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。

固定Ionic liquid/Silica sol/Nafion膜中的联吡啶钌电化学发光行为的研究及应用

制备了Ionic liquid/Silica sol/Nafion-联吡啶钌复合物膜修饰金电极。采用循环伏安(CV)和电致化学发光(ECL)法,考察了联吡啶钌和左氧氟沙星在此修饰电极上的电化学及其发光行为。结果表明,此修饰电极表现出很好的电化学活性和电化学发光响应。基于左氧氟沙星对固定化联吡啶钌在0.1 mol/L磷酸盐缓冲液中的弱电化学发光信号有较强的增敏作用,建立了电化学发光检测盐酸左氧氟沙星的新方法。在最佳实验条件下,左氧氟沙星浓度在1.0×10-7～1.0×10-4mol/L范围内与相对发光强度呈线性关系(r2=0.998 4),检出限(S/N=3)为1.59×10-9mol/L。连续平行测定2.2×10-5mol/L的左氧氟沙星溶液10次,发光强度的相对标准偏差(RSD)为3.6%。对样品进行回收率试验,回收率在95.6%～103.5%之间,RSD(n=5)为3.0%。该方法具有较高的选择性和灵敏度,样品处理简单快速,用于盐酸左氧氟沙星的测定,结果满意。

Nano-Au/Silica sol/PVP修饰金电极上电化学发光测定盐酸硫必利

采用溶胶-凝胶法制备了Nano—Au／Silicasol／PVP修饰金电极，并基于盐酸硫必利对联吡啶钌（Ru（bpy）2/3＋）在该修饰电极上弱电化学发光具有较强的增敏作用，建立了电化学发光检测盐酸硫必利的新方法。在最佳实验条件下，盐酸硫必利浓度在1．0×10-7～1．0×0-4mol／L范围内与相对发光强度呈线性关系（r2=0．9978），检出限（S／N-3）为6．7×10-10mol／L。连续平行测定1．0×10-5mol／L盐酸硫必利溶液10次，发光强度的相对标准偏差（RSD）为1．789／6。对样品进行回收率试验，其回收率在97．7％～103．9％之间，RSD为2．62％。该方法具有较高的选择性和灵敏度，样品处理简单快速，用于盐酸硫必利的测定，结果满意。

Effect of SiO_2 concentration in silica sol on interface reaction during titanium alloy investment casting

Using silica sol as a binder for titanium investment casting is very attractive due to its good stability and reasonable cost as compared with yttrium sol and zirconium sol. However, the mechanism of interface reaction in the related system remains unclear. In this investigation, the interface reaction between Y_2O_3-SiO_2(YSi) shell mold and titanium alloys was studied. A group of shell molds were prepared by using Y_2O_3 sand and silica sol with different contents of SiO_2. Ti-6Al-4V alloy was cast under vacuum by gravity casting through cold crucible induction melting(CCIM) method. Scanning electron microscopy(SEM) and energy dispersive x-ray spectroscopy(EDS) were employed to characterize the micromorphology and composition of the reaction area, respectively X-ray photoelectron spectroscopy(XPS) was used to confirm the valence state of relevant elements. White ligh interferometer(WLI) was used to obtain the surface topography of Y-Si shells. The results show that the thickness of reaction layers is below 3 μm when the SiO_2 content of silica sol is below 20 wt.%. Whereas, when the SiO_2 content increases to 25 wt.%, the thickness of the reaction layer increases sharply to about 15 μm. There is a good balance between chemical inertness and mechanical performance when the SiO_2 content is between 15 and 20 wt.%. Moreover, it was found that the distribution of SiO_2 and the roughness at the surface of the shell are the key factors that determine the level of reaction.

Preparation and Characterization of Hybrid Aqueous Dispersions Composed of Silica Sol and Poly(styrene-co-acrylate)

A stable silica sol with 3-5 nm in diameter, which can form homogeneous film without crack, was prepared and characterized. Then, the inorganic-organic hybrid aqueous dispersion composed of such a silica sol and an emulsion of styrene （St） and acrylate （Ac） copolymer was prepared and the hybrid effect between the silica sol and poly（St-co-Ac） was observed by Fourier transform infra-red （FT-IR） spectroscope. The toughness of the film prepared by this kind of hybrid aqueous dispersion was excellent, as it was enhanced appreciably by commixing with a small amount of poly（St-co-Ac） emulsion. Some amino-polysiloxane modified hybrid aqueous dispersions were also prepared and the properties of the modified dispersions and their films were investigated. The experimental results showed that the film prepared with such an amino-polysiloxane modified hybrid dispersion exhibited excellent hydrophobicity and low surface energy after heat treatment for 1.5 h, during which the formation of the graft copolymer was observed. The surface energy of this film decreases as a result of the enrichment of siloxane segments on the film surface.

Research on New Silica Sol Matrix Used in Fluid Catalytic Cracking Reaction

A new silica sol binder was obtained by mixing the acid-modified aluminium sulfate and water glass. The effect of SiO2 concentration in sodium silicate, pH value and polymerization was investigated. The new silica sol binder, which possessed abundant pore volume and suitable acid amount, was an ideal component for preparing cracking catalyst. As a result, the corresponding catalyst comprising the new binder showed excellent performance. Compared with the reference sample, the liquefied petroleum gas(LPG) and propylene yield obtained over this catalyst increased by 3.49 and 1.20 percentage points, respectively. The perfect pore structure and suitable Lewis acid amount of new silica sol were the possible reason leading to its outstanding performance.

Application of Vacuum Drying to Silica Sol Ceramic Mold

Silica sol ceramic mold was made at room temperature with JN-30 silica sol, silica powder and NH4Cl. It is found that the harden time of silica sol ceramic mold is only 0.5 to 1.5 h under the amount of NH4Cl solution of 7% to 8% with 15% concentration, and less surface cracks occur by using vacuum drying. The proper vacuum drying process parameters： vacuum drying temperature is 80 to 100℃, drying time is 5 h and vacuum is 0.06 to 0.07MPa. The harden mechanics, vacuum drying mechanics and the reason of less surface cracks of silica sol ceramic mold by vacuum drying： were also analyzed in this paper.

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.

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.

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.

Effects of Silica Sol on Structure and Properties of Core-Shell Silicon-Acrylic Materials

Silica sol prepared by sol-gel method was introduced into poly (butyl acrylate) (PBA)/poly (butyl acrylate-styrene-methacryloxypropyl trimethoxysilane) (PSBM) core-shell emulsions to prepare a series of paper surface sizing agents. The rheological measurement indicated that PSBM emulsions exhibited shear-thinning behavior, and the phenomena became more pronounced with increasing silica sol concentration. Dynamic mechanical analysis (DMA) demonstrated that the stronger interfacial interaction between silica sol and polymer matrix, but microphase separation took place with excess silica sol. Thereby the tensile strength and thermal stability of emulsion films were increased with desirable silica sol concentration, and when silica sol concentration was greater than 6 wt%, the tensile strength leveled off and the decomposition temperature decreased from 351.19℃ to 331.63℃. The degree of crystallinity increased from 5.12% to 10.98% with 4% silica sol addition, resulting in enhanced rigidity of films. Furthermore, the interaction between polymer and fiber was improved with certain amount of silica sol, resulting in improved sizing degree, ring crush strength, surface strength and folding strength. However, excessive crosslinking will be harmful for the properties of sized paper.

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.

Preparation and characterization of silica microcapsules containing butyl-stearate via sol-gel method

For thermal energy storage application in energy-saving building materials,silica microcapsules containing phase change material were prepared using sol-gel method in O/W emulsion system. In the system droplets in microns are formed by emulsifying an organic phase consisting of butyl-stearate as core material. The silica shell was formed via hydrolysis and condensation from tetraethyl silicate with acetate as catalyst. The SEM photographs show the particles possess spherical morphology and core-shell structure. The as-prepared silica microcapsules mainly consist of microsphere in the diameter of 3-7 μm and the median diameter of these microcapsules equals to 5.2 μm. The differential scanning calorimetry(DSC) curves indicate that the latent heat and the melting point of microcapsules are 86 J/g and 22.6 ℃,respectively. The results of DSC and TG further testify the microcapsules with core-shell structure.

STUDIES ON SYNTHESIS OF SILICA SOL-ORGANIC POLYMER COMPOSITE EMULSION

An emulsion of polystyrene/poly (butylacrylate-methyl methacrylate acrylic acid) core/shell latex particles (PS/P (BA-MMA-AA)) has been prepared by use of three synthetic methods. The effects of synthetic methods on the distribution of carboxyl groups in latex particles were studied. The results show that the seed emulsion polymerization in which the pre-emulsified monomers were added by dropping method to the second stage is the best technique for obtaining the optimum distribution of carboxyl groups on the surface of the latex particles. Furthermore, by using PS/P (BA-MMA-AA), a type of novel composite emulsion of silica sol-PS/P (BA-MMA-AA) was synthesized with the above method. By observation through transmission EM, the morphology of the latex particles obtained shows that a composite structure has been formed between silica sol particles and organic polymer particles.

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.

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.

The preparation of high concentration alkaline silica sol with the method of vacuum distillation

High concentration alkaline silica sol has been prepared by the method of vacuum distillation, which shows that the stable and high concentration silica sol can be obtained under conditions as follows： 70℃, vacuum degree of 0.095Mpa and dispersant of SDS. The experimental results show that the sol particles size decreases with mass concentration first and then increase, sol viscosity increases with mass concentration during the concentrating process. The TEM method was used to study the dispersion behavior of sol particles, its result showed that sol particles dispersed more uniformly after concentrating process than before concentrating distinctly. It could be concluded that the disperse degree of alkaline silica sol could be increased by addition of right dispersant. The dispersion mechanism of dispersant in alkaline silica sol was also discussed.

Preparation of Magnesia Insulation Materials by Walnut Shell Powder Impregnated with Silica Sol

In order to reduce the thermal energy loss of high temperature kilns and furnaces and lower the surface temperature of the kiln body,magnesia insulation materials were prepared using self-made magnesia porous aggregates(using high purity magnesia powder as starting material and potassium oleate as the foaming agent),middle grade magnesia powder,calcium aluminate cement,and SiO_(2) micropowder as starting materials,introducing walnut shell powder impregnated with silica sol(short for Sws)as a pore-forming agent.The effects of the Sws addition(0,10%,15%,and 20%,by mass)and the sintering temperature(1300,1350,1400,and 1480℃)on the properties of magnesia insulation materials were studied.The results show that(1)for the specimens fired at 1480℃,when the Sws addition is 10%,the cold compressive strength is 22 MPa;when the Sws addition is 20%,the thermal conductivity is 0.368 W·m^(-1)·K^(-1)(350℃);(2)nano-silica in the silica sol reacts with MgO in the matrix to form forsterite,which encapsulates the pores volatilized from the walnut shell powder and forms closed pores.

APPLICATION OF BORON MODIFIED SILICA SOL ON RETENTION AND DRAINAGE

In this paper it was studied that these dosage effects of CPAM, cationic starch?boron modified silica sol(BMS), Al2(SO4)3, pH value and electrolyte on the retention and drainage of different microparticulate systems including CPAM, cationic starch and boron silica sol. The research results indicated that CPAM had no good retention when used with boron silica sol. The best retention efficiency was the microparticulate system of CPAM + cationic starch with boron modified silica sol; Secondly was that of cationic starch with boron modified silica sol; The worst was that of CPAM with boron modified silica sol. The retention efficiency had no relation with the addition order between CPAM and cationic starch. It was also found that the microparticulate retention system of boron modified silica sol could be used in alum-rosin sizing and in acidity, neutral or alkaline papermaking conditions. This system also could be used with close circulate water so that it could reduce the water pollution and waste.

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.