Preparation and Characterization of Silica Aerogels Derived from Ambient Pressure

Silica aerogels were prepared by sol-gel technique from industrial silicon derivatives （polyethoxydisiloxanes, E40）, followed by silylation and drying under ambient pressure. The specific surface area, pore size distribution and thermal conductivity of the silica aerogels were investigated and the results showed that the diameter of the silica particles is about 6 nm and the average pore size of the silica aerogels is 14.7 nm. The specific surface area of which is about 1000 m^2.g^-1 and the thermal conductivity is about 0.014 wm^-l.K^-1 at room temperature and pressure of 1.01×10^5 Pa. The Si-CH3 groups were also detected on the internal surface of the silica aerogels, which show hydrophobic. Silica aerogels derived by this technique is low cost and have wide applications.

Microstructure Control of Nanoporous Silica Thin Film Prepared by Sol-gel Process

Nanoporous silica films were prepared by sol-gel process with base, acid and base/acid two-step catalysis.Transmission electron microscope （TEM） and particle size analyzer were used to characterize the microstructure and the particle size distribution of the sols. Scanning electron microscopy （SEM）, atomic force microscopy （AFM） and spectroscopic ellipsometer were used to characterize the surface microstructure and the optical properties of the silica films. Stability of the sols during long-term storage was investigated. Moreover,the dispersion relation of the optical constants of the silica films, and the control of the microstructure and properties of the films by changing the catalysis conditions during sol-gel process were also discussed.

SYNTHESIS OF MESOPOROUS POLY(STYRENE-co-MALEIC ANHYDRIDE)/SILICA HYBRID MATERIALS VIA A NONSURFACTANT-TEMPLATED SOL-GEL PROCESS

Mesoporous poly(styrene-co-maleic anhydride)/silica hybrid materials have been prepared. The synthesis was achieved by the HCl-catalyzed sol-gel reactions of tetraethyl orthosilicate (TEOS) and styrene-maleic anhydride copolymer in the presence of 3-aminopropyl triethoxysilane (APTES) as a coupling agent and citric acid as a nonsurfactant template or pore-forming agent, followed by ethanol extraction. Characterization results from nitrogen sorption isotherms and powder X-ray diffraction indicate that polymer-modified mesoporous materials with large specific surface areas (e.g. 900 m(2)/g) and pore volumes (e.g. 0.6 cm(3)/g) could be prepared. As the citric acid concentration is increased, the specific surface areas, pore volumes and pore diameters of the hybrid materials increase.

Study on roasting process of zircon-silica sol ceramic mould

Dry stock of silica sol ceramic mould was prepared by using of colloidal moulding technique with an optimized vacuum drying process.Effect of roasting process on the shrinkage rate and compressive strength of zircon-silica sol ceramic mould,and the relationship between the roasting temperature and microstructure of zircon-silica sol ceramic mould were studied.The optimum roasting temperature of zircon-silica sol ceramic mould gained by the experiments is 900℃ and the holding time is 2 h.The scanning electron microscope(SEM) observation showed the growth of refractory particles during the roasting process.The occurrence of sintering was observed in the zircon-silica sol ceramic mould when roasting temperature was above 1,000℃.

Facile and Controlled Synthesis of Silica Sol Nanospheres Through a Modifi ed Sol-Gel Process

An effective and reproducible preparation of silica sol nanospheres via a modified sol-gel process has been described. Monodisperse and stable silica sol nanospheres with uniformsize were successfully obtained through the optimized synthesis in which the mixture of tetraethyl orthosilicate （TEOS） and ethanol was followed by the addition of water and ammonium hydroxide （NH3） separately, and the size of silica sol spheres was strictly controlled in the range of 25-119 nm with a narrow size distribution by fine adjustment of several reaction parameters. Results showed that in the presence of low concentration of TEOS, spheres size rose first and reached maximum when H2O concentration was up to 66 g/L. However, the diameter of silica sol spheres decreased above 66 g/L of H2O concentration. Furthermore, it was also found that the size and size distribution of silica sol nanospheres were affected by NH3 concentration. As NH3 concentration increased from 15 to 35 g/L, the diameter declined from 83 to 64 nm. Nevertheless, higher NH3 concentration would result in relatively broad size distribution, and gelation occurred when NH3 concentration reached 44 g/L. In addition, the effect of the different feed rates ofNH3 on the size growth of silica sol nanospheres was also discussed.

Experiment on the silica sol imbibition of low-permeability rock mass:With silica sol particle sizes and rock permeability considered

It’s a universal engineering problem to seal micro-cracks of low-permeability argillaceous rock mass by grouting in the fields of civil engineering and mining.This paper achieved the grouting sealing of lowpermeability artificial rocks with the permeability of 0.1–40 mD by adopting silica sol imbibition grouting.The variation characteristics of particle size,viscosity,and contact angle of silica sol during solidification and the pore size distribution of low-permeability artificial rocks were measured,and spontaneous imbibition tests of the artificial rocks were carried out.Finally,combined with the imbibition theory,percolation theory,and fracture medium grouting principle,the silica sol imbibition mechanism of lowpermeability rocks and soil was discussed.The results show that:(1)Silica sol can be injected into artificial rocks with the minimum permeability of 0.1 mD through spontaneous imbibition;(2)The particle size increase of silica sol leads to decreased wettability,affinity,and injectability in grouting materials;and(3)In the range of 0.1–40 mD,the grout absorption first increases and then decreases with increased permeability.The number of large pores and fractures in the rock mass is related to injectability,and the number of small and medium pores is related to the internal driving force of imbibition.This study provides a theoretical basis for silica sol grouting sealing of low-permeability argillaceous rocks and is,therefore,an important reference for application.

Effect of Catalyst on the Formation of Silica Coating on Nickel Substrate by Sol-Gel Processing

In this research work silica coating was produced on nickel substrates by a sol-gel process. In order to increase the rate of hydrolysis and to reduce the rate of polymerization several acid catalysts including nitric acid-hydrochloric acid, acetic acid, hydrochloric acid and nitric acid were add to silica sol. Conversely, in order to control the rate of hydrolysis and to increase the rate of polymerization, basic catalyst of ammonia and ammonia hydroxyl were introduced in to the solution. Nickel specimens of known surface roughness were chemically cleaned and prepared by dipping in the sols. In order to produce a suitable silica coating the drying and firing cycles were optimized on these substrates. The structure and uniformity of the coatings produced were examined by scanning electron microscopy. Coatings composition was determined using glow discharge optical spectroscopy and EDAX microanalysis. Experimental result showed that hydrochloric acid, acetic acid, ammonia and acetic acid - ammonia are suitable catalytic agents for silica coating formation on nickel type substrate.

RHEOLOGICAL MODIFICATION OF EPOXY RESINS WITH NANO SILICA PREPARED BY THE SOL-GEL PROCESS

Nano silica-modified epoxy resins were synthesized by the sol-gel process, The materials have the morphological structure of nano particales dispersed in the epoxy matrix. The dispersed phase formed a physical network in the resin and thus influenced the rheological behavior greatly. However, the nano silica did not show a significant influence on the mechanical properties of the cured resins.

Synthesis of Mesoporous Carbon Monolith by Direct Carbonization of Compressed Sucrose/Silica Composite

Mesoporous carbon monolith was synthesized by the direct carbonization of compressed sucrose/silica composite, which was prepared by using sol-gel method. The structural and textural properties of the materials were investigated by XRD, DRIFT, N2-adsorption and SEM. The characterization study shows that the resultant carbon monolith possesses a relatively high surface area, large pore volume and well interconnected pore system. Addition of a certain amount of citric acid or aluminum nitrate into the sol-gel precursor of sucrose/silica composite could considerably change the structure parameters of the carbon monolith.

Preparation of Scratch-Resistant Nano-Porous Silica Films Derived by Sol-Gel Process and Their Anti-reflective Properties

Structural strengthening of the nano porous silica films has been reported. The films were prepared with a base/acid two-step catalyzed TEOS-based sol-gel processing and dip-coating, and then baked in the mixed gas of ammonia and water vapor. The silica films were characterized with TEM, AFM, FTIR, spectrophotometer, ellipsometer, and abrasion test, respectively. The experimental results have shown that the films have a nanostructure with a low refractive index and can form an excellent scratch-resistant broadband anti-reflectance. The two-step catalysis noticeably strengthens the films, and the mixed gas treatment further improves mechanical strength of the silica network. Finally the strengthening mechanism has been discussed.

A comparative study of drying techniques on the morphology of porous silica gels synthesized via sol-gel process

The effect of drying techniques on the microstructure,morphology and pore structure of porous silica gels was studied in the paper.The gels were prepared by using sol-gel process and different drying routes:freeze-drying (FD),low pressure drying (LPD),high temperature drying (HTD) and chemical modification & ambient drying (CMD) techniques.Observation under pore distribution and structural properties showed that CMD technique leads to homogenous mesoporous silica material with specific surface area of 745 m2/g,and the average pore size around 20 nm,while LPD and HTD result in loosely packed particles with non-isotropic aggregation pattern.The specific surface areas of LPD and HTD samples are 419 and 513 m2/g respectively,and the pore size distribution of the samples are observed distributing widely in range of 10-100 nm.Freeze drying method is a new but prospective way to prepare mesoporous silica.The specific area of FD sample is around 500 m2/g.By the comparison for the properties of the gels,this paper wants to induce a further interest in finding a proper method to synthesize the porous silica gels for low price use.

溶胶-凝胶法改良人工林马尾松尺寸稳定性及其机理研究

马尾松是广西地区重要的人工林资源之一,但其尺寸稳定性较差,极大地限制了其在木材工业中的使用。本研究选用基于SiO_(2)的溶胶-凝胶法对马尾松进行改良,探讨了浸渍时间对马尾松尺寸稳定性的影响,并通过扫描电子显微镜(SEM)、X射线能谱(EDS)、傅里叶变换红外光谱(FT-IR)、X射线光电子能谱(XPS)、X射线衍射(XRD)揭示了溶胶-凝胶法对马尾松的改良机理。研究结果表明:经过6 h溶胶浸渍处理的改性马尾松尺寸稳定性最好,相较于未处理的马尾松,浸渍6 h的改性马尾松的浸渍率为5%,60 h吸水质量增加率由34.7%降低至28.2%,60 h吸湿体积膨胀率由16.5%降低至11.1%,72 h抗老化性能由18.02的色差值降低为11.9。溶胶-凝胶法对马尾松尺寸稳定性的改善机理体现在两个方面:其一,通过形成玻璃层状及膨胀结构可以阻挡水分的进入;其二,通过氢键及化学键的形式与细胞壁进行结合,以起到永久的润胀作用。

纳米硅溶胶−EVA−粉煤灰水泥基复合浆材配比正交优化及对其物性的影响

针对传统水泥基浆材不能满足煤矿大变形巷道注浆加固实际需求的难题,通过添加纳米硅溶胶、乙烯−醋酸乙烯共聚物(EVA)和粉煤灰对普通硅酸盐水泥进行改性获得高性能复合浆材。采用正交试验和极差分析法系统研究复合浆材物理力学性能的变化规律,确定最优配比,并进一步分析最优配比复合浆材与纯水泥的物性差异,构建复合浆材的水化反应机理模型,阐明其加固破碎岩石的力学特性。研究结果表明,复合浆材最优配比为:水灰比0.7,粉煤灰掺量15%,硅溶胶掺量2%,EVA掺量7.5%;相较于纯水泥,复合浆材流变性略有下降,但浆液稳定性、力学性能等均有显著提升,初凝时间缩短了38.9%,终凝时间缩短了53.8%,析水率降低了60%,结石率提高了3.3%,单轴抗压强度提高了39.1%,抗拉强度提高了97.2%,拉压比提高了41.7%;硅溶胶和粉煤灰在不同时期与Ca(OH)2发生火山灰反应生成更多水化硅酸钙(C-S-H)和水化铝酸钙(CA-H),促进复合浆材的水化反应,并加速EVA成膜,使结石体更加致密;复合浆材注入量和胶结体单轴抗压强度均随注浆压力的增大而增加,随Talbot指数的增加,抗压强度先增大后减小,破坏形式多呈鼓状,剪胀变形明显;当注浆压力大于2 MPa,Talbot指数为0.5时,胶结体强度较大,破坏较小。本研究为水泥基复合浆材早期强度、增韧改性提供了可行途径。

改性硅溶胶封孔剂对多孔Al_(2)O_(3)陶瓷绝缘性能和微观结构的影响

采用甲基三甲氧基硅烷和二甲基二甲氧基硅烷对硅溶胶进行改性制得有机硅改性硅溶胶封孔剂,并通过浸渍和加热固化的方法对多孔Al_(2)O_(3)陶瓷片进行封孔处理。研究了固化温度和固化时间对封孔Al_(2)O_(3)陶瓷片绝缘性能的影响,并对多孔Al_(2)O_(3)陶瓷片封孔前后的微观结构进行了表征。结果表明,较佳封孔条件为固化温度120℃、固化时间60 min,此时封孔Al_(2)O_(3)陶瓷片的直流和交流击穿电压分别达到最大值10.76 kV和6.01 kV,1000 V绝缘电阻不低于9999 MΩ。封孔Al_(2)O_(3)陶瓷片表面为改性硅溶胶涂层,呈致密无孔隙状态且与基体结合紧密,涂层厚度约为25μm,表面水接触角提高到86.93°,封孔层深度约为10μm。

硅溶胶-异丁基三乙氧基硅烷复合乳液对泡沫混凝土防水性能的影响

[目的]研究硅溶胶-异丁基三乙氧基硅烷(IBTS)复合乳液对泡沫混凝土防水性能的影响,为拓宽其应用提供实验数据。[方法]通过宏观力学特性试验和微观结构分析,综合考察了该复合乳液对泡沫混凝土的防护效果。[结果]涂抹了复合乳液的泡沫混凝土表现出比涂抹了单一IBTS乳液的泡沫混凝土更优异的抗渗透性能和耐久性,其水渗透深度和碳化深度更小,浸水48 h后的吸水率为0.46%,氯离子迁移系数为1.1×10^(-12)m^(2)/s,冻融240次后的质量损失率为0.55%,且动弹性模量仍维持冻融试验前的85.34%。[结论]复合乳液的防水机理涉及表面效应、化学反应、物理效应等多个方面,通过形成致密的防水层、填充孔隙和微裂纹、吸附并包固水分子等方式来防止水分渗透和扩散,从而提高泡沫混凝土的防水性能。

水性饰面型防火涂料的制备及其耐火性能研究

[目的]配方对防火涂料的性能有很大影响。[方法]以苯丙乳液和硅溶胶作为基料,聚磷酸铵、季戊四醇和三聚氰胺作为阻燃体系,二氧化钛作为颜填料,六偏磷酸钠作为分散剂,磷酸三丁酯作为消泡剂,羧甲基纤维素作为增稠剂,研制了一种适用于钢结构的水性饰面型复合膨胀防火涂料。利用模拟大板燃烧试验考察了各组分的质量分数对涂料性能的影响,并采用扫描电镜(SEM)对防火涂层燃烧后的微观结构进行表征。[结果]最佳配方为:苯丙乳液20.0%,硅溶胶4.0%,聚磷酸铵27.0%,季戊四醇22.0%,三聚氰胺21.0%,颜填料4.0%,助剂2.0%。此时涂料的耐燃时间长达57 min,燃烧后形成的炭层致密。[结论]该涂料具有良好的防火阻燃效果。

硅溶胶包覆制备核壳结构VO_(2)(M)@SiO_(2)研究

通过SiO_(2)包覆VO_(2)(M)材料形成核壳结构,可以显著提高其可见光透过率(T_(lum)),有效减缓VO_(2)(M)的氧化过程,对于增强智能窗的应用价值具有重要意义。Stöber法是制备核壳结构VO_(2)(M)@SiO_(2)的传统方法,采用硅溶胶凝胶法来简化制备工序、降低生产成本并减少工艺调控要素。通过对硅溶胶凝胶实验的初步研究,探讨硅溶胶凝胶包覆VO_(2)(M)的工艺参数,并通过实验验证硅溶胶凝胶包覆VO_(2)(M)的可行性。研究结果表明,当pH为5~6、固含量为15%~20%(质量分数)时,硅溶胶的凝胶化能力最佳。此外,随着凝胶温度升高,凝胶时间缩短,焙烧后得到的SiO_(2)粉体结晶性和热稳定性增加。根据优化后的硅溶胶凝胶工艺参数成功制备了致密稳定的核壳结构VO_(2)(M)@SiO_(2)材料,其包覆程度达到93.3%,薄膜的光学透过率提升至65%,且其相变温度降低和热滞后回线宽度变窄。因此,硅溶胶凝胶法为制备高性能的核壳结构VO_(2)(M)@SiO_(2)材料提供了一种简化工艺和降低成本的方法,对于智能窗等应用具有重要潜力。

Silica sol/Nano-Au/PVP修饰金电极电致化学发光测定槐定碱

基于槐定碱对联吡啶钌（Ru（bpy）3^2＋）在电致化学发光中的增敏机理,通过传感器修饰技术,将Silica sol/Nano-Au/PVP修饰到金电极表面,建立了简单、快捷测定槐定碱的新方法。实验表明,最佳实验条件下,在1.6×10^-7-1.6×10^-4mol/L范围内,槐定碱的浓度与其对应的电化学发光强度值呈良好的线性关系,I=4.000×10^7c＋262.2,r^2=0.994 5,检出限（S/N=3）为3.5×10^-9mol/L。连续平行测定浓度为1.6×10^-5mol/L的槐定碱溶液6次,其相对标准偏差（RSD）为2.9%。该方法具有较高的选择性和灵敏度,样品处理简单快速,用于槐定碱的测定,结果满意。

二氧化硅微球制备方法研究进展

二氧化硅微球是一种无机填料,由于其比表面积大、化学稳定性高、耐温性能优良、机械强度高以及环保无污染等优点,在电子封装、生物医药、机械抛光以及流体输送等领域中有着广泛应用。主要综述了当前常见的制备方法,如溶胶-凝胶法、气相法和高温球化法等,并指出了以上方法的优缺点,同时介绍了二氧化硅微球在复合材料中的应用,并对这些方法的改进以及后续研究方向提出了观点。此外,还简要介绍了独创的气相氧化法的原理、优势和应用。