New Process for the Preparation of Monodispersed, Spherical Silica Particles

A new method is presented for preparing highly monodispersed silica particles using a two-stage semibatch/batch hydrolysis reaction of Si(OC₂H₅)₄. The slower rate of hydrolysis of the tetraethylorthosilicate (TEOS) that occurred during the semibatch process resulted in larger silica particles with a higher yield and narrower size distribution. This was in direct contrast to the batch process. In addition, the ability of four different mixed processes to produce silica particles with good packing density, narrower particle-size distribution, and higher yield were evaluated. These were batch/batch (B-B), batch/semibatch (B-S), semibatch/batch (S-B), and semibatch/semibatch (S-S) processes. The S-S system produced the largest particles with the highest yields. The size of the silica particles obtained by the S-B method decreased with increasing reaction time, while the particles obtained by the B-S process had the best particle-size distribution and packing density. In conclusion, a mixed batch/semibatch system was the best way to produce an extremely narrow particle-size distribution and a good packing density.     

Cycling of lithium/metal oxide cells using composite electrolytes containing fumed silicas

The effect on cycle capacity is reported of cathode material (metal oxide, carbon, and current collector) in lithium/metal oxide cells cycled with fumed silica-based composite electrolytes. Three types of electrolytes are compared: filler-free electrolyte consisting of methyl-terminated poly(ethylene glycol) oligomer (PEGdm, M_w=250)+lithium bis(trifluromethylsufonyl)imide (LiTFSI) (Li:O=1:20), and two composite systems of the above baseline liquid electrolyte containing 10-wt% A200 (hydrophilic fumed silica) or R805 (hydrophobic fumed silica with octyl surface group). The composite electrolytes are solid-like gels. Three cathode active materials (LiCoO₂, V₆O₁₃, and Li_xMnO₂), four conducting carbons (graphite Timrex® SFG 15, SFG 44, carbon black Vulcan XC72R, and Ketjenblack EC-600JD), and three current collector materials (Al, Ni, and carbon fiber) were studied. Cells with composite electrolytes show higher capacity, reduced capacity fade, and less cell polarization than those with filler-free electrolyte. Among the three active materials studied, V₆O₁₃ cathodes deliver the highest capacity and Li_xMnO₂ cathodes render the best capacity retention. Discharge capacity of Li/LiCoO₂ cells is affected greatly by cathode carbon type, and the capacity decreases in the order of Ketjenblack>SFG 15>SFG 44>Vulcan. Current collector material also plays a significant role in cell cycling performance. Lithium/vanadium oxide (V₆O₁₃) cells deliver increased capacity using Ni foil and carbon fiber current collectors in comparison to an Al foil current collector.     

Mn2+在Zn2SiO4中的发光

利用Sol-gel法制备掺Mn^2 的Zn2SiO4的前驱体，并将前躯体在弱氧化气氛下在1000℃煅烧2h，得到掺Mn^2 的Zn2SiO4试样。X射线衍射分析确定试样为α-Zn2SiO4晶相。荧光分析测定试样的激发光谱和发射光谱。结果显示Mn^2 掺杂的α-Zn2SiO4可发蓝色和绿色荧光，这一结果显然不同于以前的文献报道。同时，我们讨论了Mn^2 在Zn2SiO4中产生这一新型发光性质的机理。     

Superfine structure,physical properties,and dyeability of alkaline hydrolyzed soly(ethylene terephthalate)/silica nanocomposite fibers prepared by in situ polymerization

In this study, poly(ethylene terephthalate) (PET)/SiO₂ nanocomposites were synthesized by in situ polymerization and melt‐spun to fibers. The superfine structure, physical properties, and dyeability of alkaline hydrolyzed PET/SiO₂ nanocomposite fibers were studied. According to the TEM, SiO₂ nanoparticles were well dispersed in the PET matrix at a size level of 10–20 nm. PET/SiO₂ nanocomposite fibers were treated with aqueous solution of sodium hydroxide and cetyltrimethyl ammonium bromide at 100°C for different time. The differences in the alkaline hydrolysis mechanism between pure PET and PET/SiO₂ nanocomposite fibers were preliminarily investigated, which were evaluated in terms of the weight loss, tensile strength, specific surface area, as well as disperse dye uptake. PET/SiO₂ nanocomposite fibers showed a greater degree of weight loss as compared with that of pure PET fibers. More and tougher superfine structures, such as cracks, craters, and cavities, were introduced, which would facilitate the certain application like deep dyeing. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 3691–3697, 2006     

Order Distance Estimation in Porous Glasses via Transformed Correlation Function of Small-Angle Scattering

A mesoporous two-phase system, consisting of colloidal silica in the cavities of the main silica frame work of a macroporous glass, was investigated by use of Small-Angle X-ray scattering. The transformed correlation function _T(r) was determined for this material for distances r<40 nm. The application of the intrinsic properties of _T(r) yields estimations for two fundamental order distances L ₁=11 nm and L ₂=120 nm of the~porous glass possessing a clear geometric interpretation: L ₁, a short-order-range, is the mean chord length of the mesopores plus the mean chord length in the secondary particles. L ₂, a long-order-range, is an estimation of the mean diameter of a macropore plus the mean free distance in the silica framework which separates two nearly parallel segments of two adjacent macropores.     

Sintering of Confined Silica in Oxidized Silicon Particles

We observed electron-beam-induced sintering of amorphous silica in oxidized submicrometer silicon particles and analyzed the nature of mass transport in linear and triangular particle assemblies. The movement of silica around the rigid crystalline cores occurs rapidly and fills the necks, but the relative core positions in the sintered product depends on the initial geometry of the confined oxide. However, a thin layer of silica remains stable against the flow.     

The Effects of Phenyltrimethoxysilane Coupling Agents on the Properties of PTFE/Silica Composites

A study on PTFE reinforced with SiO₂ was described. This study included the manufactural process of SiO₂-reinforced PTFE and the effects of the content of silane (Z6124) on the properties of the composites material, such as thermal, dielectric properties, tensile strength and morphology, etc. PTFE/silica composites of 60 wt% SiO₂ loaded with a different coupling agent content were mixed by a high-speed dispersion machine and prepared by a two-roll milling machine. Our results show that the sample treated with 3 wt% silane has the highest tensile strength and optimum dielectric properties. Furthermore, the tensile strength and coefficient of thermal expansion (CTE) increase, and the water absorption decreases, with an increasing silane content. These experiments reveal that silane treatment can reduce the overall hydrophilicity of the composites. Finally, predictions on dielectric and CTE properties are discussed. It has been found that experimental values of the dielectric constant agree well with those predicted by the rule of mixture.     

Use of mesoporous SBA-15 for nanostructuring titania for photocatalytic applications

SBA15–TiO₂ samples prepared by introducing titanium with a grafting method and having TiO₂ loadings below 15 wt.% have been characterized by XRF, XRD, IR, porosimetry, SEM, HRTEM, and UV–Visible diffuse reflectance. Differently from the samples reported in the literature characterized by a high TiO₂ loading, no evidences have been found for the presence of titania particles inside or outside the mesopores of SBA-15. Three different titanium species were instead evidenced to be present. The first two derive from the reaction of titanium with silanol groups in the corona area of inner SBA-15 walls leading to the formation of either TiO₄ tetrahedral sites (by reaction by hydroxyl nests of surface defect sites) and/or pseudo-octahedral surface sites anchored by two (or more) Si or Ti ions through bridging oxygens. The third species derives from the reaction of titanium in the regions with high sylanol density, e.g. in the micropores located in the corona of SBA-15 channels, leading to the formation of TiO₂-like nanoareas (probably Si-doped) with dimensions of around 1–2 nm maximum. The potential interest of these materials as photocatalysts, for the presence of a TiO₂-like nanoareas highly accessible by reactants, is discussed.     

Porous mullite ceramics through diphasic gels of large boehmite and small silica particles

Mullite formation process has been studied in stoichiometric mullite (3Al₂O₃·2SiO₂) diphasic gel containing large boehmite (1 m) and small silica (10 nm) particles. It has been found that initial mullitization did not take place inside the silica phase (cristobalite), but took place in the defect -alumina phase. -alumina was stabilized by silica when the temperature was below 1350°C. At temperatures above 1350°C, mullite crystallized directly. It was suggested that silica diffused into the pores (<1.8 nm) of -alumina and prevented the collapse of -alumina pore structure. On the other hand, when silica was not present, the pore structure of -alumina collapsed and -alumina crystallized at 1100°C. Porous mullite ceramics were obtained by using special diphasic gels containing large boehmite and small silica particles.     

A polyamide-silica composite prepared by the sol-gel process

Summary A new kind of organic-inorganic hybrid composite was prepared by means of the sol-gel process. The polymer employed was a mixed-isomer aromatic polyamide having good solubility and thermal stability. The silica constituting the inorganic phase was produced by the hydrolysis and condensation of tetramethoxysilane. The bonding between the phases involved aminophenyl-trimethoxysilane, in which the amino group can react with the phthaloyl chloride end-capped polymer, and the methoxysilane groups undergo hydrolysis. The composition of these composites was varied by changing the linear polymer chain length and relative amount of tetramethoxysilane. The gelation time was found to range from a few minutes to several days. Thermogravimetric analyses showed that decomposition starts at approximately 450 °C. Thin films cast from materials having a relatively high silica content were opaque and rigid, but those with low silica content were flexible and transparent.