Preparation and characterization of mesoporous silica thin films from polyethoxysiloxanes

Tetraethoxysilane (TEOS) and polyethoxysiloxanes (PEOSs; prepared by the acid‐catalyzed hydrolytic polycondensation of TEOS) were subjected to the sol–gel process in the presence of cetyltrimethylammonium bromide (CTAB), respectively. The PEOSs with M_w 700–26,000, as prepared by sol–gel coating of TEOS and PEOS under various conditions, were used. Uniform and crack‐free thin films of thickness 276–613 nm were prepared by spin‐coating of a PEOS solution containing CTAB. When the coating films were sintered at 400 °C, the combustion of ethoxy groups and CTAB took place to provide porous silica thin films. The structure of the thin films was found to be dependent on the molecular weight of PEOS and the molar ratio of CTAB/Si: lamellar or hexagonal phase was observed for M_w less than 15,000 and for CTAB/Si molar ratios greater than 0.10. Honeycomb structures were observed for M_w less than 5000 and for CTAB/Si molar ratios of 0.15. The honeycomb structure was also observed by atomic force microscopy and transmission electron microscope. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 2542–2550, 2006     

On the origin of 1.5 μm luminescence in porous silicon coated with sol–gel derived erbium-doped Fe2O3 films

Sol–gel derived Fe₂O₃ films containing about 10 wt% of Er₂O₃ were deposited on porous silicon by dipping or by a spin-on technique followed by thermal processing at 1073 K for 15 min. The samples were characterized by means of PL, SEM and X-ray diffraction analyses. They exhibit strong room-temperature luminescence at 1.5 μm related to erbium in the sol–gel derived host. The luminescence intensity increases by a factor of 1000 when the samples are cooled from 300 to 4.2 K. After complete removal of the erbium-doped film by etching and partial etching the porous silicon, the erbium-related luminescence disappears. Following this, luminescence at 1.5 μm originating from optically active dislocations (“D-lines”) in porous silicon was detected. The influence of the conditions of synthesis on luminescence at 1.5 μm is discussed.     

钢中Si、Mn的电子探针定量分析与标样

采用特制的Fe-Si、Fe-Mn合金系列标样，用电子探针测定了钢或铁基合金中低含量的Si和Mn元素、与用纯元素作标样、经ZAF修正的结果相比较，提高了分析准确度．     

Elimination of matrix effects for headspace solid-phase microextraction of important volatile compounds in red wine using a novel coating

In this paper, hydroxy-terminated silicone oil-butyl methacrylate-divinylbenzene (OH-TSO-BMA-DVB) copolymer was first synthesized and used as stationary phase with the aid of γ-methacryloxypropyltrimethoxylsilane (KH-570) as bridge in solid-phase microextraction (SPME) using sol–gel method and cross-linking technique. It has high extraction efficiency for both polar alcohols and fatty acids and nonpolar esters in comparison with commercial PDMS, PDMS-DVB and PA fibers. A simple and sensitive headspace SPME-gas chromatography (HS-SPME-GC) method using the novel fiber was presented for the simultaneous analysis of both polar alcohols and fatty acids and nonpolar esters in wine. To check the matrix effects, various model wine matrices, including distilled water; 11.5% ethanol/water (v/v) solution; a concentrated synthetic wine; a ‘volatile-free’ wine and a real wine were investigated in detail. Matrix effects were compensated for by using internal standard method and selecting the ‘volatile-free’ wine as working standard. The method presented in this study showed satisfactory linearity, precision, detection limits and accuracy. The recoveries obtained ranged from 85.87 to 104.2%, and the relative standard deviation values were below 9%. The results obtained indicated that the present method is a validated and accurate procedure for the simultaneous determination of both polar and nonpolar aroma compounds in wine.     

Immobilization of thiabendazole-specific monoclonal antibodies to silicon substrates via aqueous silanization

Monoclonal antibodies specific for thiabendazole were immobilized to silicon, silicon dioxide, stoichiometric silicon nitride, and silicon-rich silicon nitride surfaces. This work provides the foundation for the development of a homogeneous sensor system for rapid detection and quantification of thiabendazole residues in produce and animal tissue. Immobilization was performed via aqueous silanization of the substrate followed sequentially by treatment with glutaraldehyde and contact with antibody solution in the presence of detergent. Surfaces were challenged with thiabendazole-horseradish peroxidase conjugate in an ELISA format to estimate immobilized antibody load. A stable and reproducible surface loading of 2 x 10¹¹ antibodies/cm² was obtained only after surfaces received postimmobilization treatments to remove nonspecifically adsorbed antibody. No difference in surface loading was noted when using 30% hydrogen peroxide rather than nitric acid for silanol activation. Little difference was noted among the antibody loadings achieved on the various silicon substrates. Bound antigen-enzyme conjugate was eluted with 0.1N acetic acid and reproducible surface activity was measured for up to four consecutive antigen challenges. Immobilized antibody surfaces were stabilized with 2% sucrose, dehydrated at 37‡C and stored in vacuum or stored at 4‡C in phosphate buffered saline containing 0.01% sodium azide without significant loss of activity.     

多孔硅的电化学制备

单晶硅在氢氟酸溶液中阳极氧化可制得多孔硅, 多孔硅是一种以新形态存在的硅, 与单晶硅相比, 它表现出独特的物理性质和化学活性。荧光光谱峰的蓝移表明, 在p-型低掺杂衬底硅上形成的多孔硅中存在量子尺寸效应, 新近获得的Raman光谱也证实了这一点。     

高效液相色谱法所用大孔硅胶填料的制备

对国产ＧＹＱＧ球形硅胶施加高压水热处理并进行扩孔，制备了用于高效液相色谱法的大孔硅胶填料，考察了扩孔压力，扩孔温度和扩孔时间对平均孔径和比表面积的影响。并将产品日本ＳＩＬ－３００３×１０＾－８ｍ硅胶进行了物理性质和孔分布的对比实验，结果表明ＧＹＱＧ硅胶扩孔后平均孔径为２０～３０ｎｍ接近日本ＳＩＬ－３００３×１０＾－８ｍ硅前平平均孔径２５ｎｍ。display structure     

XPS,AFM, ATR and TPD evidence for terraced,dihydrogen terminated, 1×1 (100) silicon

Heating (100) silicon at high temperature (say, higher than 850 °C) in H₂, cooling to 670–700 °C in the same ambient, and quenching to room temperature in N₂ results in environmentally robust, terraced 1 × 1 (100) SiH₂. Evidence for this conclusion is based on angle‐resolved x‐ray photoelectron spectroscopy, atomic force microscopy, infrared absorption spectroscopy in the attenuated total reflection mode, thermal programmed desorption, and reflection high‐energy electron diffraction. Copyright © 2005 John Wiley & Sons, Ltd.