87 resultados para Preparation process


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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.

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Barium titanate (BaTiO3) powders with particle sizes of 30 similar to 50 nm were prepared from barium stearate, titanium alkoxides and stearic acid by stearic acid-gel method. Dispersing the agglomerate of BaTiO3 nanoparticles into poly(amic acid) solution followed by curing led to the formation of polyimide hybrid films. The hybrid films were transparent and well distributed with BaTiO3 nanoparticles when the BaTiO3 content was less than 1 wt%. Highly loaded hybrid film containing 30 wit % BaTiO3 was tough, had a smooth surface and possessed much higher dielectric and piezoelectric constants than the parent polyimide.

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In-situ synthesis of terbium complex with salicylic acid (Sal) in silica matrix was made by a two-step sol-gel process. The terbium complex with salicylic acid was formed in sol-gel derived silica gel, and confirmed by the luminescence excitation spectra and infrared(IR) spectra. As compared to the pure terbium complex powder, the silica gel containing terbium complex exhibits its characteristic emission and presents a longer fluorescence lifetime than that for the pure complex. The luminescence properties of the complex containing;silica gel were investigated and compared with that of both terbium doped the silica gel and thp pure complex powder. The reasons leading to the above results were also discussed.

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An in-situ modified sol-gel method for the preparation of a Ni-based monolith-supported catalyst is reported. With the presence of a proper amount of plasticizer and binder, and at an optimized pH value, the stable boehmite sol was modified with metal ions (Ni, Li, La) successfully without distinct growth of the particle size. Monolith-supported Ni-based/gamma-Al2O3 catalysts were obtained using the modified sol as the coating medium with several cycles of dip-coating and calcination. Combined BET, SEM-EDS, XRD and H-2-TPR investigations demonstrated that the derived monolith catalysts had a high specific surface area, a relatively homogeneous surface composition, and a high extent of interaction between the active component and the support. These catalysts showed relatively stable catalytic activities for partial oxidation of methane (POM) to syngas under atmospheric pressure. The monolith catalysts prepared by this sol-gel method also demonstrated an improved resistance to sintering and loss of the active component during the reaction process.

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Two kinds of silanes, 3-glycidoxypropyltrimethoxysilane (GLYMO) and 3-trimethoxysililpropylmethacrylate (TMSPM), were used to prepare ormosil waveguide films by the sol-gel method. Thirty percent Ti(OBu)(4) and 70% silane were contained in the precursor sets. The properties of films were measured by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), UV/VIS/NIR spectrophotometer (UV-vis), atomic force microscopy (AFM), m-line and scattering-detection method. The films from GLYMO and TMSPM precursors exhibit similar thickness (2.58 mu m for GLYMO, 2.51 mu m for TMSPM) and refractive index (1.5438 for GLYMO, 1.5392 for TMSPM, lambda=632.8 nm), but the film from TMSPM precursor has higher propagation loss (1.024 dB/cm, lambda=632.8 nm) than the film prepared from GLYMO (0.569 dB/cm, lambda=632.8 nm). Furthermore, the film prepared from TMSPM is easy to be opaque and cracks during coating whereas the same phenomenon was not found for the film prepared with GLYMO. It is confirmed that GLYMO is a better precursor than TMSPM for waveguide film preparation. (C) 2005 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

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Hybrid ZnO/ormosils Elms are prepared by the sol-gel method. A FT-IR spectrometer, 900 UV/VIS/NIR spectrophotometer, atomic force microscope, and ellipsometer are employed to investigate microstructure and optical properties of the films fired at different temperatures. The results show that the films with high transmittance and low surface roughness could be obtained at the heat-treatment temperature of 150 degrees C, the refractive index and thickness of the film are 1.413, 2.11 mu m, respectively. Higher temperatures (350 degrees C, 550 degrees C) change the Elm microstructure severely, and then decrease the transmittance of the films.

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In this work, alpha-Al2O3:C, a highly sensitive thermoluminescence dosimetry crystal, was grown by the EFG method in which a graphite heating unit and shield acted as the carbon source during the growth process. The optical, luminescent properties and dosimetric characteristics of the crystal were investigated. The as-grown crystal shows a single glow peak at 536 K, which is associated with Cr3+ ions. After annealing in H-2 at 1673 K for 80 h, the crystal shows a single glow peak at 460 K and a blue emission band at 415 nm. The thermoluminescent response of the annealed crystal shows linear-sublinear-saturation characteristics in the dose range from 5 x 10(-6) to 100 Gy.

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Silicon sheets from powder (SSP) ribbons have been prepared by modified SSP technique using electronic-grade (9N purity) silicon powder. The surface morphology, crystallographic quality, composition and electric properties of the SSP ribbons were investigated by surface profiler, X-ray diffraction (XRD), scanning electron microscopy (SEM), metallurgical microscope, Auger electron spectroscopy (AES) and four-point probe apparatus, respectively. The results show that the SSP ribbon made from electronic-grade silicon powder is a suitable candidate for the substrates of crystalline silicon thin film (CSiTF) solar cells, which could meet the primary requirements of CSiTF solar cell process on the substrates, including surface smoothness, crystallographic quality, purity and electric conductivity, etc. (C) 2004 Elsevier B.V. All rights reserved.

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Self-ordered porous alumina films on a semi-insulated GaAs substrate were prepared in oxalic acid aqueous solutions by three-step anodization. The I-t curve of anodization process was recorded to observe time effects of anodization. Atomic force microscopy was used to investigate structure and morphology of alumina films. It was revealed that the case of oxalic acid resulted in a self-ordered porous structure, with the pore diameters of 60-70 nm, the pore density of the order of about 10(10) pore cm(-2), and interpore distances of 95-100nm. At the same time the pore size and shape change with the pore widening time. Field-enhanced dissolution model and theory of deformation relaxation combined were brought forward to be the cause of self-ordered pore structure according to I-t curve of anodization and structure characteristics of porous alumina films. (c) 2006 Elsevier Ltd. All rights reserved.

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Self-ordered porous alumina films on a semi-insulated GaAs substrate were prepared in oxalic acid aqueous solutions by three-step anodization. The I-t curve of anodization process was recorded to observe time effects of anodization. Atomic force microscopy was used to investigate structure and morphology of alumina films. It was revealed that the case of oxalic acid resulted in a self-ordered porous structure, with the pore diameters of 60-70 nm, the pore density of the order of about 10(10) pore cm(-2), and interpore distances of 95-100nm. At the same time the pore size and shape change with the pore widening time. Field-enhanced dissolution model and theory of deformation relaxation combined were brought forward to be the cause of self-ordered pore structure according to I-t curve of anodization and structure characteristics of porous alumina films. (c) 2006 Elsevier Ltd. All rights reserved.

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A novel inorganic-organic hybrid hydrophobic anti-reflection silica film used for laser crystal was obtained by sol-gel process. The film consisted of silica sols mixed with a small amount of polymethyl methacrylate (PMMA) or polystyrene (PS). The optical transparency, hydrophobic property and surface morphology of the film were characterized by UV-VIS-NIR spectrophotometer; contact angle instrument and Scanning Electron Microscopy (SEM), respectively. The results showed that the anti-reflection coating had good hydrophobility and optical transparency from 400 nm to 1200 nm. The contact angle reached to 130-140 degrees. SEM images indicated the hydrophobic films modified with PMMA or PS had compact structure compared to the pure silica sol film. (C) 2008 Elsevier B.V. All rights reserved.

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Erbium-doped silica glasses were made by sol-gel process. Intensive photoluminescence (PL) spectra from the Er-doped silica glasses at room temperature were measured. A broadband peak at 1535 ma, corresponding to the I-4(13/2)-I-4(15/2) transition, its full width at half-maximum (FWHM) of 10 nm, and a shoulder at 1546 nm in the PL spectra were observed. At lower temperatures, main line of 1535 nm and another line of 1552 Mn instead of 1546 nm appear. So two types of luminescence centers must exist in the samples at different temperature. The intensity of main line does not decrease obviously with increasing temperature. By varying the Er ion concentration in the range of 0.2 wt% - 5wt%, the highest photoluminescence intensity was obtained at 0.2wt% erbium doped concentration. Luminescence intensity decreases with increasing erbium concentration. Cooperative upconversion was used to explain the concentration quenching of luminescence from silica glass with high erbium concentration. Extended X-ray absorption fine structure measurements were carried out. It was found that the majority of the erbium impurities in the glasses have a local structure of eight first neighbor oxygen atoms at a mean distance of 0.255 nm, which is consistent with the typical coordination structure of rare earth ion.

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The preparation of light alkenes by the gas phase oxidative cracking (GOC) or catalytic oxidative cracking (COC) of model high hydrocarbons ( hexane, cyclohexane, isooctane and decane in the GOC process and hexane in the COC process) was investigated in this paper. The selection for the feed in the GOC process was flexible. Excellent conversion of hydrocarbons ( over 85%) and high yield of light alkenes ( about 50%) were obtained in the GOC of various hydrocarbons including cyclohexane at 750 degreesC. In the GOC process, the utilization ratio of the carbon resources was high; CO dominated the produced COX (the selectivity to CO2 was always below 1%); and the total selectivity to light alkenes and CO was near or over 70%. In the COC of hexane over three typical catalysts (HZSM-5, 10% La2O3/HZSM-5 and 0.25% Li/MgO), the selectivity to COX was hard to decrease and the conversion of hexane and yield of light alkenes could not compete with those in the GOC process. With the addition of H-2 in the feed, the selectivity to COX was reduced below 5% over 0.1% Pt/HZSM-5 or 0.1% Pt/MgAl2O4 catalyst. The latter catalyst was superior to the former catalyst due to its perfect performance at high temperature, and with the latter, excellent selectivity to light alkenes ( 70%) and the conversion of hexane (92%) were achieved at 850 degreesC ( a yield of light alkenes of 64%, correspondingly).

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A sol-gel coating method for the preparation of extractive phase on bars used in sorptive microextraction is described. The extraction phase of poly(dimethylsiloxane) is partially crosslinked with the sol-gel network, and the most part is physically incorporated in the network. Three aging steps at different temperatures are applied to complete the crosslinking process. Thirty-micrometer-thick coating layer is obtained by one coating process. The improved coating shows good thermal stability up to 300degreesC. Spiked aqueous samples containing n-alkanes, polycyclic aromatic hydrocarbons and organophosphorus pesticides were analyzed by using the sorptive bars and GC. The results demonstrate that it is suitable for both aploar and polar analytes. The detection limit for chrysene is 7.44 ng/L, 0.74 ng/L for C-19 and 0.9 ng/L for phorate. The extraction equilibration can be reached in less than 15 min by supersonic extraction with the bars of 30 mum coating layer. (C) 2004 Elsevier B.V. All rights reserved.

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With the objective of making calcium alginate gel beads with small and uniform size, membrane emulsification coupled with internal gelation was proposed. Spherical gel beads with mean size of about 50 mum, and even smaller ones in water, and with narrow size distribution were successfully obtained. Experimental studies focusing mainly on the effect of process parameters on bead properties were performed. The size of the beads was mainly dependent on the diameter of the membrane pores. High transmembrane pressure made for large gel beads with wide size distribution. Low sodium alginate concentration produced nonspherical beads, whereas a high concentration was unsuitable for the production of small beads with narrow distribution. Thus 1.5% w/v was enough. A high surfactant concentration favored the formation of small beads, but the adverse effect on mass transfer should be considered in this novel process. (C) 2002 Wiley Periodicals, Inc.