制备高比表面多孔Ti-Si复合氧化物材料的新方法

A new method named peptizinggelation method was used to synthesize TiSi dioxide composite, whose surface area is above 1 000 m2/g. The character of this method is that Ti exists in the form of ion and ion cluster during the hydrolysis of Si(OC 2H 5) 4 . This is the progress on the cohydrolysis of Si(OC 2H 5) 4 and Ti(OC 4H 9) 4. During the calcination of gelation, Ti—O—Si was formed with Ti element in the situation of SiO 2 crystal cell. This is confirmed by FTIR analysis. TiSi dioxide composite with Ti molar fraction of 13.1% is mainly in the form of amorphous based on XRD analysis, which reveals that TiSi dioxide composite is uniform in structure. Furthermore, extra Ti element presents on the surface layer of TiSi dioxide composite examined by Raman and EES analysis. Owning to these two characters, TiSi dioxide composite prepared by peptizinggelation method becomes a good catalyst in the field of catalysis.

Hydrophilic and photocatalytic activities of Nd-doped titanium dioxide thin films

The Nd-doped TiO2 thin films with higher hydrophilic and photocatalytic activities were prepared on glass slides by an acid-catalyzed sol？gel method. The effects of Nd doping on crystalline phase, surface composition and optical property were investigated by means of techniques such as X-ray diffraction （XRD）, scanning electron microscopy （SEM）, transmission electron microscopy （TEM）, Fourier transform infrared spectroscopy （FT-IR）, optical contact angle tester and UV-Vis spectroscopy. The results show that Nd doping obviously influences the hydrophilic and photocatalytic activities of TiO2thin films. Nd doping could cause the TiO2 lattice distortion, inhibit phase transition from anatase to rutile, cause red shift of the absorption spectrum edge, produce hydroxyl radicals （·OH）, and accelerate surface hydroxylation, which result in a significant improvement in the hydrophilicity and photoreactivity of Nd-doped TiO2 thin films. When the content of Nd is 0.1% （mass fraction）, TiO2 thin films achieve the smallest grain size （about 15 nm）, and the hydrophilic and photocatalytic activities of TiO2 thin film reach the maximum, the contact angle is only 8.1°, and 92% of methylene blue is finally degraded. Moreover, the modification mechanism of Nd doping was also discussed.

Surface modification of NiTi alloy by sol-gel derived porous TiO_(2)film

Titania films with nano-sized pores were prepared on the NaOH？HCl pretreated NiTi alloy substrate by sol？gel method.A crack-free film is obtained for the sample with a dense inner layer and a porous outside layer（sample TC1＋1）.The X-ray diffraction shows that the titania films are composed of anatase,and a little Ni4Ti3 phase in the heat treated substrate is also detected.The X-ray photoelectron spectroscopy results indicate that the titania film completely covered the NiTi substrate for sample TC1＋1.The sample TC1＋1 is hydrophilic with a contact angle about 20°,and UV illumination treatment for 15 min further decreases the contact angle to（9.2±3.2）°.The potentiodynamic polarization test in 0.9% NaCl solution reveals a better corrosion resistance of sample TC1＋1 than the polished NiTi sample.

Preparation of long alumina fibers by sol-gel method using malic acid

The precursor sol of alumina was prepared by sol-gel method with aluminum nitrate and malic acid as raw materials.The effects of content of malic acid and polyvinylpyrrolidone （PVP） on sol spinnability were explored.The gel fibers with above 80 cm in length were obtained by mixing aluminum nitrate,malic acid and PVP on mass ratio of 10 3 1.5.Thermogravimetry-differential scanning calorimetry （TG-DSC）,Fourier transform infrared （FTIR） spectrum,X-ray diffractometry （XRD）,and scanning electron microscopy （SEM） were used to characterize the properties of the gel and ceramic fibers.The alumina fibers with a smooth surface and about 20μm in diameter were obtained by sintering at 1 200℃,and their main phase was indentified to be α-Al2O3.

Synthesis of LiMnPO_4/C composite material for lithium ion batteries by sol-gel method

The LiMnPO4/C composite material was synthesized via a sol-gel method based on the citric acid. The X-ray diffraction （XRD）, scanning electron microscopy （SEM） and electrochemical performance tests were adopted to characterize the properties of LiMnPO4/C. The XRD studies show that the pure olivine phase LiMnPO4 can be obtained at a low temperature of 500 °C. The SEM analyses illustrate that the citric acid used as the chelating reagent and carbon source can restrain the particle size of LiMnPO4/C well. The LiMnPO4/C sample synthesized at 500 °C for 10 h performs the highest initial discharge capacity of 122.6 mA-h/g, retaining 112.4 mA-h/g over 30 cycles at 0.05C rate. The citric acid based sol-gel method is favor to obtain the high electrochemical performance of LiMnPO4/C.

A Novel Approach to Synthesizing Porous ZnO Films: Inorganic Chelating Sol-Gel Method

Porous ZnO films are synthesized by inorganic chelating sol-gel method,which is a novel sol-gel technique using zinc nitrate as starting materials and citric acid as the chelating reagent.The crystal structure,surface morphology,porous and optical properties of the deposited films are investigated.X-ray diffraction pattern analysis shows that crystal structure of the ZnO films is hexagonal wurtzite.Scanning electron microscopy (SEM) shows that the ZnO film is porous.The curve of pore size distribution has two peak values at about 2.02nm and 4.97nm and BET surface area of the ZnO film is 27.57m2/g.In addition,the transmittance spectrum gives a high transmittance of 85% in the visible region and optical bandgap of the ZnO film (fired at 500℃) is 3.25eV.

Effect of Cu-Excess on the Electrical Properties of Cu_xAlO_2(1≤x≤1.06)

Cu-excess CuxAlO2 ceramics with delafossite phases were synthesized using sol-gel. In the composition range of 1≤x〈1. 04,there are no detectable non-delafossite phases. Weak diffraction peaks of CuO are observed when x ≥1.04. The room temperature conductivity of the CU1.04AlO2 sample is improved by nearly an order of magnitude over that of the CuAlO2 sample. The major defect mechanism responsible for the conductivity enhancement is proposed to be substitution defects of CuAl （Cu^2 ＋ ions substitute Al^3 ＋ ions）. The composition formula unit for Cu-excess Cux AlO2 may be expressed as Cu（All yCuy）O2.

Influence of lanthanum-doping on photocatalytic properties of BiFeO_3 for phenol degradation

A series of BiFeO3 and lanthanum‐doped BiFeO3 photocatalysts were synthesized by a facile sol‐gel method using citric acid as complexing agent, and used to remove phenol in industrial wastewater under simulated sunlight irradiation. The samples were characterized by X‐ray diffraction, energy dispersive spectroscopy, X‐ray photoelectron spectroscopy, UV‐Vis diffuse reflectance spectroscopy and photoluminescence spectroscopy. The introduction of La effectively suppressed the generation of an impurity phase. All the metals （La, Bi and Fe） are well distributed. Under simulated sunlight irradiation, the La‐doped BiFeO3 photocatalysts exhibited superior photocatalytic activity to pure BiFeO3. The 15%La‐doped BiFeO3 photocatalyst exhibited the best activity, with a degradation rate of 96%and COD removal rate of 81.53%after irradiation for 180 min, and it showed good recycling stability. The enhanced photocatalytic ability of 15% La‐doped BiFeO3 was attributed to the in‐crease of adsorbed surface hydroxyl groups, enhancement of visible light absorption and reduction of electron‐hole recombination. We confirmed that the primary active species was -OH by adding different scavengers during the photodegradation of phenol and proposed a reaction mechanism based on these experiments.

Effect of Er substituting sites on upconversion luminescence of Er^(3+)-doped BaTiO_3 films

Erbium-doped BaTiO3 films on LaNiO3/Si substrates were fabricated by sol-gel method. The crystalline structure, morphologies and upconversion （UC） luminescence properties of films were respectively investigated by X-ray diffraction （XRD）, atomic force microcopy （AFM） and photoluminescence （PL）. The results indicate that both of the microstructure and luminescence are found to be dependent on Er^3＋ substituting sites. The samples with A-site substitution have smaller lattice constants, larger grains and smoother surface than those with B-site substitution. The photoluminescence spectra show that both of the samples have two stronger green emission bands centered at 528 and 548 nm and a weak red emission band centered at 673 nm, which correspond to the relaxation of Er^3＋ from ^2H11/2, ^4S3/2, and ^4F9/2 levels to the ground level ^4I15/2, respectively. Compared with B-site doped films, A-site doped films have a stronger integrated intensity of green emissions and a weaker relative intensity of red emissions. The differences could be explained by the crystalline quality and cross relaxation （CR） process.

Synthesis and electrochemical performance of Li_(3-2x)Mg_xV_2(PO_4)_3/C composite cathode materials for lithium-ion batteries

The Li3 2xMgxV2（PO4）3/C （x-=0, 0.01, 0.03 and 0.05） composites were prepared by a sol-gel method and characterized by X-ray diffraction （XRD）, scanning electron microscopy （SEM） and electrochemical measurements. The XRD results reveal that a small amount of Mg2＋ doping into Li sites does not significantly change the monoclinic structure of Li3V2（PO4）3, but Mg-doped Li3W2（PO4）3 has larger cell volume than the pristine Li3V2（PO4）3. All Mg-doped composites display better electrochemical performance than the pristine one, and Liz.94Mgo.03Vz（P04）3/C composite exhibits the highest capacity and the best cycle performance among all above-mentioned composites. The analysis of Li＋ diffusion coefficients in Li3V2（PO4）3/C and Li2.94Mgo.03V2（P04）3/C indicates that rapid Li＋ diffusion results from the doping of Mg2＋ and the rapid Li＋ diffusion is responsible for the better electrochemical performance of Mg-doped Li3V2（PO4）3/C composite cathode materials.

Effects of Ni doping contents on photocatalytic activity of B-BiVO_4 synthesized through sol-gel and impregnation two-step method

To enhance the photocatalytic activity of B-BiVO4,Ni-doped B?BiVO4photocatalyst(Ni-B-BiVO4)was synthesized through sol-gel and impregnation method.The photocatalysts were characterized by XPS,XRD,SEM,EDS,BET and UV-Vis DRS techniques.The results showed that single or double doping did not change the crystalline structure and morphology,but the particle size decreased with Ni doping.The band gap energy absorption edge of Ni-B-BiVO4shifted to a longer wavelength compared with undoped,B or Ni single doped BiVO4.More V4+and surface hydroxyl oxygen were observed in BiVO4after Ni-B co-doping.When the optimal mass fraction of Ni is0.30%,the degradation rate of MO in50min is95%for0.3Ni-B-BiVO4sample which also can effectively degrade methyl blue(MB),acid orange(AOII)II and rhodamine B(RhB).The enhanced photocatalytic activity is attributed to the synergistic effects of B and Ni doping.

Direct Synthesis of Diphenyl Carbonate with Heterogeneous Catalyst and Optimal Synthesis Conditions of the Support Prepared by Sol-gel Method

The support of catalyst for the direct synthesis of diphenyl carbonate （DPC） by heterogeneous catalytic reaction was prepared by the sol-gel method. Compared with activated charcoal, molecular sieve, porous ceramics, hopcalite, the support prepared by the sol-gel method has higher activity. The characterization of the support by X-ray diffraction （XRD） and transmission electron microscope （TEM） show that the mare crystal phase is Co2MnO4 and the average particle diameter is about 40 nm. The optimum conditions for synthesis of the support were determined by orthogonal experiments, which indicate that the proportion of Cu, Mn, and Co is the first important factor influencing the yield and selectivity of DPC. Temperature of calcination is the second one. The optimum conditions are： molar proportion of Cu, Mn, and Co being 1 ： 1 ： 1, temperature of calcination 700℃, drying at 100~C, temperature of water bath 85~C. The yield and selectivity of DPC in the process can reach 38% and 99% in the batch operation, respectively. The copper cobalt manganese mixed oxides chosen as the support contribute more to the high catalytic activity than the sol-gel method.

Sintering and microstructure of silicon carbide ceramic with Y_3Al_5O_(12) added by sol-gel method

Silicon carbide (SiC) ceramic with YAG (Y3Al5O12) additive added by sol-gel method was liquid-phase sintered at different sintering temperatures, and the sintering mechanism and microstructural characteristics of resulting silicon carbide ceramics were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM) and elemental distribution of surface (EDS). YAG (yttrium aluminum garnet) phase formed before the sintering and its uniform distribution in the SiC/YAG composite powder decreased the sintering temperature and improved the densification of SiC ceramic. The suitable sintering temperature was 1860 °C with the specimen sintered at this temperature having superior sintering and mechanical properties, smaller crystal size and fewer microstructure defects. Three characteristics of improved toughness of SiC ceramic with YAG added by sol-gel method were microstructural densification, main-crack deflection and crystal ‘bridging’.

Characterization and photoelectrochemical performance of Zn-doped TiO_2 films by sol-gel method

Zn-doped TiO2 (Zn?TiO2) thin films were prepared by the sol?gel method on titanium substrates with heat treatment at different temperatures. The effects of heat treatment temperatures and Zn doping on the structure, photocathodic protection and photoelectrochemical properties of TiO2 thin films were investigated. It is indicated that the photoelectrical performance of the Zn?TiO2 films is enhanced with the addition of Zn element compared with the pure-TiO2 film and the largest decline by 897 mV in the electrode potential is achieved under 300 °C heat treatment. SEM?EDS analyses show that Zn element is unevenly distributed in Zn?TiO2 films; XRD patterns reveal that the grain size of Zn?TiO2 is smaller than that of pure-TiO2; FTIR results indicate that Zn - O bond forms on Zn?TiO2 surface. Ultraviolet visible absorption spectra prove that Zn?TiO2 shifts to visible light region.Mott?Shottky curves show that the flat-band potential of Zn?TiO2 is more negative and charge carrier density is bigger than that ofpure-TiO2, implying that under the synergy of the width of the space-charge layer, carrier density and flat-band potential, Zn?TiO2 with 300 °C heat treatment displays the best photocathodic protection performance.

A new solid acid SO_4^(2-)/TiO_2 catalyst modified with tin to synthesize 1,6-hexanediol diacrylate

A new solid acid catalyst,SO4^2-/TiO2 modified with tin,was prepared using a sol-gel method and its physicochemical properties were revealed by nitrogen adsorption-desorption,X-ray powder diffraction,scanning electron microscopy,Fourier transform infrared spectroscopy,infrared spectroscopy of adsorbed pyridine,temperature-programmed desorption of ammonia and thermal gravimetric analysis.The structure,acidity and thermal stability of the SO4^2-/TiO2-SnO2 catalyst were studied.Incorporating tin enlarged the specific surface area and decreased crystallite size of the SO4^2-/TiO2 catalyst.The total acid sites of the modified catalyst increased and Bronsted acid strength remarkably increased with increasing tin content.The decomposition temperature of sulfate radical in the modified catalyst was 100 ℃ greater and its mass loss was more than twice that of the SO4^2-/TiO2 catalyst.The SO4^2-/TiO2-SnO2 catalyst was designed to synthesize 1,6-hexanediol diacrylate by esterification of 1,6-hexanediol with crylic acid.The yield of 1,6-hexanediol diacrylate exceeded 87% under the optimal reaction conditions：crylic acid to 1,6-hexanediol molar ratio = 3.5,catalyst loading = 7%,reaction temperature = 130 ℃ and reaction time = 3 h.The modified catalyst exhibited excellent reusability and after 10 cycles the conversion of 1,6-hexanediol was above 81%.

Preparation of dual-shell Si/TiO_(2)/CFs composite and its lithium storage performance

A dual-shell Si/TiO2/CFs composite was synthesized through a simple method to deal with the intrinsic drawbacks of silicon-based anode,in terms of huge volume change,unstable SEI films,and low electronic and ionic conductivity.The inner rigid TiO2 shell alleviates the huge volume expansion of the nano silicon,and the outer resilient carbon fiber,which is porous and staggered,is beneficial to the rapid transport of electrons and ions.The as-prepared Si/TiO2/CFs composite displays a superior reversible specific capacity of 583.4 mA·h/g,high rate capability and decent cycling performance.The dual-shell encapsulation method provides a guideline for other anode materials with huge volume expansion during the cycling process.

Facile synthesis of high capacity P2-type Na_(2/3)Fe_(1/2)Mn_(1/2)O_(2) cathode material for sodium-ion batteries

P2-type Na_(2/3)Fe_(1/2)Mn_(1/2)O_(2) was synthesized by a facile sol−gel method,and the effect of calcination temperature on the structure,morphology and electrochemical performance of samples was investigated.The results show that the sample obtained at 900℃ is pure P2-type Na_(2/3)Fe_(1/2)Mn_(1/2)O_(2) phase with good crystallization,which consists of hexagon plate-shaped particles with the size and thickness of 2−4μm and 200−400 nm,respectively.The sample exhibits an initial specific discharge capacity of 243 mA·h/g at a current density of 26 mA/g with good cycling stability.The high specific capacity indicates that P2-type Na_(2/3)Fe_(1/2)Mn_(1/2)O_(2) is a promising cathode material for sodiumion batteries.

Sol-gel synthesis and photoluminescence of LaPO_4:Eu^(3+) nanorods

Monoclinic LaPO4 nanostructures with uniform rod shape have been successfully synthesized by a simple sol-gel method.The procedure involves formation of homogeneous,transparent,metal-citrate-EDTA gel precursors,followed by calcination to promote thermal decomposition of the gel precursors to yield the LaPO4 nanoparticles.Their morphologies and structures were characterized by XRD,TEM,TG-DSC and HRTEM.The results indicate that single monoclinic phase LaPO4 nanorods are readily obtained at 800 ℃ within 3 h.Furthermore,photoluminescence(PL) characterization of the Eu3+-doped LaPO4 nanocrystals was carried out.The effects of calcination temperatures and Eu3+ doping content on the PL properties were elaborated in detail.Room-temperature photoluminescence(PL) characterization reveals that the optical brightness as well as the intensity ratio of 5D0-7F1 to 5D0-7F2 is highly dependent on the calcination temperature,and the Eu0.05La0.95PO4 nanophosphor shows the relatively promising PL performance with the most intense emission.

Hydrous Ruthenium Oxide with High Rate Pseudo-Capacitance Prepared by a New Sol-Gel Process

A kind of ruthenium oxide with smaller particles and higher porosity was prepared by a sol-gel process with RuCl3·xH2O and NaHCO3 solution. Several details concerning this new material, including crystal structure, particle size as functions of the temperature, and electrochemical properties were also reported. The optimal annealing temperature was 210 ℃ and the powder annealed at this temperature had a rate capacitance of 541 F/g. In addition, the rate capacitance of the composite electrode reached 802 F/g after 10% carbon black was added, much higher than any previously reported value. High energy density supercapacitors were built with the newly discovered electrode material. Energy densities as high as 67 J/g were obtained based on the RuO2·xH2O alone. By introducing the highly porous carbon black into the electrode, energy densities great than 100 J/g could be achieved. The power density of the capacitor was enhanced significantly.

Preparation of Organic/Inorganic Hybrid Polymer Emulsions with High Silicon Content and Sol-gel-derived Thin Films

A novel polymer/SiO2 hybrid emulsion(PAES)was prepared by directly mixing colloidal silica with polyacrylate emulsion(PAE)modified by a saline coupling agent.The sol-gel-derived thin films were obtained by addition of co-solvents into the PAES.The effects ofγ-methacryloxypropyltrimethoxysilane(KH-570)content and co-solvent on the properties of PAES films were investigated.Dynamic laser scattering(DLS)data indicate that the average diameter of PAES(96 nm)is slightly larger than that of PAE(89 nm).Transmission electron microscopy (TEM)photo discloses that colloidal silica particles are dispersed uniformly around polyacrylate particles and some of the colloidal silica particles are adsorbed on the surface of PAE particles.The crosslinking degree data and Fourier transform infrared(FT-IR)spectra confirm that the chemical structure of the PAES is changed to form Si-O-Si-polymer crosslinking networks during the film formation.Atomic force microscope(AFM)photos show the solvent induced sol-gel process of colloidal silica and the Si-based polymer distribution on the film surface of the dried PAES.Thermogravimetric analysis(TGA)curves demonstrate that the PAES films display much better thermal stability than PAE.