A study of NiZnCu-ferrite/SiO2 nanocomposites with different ferrite contents synthesized by sol-gel method

Ni0.65Zn0.35Cu0.1Fe1.9O4/SiO2 nanocomposites with different weight percentages of NiZnCu-ferrite dispersed in silica matrix were successfully fabricated by the sol-gel method using tetraethylorthosilicate (TEOS) as a precursor of silica, and metal nitrates as precursors of NiZnCu ferrite. The thermal decomposition process of the dried gel was studied by thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The obtained Ni0.65Zn0.35Cu0.1Fe1.9O4/SiO2 nanocomposites were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), scanning electron microscope (SEM), Mossbauer spectroscopy and vibrating sample magnetometry (VSM). The formation of stoichiometric NiZnCu-ferrite dispersed in silica matrix is confirmed when the weight percentage of ferrite is not more than 30%. Samples with higher ferrite content have small amount of alpha-Fe2O3. The transition from the paramagnetic to the ferromagnetic state is observed as the ferrite content increases from 20 to 90wt%.

Effects R3+ on the photoluminescent properties of Ca2R8(SiO4)(6)O-2 : A (R = Y, La, Gd; A= Eu3+, Tb3+) phosphor films prepared by the sol-gel process

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.

Fabrication and luminescent properties of rare earths-doped Gd-2(WO4)(3) thin film phosphors by Pechini sol-gel process

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.

Fabrication, patterning and luminescence properties of X-2-Y2SiO5 : A (A = Eu3+, Tb3+, Ce3+) phosphor films via sol-gel soft lithography

X-2-y(2)SiO(5):A (A = Eu3+, Tb3+, Ce3+) phosphor films and their patterning were fabricated by a sol-gel process combined with a soft lithography. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), atomic force microscopy (AFM), scanning electron microscopy (SEM) optical microscopy and photoluminescence (PL) were used to characterize the resulting films. The results of XRD indicated that the films began to crystallize at 900 degreesC with X-1-Y2SiO5, which transformed completely to X-2-Y2SiO5 at 1250 degreesC. Patterned thin films with different band widths (5 pin spaced by 5 pm and 16 pm spaced by 24 pm) were obtained by a soft lithography technique (micromoulding in capillaries, MIMIC). The SEM and AFM study revealed that the nonpattemed phosphor films were uniform and crack free, and the films mainly consisted of closely packed grains with an average size of 350 run. The doped rare earth ions (A) showed their characteristic emissions in X-2-Y2SiO5 phosphor films, i.e., D-5(0)-F-7(J) (J = 0, 1, 2,3,4) for Eu3+, D-5(3), (4)-F-7(J) (J = 6, 5, 4, 3) for Tb3+ and 5d (D-2)-4f (F-2(2/5),(2/7)) for Ce3+, respectively. The optimum doping concentrations for EU3+, Tb3+ were determined to be 13 and 8 mol% of Y3+ in X-2-Y2SiO5 films, respectively.

Luminescent properties of Gd2Ti2O7 : Eu3+ phosphor films prepared by sol-gel process

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.

Luminescent sol-gel thin films based on europium-substituted heteropolytungstates

Polyester thin films containing europium-substituted heteropolytungstate were obtained on quartz plate by the sol-gel method. The films exhibited the characteristic emission bands of the europium ion. The red to orange intensity ratio (R:O) of Eu3+ in the films increased as compared to the corresponding heteropolytungstate solids. The fluorescence lifetime of europium is shorter in the thin film than in the heteropolytungstate solid. The results indicated that the formation of europium-substituted heteropolytungstate/polyester thin film has great effect on the luminescence of europium- substituted heteropolytungstate.

IrO2/SnO2 electrodes: prepared by sol-gel process and their electrocatalytic for pyrocatechol

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.

Sol-Gel Preparation of Zn2 Si04：Mn Phosphor Layers on Silica Spheres and Their Luminescent Properties

The synthesis and luminescence properties of Zn2SiO4:Mn phosphor layers on spherical silica spheres,i.e.,a kind of core-shell complex phosphor,Zn2SiO4:Mn@SiO2 were described.Firstly,monodisperse silica spheres were obtained via the Stober method by the hydrolysis of tetraethoxysilane(TEOS)Si(OC2H5)4 under base condition (using NH4OH as the catalyst).Secondly,the silica spheres were coated with a Zn2SiO4:Mn phosphor layer by a Pechini sol-gel process.X-ray diffraction(XRD),scanning electron microscope(SEM),energy-dispersive X-ray spectrum(EDS) and photoluminescence(PL) were employed to characterize the resulting complex phosphor.The results comfirm that 1000℃ annealed sample consists of crystalline Zn2SiO4:Mn shells and amorphous SiO2 cores.The phosphor show the green emission of Mn2+ at 521nm corresponding 4T1(4G)-6A1(6S) transition,and the possible luminescence mechanism is proposed.

Sol-gel-derived BPO4/Ba2+ as a new efficient and environmentally-friendly bluish-white luminescent material

In this paper, BPO4 and Ba2+-doped BPO4 powder samples were prepared by the sol-gel process using glycerol and poly(ethylene glycol) as additives. The structure and optical properties of the resulting samples were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, field emission scanning electron microscopy (FESEM), diffuse reflection spectra, photoluminescence (PL) excitation and emission spectra, quantum yield, kinetic decay, and electron paramagnetic resonance (EPR), respectively. It was found that the undoped BPO4 showed a weak purple blue emission (409 nm, lifetime 6.4 ns) due to the carbon impurities involved in the host lattice. Doping Ba2+ into BPO4 resulted in oxygen-related defects as additional emission centers which enhanced the emission intensity greatly (> 10x) and shifted the emission to a longer-wavelength region (lambda(max) = 434 nm; chromaticity coordinates: x = 0.174, y = 0. 187) with a bluish-white color. The highest emission intensity was obtained ;when doping 6 mol % Ba2+ in BPO4, which has a quantum yield as high as 31%. The luminescent mechanisms of BPO4 and Ba2+-doped BPO4 were discussed in detail according to the existing models for silica-based materials.

Investigation of sol-gel transition in Pluronic F127/D2O solutions using a combination of small-angle neutron scattering and Monte Carlo simulation

Physical gelation in the concentrated Pluronic F127/D2O solution has been studied by a combination of small-angle neutron scattering (SANS) and Monte Carlo simulation. A 15% F127/D2O solution exhibits a sol-gel transition at low temperature and a gel-sol transition at the higher temperature, as evidenced by SANS and Monte Carlo simulation studies. Our SANS and simulation results also suggest that the sol-gel transition is dominated by the formation of a percolated polymer network, while the gel-sol transition is determined by the loss of bound solvent. Furthermore, different diffusion behaviors of different bound solvents and free solvent are observed. We expect that this approach can be further extended to study phase behaviors of other systems with similar sol-gel phase diagrams.

Sol-gel synthesis and characterization of SiO2@CaWO4, SiO2@CaWO4 : Eu3+/Tb3+ core-shell structured spherical particles

Nanocrystalline CaWO4 and Eu3+ (Tb3+)-doped CaWO4 phosphor layers were coated on non-aggregated, monodisperse and spherical SiO2 particles by the Pechini sol-gel method, resulting in the formation of SiO2@CaWO4, SiO2@CaWO4:Eu3+/Tb3+, core-shell structured particles. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), photoluminescence (PL), low-voltage cathodoluminescence (CL), time-resolved PL spectra and lifetimes were used to characterize the core-shell structured materials. Both XRD and FT-IR indicate that CaWO4 layers have been successfully coated on the SiO2 particles, which can be further verified by the FESEM and TEM images. The PL and CL demonstrate that the SiO2@CaWO4 sample exhibits blue emission band WO42- with a maximum at 420 nm (lifetime = 12.8 mu s) originated from the 4 groups, while SiO2@CaWO4:Eu3+ and SiO2@CaWO4:Tb3+ show additional red emission dominated by 614 nm (Eu3+:D-5(0)-F-7(2) transition, lifetime = 1.04 ms) and green emission at 544 nm (Tb3+:D-5(4)-F-7(5) transition, lifetime = 1.38 ms), respectively.

Sol-gel synthesis and photoluminescence properties of spherical SiO2@LaPO4 : Ce3+/Tb3+ particles with a core-shell structure

LaPO4: Ce3+ and LaPO4: Ce3+, Tb3+ phosphor layers have been deposited successfully on monodispersed and spherical SiO2 particles of different sizes ( 300, 500, 900 and 1200 nm) through a sol - gel process, resulting in the formation of core - shell structured SiO2@ LaPO4: Ce3+/ Tb3+ particles. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microcopy (SEM), transmission electron microscopy (TEM), and general and time-resolved photoluminescence (PL) spectra as well as lifetimes were used to characterize the resulting SiO2@ LaPO4: Ce3+/ Tb3+ samples. The XRD results demonstrate that the LaPO4: Ce3+, Tb3+ layers begin to crystallize on the SiO2 templates after annealing at 700 degrees C, and the crystallinity increases on raising the annealing temperature. The obtained core - shell phosphors have perfectly spherical shape with a narrow size distribution, non-agglomeration, and a smooth surface. The doped rare-earth ions show their characteristic emission in the core - shell phosphors, i.e. Ce3+ 5d - 4f and Tb3+5D4 - F-7(J) (J = 6 - 3) transitions, respectively. The PL intensity of the Tb3+ increased on increasing the annealing temperature and the SiO2 core particle size.

Electrogenerated chemiluminescence biosensor based on Ru(bpy)(3)(2+) and dehydrogenase immobilized in sol-gel/chitosan/poly(sodium 4-styrene sulfonate) composite material

A new electrogenerated chemiluminescence biosensor was fabricated by immobilizing ECL reagent Ru(bPY)(3)(2+) and alcohol dehydrogenase in sol-gel/chitosan/poly(sodium 4-styrene sulfonate) (PSS) organically modified composite material. The component PSS was used to immobilize ECL reagent Ru(bpy)(3)(2+) by ion-exchange, while the addition of chitosan was to prevent the cracking of conventional sol-gel-derived glasses and provide biocompatible microenvironment for alcohol dehydrogenase. Such biosensor combined enzymatic selectivity with the sensitivity of ECL detection for quantification of enzyme substrate and it was much simpler than previous double-layer design. The detection limit was 9.3 x 10(-6) M for alcohol (S/N = 3) with a linear range from 2.79 x 10(-5) to 5.78 x 10(-2) M. With ECL detection, the biosensor exhibited wide linear range, high sensitivity and good stability.

Silica supported submicron SiO2@Y2SiO5 : Eu3+ and SiO2@Y2SiO5 : Ce3+/Tb3+ spherical particles with a core-shell structure: Sol-gel synthesis and characterization

X-1-y(2)SiO(5):Eu3+ and X-1-Y2SiO5:Ce3+ and/or Tb3+ phosphor layers have been coated on nonaggregated, monodisperse, submicron spherical SiO2 particles by a sol-gel process, followed by surface reaction at high temperature (1000 degrees C), to give core/shell structured SiO2@Y2SiO5:Eu3+ and SiO2@Y2SiO5:Ce3+/Tb3+ particles. X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), TEM, photoluminescence (PL), low voltage cathodoluminescence (CL), and time-resolved PL spectra and lifetimes are used to characterize these materials. The XRD results indicate that X-1-Y2SiO5 layers have been successfully coated on the sur- face Of SiO2 particles, as further verified by the FESEM and TEM images. The PL and CL studies suggest that SiO2@Y2SiO5:Eu3+, SiO2@Y2SiO5:Tb3+ (or Ce3+/Tb3+), and SiO2@Y2SiO5:Ce3+ core/shell particles exhibit red (Eu3+, 613 rim: D-5(0)-F-7(2)), green (Tb3+, 542nm: D-5(4)-F-7(5)), or blue (Ce3+, 450nm: 5d-4f) luminescence, respectively. Pl, excitation, emission, and time-resolved spectra demonstrate that there is an energy transfer from Ce3+ to Tb3+ in the SiO2@Y2SiO5:Ce3+,Tb3+ core/shell particles.

Luminescence properties of sol-gel derived spherical SiO2@Gd-2(WO4)(3): Eu3+ particles with core-shell structure

Monodisperse, core-shell structured SiO2@Gd-2(WO4)(3):Eu3+ particles were prepared by the sol-gel method. The samples were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy, transmission electron microscopy, photoluminescence (PL) and low-voltage cathodoluntinescence (CL). PL and CL study revealed that the core-shell structured SiO2@Gd-2(WO4)(3):Eu3+ particles show strong red emission dominated by the D-5(0)-F-7(2) transition of Eu3+ at 615 nm with a lifetime of 0.89 ins. The PL and CL emission intensity can be tuned by the coating number of Gd-2(WO4)(3):Eu3+ phosphor layers on SiO2 particles, the size of the SiO2 core particles, and by accelerating voltage and the filament current, respectively.