巯基表面修饰磁性复合纳米粒子用于重金属离子去除的研究

采用化学共沉淀法合成磁性Fe3O4纳米粒子,并且利用正硅酸乙酯（TEOS）的水解和凝聚作用在Fe3O4纳米粒子表面沉积包覆一层SiO2,合成核壳式的Fe3O4@SiO2复合纳米粒子。以Fe3O4@SiO2纳米粒子为基体,将（3-巯基丙基）三乙氧基硅烷嫁接到纳米粒子表面,制备出巯基功能化的纳米材料,将其应用于对重金属离子...     

含叔胺结构可聚合纳米SiO2杂化粒子的制备及其光固化性能

用3-氨丙基三乙氧基硅烷对纳米SiO2行表面修饰,并与三羟甲基丙烷三丙烯酸酯进行Micheal 加成反应制备含叔胺结构的可聚合纳米SiO2杂化粒子.FT-IR和TGA分析表明:含叔胺结构的有机化合物接枝到了纳米SiO2表面,接枝率为22.6%.将其应用于光固化涂料中,纳米SiO2杂化粒子在涂料中分散均匀,可克服涂料光固...     

纳米硅溶胶、苯丙复合乳液的合成及性能研究

自制纳米SiO2溶胶,用硅烷偶联剂(乙烯基三乙氧基硅烷)进行表面处理,然后合成以纳米SiO2溶胶为核,聚苯乙烯、丙烯酸酯为壳的无机-有机复合乳液。结果表明,复合乳液制成的凃膜的力学性能及耐水性都得到了提高笛榛寡芯苛嗽谖藁⒘4嬖谙?苯丙乳液聚合的工艺条件。     

纳米SiO2/聚丙烯酸酯复合乳液的制备及应用

将经正硅酸乙酯原位水解形成的纳米SiO2引入到丙烯酸酯乳液合成过程中,可制备具有互穿网络结构的纳米SiO2／聚丙烯酸酯复合乳液。将复合乳液配入到市售的硅丙乳液中制备了水性涂料,并表征了复合乳液涂膜和涂料的性能。结果表明,复合乳液涂膜的表面性能和热稳定性能均优于普通的丙烯酸酯类乳液;加入部分合成的复合乳液制备的涂料,可显著提高其耐候性与耐污性。     

紫外辐照对EVOH/纳米SiO2复合材料性能的影响

用硅烷偶联剂y-氨丙基三乙氧基硅烷（KH550）对纳米SiO2进行改性,采用熔融共混法制备了合SiO2的质量分数为5％的乙烯-乙烯醇共聚物（EVOH）／纳米SiO2复合材料,并吹塑成薄膜,将复合膜进行不同时间、不同强度的紫外辐照处理。利用FTIR、TEM、SEM对纳米SiO2和复合材料进行了表征分析,测试了复合材料紫外辐照处理前后的阻隔性能和力学性能。结果表明：纳米SiO2与偶联剂KH550形成化学键合,经紫外辐照处理的EVOH／纳米SiO2复合膜的力学性能、阻隔性能得到了较大地提高。     

羟基封端的有机硅低聚物的合成

采用甲基三乙氧基硅烷,二甲基二乙氧基硅烷,苯基三乙氧基硅烷为原料,通过水解-缩合反应合成一种羟基封端的有机硅低聚物,并初步研究了有机硅低聚物的合成条件。实验表明:反应温度为70℃,时间为4h,pH为3,可合成羟基封端的有机硅低聚物。红外光谱表明,合成的有机硅低聚物在Si-OC2H5及Si-O-Si处都出现吸收峰,其结构与理论基本相符。     

溶胶-凝胶法制备可溶性聚酰亚胺/二氧化硅纳米复合材料的研究──Ⅰ.溶胶一凝胶转变过程和反应机理的研究

选取可溶性聚酰亚胺（PI）作为有机高聚物基体．通过正硅酸四乙酯（TEOS）在聚酰胺酸（PAA的N-甲基-2-吡咯烷酮（NMP）溶液中进行溶胶-凝胶反应．制备出新型的聚酰亚胺／二氧化硅（PI／SiO2）纳米复合材料。并用UV－Vis、XPS、IR和SEM等方法对其溶胶-凝胶转变过程和水解-缩合反应机理进行了研究。结果表明,在水解-缩合反应过程中,TEOS与聚酰胺酸发生反应,生成较为稳定的中间产物;在高温亚胺化的同时完成溶胶-凝胶转变,原位（in－situ）生成SiO2凝胶网络,最终制得PI／SiO2纳米复合材料。     

改性纳米SiO2/环氧树脂涂料的制备及其性能

为提高纳米SiO2在环氧树脂中的分散程度,充分发挥纳米SiO2的力学性能和耐热性,采用乙烯基三乙氧基硅烷与丙烯酸对纳米SiO2表面进行接枝改性,利用红外光谱对改性纳米SiO2的结构进行了表征;将改性纳米SiO2添加到环氧树脂中混合固化,得到改性纳米SiO2/环氧树脂复合涂料(SAE),并通过附着力、吸水率、电化学试验等方法对SAE涂层的耐蚀性能进行了评价。结果表明:改性后的纳米SiO2出现新的吸收峰;SAE具有附着力高、抗渗透性强、极化电流小等优良的耐腐蚀性能。     

硅烷偶联剂在PPy/SiO2纳米导电复合材料制备中的应用

描述了一种合成PPy／SiO2纳米复合材料的新方法。首先用不同百分含量的氨丙基三乙氧基硅烷(APS)处理SiO2,然后通过化学氧化聚合法合成PPy／APS—SiO2纳米复合材料。文中讨论了偶联剂的使用对复合材料的影响及其作用机理。结果表明,用APS处理过的SiO2合成的复合材料其PPy含量、电导率和稳定性都有很大提高,其中用1％APS—SiO2合成的复合材料电导率最高,为38．4S／cm。文中还阐述了偶联剂的预处理对PPy／SiO2纳米复合材料形貌的影响。     

聚合物改性SiO_2气凝胶的常压干燥制备及表征

以TEOS（四乙氧基硅烷）和APTES（3-氨丙基三乙氧基硅烷）共缩聚制备SiO2凝胶后采用N3200（1,6-环己烷二异氰酸酯低聚物）对其改性,经常压干燥制备了聚合物改性SiO2气凝胶。采用TGA、N2吸附-脱附、SEM和单轴抗压实验等测试方法对所制备的气凝胶进行了表征。结果表明：随气凝胶中聚合物含量的增加,气凝胶制...     

Sol-gel coating technology for the preparation of solid-phase microextraction fibers of enhanced thermal stability

A novel sol-gel method is described for the preparation of solid-phase microextraction (SPME) fibers. The protective polyimide coating was removed from a 1-cm end segment of a 200 μm o.d. fused-silica fiber, and the exposed outer surface was coated with a bonded sol-gel layer of poly(dimethylsiloxane) (PDMS). The chemistry behind this coating technique is presented. Efficient SPME-GC analyses of polycyclic aromatic hydrocarbons, alkanes, aniline derivatives, alcohols, and phenolic compounds in dilute aqueous solutions were achieved using sol-gel-coated PDMS fibers. The extracted analytes were transferred to a GC injector using an in-house-designed SPME syringe that also allowed for easy change of SPME fibers. Electron microscopy experiments suggested a porous structure for the sol-gel coating with a thickness of ～10 μm. The coating porosity provided higher surface area and allowed for the use of thinner coatings (compared with 100-μm-thick coatings for conventional SPME fibers) to achieve acceptable stationary-phase loadings and sample capacities. Enhanced surface area of sol-gel coatings, in turn, provided efficient analyte extraction rates from solution. Experimental results on thermal stability of sol-gel PDMS fibers were compared with those for commercial 100-μm PDMS fibers. Our findings suggest that sol-gel PDMS fibers possess significantly higher thermal stability (>320 °C) than conventionally coated PDMS fibers that often start bleeding at 200 °C. This is due, in part, to the strong chemical bonding between the sol-gel-generated organic-inorganic composite coating and the silica surface. Enhanced thermal stability allowed the use of higher injection port temperatures for efficient desorption of less-volatile analytes and should translate into extended range of analytes that can be handled by SPME-GC techniques. Experimental evidence is provided that supports the operational advantages of sol-gel coatings in SPME-GC analysis.     

Solid-phase microextraction using fused-silica fibers coated with sol-gel-derived hydroxy-crown ether

A novel solid-phase microextraction (SPME) fiber containing hydroxydibenzo-14-crown-4 (OH-DB14C4)/hydroxy-terminated silicone oil (OH-TSO) was first prepared by a sol-gel method and investigated for the determination of phenols. The possible mechanism is discussed and confirmed by IR spectra. The coating has stable performance in high temperature (to 350 degrees C) and solvents (organic and inorganic) due to the chemical binding between the coating and the fiber surface. The addition of crown ether enhances the polarity of the coating compared with that of the sol-gel OH-terminated silicone oil fiber and, accordingly, provides higher extraction efficiency for polar phenolic compounds. On the other hand, OH-terminated silicone oil in the coating can not only increase the length of network but also help to spread the stationary phase on the silica surface uniformly. The fluorescence microscopy experiment suggests the benefit the more uniform surface of the sol-gel-derived OHDB14C4/OH-TSO fiber in comparison with sol-gelderived OH-DB14C4 fiber. Some parameters of the SPME fiber for the determination of phenols were investigated. Limits of detection of the phenols are below 1.0 ng/mL, and the precisions are from 2.9 to 4.6% (n = 6). Linear ranges were found to be 0.1-10 microg/mL The sensitivity of the method is enhanced at a low-pH level (pH approximately 1) and with the addition of salt. The method was applied to the analysis of wastewater sample from a paper mill.     

Sol-gel poly(ethylene glycol) stationary phase for high-resolution capillary gas chromatography

A sol-gel chemistry-based method was developed for the preparation of highly stable capillary gas chromatography (GC) columns with surface-bonded poly(ethylene glycol) (PEG) stationary phase. Through a single-step procedure, it concurrently provided column deactivation, stationary-phase coating, and chemical immobilization of the coated film. Sol-gel reactions were carried out within fused-silica capillaries that were filled with properly designed sol solutions containing two sol-gel precursors, two different triethoxysilyl-derivatized poly(ethylene glycol)s, two sol-gel catalysts, and a deactivation reagent. Hydrolytic polycondensation reactions led to the formation of a sol-gel coating chemically bonded to the inner walls of the capillary. A number of sol-gel coated fused-silica capillary columns were prepared using sol-gel-active PEG derivatives. These columns demonstrated many inherent advantages, the main being the strong anchoring of the coating to the capillary wall resulting from chemical bonding with the silanol groups on the fused-silica capillary inner surface. This chemical bonding yielded strongly immobilized PEG coatings with outstanding thermal stability (up to 320 degrees C). To our knowledge, such a high thermal stability has not been achieved so far on conventionally prepared PEG GC columns. Sol-gel PEG columns provided excellent chromatographic performances: high number of theoretical plates, excellent run-to-run and column-to-column reproducibility, and pronounced selectivity for a wide range of test solutes. Using n-octadecane as a test solute (k = 7.14), an efficiency value of 3200 theoretical plates/m was obtained on a 10 m x 0.25 mm i.d. fused-silica capillary column. Five sol-gel PEG columns provided RSD values of 1.09% for column efficiency (solute, n-octadecane), 1.37% for retention factor (solute, n-octadecane), and 0.9% for separation factor (for solute pair o- and p-xylene). In five replicate measurements using the same column, RSD values of less than 0.50% for the retention time and 1.36% for retention factor (k) were obtained.     

Al/SiC composite coatings of steels by thermal spraying

Thermal spraying has been used to coat carbon steels (F112) and austenitic stainless steels (AISI 304) with aluminium matrix composites. Mixtures of aluminium powder and SiC particles were used as spraying material. A sol-gel silica coating was laid on SiC particles to reduce the porosity of the composite coatings and to inhibit the formation of aluminium carbide. The sol-gel silica coating acts as an active barrier enhancing the wettability of the reinforcement by molten aluminium. Coatings with a reinforcement volume fraction up to 30 vol.% were obtained with porosities of about 1.0 vol.%. The incorporation of sol-gel silica coated SiC particles reduces the coefficient of thermal expansion of the composite coating and enhances its adhesion to the substrates more than when uncoated SiC particles were used.     

用溶胶-凝胶法制备保护涂层的研究进展

溶胶-凝胶(Sol-gel)法用于金属及合金表面制备保护涂层可明显提高材料在各种环境下的耐蚀性、抗高温氧化性、耐磨性等性能,从而扩大金属及其合金的应用范围.介绍了Sol-gel涂层的制备技术、涂覆工艺以及涂层热处理的一般原理及特点,总结了该技术制备保护涂层的应用现状及最新研究进展,讨论了制备单组分氧化物涂层如ZrO2涂层、SiO2涂层、CeO2涂层、Al2O3涂层、TiO2涂层,双组分氧化物涂层如ZrO2-CeO2涂层、SiO2-ZrO2涂层以及多组分氧化物涂层的制备方法及涂层对基体材料的保护作用,并对其保护机理进行了初步探讨.     

Positively charged sol-gel coatings for on-line preconcentration of amino acids in capillary electrophoresis

A novel on-line method is presented for the extraction and preconcentration of amino acids using a sol-gel-coated column coupled to a conventional UV/visible detector. The presented approach does not require any additional modification of the commercially available standard CE instrument. Extraction, stacking, and focusing techniques were used in the preconcentration procedures. Sol-gel coatings were created by using N-octadecyldimethyl[3-(trimethoxysilyl)propyl]ammonium chloride (C18-TMS) in the coating sol solutions. Due to the presence of a positively charged quaternary ammonium moiety in C18-TMS, the resulting sol-gel coating carried a positive charge. For extraction, the pH of the samples was properly adjusted to impart a net negative charge to amino acids. A long plug of the sample was then passed through the sol-gel-coated capillary to facilitate extraction via electrostatic interaction between the positively charged sol-gel coating and the negatively charged amino acid molecules. Focusing of the extracted amino acids was accomplished through desorption of the extracted amino acid molecules carried out by local pH change. Two different methods are described. Both methods showed excellent extraction and preconcentration effects. Preconcentration results obtained on sol-gel-coated columns were compared with the CZE analysis performed on bare fused-silica columns with traditional sample injections. The described procedure provided a 150,000-fold enrichment effect for alanine. The two methods provided acceptable repeatability in terms of both peak height and migration time.     

Effect of TiO2-SiO2 sol-gel coating on the cpTi-porcelain bond strength

The effects of TiO₂-SiO₂ sol-gel coating with different firing temperatures (300 °C, 500 °C, and 750 °C) on the cpTi-porcelain bond strength were investigated in the present study. Prior to applying the low-fusing dental titanium porcelain, the phase, surface morphology, surface roughness and static water contact angle of the intermediate layer were evaluated. The cpTi-porcelain bond strength was measured using the three-point flexure test according to ISO 9693 standard. Statistical analyses were made using one-way ANOVA and Dunnett-t test. Significantly higher bond strength of TiO₂-SiO₂/750 °C (specimens coated with TiO₂-SiO₂ sol-gel coating and fired at 750 °C for 1 h) when compared to the control group was observed (p < 0.05). No rutile phase was found in all the tested specimens coated with TiO₂-SiO₂ sol-gel coating. The surface morphology of the intermediate layer was apparently different with different firing temperatures. It was found that the static water contact angle of TiO₂-SiO₂/750 °C significantly decreased (p < 0.05). However, no markedly different R_a of TiO₂-SiO₂/500 °C and TiO₂-SiO₂/750 °C in comparison to that of the control group was observed (p > 0.05). The results show that the TiO₂-SiO₂ sol-gel coating fired at 750 °C for 1 h can notably improve the cpTi-porcelain bond strength and may be suitable for clinical use.     

Direct coating of bioactive sol-gel derived silica on poly(ε-caprolactone) nanofibrous scaffold using co-electrospinning

This study reports a novel way of directly coating a poly(ε-caprolactone) (PCL) nanofibrous scaffold with bioactive sol-gel derived silica by directly co-electrospinning (Co-ES) a PCL solution and silica sol, used as the core and shell materials, respectively. In particular, the silica sols prepared using a sol-gel process at room temperature were heat-treated at 60 °C for various times, ranging from 0 to 9 h, in order to improve their spinability. The surface of the individual PCL nanofibers could be covered completely with a bioactive silica layer using a silica sol heat-treated at 60 °C for more than 6 h, whilst preserving the nanofibrous structure. Fourier-transform infrared spectroscopy (FT-IR) revealed only the characteristic bands associated with the PCL and sol-gel derived silica materials without any noticeable band shift.     

Hardness recovery of ceramic coated aluminium matrix composites using thermal-shock resistant sol-gel silica coatings

Sol-gel silica coatings increase wear and corrosion resistance of aluminium matrix composites, but a heat treatment stage at temperatures as high as 500 °C is usually required to consolidate the ceramic coating. Under these thermal conditions, sol-gel ceramic coatings tend to crack and the aluminium matrix hardness strongly reduces. Present paper describes how the combination of a certain sol-gel procedure accompanied with quenching treatment in silicone oil allows recovering most of the hardness of the substrate, while keeping undamaged the sol-gel silica coating deposited.     

The microwave effect on the properties of silica-coated TiO2 fine particles prepared using sol-gel method

The silica coating of TiO₂ fine particle was conducted using microwave assisted sol-gel method and conventional sol-gel method to suppress its photo-catalytic activity. The amount and uniformity of silica coating on TiO₂ surface were characterized by X-ray photoelectron spectroscopy (XPS), X-ray fluorescence spectroscopy (XRF), infrared spectroscopy (IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and zeta potential measurements. XPS and XRF results showed that the presence of catalyst and reaction time were important factors to reach high silica amounts. SEM, TEM, and zeta potential results indicated that dense film coating of SiO₂ layer formed on TiO₂ surface in conventional sol-gel method, whereas the nucleation coating was observed on sample prepared by microwave assisted sol-gel method. When photo-catalytic activities and ultraviolet (UV) shielding abilities of these samples were evaluated, the sample prepared by microwave processing showed higher inhibition of photo-catalytic activity and better UV shielding ability than the sample prepared by conventional method. These results suggested that the coating method significantly affected the photo-catalytic activity and UV shielding ability of coated TiO₂.