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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Journal of sol gel science and technology 17 (2000), S. 191-210 
    ISSN: 1573-4846
    Keywords: silica ; phase separation ; pore structure ; mesopores ; chromatography columns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract By inducing a phase separation parallel to the sol-gel transition of alkoxy-derived silicate systems, gels with well-defined macroporous structure can be prepared. Depending on the post-gelation treatment such as aging and solvent exchange, the final pore structure in the nanometer range of dried and heat-treated gels exhibits a considerable variation. With an aim of completely controlling the hierarchical pore structure in the discrete size ranges of nanometers and micrometers, systematic experimental studies have been performed. The macroporous nature of the wet gels allows an efficient solvent exchange process compared with conventional gels only with mesopores. In addition, the surface chemistry of the wet gel skeleton affects the mesopore formation process by the solvent exchange to a great extent. The median size of mesopores larger than 5 nm can be controlled by adjusting the basic solvent exchange conditions such as pH value, temperature and bath ratio for any kind of macroporous silica gel. On the other hand, the control of pore volume independent of the mesopore size is possible only in the system incorporated with the micelle-forming surfactant. Some examples of the effects of controlled mesopores on the analytical performance of monolithic-type chromatographic columns are also presented.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Journal of sol gel science and technology 19 (2000), S. 769-773 
    ISSN: 1573-4846
    Keywords: silica ; macropores ; deposition ; silicalite-1 ; microporous crystals
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Microcrystalline silicalite-1 was formed on the inner surface of macroporus silica glasses prepared by the sol-gel process. By heating a homogeneous precursor solution at 100°C under a hydrothermal condition, 2–5 μm of plate-like particles of silicalite-1 were deposited. With an increase of mixing time of the precursor solution, the number of silicalite-1 particles increased, accompanied by the relative decrease of the particle size. Depending on the temperature and the duration of the heat-treatment of the macroporous silica, the amount of deposited silicalite-1 varied. Below 1000°C, the amount increased with the heat-treatment temperature, as a result of the competition between the precipitation of silicalite-1 and the dissolution of silica from the macroporous silica glass under a strongly basic condition. On the other hand, above 1000°C the amount of deposited silicalite-1 decreased in accordance with the decrease of the macropore diameter by the heat-treatment, because of the limited transport of the dissolved silicate species through the smaller macropores.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Journal of sol gel science and technology 19 (2000), S. 371-375 
    ISSN: 1573-4846
    Keywords: phase separation ; silica ; capillary column ; HPLC ; CEC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Continuous macroporous silica gel networks were prepared in a fused silica capillary, and evaluated in reversed-phase liquid chromatography. Under pressure-driven conditions, considerable dependence of column efficiency on the linear velocity of the mobile phase was observed in spite of the small size of the silica skeletons. A major source of band broadening in the pressure-driven mode was found in the A-term of van Deemter equation. The performance of the continuous silica capillary column in the electro-driven mode was much better than that in the pressure-driven mode.
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  • 4
    ISSN: 1573-4846
    Keywords: silica ; poly(ethylene oxide) ; light scattering ; spinodal decomposition ; initial stage
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Domain formation kinetics in gelling alkoxy-derived silica solutions containing polyethylene oxide (PEO) has been investigated. The time-resolved light scattering measurement was performed for the polymerizing solutions which underwent phase separation in the length scale of micrometer. Domain formation processes which resulted in various sizes of inter-connected morphology were examined, focusing mainly on the initial stage. For all the samples, the scattering intensity grew exponentially with time forming a single peak at a fixed wave-number in the first few tens seconds, which is the characteristic of the linearized regime of the spinodal decomposition. An analysis based on the linearized theory proposed by Cahn gave a reasonable description of the kinetic parameter of phase separation induced in various stages of the sol-gel transition.
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  • 5
    Electronic Resource
    Electronic Resource
    Springer
    Journal of porous materials 5 (1998), S. 103-110 
    ISSN: 1573-4854
    Keywords: silica ; sol-gel ; phase separation ; solvent exchange ; surfactant
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract The principle of designing double-pore structure in alkoxy-derived silica is described with the experimental system containing polyoxyethylene nonylphenylether. The formation of macropores is consistently explained in terms of the concurrence of a phase separation and a sol-gel transition in the polymerizing silica-surfactant-solvent system. The composition-morphology relationship exhibited a substantial variation depending on the length of oxyethylene units in the surfactant molecule. The mesopore volume obtained after basic solvent exchange and a heat-treatment suggested that the surfactant with shorter oxyethylene chain tends to be incorporated more in the gel phase to give higher mesopore volume. The small-angle X-ray scattering measurement of the gelling and aging system supported this hypothesis indicating micelle formation in the system containing a surfactant with shorter oxyethylene chain.
    Type of Medium: Electronic Resource
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