the magnitude of measured resistivity is still very high. The only way to combine such a high free carrier concentration with a rather low conductivity is to have a very low mobility. It becomes possible when the crystallite dimensions are taken into account. We obtain grains with 5 nm of average size by estimating the grain size from X-ray diffraction data, and by using line broadening in the diffraction pattern. The low conductivity is due to very intense scattering at the grain boundary, which is created by the presence of a large amount of nanoscopic crystallites. Such a result is in accordance with X-ray photoemission spectroscopy data that pointed to Sb incorporation proportional to the free electron concentration, evaluated according to Drude's model. (c) 2006 Elsevier Ltd. All rights reserved.

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In this paper, we report the synthesis of barium zirconate, BaZrO3, (BZ) nanotubes fabricated by the modified sol-gel method within the nanochannels of anodic aluminum oxide (AAO) templates. The morphology, structure, and composition of as prepared nanotubes were characterized by means of X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM), transmission electron microscope (TEM), selected-area electron diffraction ( SAED), high resolution TEM (HRTEM) and energy-dispersive X-ray spectroscopy (EDX). The results of XRD and SAED indicated that postannealed (at 650 degrees C for 1 h) BZ nanotubes (BZNTs) exhibited a polycrystalline cubic perovskite crystal structure. SEM and TEM analysis revealed that BZNTs possessed a uniform length and diameter (similar to 200 nm) and the thickness of the wall of the BZNTs was about 20 nm. Y-junctions, multiple branching and typical T-junctions were also observed in some BZNTs. EDX analysis demonstrated that stoichiometric BaZrO3 was formed. HRTEM image confirmed that the obtained BZNTs were composed of nanoparticles in the range of 5-10 nm. The possible formation mechanism of BZNTs was discussed.

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Highly crystalline CaMoO4:Tb3+ phosphor layers were grown on monodisperse SiO2 particles through a simple sol-gel method, resulting in formation of core-shell structured SiO2@CaMoO4:Tb3+ submicrospheres. The resulting SiO2@CaMoO4: Tb3+ core-shell particles were fully characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectra (EDS), transmission electron microscopy (TEM), photoluminescence (PL), low-voltage cathodoluminescence (CL), and kinetic decays. The XRD results demonstrate that the CaMoO4:Tb3+ layers begin to crystallize on the SiO2 spheres after annealing at 400 degrees C and the crystallinity increases with raising the annealing temperature. SEM and TEM analysis indicates that the obtained submicrospheres have a uniform size distribution and obvious core-shell structure. SiO2@CaMoO4:Tb3+ submicrospheres show strong green emission under short ultraviolet (260 nm) and low-voltage electron beam (1-3 kV) excitation, and the emission spectra are dominated by a D-5(4) -F-7(5) transition of Tb3+(544 nm, green) from the CaMoO4:Tb3+ shells.

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A series of Eu3+-doped ZnO films have been prepared by a sol-gel method. These films were characterized by X-ray diffraction (XRD) and photoluminecent spectra (PL). Effects of synthetic parameters, such as annealing atmosphere, temperature and concentration of doped ions, on the highly oriented crystal growth were studied in detail. The crystalline structures of films annealed in vacuum have a wurtzite symmetry with highly c-axis orientation. A characteristic D-5(0) -> F-7(J)(J = 1, 2, 3 and 4) red emission is observed due to energy transfer from the ZnO host to the doped Eu3+ in the c-oriented ZnO films.

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Supported ceramic membranes have been produced by the sol-casting procedure from aqueous colloidal suspensions prepared by the sol-gel route. Coatings on a tubular alumina support have been successfully performed leading to crack free layers. Samples have been sintered at 400, 500 and 600 degreesC, and the effect of heating treatment on the nanostructure and on the ultrafiltration properties are analyzed. The characterization has been done by high resolution scanning electron microscopy, nitrogen adsorption-desorption isotherms, water permeation and cut-off determination using polyethylene glycol standard solutions. The micrographs have revealed that grains and pore size increase with the temperature, whereas their shape remains invariant. This results is in agreements with N-2 adsorption-desorption analyses, which have revealed that the mean pore size diameter increases from 4 to 10 nm as the sintering temperature increases from 400 to 600 degreesC, while the total porosity remains constant. Furthermore, the tortuosity, calculated from water permeability, is essentially invariant with the sintering temperatures. The membranes cut-off, determined with a retention rate equal to 95%, are 3500, 6500 and 9000 g . mol(-1) for 400, 500 and 600 degreesC, respectively, showing that the permeation properties of SnO2 ultrafiltration membranes can easily be controlled by sintering condition.

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Sol-gel route was employed to grow polycrystalline thin films of Li-doped ZnO thin films (Zn1-xLixO, x=0.15). Polycrystalline films were obtained at a growth temperature of 400-500 degrees C. Ferroelectricity in Zn0.85Li0.15O was verified by examining the temperature variation of the real and imaginary parts of dielectric constant, and from the C-V measurements. The phase transition temperature was found to be 330 K. The room-temperature dielectric constant and dissipation factor were 15.5 and 0.09 respectively, at a frequency of 100 kHz. The films exhibited well-defined hysteresis loop, and the values of spontaneous polarization (P-s) and coercive field were 0.15 mu C/cm(2) and 20 kV/cm, respectively, confirming the presence of ferroelectricity.

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EU3+ -doped Y3Al5O12 (YAG:Eu3+) phosphors were synthesized by a facile sol-gel combustion method. In this process, citric acid traps the constituent cations and reduces the diffusion length of the precursors. YAG phase is obtained through sintering at 900 degrees C for 2h. There were no intermediate phases such as YAlO3 (YAP) and Y4Al2O9 (YAM) observed. The charge transfer band of nanocrystalline phosphors shows a shift toward the high-energy side, compared with that of amorphous ones due to lower covalency of Eu-O bond for nanocrystalline phosphors. The higher concentration quenching in YAG:EU3+ nanophosphors may be caused by the confinement effect on resonant energy transfer of nanocrystalline. It also indicates that the sol-gel combustion synthesis method provides a good distribution of Eu3+ activators in YAG host. (c) 2005 Elsevier B.V. All rights reserved.

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High-quality Ce3+-doped Y3Al5O12 (YAG:Ce3+) phosphors were synthesized by a facile sol-gel combustion method. In this sol-gel combustion process, citric acid acts as a fuel for combustion, traps the constituent cations and reduces the diffusion length of the precursors. The XRD and FT-IR results show that YAG phase can form through sintering at 900 degrees C for 2 h. This temperature is much lower than that required to synthesize YAG phase via the solid-state reaction method. There were no intermediate phases such as YAlO3 (YAP) and Y4Al2O9 (YAM) observed in the sintering process. The average grain size of the phosphors sintered at 900-1100 degrees C is about 40 nm. With the increasing of sintering temperature, the emission intensity increases due to the improved crystalline and homogeneous distribution of Ce3+ ions. A blue shift has been observed in the Ce3+ emission spectrum of YAG:Ce3+ phosphors with increasing sintering temperatures from 900 to 1200 degrees C. It can be explained that the decrease of lattice constant affects the crystal field around Ce3+ ions. The emission intensity of 0.06Ce-doped YAG phosphors is much higher than that of the 0.04Ce and 0.02Ce ones. The red-shift at higher Ce3+ concentrations may be Ce-Ce interactions or variations in the unit cell parameters between YAG:Ce3+ and YAG. It can be concluded that the sol-gel combustion synthesis method provides a good distribution of Ce3+ activators at the molecular level in YAG matrix. (c) 2005 Elsevier B.V. All rights reserved.

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Polycrystalline nano-grain-boundary multi-doping ZnO-based nonlinear varistors with higher concentration additives have been fabricated by sol-gel and standard solid-state reaction method, of which the best sample has a very high threshold voltage of E-b = 3300 V/mm. The effect of sintering processes, sintering temperature and sintering time, and that of additive concentration of Bi2O3 on E-b of the samples are systematically investigated. The results show that the great merit of sol-gel method is its high threshold voltage obtained by a lower sintering temperature than the solid-state reaction method. The present work also shows that five phases including solid-state sintering, rich Bi liquid phase formation and ZnO as well as other additive dissolution, ZnO grain growth, the secondary phase sufficient formation and evolution have been experienced at different sintering temperatures. The hole type defect and nonhomogeneity of the microstructure will lead to the decrease of threshold voltage, i.e., the grain size and the homogeneity of the material will be important factors and directly affect the characteristic of the varistor. The sintering characteristic and the influence of Bi2O3 content on the threshold voltage are also discussed. (c) 2004 Elsevier B.V. All rights reserved.

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Lu3Ga5O12:Eu3+, Lu3Ga5O12:Tb3+, and Lu3Ga5O12:Pr3+ phosphors were prepared through a Pechini-type sol-gel process. X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), photoluminescence, and cathodoluminescence spectra were utilized to characterize the synthesized phosphors. The XRD results reveal that the sample begins to crystallize at 800 degrees C and fully crystallined pure Lu3Ga5O12 phase can be obtained at 1000 degrees C. The FESEM image indicates that the phosphor sample is composed of aggregated rice grainlike particles with sizes around 80-120 nm.

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LaAlO3:Tm3+ and LaAlO3:Tb3+ phosphors were prepared through a Pechini-type sol-gel process. X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), photoluminescence, and cathodoluminescence (CL) spectra were utilized to characterize the synthesized phosphors. The XRD results reveal that the fully crystalline pure LaAlO3 Phase can be obtained at 800 degrees C. The FE-SEM image indicates that the phosphor samples are composed of aggregated spherical particles with sizes ranging from 40 to 80 nm. Under the excitation of ultraviolet light (230 nm) and low-voltage electron beams (1-3 kV), the LaAlO3:Tm3+ and LaAlO3:Tb3+ phosphors show the characteristic emissions of Tb3+ (D-1(2)-> H-3(6,4),F-3(4) transitions) and Tm3+ (D-5(3,4)-> F-7(6,5,4,3) transitions) respectively. The CL of the LaAlO3:Tm3+ phosphors have high color purity and comparable intensity to the Y2SiO5:Ce3+ commercial product, and the CL colors of Tb3+-doped LaAlO3 phosphors can be tuned from blue to green by changing the doping concentration of Tb3+ to some extent.