溶胶－凝胶法制备超细SiO_2──制备参数对气凝胶织构性质的影响

ＳｉＯ_２气凝胶超细粉由ＴＥＯＳ（正硅酸乙酯）在乙醇溶液中水解聚合后经超临界流体干燥（ＳＣＦＤ）制得。本文考察了ＴＥＯＳ的浓度、水和ＴＥＯＳ的摩尔比以及焙烧温度对超细粉织构性能的影响。结果表明，超细ＳｉＯ_２的比表面积、总孔容、孔分布、最可几孔径及表现堆密度均随制备参数而改变。而以ＳｉＯ_２气凝胶超细粉体为基本载体材料的Ｃｏ／ＺｒＯ_２－ＳｉＯ_２催化剂显示出高的ＣＯ＋Ｈ_２合成重质烃的活性和选择性。     

溶胶—凝胶法制备有机—无机纳米复合材料

溶胶－凝胶法以其温和的反应条件，尤其是低的反应温度成为有机－无机纳米复合材料制备的最有效的方法．本文根据合成路线的不同，分５个方面对用溶胶－凝胶法制备复合材料进行概要介绍．     

溶胶-凝胶法制备纳米二氧化钛颗粒的研究

本文采用钛酸丁脂等原料,利用sol-gel方法制备了TiO2纳米颗粒.研究了不同实验顺序(滴入方式)和工艺参数对制备效果的影响.通过实验和对TiO2纳米粉末的TEM分析,获得了粒度(30-40nm)比较均匀的球型TiO2纳米颗粒.     

溶胶凝胶法制备纳米LiCoO2

纳米微粒;放电初容量;循环稳定性;溶胶凝胶法制备纳米LiCoO2     

溶胶-凝胶工艺制备发光薄膜研究进展

本文综述了通过深胶－凝胶工艺制备发光薄膜的基本过程、薄膜的表征方法、发光薄膜的当前发展及应用情况。依据组成特点,对溶胶－凝胶法制备的发光薄膜乾地了分类阐述,并预言了今后该法制备发光薄膜的发展趋势。     

溶胶-凝胶法制备纳米二氧化硅微球

在不同醇介质中,以氨水作为催化剂,正硅酸乙酯为硅源,利用溶胶-凝胶法制备了单分散纳米SiO2微球,利用激光粒度仪得到了微球粒径,利用扫描电镜得到了SiO2形貌,用能谱仪进行了元素成分分析。研究表明,随着氨水用量提高,溶液中OH-浓度增大,SiO2微球粒径增大;随着水用量增加,SiO2粒径有所增大,当水量太多时,粒径反而有下降趋势;在不同介质中,随着烃基中碳数和粘度改变,SiO2粒径会呈现不同变化。     

溶胶-凝胶法制备层状Ti/Si复合材料的研究

在水热体系下,通过溶胶-凝胶法,以阳离子表面活性剂十六烷基三甲基溴化铵作为模板剂,正硅酸乙酯作为硅源,三氯化钛作为钛源,制备出Ti/Si复合材料。样品的结构和形貌采用X射线衍射、扫描电子显微镜和透射电子显微镜进行表征,结果表明,所得样品呈现10 nm左右的层状形貌,同时具有相对规则的微孔结构,为其在催化氧化方面提供了有利条件,也为实验教材中Ti/Si复合材料的制备奠定了理论基础。     

TiO2纳米薄膜的溶胶-凝胶工艺制备和表征

通过sol-gel工艺在普通钠钙玻璃表面制备了均匀透明的锐钛矿型TiO2纳米薄膜.TiO2薄膜的X射线衍射分析表明,当薄膜的厚度小于0.46μm时,薄膜中未出现锐钛矿的衍射峰.随着镀膜次数或薄膜厚度的增加,薄膜中TiO2纳米微晶的平均晶粒大小逐渐增大,TiO2薄膜的透光率略有减小,其吸收阈值发生了明显的红移.XPS实验结果表明：薄膜中除含有Ti、O元素外,还有一定量来自有机前驱物中未完全燃烧的碳和少量从玻璃表面扩散到薄膜中的Na和Ca元素.     

溶胶-凝胶法制备纳米Pb(Zr0.52Ti0.48)O3

溶胶-凝胶法;纳米晶;溶胶-凝胶法制备纳米Pb(Zr0.52Ti0.48)O3     

新颖的玻璃制备方法—溶胶—凝胶法

长期以来,玻璃和光学纤维玻璃的制备几乎都是使用熔融—冷却法。这种方法不仅需要昂贵的生产设备,而且难以得到高纯度和高均匀度的材料。尤其是对于一些具有特殊结构和高熔点的玻璃材料,熔融—冷却法往往无能为力。     

Pyrolysis study of sol-gel derived zirconia by TG-GC-MS

Summary A homogeneous ZrO₂ gel was obtained by hydrolysis-condensation of zirconium(IV) n-propoxide previously reacted with acetic acid. Dried zirconia powders were characterized by Fourier transformed infra-red (FTIR) and X-ray diffraction (XRD) analyses. Thermogravimetric (TG) and differential thermal analysis (DTA) coupled with mass spectrometric (MS) and gas chromatographic (GC) measurements were carried out in order to identify and quantify the organic products released during the ZrO₂ gel pyrolysis. The TG-MS semi-quantitative analysis of the main released species allowed to describe the chemical rearrangement occurring in the solid during heating and to determine the chemical composition of the initial gel.     

Synthesis of silica glass using solventless sol-gel process

Silica glass was synthesized form TEOS and deionized water using sol-gel process. To introduce the physicochemical effects of ultrasonic waves, an ultrasonic homogenizer was used to mix reactants instead of adding cosolvents. 2-step method was chosen to separate hydrolysis reaction and condensation reaction, and thus to control the microstructure of wet gels. Wet gels were dried in 5–8 hours without cracks using supercritical drying with ethanol at 300°C and 10.34 MPa. Aerogels thus obtained have hydrophobic surfaces due to the reesterification reactions during supercritical drying. Aerogels were sintered in a tube furnace in the changing atmosphere from N₂ through O₂ to He. Sudden volume change was started at 1050°C and sintering was completed at 1100°C as expected. Large pores of aerogels allowed fast sintering in 16 and a half hours. Incomplete extraction in supercritical drying step produced crystals during sintering.     

sol-gel 法在有机-无机杂化体系中制备二氧化硅微粒

利用sol-gel法,通过正硅酸乙酯（tetraethyl orthosilicate（TEOS））在聚氧化乙烯／二甲基甲酰胺溶液中水解、缩聚,制备了粒径分布均匀的微米级二氧化硅粒子;利用扫描电子显微镜观测了制备条件对二氧化硅粒子的粒度和形貌的影响;研究了这一方法在制备无机粒子过程中的原理．     

Synthesis of porphyrin-introduced silica gels by sol-gel process

Using a hydroxyl group appended free base porphyrin derivative (HP), porphyrin-introduced silica gels were synthesized by a sol-gel process. The HP content in the materials linearly increased with increasing the HP concentration. Meanwhile, free base tetraphenylporphyrin (TPP) with no hydroxyl groups were almost not incorporated into the silica gels. These facts suggested that the interaction between hydroxyl groups of the HP molecules and silica network is considerably strong. The UV-vis characters of HP-introduced materials were almost the same as pure HP molecules. The Beer's plot indicated that the HP molecules in the materials are dispersed.     

Synthesis of mesoporous silica materials with ascorbic acid as template via sol-gel process

Mesoporous silica materials with pore diameters of 2-5 nm have been prepared using ascorbic acid as a nonsurfactant template or pore-forming agent in HCl-catalyzed sol-gel reactions of tetraethylorthosilicate,followed by removing the ascorbic acid compound by extraction with ethanol.Characterization results from nitrogen sorption isotherm,powder X-ray diffraction and transmission electron microscopy indicate that the materials have large specific surface areas (e.g.1000 m2/g) and pore volumes (e.g.0.8 cm3/g).The rnesoporosity is arisen from interconnecting disordered wormlike channels and pores with relatively broad size distributions.As the ascorbic acid concentration is increased,the pore diameters and pore volumes of the materials increase.     

New Photoluminescence Phenomena of Ge／SiO2 Glass Synthesized by Sol-gel Method

New Ge/SiO2 glasses have been synthesized by heating the GeO2/SiO2 dry gels under H2 gas at 700℃. The resulting fluorescence spectra show that this kind of Ge/SiO2 glasses emit strong photoluminescence at 392 nm (3.12 eV), medium strong photoluminescence at 600 nm (2.05 eV) and weak photoluminescence at 770 nm (1.60 eV) respectively. Possible photoluminescence mechanisms are also discussed based on the results of X-ray diffraction (XRD) and X-ray photoelectron spectra (XPS).     

Pyrolysis study of fluorinated sol-gel silica

Fluorinated silica gels at various fluorine content were prepared via sol-gel by hydrolysis of 3,3,3-trifluoropropyltrimethoxysilane and tetraethoxysilane mixtures. The gels, of nominal stoichiometry Si(CH₂CH₂CF₃)_XO_(2-X/2)(X=0.1-1), were characterized by FT-IR, X-ray photoelectron spectroscopy (XPS) and N₂ adsorption analysis. The thermal stability of the fluorinated samples was investigated by coupling thermogravimetric measurements with mass spectrometric and gas chromatographic analyses of the evolved gaseous species. The chemical reactions occurring in the gel matrices during heating were siloxane chain rearrangements involving condensation between residual hydroxyl and ethoxyl groups in the 100-350°C temperature range, whereas the thermal decomposition of the fluoroalkyl groups were observed at higher temperatures (450-600°C). The release of the fluoroalkyl moieties also involved C-F/Si-O bond exchanges inside the siloxane chains, with gas-phase evolution of different fluorinated silicon units. This revised version was published online in July 2006 with corrections to the Cover Date.     

含氟二芳基取代乙炔的合成

含氟二芳基取代乙炔的合成;ZnCl2/SiO2;含氟芳基取代乙炔;合成     

Flexible free-standing films morphology characterization: PVA/silica polymer network dispersed cholesteric liquid crystals films by sol-gel method

A novel flexible free-standing films of polyvinyl alcohol (PVA)/silica polymer network dispersed cholesteric liquid crystals (CLC) have been prepared by the sol-gel process. In the hydrolysis of silicon alkoxides tetraethoxysilane (TEOS) processes, the silica having -OH with the -OH groups on PVA formed polymer networks with Si-O-C bonds by dehydration. The cholesteric liquid crystals were incorporated into the networks. The free-standing films were obtained by the spin-coating method. In order to improve the compatibility and microstructure of the cholesteric liquid crystals with PVA/silica polymer networks, the amphiphilic compound of hexadecyl trimethyl ammonium bromide (HDTMA) was introduced into the forming film solutions. Effects of the different ratios of raw materials on the structure of films were investigated. The microscopic morphology of free-standing films and the uniform dispersion of CLCs in the films have been characterized by polarizing optical microscopy (POM), the field emission scanning electron microscope (FESEM), Fourier transform infrared (FT-IR) spectrometer and atomic force microscope (AFM). The free-standing films exhibiting excellent CLC droplets dispersion, mechanical stability, and good flexibility could be useful for flexible displays, switchable optical elements and smart windows.     

Synthesis and properties of sol-gel submicron silica powders doped with partly oxidized iron particles

Magnetic powders based on metallic iron crystallites encapsulated in submicron-sized spherical silica particles have been obtained and investigated. The metallic iron clusters have been produced by the exploding wire method. The silica shells have been prepared via the modified sol-gel Stöber method and the metallic particles have been entrapped by occlusion during the silica powder formation. The entrapped iron particles are partially oxidized due to the nature of the synthetic methods employed. The obtained hybrid materials have been investigated by electron microscopy, X-ray diffraction, magnetic and ζ-potential techniques. Such materials can be employed in such applications as e.g. magnetically-controlled drug vectors or electromagnetic field-shielding.