938 resultados para SOL-GEL PROCESS


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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.

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This feature article highlights work from the authors' laboratories on the various kinds of oxide optical materials, mainly luminescence and pigment materials with different forms (powder, core-shell structures, thin film and patterning) prepared by the Pechini-type sol-gel (PSG) process. The PSG process, which uses the common metal salts (nitrates, acetates, chlorides, etc.) as precursors and citric acid (CA) as chelating ligands of metal ions and polyhydroxy alcohol (such as ethylene glycol or poly ethylene glycol) as a cross-linking agent to form a polymeric resin on molecular level, reduces segregation of particular metal ions and ensures compositional homogeneity. This process can overcome most of the difficulties and disadvantages that frequently occur in the alkoxides based sol-gel process.

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Nanocrystalline ZrO2 fine powders were prepared via the Pechini-type sol-gel process followed by annealing from 500 to 1000 degrees C. The obtained ZrO2 samples were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), electron paramagnetic resonance (EPR), and photoluminescence spectra (PL), respectively. The phase transition process from tetragonal (T) to monoclinic (M) was observed for the nanocrystalline ZrO2 powders in the annealing process, accompanied by the change of their photoluminescence properties. The 500 degrees C annealed ZrO2, powder with tetragonal structure shows an intense whitish blue emission (lambda(max) = 425 nm) with a wide range of excitation (230-400 nm). This emission decreased in intensity after being annealed at 600 degrees C (T + M-ZrO2) and disappeared at 700 (T + M-ZrO2), 800 (T + M-ZrO2), and 900 degrees C (M-ZrO2). After further annealing at 1000 degrees C (M-ZrO2), a strong blue-green emission appeared again (lambda(max) = 470 nm).

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One-dimensional SrAl2O4:Eu2+, Dy3+ fibers were fabricated by a simple electrospinning combined with sol-gel process. X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy and photoluminescence were used to characterize the fibers. The results show that the phase structure of SrAl2O4:Eu2+, Dy3+ belongs to a monoclinic one, the composite fibers and fibers calcined at high temperature remain the original one-dimensional texture, and the SrAl2O4:Eu2+, Dy3+ was a green emission. (C) 2010 Elsevier Inc. All rights reserved.

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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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Nanocrystalline Pb(Zr0.52Ti0.48)O-3 was prepared from lead acetate, zirconium oxynitrate and titanium tetra-n-butoxide by a sol-gel method. It is found that both the crystallization temperature of precursor PZT and PZT product size were increased with increase of V(C3H8O2)/V(H2O) ratio in solution used. At V(C3H8O2)/V(H2O) = 4.47 the gel was formed moderately quick, and the nanocrystalline PZT with uniform granularity and low crystallizing temperature could be obtained. The diameter of the final nanocrystalline was ranged 60similar to70 nm as measured by atomic force microscopy (AFM). The crystallizing temperature of the precursor PZT was 443degreesC and the crystallization reaction was completed at 500degreesC by DTA and TG. The sol-gel reaction process was monitored by FT-IR and XRD.

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Using CaCO3, metal oxides (all dissolved by nitric acid) and tetraethoxysilane Si(OC2H5)(4) (TEOS) as the main starting materials, Ca2R8(SiO4)(6)O-2:A (R = Y, La, Gd; A = EU3+, Tb3+) phosphor films have been dip-coated on quartz glass substrates through the sol-gel process. X-ray diffraction (XRD), atomic force microscope (AFM), scanning electron microscope (SEM) and photoluminescence (PL) spectra as well as lifetimes were used to characterize the resulting films. The results of XRD indicated that the 1000 degreesC annealed films are isomorphous and crystallize with the silicate oxyapatite structure. AFM and SEM studies revealed that the phosphor films consisted of homogeneous particles ranging from 30 to 90 nm, with an average thickness of 1.30 mum. The Eu3+ and Tb3+ show similar spectral properties independent of R 3, in the films due to their isomorphous crystal structures. However, both the emission intensity and lifetimes of Eu3+ and Tb3+ in Ca2R8(SiO4)(6)O-2 (R = Y, La, Gd) films decrease in the sequence of R = Gd > R = Y > R = La, which have been explained in accordance with the crystal structures.

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Rare earth ions (Eu3+ and Dy3+)-doped Gd-2(WO4)(3) phosphor films were prepared by a Pechini sol-gel process. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), atomic force microscopy (AFM) and photoluminescence (PL) spectra as well as lifetimes were used to characterize the resulting powders and films. The results of XRD indicate that the films begin to crystallize at 600degreesC and the crystallinity increases with the elevation of annealing temperatures. The film is uniform and crack-free, WO(4)(2-)mainly consists of closely packed fine particles with an average grain size of 80 nm. Owing to an energy transfer from 4 groups, the rare earth ions show their characteristic emissions in crystalline Gd-2(WO4)(3) phosphor films, i.e., D-5(J) -F-7(J), (J = 0, 1, 2, 3; J' = 0 1, 2, 3, 4, not in all cases) transitions for Eu3+ and F-4(9/2)-H-6(J) (J = 13/2, 15/2) transitions for D Y3+, with the hypersensitive transitions D-5(0)-F-7(2) (Eu3+) and F-4(9/2) - H-6(13/2) (Dy3+) being the most prominent groups, respectively.

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Gd2Ti2O7: Eu3+ thin film phosphors were fabricated by a sol-gel process. X-ray diffraction (XRD), atomic force microscopy (AFM) and photoluminescence (PL) spectra as well as lifetimes were used to characterize the resulting films. The results of XRD indicated that the films began to crystallize at 800 degreesC and the crystallinity increased with the elevation of annealing temperatures. Uniform and crack free phosphor films were obtained, which mainly consisted of grains with an average size of 70 nm. The doped Eu3+ showed orange-red emission in crystalline Gd2Ti2O7 phosphor films due to an energy transfer from Gd2Ti2O7 host to them. Both the lifetimes and PL intensity of the Eu3+ increased with increasing the annealing temperature from 800 to 1000 degreesC, and the optimum concentrations for Eu3+ were determined to be 9 at.%. of Gd3+ in Gd2Ti2O7 film host.

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IrO2/SnO2 (10%:90%, molar ratio) electrodes (ITEs) were prepared by the sol-gel method as an alternative to the electrode-position and thermal decomposition process. The electrodes were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), atomic force microscope (AFM), cyclic voltammetry (CV) and electrochemical impedance spectra (EIS). From the results of XRD, oxide films prepared at low temperature were in amorphous state, while hydrous IrO2 crystal and cassiterite phase SnO2 were formed at 300 degreesC or even to 500 degreesC. The highly porous structure was confirmed by AFM. The electrochemical experiments demonstrated that the sol-gel method made the ITEs having a fast electron transfer process with good stability and the optimal preparation temperature was 400 degreesC for the highest electroactivity. Furthermore, the electrocatalysis of pyrocatechol on the electrodes was investigated. A quasi-reversible process occurred and a linear range over three orders magnitude (1 x 10(-2) - 10 mM) was obtained by differential pulse voltammetry (DPV). Meanwhile the detection limit of pyrocatechol was 5 x 10(-3) mM. This study indicated that the sol-gel method was an appropriate route to prepare the IrO2/SnO2 electrodes for the electrocatalytic of pyrocatechol.

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Europium-doped nanocrystalline GdVO4 phosphor layers were coated on the surface of preformed submicron silica spheres by sol-gel method. The resulted SiO2@Gd0.95Eu0.05VO4 core-shell particles were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (FESEM), energy-dispersive X-ray spectra (EDS), transmission electron microscopy (TEM), photoluminescence (PL) spectra, low voltage cathodoluminescence (CL), time resolved PL spectra and kinetic decays. The XRD results demonstrate that the Gd0.95Eu0.05VO4 layers begin to crystallize on the SiO2 spheres after annealing at 600 C and the crystallinity increases with raising the annealing temperature. The obtained core-shell phosphors have spherical shape, narrow size distribution (average size ca. 600 nm), non-agglomeration. The thickness of the Gd0.95Eu0.05VO4 shells on the SiO2 cores could be easily tailored by varying the number of deposition cycles (50 nm for four deposition cycles). PL and CL show that the emissions are dominated by D-5(0)-F-7(2) transition of Eu3+ (618 nm, red).

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(YSiWO8)-Si-2:Dy3+ phosphors were prepared through a sol-gel process. XRD and photoluminespectra were used to characterize the resulting phosphors. The results indicated that the phosphors crystallized completely at 1000 degrees C. In Y2SiWO8:Dy3+ phosphors, the Dy3+ showed its characteristic yellow emission at 483nm (F-4(9/2)-H-6(5/2)) and 575nm (F-4(9/2)-H-6(13/2)) upon excitation into 275nm.

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CaWO4 phosphor films doped with rare-earth ions (Eu3+, Dy-,(3+) Sm3+, Er3+) were prepared by the Pechini sol-gel process. X-ray diffraction (XRD), Fourier transform infrared spectroscopy, thermogravimetric and differential thermal analysis, atomic force microscopy, and photoluminescence spectra, as well as lifetimes, were used to characterize the resulting powders and films. The results of the XRD analysis indicated that the films began to crystallize at 400degreesC and that the crystallinity increased with elevation of the annealing temperature. The doped rare-earth ions showed their characteristic emissions in crystalline CaWO4 phosphor films due to energy transfer from WO42- groups to them. Both the lifetimes and PL intensities of the doped rare-earth ions increased with increasing annealing temperature, from 500 to 900degreesC, and the optimum concentrations for Eu3+, Dy3+, Sm3+, Er3+ were determined as 30, 1.5, 1.5, 0.5 at.% of Ca2+ in CaWO4 films annealed at 900degreesC, respectively.