Synthesis of Nanometer-sized Mesoporous Oxide Spheres

A few hundreds nanometer-sized mesoporous silica and alumina spheres were synthesized in organic solvents. The impacts of ammonia, N, N-dimethylformamide (DMF) and stirring speed were also investigated.

THE MECHANISM FOR NANOMETER-SIZED TiC SYNTHESIZING BY MECHANICAL & THERMAL ACTIVATION PROCESSING

A novel process for synthesizing nano-ceramics powders, named mechanical & therm al activation processing, is discussed in the present paper. It is a processing based on thermal activation in liquid phase (molten salt) after mechanical activ ation. The nanometer-sized TiC particles (15-20nm) have been synthesized by the method, and analyzed by X-ray diffraction (XRD), transmission electron microscop e (TEM), scanning electron microscopy (SEM) and energy dispersion X-ray (EDX) sp ectroscopy. An interface interaction between liquid (molten salt) and solid (fin al product particles) phases plays a dominating role for the control of product particles size. The mechanism for the formation of nanometer-sized TiC particles has been discussed.

Synthesis and Luminescent Properties of Novel Nanometer-sized ScAlMgO_4:Eu^(3+) Phosphors for PDP

Novel nanometer-sized ScAlMgO4：Eu3＋ phosphors were successfully synthesized by the citric acid complexation method.The mean particle size of the obtained powders was within the range of 100～150 nm according to the SEM patterns.In ScAlMgO4：Eu3＋ showed strong characteristic red emission,of which the maximum emission peak was located at 629 nm for ultraviolet（UV） excitation.The dependence of photoluminescence intensity on Eu3＋ concentration was also studied in detail,and the emission intensity of Sc1-xEuxAlMgO4 was about 10% at optimized Eu3＋ concentration.Furthermore,the luminescence decay measurements showed that the lifetimes of Eu3＋ were in the range of millisecond.The obtained ScAlMgO4：Eu3＋ phosphors with nanometer size and excellent luminescence efficiency would be potential red phosphors in plasma display panels.

Preparation and Gas Sensitive Properties of Nanometer-Sized SnO_(2)

Nanometer-sized SnO_(2) particles were prepared by a sol-gel method using inorganic salt as a precursor material. Its crystallization was investigated by means of TG-DTA,IR absorption spectra, X-ray diffractometry and TEM as well as its resistivity change and the gas sensitivity varied with temperature were measured in various reducing gas. The results indicate that well-crystallized nano-sized SnO_(2)with size around 15nm can be obtained at annealing temperature 600℃. The activation energy for the growth of nano-SnO_(2) was calculated to be 26.55kJ.mol^(-1) when the annealing temperature was higher than 500℃. The measurements also show that there is a peculiar resistance change varied with temperature for nano SnO_(2).It has relevance to the increase in surface adsorbed oxygen. The selective detectivities to C_(4)H_(10) and petrol can be increased when ruthenium ion was doped in nano SnO_(2)as a catalyst and so do the gas sensitivity to CO,CH_(4),H_(2) etc. when rhodium ion was doped in.The detection to the several reducing gas can be realized when the temperature ranged from 260℃ to 400℃.

INVESTIGATIONS ON NANOMETER-SIZED ULTRAMICRO-ELECTRODES(Ⅱ)—FABRICATION, CHARACTERIZATION OF CARBON FIBER CYLINDER ULTRAMICROELECTRODES

Described here are the fabrication and characterization of carbon fiber cylinder ultramicroelectrodes with cylinder length of less than 100 am, total tip diameter of several hundreds nanometers. The electrodes have been fabricated by direct etching of carbon fiber using an ion beam thinner. Optical microscopy, scanning electron microscopy (SEM), cyclic voltammetry have been employed to characterize those electrodes. The experimental results obtained indicate the electrodes can be used for in vivo detection of neurotransmitters such as dopamine, 5—hydroxytryptamine in a single cell.

Simulation of Electrical Discharge Initiated by a Nanometer-Sized Probe in Atmospheric Conditions

In this paper, a two-dimensional nanometer scale tip-plate discharge model has been employed to study nanoscale electrical discharge in atmospheric conditions. The field strength dis- tributions in a nanometer scale tip-to-plate electrode arrangement were calculated using the finite element analysis （FEA） method, and the influences of applied voltage amplitude and frequency as well as gas gap distance on the variation of effective discharge range （EDR） on the plate were also investigated and discussed. The simulation results show that the probe with a wide tip will cause a larger effective discharge range on the plate; the field strength in the gap is notably higher than that induced by the sharp tip probe; the effective discharge range will increase linearly with the rise of excitation voltage, and decrease nonlinearly with the rise of gap length. In addition, probe dimension, especially the width/height ratio, affects the effective discharge range in different manners. With the width/height ratio rising from 1 ： 1 to 1 ： 10, the effective discharge range will maintain stable when the excitation voltage is around 50 V. This will increase when the excitation voltage gets higher and decrease as the excitation voltage gets lower. Fhrthermore, when the gap length is 5 nm and the excitation voltage is below 20 V, the diameter of EDR in our simulation is about 150 nm, which is consistent with the experiment results reported by other research groups. Our work provides a preliminary understanding of nanometer scale discharges and establishes a predictive structure-behavior relationship.

纳米二氧化钛/玻璃鳞片协同增强环氧树脂的耐磨性研究

[目的]环氧树脂(EP)复合材料虽有良好的力学性能和化学稳定性,但脆性大、摩擦因数高、耐磨性差,使其难以满足运动摩擦部件的性能要求。[方法]通过向EP基体中添加改性纳米TiO_(2)和玻璃鳞片(GF)制备了TiO_(2)/GF/EP复合材料,研究了纳米TiO_(2)添加量对复合涂层性能的影响。采用扫描电子显微镜(SEM)和傅里叶变换红外光谱仪(FT-IR)对涂层的断面形貌和分子结构进行了表征。[结果]利用KH-550硅烷偶联剂对纳米TiO_(2)进行改性处理消耗了其表面大量的羟基,有效减少了纳米TiO_(2)的团聚。GF和改性纳米TiO_(2)与EP基体的界面相容性良好,TiO_(2)/GF/EP复合涂层的致密性与纯EP涂层相比明显提高。对于添加了相对于EP质量4%的纳米TiO_(2)和30%的GF的复合涂层,其显微硬度比纯EP提高了46.8%,摩擦因数和磨损后的质量损失分别比纯EP减小了46.1%和52.0%。[结论]改性纳米TiO_(2)和GF共同作为填料加入,可使EP的显微硬度和耐磨性得到明显提高,摩擦因数明显减小,综合性能得到提升。

TiO_(2)包覆高镍NCM811的电化学性能研究

高镍材料具有较好的电化学性能,但其存在着表面稳定性较差的问题,通过钛酸四丁酯在NCM811材料表面水解生成TiO_(2),改善了高镍材料的表面稳定性。利用SEM和TEM对改性后的材料进行表面分析,结果表明,实验成功将TiO_(2)层均匀地包覆在高镍NCM811表面,并且发现,在表面包覆过程中,还发生了体相掺杂。利用表面包覆和体相掺杂的共同作用,在1C放电的条件下,循环200圈后,材料的容量保持率从81.40%提升至92.39%,改善了材料的电化学性能。

适用于地面装备的特种降温涂层研究与应用

[目的]为了有效降低太阳辐射引起的导弹温升,考察了一种针对地面装备的特种涂层的降温性能。[方法]通过基料与颜填料的筛选,确定以环氧树脂搭配固化剂作为基料,金红石型二氧化钛作为主要颜填料。对涂层方案及其作用机理进行分析后,确定了特种降温涂层的设计原则。对涂层建立了热传导模型,分析辐射来源,对地面装备进行了仿真分析。[结果]通过试样级试验验证了特种涂层的环境适应性与降温性能。[结论]该特种降温涂层解决了太阳辐射下地面装备内部升温较高的问题,为地面装备的应用打下了基础。

光催化二氧化钛超亲水无机涂层的制备及性能

[目的]超亲水涂层具有自清洁、防雾、防污等特性,但在玻璃上应用时透光性往往不够理想。[方法]以钛酸丁酯为前驱体,乙酰丙酮为抑制剂,无水乙醇和去离子水为溶剂,加入硝酸进行催化,合成了TiO2溶胶,并将其涂覆在玻片上,经煅烧处理后获得超亲水性透明涂层。分别考察了溶胶的粒径及涂层的表面形貌、水接触角、透明度和热稳定性。[结果]TiO2亲水涂层的水接触角为8.0°,400~700 nm波长范围内的透光率仅比空白玻璃低4个百分点,加热至800℃的过程中质量损失仅为8%。[结论]该涂层具有良好的亲水性和防雾性能。

低膨胀石英玻璃的制备技术与发展趋势

低膨胀石英玻璃(Low-expansion quartz glass)是指掺有低膨胀氧化物的石英玻璃,其热膨胀系数比一般的石英玻璃低一个或两个数量级,基于这种特质,低膨胀石英玻璃受到了许多人的关注。然而,随着高新技术的快速发展,低膨胀石英玻璃的性能已不能满足新技术领域的需求,直到1968年研制出SiO_(2)-TiO_(2)石英玻璃。相较于其他低膨胀石英玻璃,SiO_(2)-TiO_(2)石英玻璃的热膨胀系数更低,在一定温度范围内甚至可以做到零膨胀或负膨胀,因此掺钛石英玻璃又被称为超低膨胀(Ultra low expansion,ULE)石英玻璃。SiO_(2)-TiO_(2)石英玻璃凭借优秀的性能被广泛应用于半导体、航空航天、电子、光学等领域。SiO_(2)-TiO_(2)石英玻璃通常有以下几种制备方法——溶胶-凝胶法、化学气相沉积法、气相轴向沉积法和等离子体化学气相沉积法等,其中,火焰水解沉积法使用较为广泛,具有成熟的工业应用。

Chemical equilibrium controlled synthesis of polyoxymethylene dimethyl ethers over sulfated titania

The chemical equilibrium and reaction kinetic behavior in the synthesis of polyoxymethylene dimethyl ethers （DMMn） were investigated over sulfated titania in order to reveal the decisive factor controlling the reaction. The results showed that the molar ratio of adjacent DMMn products in equilibrium solution had the same value, which depended absolutely on the reaction temperature. Meanwhile, the reactions had the same DMMn products distributions under varied reaction conditions. The equilibrium constants of the related step-wise reactions for DMMn formation were equal, which were calculated based on the bulk compositions of the reaction solution. And thus, the selectivity to DMMn was mainly controlled by the chemical equilibrium, i.e., thermodynamic control. In brief, the present results provide some guidance for future synthesis of DMMn.

Enhancement of formaldehyde degradation by amine functionalized silica/titania films

Doping amine functional groups into SiO2/TiO2 films for enhancing the decomposition of formaldehyde has been investigated using the modified sol-gel method to prepare organic-inorganic hybrid photocatalysts via the co-condensation reaction of methyltrimethoxysilane （MTMOS） and amine functional groups, n-（2-Aminoethyl）-3-aminopropyl-trimethoxysilane （AEAPTMS） and 3-aminopropyl-trimethoxysilane （APTMS） were selected to study the effect of amine functional groups on the enhancement of formaldehyde adsorption and degradation under a UV irradiation process. Physicocbemical properties of prepared photocatalysts were characterized with nitrogen adsorption-desorption isotherms measurement, X-ray diffraction （XRD） and Fourier transform infrared （FT-IR） spectroscopy. The results indicated that the APTMS/SiO2/TiO2 film demonstrated a degradation efficiency of 79% superior to those of SiO2/TrO2 and AEAPTMS/SiO2/TiO2 films due to the synergetic effect of adsorption and photocatalytic properties. The APTMS/SiO2/TiO2 film can be recycled with about 7% decreasing of degradation efficiency after seven cycles.

Preparation of nitrogen-doped titania and its photocatalytic activity

Yellowish nitrogen-doped titania was produced through sol-gel method in mild condition, with the elemental nitrogen derived from aqua ammonia. The titania catalysts were characterized using XRD, BET, TEM, XPS, and UV-Vis diffuse reflectance spectrophotometer, and their photocatalytic activities were evaluated under UV and visible light, respec tively. The XRD results showed that all titania catalysts were anatase. More significantly, the crystallite size of nitrogen-doped titania increased with an increase in N/Ti proportion, and the doping of nitrogen could extend the absorption shoulder into the visible-light region, thus it possessed a higher visible-light activity illustrated by decolorization of methyl orange （65.3%） under the irradiation of visible light, whereas pure titania showed little of such kind of visible light activity. The UV-light activity of nitrogen-doped titania catalysts was worse than that of pure titania and Degussa P25. In the range of N/Ti proportion of 4-10 mol%, the activity of nitrogen-doped titania weakened appreciably in the visible-light region as the N/Ti proportion increased, whereas a reverse relationship existed under the irradiation of UV light.

Molybdosphoric Acid Mixed with Titania Used as a Catalyst to Synthesize Diphenyl Carbonate via Transesterification of Dimethyl Carbonate and Phenol

The 12-molybdosphoric acid mixed with titania （MPA-TiO2） was found to be a novel and efficient catalyst for the synthesis of diphenyl carbonate （DPC） via transesterification of dimethyl carbonate （DMC） and phenol. The X-ray diffraction （XRD） and infrared （IR） techniques were employed to characterize the prepared catalysts. The effect of the weight ratio of the 12-molybdosphoric acid to titania on the transesterification was investigated. A 13.1% yield of DPC and an 11.6% yield of methyl phenyl carbonate （MPC） were obtained over MPA-TiO2 with the weight ratio of MPA to TiO2 as 5：1.

Synthesis and Characterization of Co-Doped Brookite Titania Photocatalysts with High Photocatalytic Activity

Transition metal-doping could effectively extend the light response range of TiO _2 photocatalysts from the ultraviolet(UV)to the visible region.Co-doped brookite titanium dioxide(Co–TiO_2)photocatalysts were synthesized via the hydrothermal method with titanium tetrachloride as the raw material and cobalt chloride hexahydrate as the dopant.The prepared Co–TiO_2 photocatalysts were characterized by X-ray diffraction(XRD),scanning electron microscopy(SEM),transmission electron microscopy(TEM),Raman spectroscopy,X-ray photoelectron spectroscopy(XPS)and UV–Vis diffuse reflectance spectroscopy(UV–Vis DRS).The photocatalytic activities of Co–TiO _2 photocatalysts were evaluated by photocatalytic degradation of isopropanol alcohol(IPA),a typical volatile organic compound(VOC),under visible light.The influences ofdifferent Co doping rates,initial concentrations of IPA gas and the amounts of photocatalyst addition were also studied.At the same time,the enhancement mechanism ofcobalt ions as a trap for photogenerated holes was discussed.Thus,we found the optimum doping rate,initial concentration of IPA gas and amount of photocatalyst to add.The results show that the mesoporous Co–TiO _2 photocatalysts possess smaller size particles,larger specific surface area,lower forbidden bandgap energy(Eg)and better photocatalytic activity than pure brookite TiO _2.When the doping of Co was 7% by mass,the initial concentration ofIPA gas was 1.0×10^(-6 )mol/L and the addition of Co–TiO_2 photocatalysts was 50 mg,the best photocatalytic activity was achieved.Furthermore,the degradation rate ofIPA was up to 91%,which shows great potential for waste water treatment.

Synthesis of Nanoscale Shell-core Titania Coated Silica Particles in the Presence of Polyether Polyamine and the Phase Transition

The nanoscale titania coated silica was prepared via a two-step precipitating approach, where the nanoscale silica nuclei were first prepared by passing an aqueous solution of sodium silicate through an ion-exchange resin bed, then coated with the precipitation from hydrolyzed butyl titanate in an ethanol-hexane mixture at a low pH value in the presence of poly(ethylene oxide) polyamine salt(PPA) at a high temperature of 90 ℃. In the second-step precipitating process, the spontaneously precipitated titania shell on the silica nuclei was stabilized in the suspension solution with the help of the adsorption of PPA on the particles. A possible precipitating mechanism was suggested. Furthermore, the amorphous titania shell could undergo crystallization from the amorphous to the anatase structure at a high temperature of 650 ℃, and a further phase transition from the anatase to the rutile structure in the different sintering processes at a rising temperature of 750 ℃.

Synthesis of Nanostructured Copper-doped Titania and Its Properties

Nanostructured pure-Ti O_2 and Cu3%-Ti O_2 were successfully synthesized via co-precipitation method. The X-ray diffraction(XRD) result proves that the synthesized sample were predominantly in anatase phase with size in the range of 8～16 nm, which are in good agreement with the transmission electron microscopy data. Owing to doping of copper, not only did the thermal stability of the Ti O_2 decrease, but also a significant decrease in its particle size and a shift of the adsorption edge to a higher wavelength region appear. The activity of both pure-Ti O_2 and Cu3%-doped Ti O_2 was tested to study their ability to decolorize congo red(CR) dye in aqueous solution. We observed that the CR dye was decolorized faster by Cu3%-Ti O_2 than pure-Ti O_2. Results of this study demonstrate a potential application of the synthesized sample for decolorizing dye pollutants from aqueous waste.

Heterogeneous Photocatalytic Mineralization of Chlorobenzene by Paratungstate-loaded Titania Catalysts in an Aqueous Medium

Paratungstate-loaded titania catalysts were prepared %via% the addition of a series of aqueous solutions of paratungstate(denoted as W_ 7) into an isopropanol solution of Ti[OCH(CH_ 3)_ 2]_ 4 by means of the sol-gel method. The catalysts were characterized by EDX, BET, FTIR, UV-Vis DRS, XRD and the results indicate that such paratungstate-loaded catalysts maintained their heptatungstate structure in the anatase titania matrix up to 400 ℃. The catalysts were tested for the heterogeneous photodegradation of chlorobenzene in aqueous media and showed a better catalytic activity than P-25 TiO_ 2 because paratungstate can prevent the recombination of the holes and electrons produced during irradiation. Moreover, the paratungstate-loaded titania catalysts can resist the disaggregation during the photoirradiation and can be easily recycled from the aqueous suspensions after reactions.

Synthesis and Characterization of Mesoporous Titania Particles and Thin Films

Well-organized mesoporous titania particles and thin films were successfully synthesized by using tetrabutyl titanate as the inorganic precursor and triblock copolymer （Pluronic P123） as the template via evaporationinduced self-assembly process. The resulting materials were characterized by high resolution transmission electron microscopy （HRTEM）, X-ray diffraction （XRD）. Fourier-transform infrared spectroscopy （FT-IR）,Brunauer-Emmett-Teller （BET） and atomic force microscopy （AFM）. Macro shape of mesoporous titania would greatly influence the mesostructure of materials, and the probable reasons were also discussed.