SYNTHESIS OF MESOPOROUS POLY(STYRENE-co-MALEIC ANHYDRIDE)/SILICA HYBRID MATERIALS VIA A NONSURFACTANT-TEMPLATED SOL-GEL PROCESS

Mesoporous poly(styrene-co-maleic anhydride)/silica hybrid materials have been prepared. The synthesis was achieved by the HCl-catalyzed sol-gel reactions of tetraethyl orthosilicate (TEOS) and styrene-maleic anhydride copolymer in the presence of 3-aminopropyl triethoxysilane (APTES) as a coupling agent and citric acid as a nonsurfactant template or pore-forming agent, followed by ethanol extraction. Characterization results from nitrogen sorption isotherms and powder X-ray diffraction indicate that polymer-modified mesoporous materials with large specific surface areas (e.g. 900 m(2)/g) and pore volumes (e.g. 0.6 cm(3)/g) could be prepared. As the citric acid concentration is increased, the specific surface areas, pore volumes and pore diameters of the hybrid materials increase.

Preparation of layered oxide Li(Co_(1/3)Ni_(1/3)Mn_(1/3))O_2 via the sol-gel process

获得同质的分层的氧化物李(Co1/3Ni1/3Mn1/3 ) 是的 O2 锂插入积极电极材料，把柠檬性的酸用作一个 chelating 代理人的大音阶的第五音胶化过程被使用。材料李(Co1/3Ni1/3Mn1/3 ) O2 在不同锻烧温度被综合。XRD 实验显示分层的李(Co1/3Ni1/3Mn1/3 ) O2 材料能在 800 的更低的温度被综合 ? 琠? 楢整漠吗？

Synthesis and Characterization of Cerium-Doped Lutetium Aluminum Garnet Phosphors by Nitrate-citrate Sol-Gel Combustion Process

Nanosized cerium-doped lutetium aluminum garnet （LuAG：Ce） phosphors were prepared by nitrate-citrate solgel combustion process using 1：1 ratio of the citrate：nitrate. The prepared LuAG：Ce phosphors were characterized by XRD, TEM, photoluminescence and radioluminescence spectra excited by UV and X-ray, respectively. The purified crystalline phase of LuAG：Ce was obtained at 900 ℃ by directly crystallizing from amorphous materials. The resultant Lu- AG：Ce phosphors were uniform and had good dispersivity with an average particle size of about 30 urn. Both photoluminescence and radioluminescence were well-known Ce^3＋ emissions located in the range of 470 -600 nm consisting of two emission bands because of the transition from the lowest 5d excited state （2D） to the 4f ground state of Ce^3＋, which matched well with the sensitivity curve of the Si-photodiode. There was a little red shift for the emission components from the UV-excited emission spectrum to the X-ray-excited emission spectrum. The fast scintillation decay component of 26 ns satisfies the requirements of fast scintillators.

Methane reforming with CO_2 to syngas over CeO_2-promoted Ni/Al_2O_3-ZrO_2 catalysts prepared via a direct sol-gel process

CeO2-promoted Ni/Al2O3-ZrO2 （Ni/Al2O3-ZrO2-CeO2） catalysts were prepared by a direct sol-gel process with citric acid as gelling agent. The catalysts used for the methane reforming with CO2 was studied by infrared spectroscopy （IR）, thermal gravimetric analysis （TGA）, microscopic analysis, X-ray diffraction （XRD） and temperature-programmed reduction （TPR）. The catalytic performance for CO2 reforming of methane to synthesis gas was investigated in a continuous-flow micro-reactor under atmospheric pressure. TGA, IR, XRD and microscopic analysis show that the catalysts prepared by the direct sol-gel process consist of Ni particles with a nanostructure of around 5 nm and an amorphous-phase composite oxide support. There exists a chemical interaction between metallic Ni particles and supports, which makes metallic Ni well dispersed, highly active and stable. The addition of CeO2 effectively improves the dispersion and the stability of Ni particles of the prepared catalysts, and enhances the adsorption of CO2 on the surface of catalysts. The catalytic tests for methane reforming with CO2 to synthesis gas show that the Ni/Al2O3-ZrO2-CeO2 catalysts show excellent activity and stability compared with the Ni/Al2O3 catalyst. The excellent catalytic activity and stability of the Ni/Al2O3-ZrO2-CeO2 are attributed to the highly, uniformly and stably dispersed small metallic Ni particles, the high reducibility of the Ni oxides and the interaction between metallic Ni particles and the composite oxide supports.

Mechanism of Phase Transformation and Formation of Barium Hexafer rite Doped with Rare-Earths in Sol-Gel Process

The phase-transformation in sol-gel preparation of barium hexaferrite and the formation of barium hexaferrite doped with La 3+ were studied by chemical p hase analysis, X-ray diffraction and infrared spectrometry analysis. The expe rimental results show that phase transformation reactions of FeCO 3, Fe 2O 3 and BaFe 2O 4, barium hexaferrite and γ-Fe 2O 3 take place in the heat tr eatment of gel. While the doping lanthanide ion replace barium ion, an equivalen t quantity of Fe 3+ are reduced to Fe 2+ to maintain the charge equili brium.

Preparation and characterization of BaMgAl_(10)O_(17)∶Eu phosphor coated with MgF_2 by sol-gel process

In order to prevent BaMgAl10O17∶Eu （BAM） phosphor from thermal degradation, MgF2-coatings on the surface of BAM were prepared by a sol-gel process. The coatings were characterized by X-ray photoelectron spectroscopy and scanning electron microscopy. The results indicate that BAM is successfully coated with homogenous, close MgF2 coatings. The photoluminescence and anti-thermal degradation properties of coated BAM were investigated under 254 and 147 nm excitations. The optimum anti-thermal degradation properties are obtained at the mass ratio of MgF2 to BAM 0.2% under 254 nm excitation and 0.5% under 147 nm excitation, respectively. It is considered that trace MgO formed after baked would cause different optimum coating thicknesses under 254 and 147 nm excitations.

Microstructure and electrical properties of La_2 O_3-doped ZnO-based varistor thin films by sol-gel process

Microstructure and electrical properties of La2 O3-doped ZnO-Bi2 O3 thin films prepared by sol–gel process have been investigated.X-ray diffraction shows that most diffraction peaks of ZnO are equal,and the crystals of ZnO grow well.Scanning electron microscopy and atomic force microscopy results indicate that the samples have a good structure and lower surface roughness.The nonlinear V–I characteristics of the films show that La2 O3 develops the electrical properties largely and the best doped content is 0.3% lanthanum ion,with the leakage current of 0.25 mA,the threshold field of 150 V/mm and the nonlinear coefficient of 4.0 in detail.

SYNTHESIS AND OPTICAL PROPERTIES OF A NOVEL ORGANIC/INORGANIC HYBRID NONLINEAR OPTICAL POLYMER VIA SOL-GEL PROCESS

A new organic/inorganic hybrid nonlinear optical (NLO) material was developed by the sol-gel process of an alkoxysilane dye with tetraethoxysilane. A NLO moiety based on 4-nitro-4 ' -hydroxy azobenzene was covalently bonded to the triethoxysilane derivative, i.e, gamma -isocyanatopropyl triethoxysilane. The preparation process and properties of the sol-gel derived NLO polymer were studied and characterized by SEM, FTIR,H-1-NMR, UV-Vis, DSC and second harmonic generation (SHG) measurement. The results indicated that the chemical bonding of the chromophores to the inorganic SiO2 networks induces low dipole alignment relaxation and preferable orientational stability. The SHG measurements also showed that the bonded polymer film containing 75 wt% of the akoxysilane dye has a high electro-optic coefficient (r(33)) of 7.1 pm/V at 1.1 mum wavelength, and exhibit good SHG stability, the r(33) values can maintain about 92.7% of its initial value at room temperature for 90 days, and can maintain about 59.3% at 100 degreesC for 300 min.

PREPARATION AND SECOND-ORDER OPTICAL NONLINEARITY OF NOVEL PHENOXYSILICON NETWORKS BY SOL-GEL PROCESS

Four phenoxysilicon networks for nonlinear optical (NLO) applications were designed and prepared by an extended sol-gel process without additional H2O and catalyst. All poled polymer network films possess high second-order nonlinear optical coefficients (d(33)) Of 10(-7)similar to 10(-8) esu. The investigation of NLO temporal stability at room temperature and elevated temperature (120 degreesC) indicated that these films exhibit high d(33) stability because the orientation of the chromophores are locked in the phenoxysilicon organic/inorganic networks.

Growth of TiO_2 Nanorods by Sol-gel Template Process

In this work, TiO2 nanorods with uniform diameter of about 100 nm and a length of several micrometers were successfully prepared by the sol-gel template method. Also the influence of molar ratios of precursor on the morphology and structure of TiO2 nanorods has been investigated. The prepared samples were characterized by Fourier transform infrared spectroscopy （FTIR）, X-ray diffraction （XRD） and scanning electron microscopy （SEM）. The XRD results indicated that the TiO2 nanorods were crystallized in the anatase and rutile phases, after annealing to 400-700℃ up to 2 h.

Luminescent Properties of Y_2O_3∶Eu Nanocrystalls Synthesized by EDTA Complexing Sol-Gel Process

Y 2O 3: Eu nanocrystals were synthesized by EDTA complexing sol gel process at a relatively low temperature, in which ethylen diamine tetraacetic acid (EDTA) and polyethylene glycol (PEG) were used as the chelating agent and polymerization agent respectively. Formation process of Y 2O 3:Eu and structure characterization were carried out by TG DTA, XRD, SEM/EDX. The results show that pure cubic phase Y 2O 3: Eu nanocrystalsere is produced after the precursor calcinated at 600 ℃ for 2 h, and the crystallinity increases with increasing calcination temperature. The nanoparticles of the Y 2O 3: Eu are basically spherical in shape. The mean particle size increases from about 30 to 70 nm when the calcination temperature increases from 600 to 1000 ℃. The luminescent properties of phosphor were analyzed by measuring the excitation and emission spectra. The main emission peak of the sample is around 612 nm, resulting in a red emission. The emission intensity increases with the calcination temperature. Compared with microsized Y 2O 3: Eu phosphors prepared by a conventional method, nanosized Y 2O 3: Eu synthesized by the present work, gives and a clear red shift in the emission spectrum. Moreover, the quenching concentration of Eu is raised.

Preparation of LiTi_2(PO_4)_3 by the Sol-gel Method and Investigation of Its Formation Process

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Facile and Controlled Synthesis of Silica Sol Nanospheres Through a Modifi ed Sol-Gel Process

An effective and reproducible preparation of silica sol nanospheres via a modified sol-gel process has been described. Monodisperse and stable silica sol nanospheres with uniformsize were successfully obtained through the optimized synthesis in which the mixture of tetraethyl orthosilicate （TEOS） and ethanol was followed by the addition of water and ammonium hydroxide （NH3） separately, and the size of silica sol spheres was strictly controlled in the range of 25-119 nm with a narrow size distribution by fine adjustment of several reaction parameters. Results showed that in the presence of low concentration of TEOS, spheres size rose first and reached maximum when H2O concentration was up to 66 g/L. However, the diameter of silica sol spheres decreased above 66 g/L of H2O concentration. Furthermore, it was also found that the size and size distribution of silica sol nanospheres were affected by NH3 concentration. As NH3 concentration increased from 15 to 35 g/L, the diameter declined from 83 to 64 nm. Nevertheless, higher NH3 concentration would result in relatively broad size distribution, and gelation occurred when NH3 concentration reached 44 g/L. In addition, the effect of the different feed rates ofNH3 on the size growth of silica sol nanospheres was also discussed.

Agglomerate control in the complexing sol-gel process

Nanometer ZrO2 - 8% Y2O3 (mole fraction, % ) powders were prepared by the EDTA (ethylenediaminetetraacetic acid) sol-gel process. Effects of the addition of ethylene glycol on agglomerate control was investigated. The results showed that because of the replacement of hydrogen bonds with ethylene glycol in the polymerized gel, gel stabilization and homogeneity were improved and close approach of gel particles was prevented, which led to reduction of hard agglomerates to some extent. Calcined at 4OO t for 2 h and 700 C for 2 h, the powders had a specific surface area of 35 m2/g, average particle size of 28 nm, and median particle size (d50) of 0. 44um with very sharp distribution, mostly being soft agglomerates.

RHEOLOGICAL MODIFICATION OF EPOXY RESINS WITH NANO SILICA PREPARED BY THE SOL-GEL PROCESS

Nano silica-modified epoxy resins were synthesized by the sol-gel process, The materials have the morphological structure of nano particales dispersed in the epoxy matrix. The dispersed phase formed a physical network in the resin and thus influenced the rheological behavior greatly. However, the nano silica did not show a significant influence on the mechanical properties of the cured resins.

Synthesis and Microstructure of Doped Alumina Composite Membrane by Sol-Gel Process

The supported membranes of Al 2O 3 and its modification membranes were prepared.Al 2O 3,Al 2O 3 SiO 2 TiO 2 and Al 2O 3 SiO 2 TiO 2 ZrO 2 membranes were mamufatured by the slip casting process using mixing boehmite,silicate,titania and zirconia sols under proper conditions,then the composite membrane was prepared.The structure and characteristics of the membrane were determined by XRD,SEM and AFM measurement.The conditions of preparation of the membrane are discussed.The thickness of the layer is about 1-2μm,the diameter of an average pore is 200-300nm and has a narrow pore distribution without crack forming.By changing the ratios of Al∶Si∶Ti∶Zr(mol),variations of surface pore size of Al 2O 3 SiO 2 TiO 2 ZrO 2 membrane can be gained.

Synthesis of Anatase TiO_2 Nanoparticles by Improved Sol-Gel Process at Low Temperature

The nanocrystalline TiO_2 powder were prepared by improved sol-gel method at low temperature under ambient pressure. The prepared TiO_2 powder was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM). It is found that the yield of anatase TiO_2 significantly increases with the reduction of pH by increasing the nucleation rate of anatase. There is an optimum amount of water in sol for the formation of anatase by combining two effects on the concentration of Ti(OH)_4 in gels. Increasing in reaction temperature also benefit to the nucleation of anatase of TiO_2.

Preparation of Scratch-Resistant Nano-Porous Silica Films Derived by Sol-Gel Process and Their Anti-reflective Properties

Structural strengthening of the nano porous silica films has been reported. The films were prepared with a base/acid two-step catalyzed TEOS-based sol-gel processing and dip-coating, and then baked in the mixed gas of ammonia and water vapor. The silica films were characterized with TEM, AFM, FTIR, spectrophotometer, ellipsometer, and abrasion test, respectively. The experimental results have shown that the films have a nanostructure with a low refractive index and can form an excellent scratch-resistant broadband anti-reflectance. The two-step catalysis noticeably strengthens the films, and the mixed gas treatment further improves mechanical strength of the silica network. Finally the strengthening mechanism has been discussed.

Synthesis mechanism of Pr doped BaTi_4O_9 powder by sol-gel process

Pr Doped BaTi4O9 gel was prepared by sol-gel method using Ti(OC4H9)4, Ba(CH3COO)2, CH3COOH and CH3OCH2CH2OH as raw materials. Through analyzing dry gel thermal treated at different temperatures, the possible synthesis mechanism of Pr doped BaTi4O9 powder was discussed. At first, Ti(OC4H9)4 hydrolyzes and three dimensional networks form, in which Ba2+ and CH3COO- are mostly in the form of ions; organic solvent is gradually volatilized through calefaction at 700 ℃, then the offspring is turned into BaTi5O11. With the temperature increasing to 850 ℃, BaTi5O11 begins resolving partly and forming BaTi4O9, and at 1000℃ Ba4Ti13O22 forms partly, but BaTi4O9 is the main crystal phase. BaTi5O11 and Ba4Ti13O30 decomposes completely at 1200℃ and forms single-phase BaTi4O9. The infrared (IR) analysis also shows that the absorbing peak of Ti-O bond is not in the characteristic absorption range of Ti-O-Ti (700-900 cm-1), but slightly shifted to the higher end (908 cm-1). It is probably because that doping Pr enters into the crystal lattice and causes the abnormal absorption of Ti-O bond.