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.

Development of Modified Glasses by Transparent, Functional Hybrid Sol-Gel Nano-Ceramic Coatings, a Comparative Study

This paper concentrates on the development of glasses with self-cleaning surfaces exhibiting high water contact angles. In this study, we prepared super-hydrophobic nano-ceramic coated glass based on titania & silica using simple sol-gel & dip coating methods and studied the best composition of the coatings by altering ratios of titanium tetraisopropoxide (TTIP)/tetraethyl orthosilicate (TEOS) with different homogenizing agents. We characterized the coatings by surface roughness measurement, percentage of optical transmission, static contact angle, near-infrared (NIR) transmission, and diffuse reflectance. The fabrication of coatings on glass substrates played an important role in increasing the water contact angle of about 95° and visible & NIR transmission of about 90%. We compared our modified glass substrate with commercial low emissivity (Low E) glass using X-ray diffraction (XRD) analysis, which showed pure amorphous surface claiming excellent wettability and thus the prepared glass substrate could have a variety of applications in different fields.

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.

Preparation of Rod-like Aluminum Doped Zinc Oxide Powders by Sol-gel Technique Using Metal Chlorides and Acetylacetone Precursors

Al-doped ZnO(AZO) powders were prepared by using metal chloride precursors and the sol-gel technique. IR peaks observed at 1590 cm-1 and 1620 cm-1indicated the formation of metal chelate as a consequence of the addition of acetylacetone to the metal chloride solution. TG-DSC analysis of the AZO gels confirmed the formation of metal chelate as evidenced by the development of several weight loss peaks accompanied by the introduction of new endothermic peaks. The resulting AZO gels were annealed at 500, 600, and 800 ℃ to study the effect of annealing temperature. XRD and SEM results showed that crystallization of AZO gels takes place around 600 ℃. Hexagonal wurtzite structure was identified as the main phase for all the samples. In addition, small shift of the XRD(002) peak coupled with XPS results from the AZO powders confirmed the successful doping of the ZnO powders. Micron sized rod-like AZO powders were uniform in dimension and morphology and remained stable even at 800 ℃.

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.

Indium doping effect on properties of ZnO nanoparticles synthesized by sol–gel method

Pure ZnO and indium-doped ZnO(In–ZO) nanoparticles with concentrations of In ranging from 0 to 5% are synthesized by a sol–gel processing technique. The structural and optical properties of ZnO and In–ZO nanoparticles are characterized by different techniques. The structural study confirms the presence of hexagonal wurtzite phase and indicates the incorporation of In^(3+) ions at the Zn^(2+) sites. However, the optical study shows a high absorption in the UV range and an important reflectance in the visible range. The optical band gap of In–ZnO sample varies between 3.16 e V and 3.22 e V. The photoluminescence(PL) analysis reveals that two emission peaks appear: one is located at 381 nm corresponding to the near-band-edge(NBE) and the other is observed in the green region. The aim of this work is to study the effect of indium doping on the structural, morphological, and optical properties of ZnO nanoparticles.

Synthesis of Lithium-cobalt Oxides by Sol-gel Method and their Cathodical Discharge Behavior at 500 ℃

Three kinds of lithium cobalt oxides with lithium to cobalt atomic ratios of 0.6, 0.8 and 1.0 respectively were prepared using nitrates and citric acid by sol gel process. During the baking of the dry gel powder, two exothermic peaks occur, followed by the formation of Li 2O and Co 3O 4 and then the combination of LiCoO 2, which is testified by DTA and XRD. The powder formed from an alkaline sol is finer than that from the acidic one. There are a single phase intercalation of lithium ion and an electrochemical reduction reaction for higher valence cobalt ion when simulating the discharging process of Li B/LiCl KCl/lithium cobalt oxides at 500 ℃, and the voltage and specific capacity are not sensitive to the initial ratios of lithium to cobalt.

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.

Thermal Stability and Luminescence Properties of Eu^(3+) and Tb^(3+) Complexes with a Silica Matrix by Sol-Gel Method

Ternary complexes of europium and terbium with benzoic acid and 1, 10 phenanthroline [RE(BA) 3phen] (BA=benzoate phen=1,10 phenanthroline) were introduced into a silica matrix by sol gel method. The thermal stability and luminescence behavior of the complexes in silica gels were studied in comparison with the corresponding solid state complexes by thermal decomposition, excitation and emission spectra. The thermal stability of the complexes is enhanced in silica gel matrix and the luminescence remaines unchanged.

PREPARATION OF ZnO CERAMIC POWDER BY SOL-GEL METHOD AND ITS VOLTAGE SENSITIVE PROPERTIES

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Preparation of Crack-free 3Y-TZP/Al_2O_3 Composite Ceramic Fiber by Electrolysis-sol-gel Method

Polycrystalline 3Y-TZP/Al2O3 tetragonal zirconia fiber was obtained by the pyrolysis of gel fibers using zirconium oxychloride octahydrate（ZOC） as the raw material. The spinnable zirconia sol was prepared by electrolyzing the zirco-nium oxychloride octahydrate（ZOC） solution in the presence of acetic acid and sugar（ sucrose, glucrose or fructose） , in which the molar ratios of CH3 COOH/ZOC and sugar/ZOC were 1.0-4.0 and 0.2-0.4, respectively. The pre- pared tetragonal zireonia fibers sintered at different temperatures showed smooth and crack-free surfaces with diame, ters of 5-10 μm. The addition of Al2O3 enhanced the sintering process and prevented the crystals from growing. Thermogravimetric analysis（TG）, X-ray diffraction （ XRD ）, Fourier transform infrared spectroscopy（FTIR）, and scanning electron microscope（SEM） techniques were used to characterize the prepared fibers.

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.

Preparation and characterization of (metal, nitrogen)-codoped TiO_2 by TiCl_4 sol-gel auto-igniting synthesis

The nitrogen-doped and （metal, nitrogen）-codoped TiO2 photocatalysts （metal = Ag, Ce, Fe, La） were synthesized by sol-gel auto-igniting synthesis （SAS） with the complex compound sol of TiCl4-NH4NO3-citri acid-metal nitrate- NH3.H20 as a precursor. The products were characterized by means of XRD, XPS, and UV-Vis diffuse reflectance spectra, and their photocatalytic activity was investigated under visible light. It was found that all the synthesized powders showed good absorption for visible light, and that the radius and alterable valence states of doping metallic cations played important roles on their photocatalytic activity. These results were discussed in detail.

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.

Upconversion properties of Y_2O_3:Er films prepared by sol-gel method

Y2O3：Er^3＋ films were prepared by a simple sol-gel process. The structural properties of Y2O3：Er^3＋ films were characterized with X-ray diffraction, Fourier transform infrared spectroscopy and field emission scanning electron microscopy. The results indicated that the Y2O3：Er^3＋ films might have high upconversion efficiency because of their low vibrational energy. Under 785 and 980 nm laser excitation, the samples showed green （^2H11/2→^4I15/2, ^4S3/2→^4I15/2） and red （^4F9/2→^4I15/2） upconversion emissions. The upconversion mechanisms were studied in detail through laser power dependence. Excited state absorption and energy transfer process were discussed as possible upconversion mechanisms. The cross relaxation process in Er^3＋ was also investigated.

Preparation and Sinterability of Mn-Zn Ferrite Powders by Sol-Gel Method

Mn-Zn spinel ferrites were synthesized by sol-gel method. Effects of calcined temperature on structure and particle size of MnZnFe2O4 were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM). XRD patterns indicate that the ultra fine Mn-Zn ferrite exhibits a spinel crystal structure. SEM images show that the powder fired at 900℃for 2 h has an average diameter of 60 ~ 90 nm. The particle size becomes larger with the increasing of calcined temperature and the distribution of particle becomes even more homogeneous. Sintering behaviors of synthesized ferrite powders depend on the powder characteristics and high temperatures have induced the good crystallization of particles.