微波辅助sol-gel法合成Bi_(0.5)Na_(0.5)TiO_(3)粉体及其压电性能研究

采用微波辅助溶胶-凝胶(sol-gel)法制备Bi_(0.5)Na_(0.5)TiO_(3)(BNT)粉体,通过DSC/TG,XRD,SEM,FT-IR等表征方法,分析BNT的反应历程,煅烧温度对BNT成分、晶粒尺寸和压电性能的影响.结果表明,当微波煅烧温度为650℃时,可合成出高纯度BNT粉体(30~120 nm),其居里温度为394℃,d_(33)=7.5 pC/N,ε_(r)=535.58,tanδ=0.29.对比传统马弗炉煅烧sol-gel法,微波辅助sol-gel法有利于提高BNT的介电性能和居里温度,降低介质损耗.

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.

Synthesis and electrochemical properties of dual doped spinels LiNi_xAl_yMn_(2-x-y)O_4 via facile novel chelated sol–gel method as possible cathode material for lithium rechargeable batteries

LiMnOand LiNiAlyMnO（x= 0.50;y = 0.05-0.50） powders have been synthesized via facile solgel method using Behenic acid as active cheiating agent.The synthesized samples are subjected to physical characterizations such as thermo gravimetric analysis（TG/DTA）,X-ray diffraction（XRD）,Fourier transform infrared spectroscopy（FT-IR）,field-emission scanning electron microscopy（FESEM）,transmission electron microscopy（TEM） and electrochemical studies viz.,galvanostatic cycling properties,electrochemical impedance spectroscopy（EIS） and differential capacity curves（dQ/dE）.Finger print XRD patterns of LiMnOand LiNiAlMnOfortify the high degree of crystallinity with better phase purity.FESEM images of the undoped pristine spinel illustrate uniform spherical grains surface morphology with an average particle size of 0.5 μm while Ni doped particles depict the spherical grains growth（50nm） with ice-cube surface morphology.TEM images of the spinel LiMnOshows the uniform spherical morphology with particle size of（100 nm） while low level of Al-doping spinel（LiNio.5Alo.05Mn1.45O4） displaying cloudy particles with agglomerated particles of（50nm）.The LiMnOsamples calcined at 850℃ deliver the discharge capacity of 130 mAh/g in the first cycle corresponds to 94%coiumbic efficiency with capacity fade of 1.5 mAh/g/cycle over the investigated 10 cycles.Among all four dopant compositions investigated,LiNiAlMnOdelivers the maximum discharge capacity of 126 mAh/g during the first cycle and shows the stable cycling performance with low capacity fade of 1 mAh/g/cycle（capacity retention of 92%） over the investigated 10 cycles.Electrochemical impedance studies of spinel LiMnOand LiNiAlMnOdepict the high and low real polarization of 1562 and 1100 Ω.

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.

Tungsten nanoparticle-strengthened copper composite prepared by a sol–gel method and in-situ reaction

Tungsten nanoparticle-strengthened Cu composites were prepared from nanopowder synthesized by a sol–gel method and in-situ hydrogen reduction.The tungsten particles in the Cu matrix were well-dispersed with an average size of approximately 100–200 nm.The addition of nanosized W particles remarkably improves the mechanical properties,while the electrical conductivity did not substantially decrease.The Cu–W composite with 6 wt%W has the most comprehensive properties with an ultimate strength of 310 MPa,yield strength of 238 MPa,hardness of HV 108 and electrical conductivity of 90%IACS.The enhanced mechanical property and only a small loss of electrical conductivity demonstrate the potential of this new strategy to prepare W nanoparticle-strengthened Cu composites.

CHANGE OF CeVALENCE STATE DURING THE PREPARATION OF CeO_2 ULTRAFINE POWDER BY SOL－GEL METHOD

CeO2 ultrafine powder was prepared by sol-gel method.XRD showed that samples were amorphous when calcination temperature was below 230℃,and single phase CeO2 ultrafine powders could be obtained above 250℃.It was found that Ce(3+) and Ce(4+)coexisted in the dried gel,the content of Ce(3+)lowered gradually and that of Ce(4+)increased in samples when calcining temperature increased.Ce(3+)was converted to Ce(4+)completel at 250℃.

Encapsulation of Eu(TTA)_3 into MCM-41 Mesoporous Molecular Sieve by Sol Gel Method

The rare earth complex Eu(TTA) 3 was successfully encapsulated into MCM 41 mesoporous molecular sieve by the addition of the complex into the sol gel mixture for the synthesis of MCM 41 mesoporous material under microwave radiation. The as synthesized MCM 41 hosted Eu(TTA) 3 mesophase was confirmed to possess hexagonally ordered mesostructure and a uniform crystal size of about 30 nm with XRD and HRTEM techniques. Moreover, the IR spectrum, photoluminescence effect and fluorescence lifetime of the Eu(TTA) 3/MCM 41 hybrid were also studied. An increase in Stokes' shift and no change in luminescence lifetime were observed to the resultant mesophase in comparison with Eu(TTA) 3 in ethanol solution.

Nanostructured Yb:GGG polycrystalline powders via gel combustion method

Gadolinium gallium gamet （GGG） nanopowders doped with ytterbium ions （Yb：GGG） were synthesized with citric acid as a fuel via gel combustion method. The optimized conditions for preparing yb^3＋：Gd3Ga5O12 nanopowders were discussed. The heat behavior, structure and morphology of powders were analyzed with thermal analysis （TG-DTA）, X-ray diffraction （XRD）, infrared spectra OR） and transmission electron microscope （TEM）. TG-DTA analysis revealed that the weight loss of the precursor occured below 800 ℃ and its crystallization temperature was 830.6℃. XRD and IR analysis showed that the precursor converted directly into pure GGG at a relatively lower temperature （900 ℃） without any other intermediate phase. The lattice constant was 1.2377 calculated by extrapolation method. TEM results indicated that the spherical powders showed good dispersity and had a relatively narrow size distribution with average particle size of approximately 40-50 ran, which was favorable for good sinterability of Yb：GGG laser ceramic.

In_2O_3 Ultrafine Powder Synthesis by Sol0Gel Method

The precursor of ultrafine In 2O 3 powder was prepared by the hydrolysis, peptization and gelation of InCl 3·4H 2O used as raw material. After calcination, ultrafine In 2O 3 powder was obtained. The particles were characterized by the methods of thermo gravimetric and differential thermal analysis (TG DTA), X ray diffractometry (XRD) and transmission electron microscopy (TEM), respectively.

Characterization of YSZ Ceramic Nanopowders Synthesized at Different Temperatures via Polyacrylamide Gel Method

Tetragonal zirconia (T-ZrO2) ceramic nanopowders stabilized with 3 mol% Y2O3 were synthesized via polyacrylamide gel method, using ZrOCl2?8H2O and Y(NO3)3?6H2O as raw materials. The effect of temperature on phase composition and morphology of YSZ nanopowders and sintering behavior of YSZ ceramics was investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Vickers hardness tester. The aging-resistance of YSZ ceramics was measured by means of aging experiments. The results demonstrated that the phase composition of YSZ ceramic nanopowders had no obvious change and it was composed of T-ZrO2. Particle size of well-dispersed YSZ ceramic nanopowders increased from 17 to 35 nm with increasing calcining temperature from 600 to 800 ℃. There was noticeable negative correlation between calcining temperature and the relative density of YSZ ceramic at the same sintering temperature. The aging experiments showed that water vapor facilitated tetragonal to monoclinic phase transformation, and the sample that had smaller grain size exhibited better aging-resistance. It can be concluded that when the calcining temperature is 600 ℃ and sintering temperature is 1550 ℃, the relative density and hardness of YSZ ceramic arrive at the peak of 96.64% and 11.135 GPa respectively, and it has less microcracks and excellent aging-resistance.

Photocatalytic Activity of Nanosized ZnWO_4 Prepared by the Sol-gel Method

Nanosized ZnWO4 photocatalysts were successfully synthesized via the sol-gel process in a temperature range of 450-800℃. The grain size, crystal size, and crystallinity of ZnWO4 particles increased with the increase of calcina- tion temperature and prolonging calcination time. The photocatalytic activity was measured for the degradation of an aqueous Rhodamine-B（RhB） solution and gaseous formaldehyde（FAD）. With the increase of calcination temperature and time, the activities increased to a maximum and then decreased. ZnWO4 photocatalyst prepared at 550℃ for I0 h showed the highest activity, which is similar to the photocatalytic activity of P25TiO2 for the degradation of gase-ous FAD. High crystallinity, large surface area, and good dispersion are responsible for the high photocatalytic per- formance of the prepared ZnWO4.

Preparation and properties of nanocrystal SmBO_3 by nitrate-citrate sol-gel combustion method

Nanocrystal SmBO3 powders were synthesized by nitrate-citrate sol-gel combustion method. The phase evolution, morphologies and absorbency of the synthesized powders were characterized by X-ray diffraction （XRD）, Field emission scanning electronic microscope （FESEM）, Fourier transform infrared spectroscopy （FFIR） and UV-3101PC spectrophotometer （UVPC）, respectively. XRD and FESEM results showed that pure SmBO3 phase was obtained at 750 ℃, with an average original particle size of about 100 nm. FTIR showed that there were apparently concentrated absorbent peaks between 500 and 1400 cm^-1. Moreover, the reflectivity of the powders apparently decreased at the wavelength between 1.05 and 1.15 μm. Therefore, SmBO3 might be a kind of absorbent material for infrared laser.

Grain Size and Photocatalytic Activity of Nanometer TiO_2 Thin Films Prepared by the Sol-gel Method

Transparent anatase TiO2 nanometer thin films with photocatalytic activity were prepared via the sol-gel method on soda-lime glass. The thickness , crystalline phase, grain size, surface hydroxyl amount and so on were characterized by scanning electron microscopy (SEM) , X-ray diffraction (XRD), transmission electron microscopy ( TEM), X-ray photoelectron spectroscopy (XPS) and UV-visible spectrophotometer ( UV-VIS). The photocatalytic activity of TiO2 thin films was evaluated for the photocatalytic decolorization of aqueous methyl orange . The effects of film thickness on the crystalline phase, grain size, transmittance and photocatalytic activity of nanometer Ti02 thin films were discussed.

Luminescence properties of red-emitting Ca_2Al_2SiO_7:Eu^(3+) nanoparticles prepared by sol-gel method

A series of red-emitting Ca2_xA12SiOT：xEu^3＋ （x = 1 mol.%-10 tool.%） phosphors were synthesized by the sol-gel method. The effects of annealing temperature and doping concentration on the crystal structure and luminescence properties of Ca2A12SiO7：Eu^3＋ phosphors were investigated. X-ray diffraction （XRD） profiles showed that all peaks could be attributed to the tetragonal Ca2A12SiO7 phase when the sample was annealed at 1000℃. Scanning electron microscopy （SEM） micrographs indicate that the phosphors have an irregularly rounded mor- phology with particles of about 200 nm. Excitation spectra showed that the strong broad band at around 258 nm and weak sharp lines in 350-490 nm were attributed to the charge transfer band of Eu^3＋-O^2- and f-f transitions within the 4f^6 configuration of Eu^3＋ ions, respectively. Emission spectra implied that the red luminescence could be attributed to the transitions from the ^5D0 excited level to the 7Fj （J = 0, 1, 2, 3, 4） levels of Eu3＋ions with the main electric dipole transition ^5D0→^7F2 （618 and 620 nm）, and Eu^3＋ ions prefer to occupy a lower symmetry site in the crystal lattice. Moreover, the photoluminescence （PL） intensity was strongly dependent on both the sintering temperature and doping concentration, and the highest PL intensity was observed at an Eu^3＋ concentration x = 7 mol.% after annealing at ll00℃. The obtained Ca2A12SiO7：Eu^＋3＋ phosphor may have potential application for the red lamp phosphor.

Progress in Research on Nanometer Al_2O_3 Fabricated by Sol-Gel Method

Nanometer Al_2O_3 is one of new types of functional materials with broad application and development prospects in the future. The basic principle and ways of nanometer Al_2O_3 fabricated using sol-gel technique were introduced, and the factors affecting nanometer Al_2O_3 fabricated using sol-gel method were analyzed. The progress in research on nanometer Al_2O_3 and the application fields of nanometer Al_2O_3 were reviewed. The existing problems and the problems prospect for nanometer Al_2O_3 were pointed out.

Barium titanate ceramic inks for continuous ink-jet printing synthesized by mechanical mixing and sol-gel methods

Ink-jet printing of ceramic thick films is one of low cost on-site ceramic pattern fabrication methods.It is necessary to investigate the rheological behaviour of ceramic inks and drying behaviour of droplets.Two kinds of BaTiO3 ceramic inks were prepared by mechanical mixing and sol-gel methods,respectively.The effect of preparation parameters,such as quantity of polyacrylic acid(PAA)and solid content,on physicochemical and rheologic properties of the ceramic inks was investigated.The results show that they satisfy the requirements of continuous ink-jet printing.The appearances of printed dots and single printed layers were observed by SEM.The SEM images indicate that dots printed with mixing method ink are in ring shape,and dots printed with sol-gel method ink are in pancake shape,so the printed layer surface with the latter ink is smoother.The causes of these phenomena were discussed.

Effects of sol-gel method and lanthanum addition on catalytic performances of nickel-based catalysts for methane reforming with carbon dioxide

The nickel-based catalysts were prepared by the sol-gel method and used for the CH4 reforming with CO2. The effects of the sol-gel method on the specific surface area, catalytic activity, desorption, and reduction performances of catalysts were investigated with BET, TPR, and TPD. Compared with the catalyst prepared by the impregnation method, the results indicated that the catalysts prepared by the sol-gel method had larger specific surface area, showing higher catalytic activities and exhibiting perfect desorption and reduction performances. In addition, the modification effects of adding La were studied, and it was found that the 0.75NLBT catalyst constituted of 5wt.%Ni-0.75wt.%La was optimal.

Fabrication and characterization of highly ordered Ni_(0.5)Zn_(0.5)Fe_2O_4 nanowire/tube arrays by sol-gel template method

Highly ordered nanowire/tube arrays of Ni0.5Zn0.5Fe2O4were fabricated by the sol-gel method in the pores of anodic alumina membrane （AAM）. Whether nanowires or nanotubes were fabricated depends on immersion time. The immersion time was 15- 40 s for nanotubes and over 60 s for nanowires. The topography and crystalline structure of the nanowire arrays were characterized by scanning electron microscopy （SEM）, transmission electron microscopy （TEM）, and X-ray diffraction （XRD）. It was found that the length and diameter of the Ni0.5Zn0.5Fe2O4 nanowires are related to the thickness of the AAM and the diameter of the pores. The results indicated that the Ni0.5Zn0.5Fe2O4 nanowires are uniform and parallel to each other.

Synthesis and Characterization of Nanocrystalline SrAl_2O_4∶Eu, Dy Long Afterglow Phosphors by Sol-Gel Method

Eu 2+, Dy 3+ co-doped nanocrystalline strontium aluminate phosphor powders with brightness and long afterglow were synthesized by the sol-gel method at 1200 ℃ for 2 h. The samples were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results of XRD show that the single crystalline phase is α-SrAl_2O_4. According to the observation of SEM, the particles of the samples are needle-like. Compared with the samples synthesized by solid state reaction, the grain size of the sol-gel method is to nanometer grade. A clear blue shift occurs in the excitation and emission spectra. The blue shift in nanocrystalline SrAl_2O_4∶Eu, Dy phosphor can be attributed to the quantum-size-effect of the luminescent particles.

Studies on impact sensitivity of nanosized trinitrotoluene (TNT) confined in silica processed by sol-gel method

Nano-sized trinitrotoluene(TNT) material restrained in silica gel has been prepared by using the sol-gel process to study the effect of varying porosity in gel on the sensitivity of TNT. The TNT content in the gel has been varied from 60 to 90 wt %(at fixed acetone/tetramethoxysilane ratio of 50). Also, for a fixed TNT content of 75 wt %, the pore structure in the gel has been varied by changing the ratio of silica gel precursor to the solvent. The resultant TNT–silica gel composites have been characterized using scanning electron microscopy, thermal analysis, small angle X-ray scattering and surface area analysis techniques. Impact sensitivity studies were carried out using Fall Hammer Impact Test. The results showed that the sensitivity of nanostructured explosives prepared by sol-gel process can be tailored precisely by controlling the process parameters.