Phase transformation and photoluminescence properties of nanocrystalline ZrO2 powders prepared via the Pechini-type sol-gel process

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).

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.

Luminescent properties of rare-earth-doped CaWO4 phosphor films prepared by the Pechini sol-gel process

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.

Co-immobilized microbial biosensor for BOD estimation based on sol-gel derived composite material

A novel type of biochemical oxygen demand (BOD) biosensor was developed for water monitor, based on co-immobilizing of Trichosporon cutaneum and Bacillus subtilis in the sol-gel derived composite material which is composed of silica and the grafting copolymer of poly (vinyl alcohol) and 4-vinylpyridine (PVA-g-P(4-VP)). Factors that influence the performance of the resulting biosensor were examined. The biodegradable substrate spectrum could be expanded by the co-immobilized microorganisms. The biosensor prepared also exhibited good reproducibility and long-term stability. Good agreement was obtained between the results of the sensor BOD measurement and those obtained from conventional BOD5 method for water samples.

Preparation and characterization of novel luminescent sol-gel films containing a RE3+ carboxylic acid complex

RE3+ (Eu3+, Tb3+) complexes with carboxylic acid (salicylic acid and benzoic acid) were introduced into the sol, which was prepared by the hydrolysis of tetraethoxysilane (TEOS). A sol-gel luminescent thin film (SG-LTF) was then prepared by dispersing the sol onto a silica substrate by a spin coating method. Multi-layer luminescent thin films were prepared by repeating the same process. The luminescent spectra, fluorescence lifetime and thermal stability of the SG-LTFs were investigated. For the reason of comparison polyvinylbutyral (PVB) was added into a N,N-dimethylformamide (DMF) solution in which the comparative RE3+ carboxylic acid complexes were previously dissolved to form the DMF/PVB solution and the PVB luminescent thin film (PVB-LTF) was prepared. The results show that a broad excitation band indicates the formation of RE complexes in the solid SG-LTFs. RE ions, which are restrained in the silica matrix, present longer lifetimes and higher thermal stability than that in the PVB-LTF containing the corresponding pure complexes. The different doping concentration of RE (III) complexes in the SG-LTFs and the different change of the emission intensities with the heat treatment temperature in the sol-gel thin film and the sol-gel bulk gel were also discussed in this paper.

Luminescence properties of Eu(phen)(2)Cl-3 doped in sol-gel-derived SiO2-PEG matrix

Rare earth complex Eu(phen)(2)Cl-3 was introduced into a SiO2-PEG-400 hybrid material by a sol-ger method. The result indicated that Poly(ethylene glycol) (PEG) could associate with Eu3+ and change the surroundings of Eu3+ in the hybrid material, greatly improving the decay time. Transparent SiO2-PEG400 hybrid doped with a very small amount of Eu(phen)(2)Cl-3 has better mechanical properties and can retain excellent luminescence properties of the rare earth complex. (C) 2000 Elsevier Science B.V. All rights reserved.

Silica sol-gel composite film as an encapsulation matrix for the construction of an amperometric tyrosinase-based biosensor

An amperometric tyrosinase enzyme electrode for the determination of phenols was developed by a simple and effective immobilization method using sol-gel techniques. A grafting copolymer was introduced into sol-gel solution and the composition of the resultant organic-inorganic composite material was optimized, the tyrosinase retained its activity in the sol-gel thin film and its response to several phenol compounds was determined at 0 mV vs. Ag/AgCl (sat. KCI). The dependences of the current response on pH, oxygen level and temperature were studied, and the stability of the biosensor was also evaluated. The sensitivity of the biosensor for catechol, phenol and p-cresol was 59.6, 23.1 and 39.4 muA/mM, respectively. The enzyme electrode maintained 73% of its original activity after intermittent use for three weeks when storing in a dry state at 4 degreesC. (C) 2000 Elsevier Science S.A. All rights reserved.

Preparation and characterization of luminescent thin films doped with rare earth (Tb3+, Eu3+) complexes derived from a sol-gel process

Sol-gel derived luminescent thin films doped with rare earth (RE) complexes were prepared using an in-situ synthesis method with a two-step hydrolysis process and the luminescence spectra were measured. Fluorescence Lifetime and thermal stability were investigated. The results show that a broad excitation band indicates the formation of RE complexes in the solid thin films. RE ions, which are restrained in a silica matrix, present longer lifetime and higher thermal stability than that in DMF/PVB films containing the corresponding pure complexes. (C) 2000 Elsevier Science B.V. All rights reserved.

Sol-gel biosensor

yA review with 44 references is presented on the development of sol-gel-based biosensor. The main discussions are devoted to the process, advantages and properties of sol-gel immobilization method, sol-gel optical biosensor and amperometric biosensor, also the trend in this field is forecasted.

Sol-gel thin-film immobilized soybean peroxidase biosensor for the amperometric determination of hydrogen peroxide in acid medium

An acid-stable soybean-peroxidase biosensor was devel oped by immobilizing the enzyme in a sol-gel thin film. Methylene blue was used as a mediator because of its high electron-transfer efficiency. The sol-gel thin film and enzyme membrane were characterized by FT-IR, and the effects of pH, operating potential, and temperature were explored for optimum analytical performance by using the amperometric method. The H2O2 sensor exhibited a fast response (5 s), high sensitivity (27.5 mu A/mM), as well as good thermostability and long-term stability. In addition, the performance of the biosensor was investigated using flow-injection analysis (FIA).

Sol-gel synthesis and electrical properties of ceria-based solid electrolytes

A series of solid electrolytes (Ce0.8RE0.2)(1-x)MxO2-delta(RE: Rare earth, M: Alkali earth) were prepared by sol-gel methods. XRD indicated that a pure fluorite phase was formed at 800 degrees C. The synthesis temperature by the sol-gel methods was about 700 degrees C lower than by the traditional ceramic method. The electrical conductivity and impedance spectra were measured. XPS showed that the oxygen vacancy increased obviously by doping MO, thus, resulting in the increase of the oxygen ionic transport number and conductivity. The performance of ceria-based solid electrolyte was improved. The effects of RE2O3 and MO on the electrical properties were discussed. The conductivity and the oxygen ionic transport number of (Ce0.8Sm0.2)(1-0.05)Ca0.05O2-delta is 0.126 S.cm(-1) and 0.99 at 800 degrees C, respectively.

Formation and characterization of tin oxide aerogel derived from sol-gel process based on tetra(n-butoxy)tin(IV)

Transparent and translucent SnO2 aerogels with high specific surface area (>300m(2)/g) have been prepared by sol-gel process using tetra(n-butoxy)tin(IV) as a starting compound, and supercritical drying technique for solvent extraction. Light scattering measurements reveal that the polymeric cluster size distribution in sol system is gradually broadened during sol-gel transition. SEM images show that the aerogels are made up of the cottonlike oxide agglomerates with a large number of Pores. TEM images show that these aerogels seem to be self-similar at different magnifications. Their pore size distribution is pretty wide ranging, from mesopore to macropore especially for that of translucent aerogel. (C) 2004 Elsevier B.V. All rights reserved.

Structural role of fluoride in aluminophosphate sol-gel glasses: High-resolution double-resonance NMR studies

The local structure of Na-Al-P-O-F glasses, prepared by a novel sol-gel route, was extensively investigated by advanced solid-state NMR techniques. Al-21{F-19} rotational echo double resonance (REDOR) results indicate that the F incorporated into aluminophosphate glass is preferentially bonded to octahedral Al units and results in a significant increase in the concentration of six-coordinated aluminum. The extent of Al-F and Al-O-P connectivities are quantified consistently by analyzing Al-27{P-31} and Al-21{F-19} REDOR NMR data. Two distinct types of fluorine species were identified and characterized by various F-19{Al-27}, F-19{Na-23}, and F-19{P-31} double resonance experiments, which were able to support peak assignments to bridging (Al-F-Al, -140 ppm) and terminal (Al-F, -170 ppm) units. On the basis of the detailed quantitative dipole-dipole coupling information obtained, a comprehensive structural model for these glasses is presented, detailing the structural speciation as a function of composition.