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  • silica  (5)
  • microporous crystals  (2)
  • silica-zirconia  (2)
  • sol-gel  (2)
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  • 1
    Digitale Medien
    Digitale Medien
    Springer
    Journal of sol gel science and technology 8 (1997), S. 71-76 
    ISSN: 1573-4846
    Schlagwort(e): silica-zirconia ; poly(ethylene oxide) ; spinodal decomposition ; light scattering
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Abstract Gels with interconnected domain morphologies in the micrometer-range have been prepared in the silica-zirconia system. The domain formation kinetics in the gelling solution have been examined. Growth of an ordered structure on the length scale of micrometers, for which the kinetics are interpreted as spinodal decomposition, was observed by time-resolved light scattering measurements. The remarkable feature of the silica-zirconia system was that a time-dependent decrease of the wavelength of compositional fluctuations was observed. This occurred in the early stage, probably because the fast condensation reaction which was induced by the addition of zirconia, lead to a substantial change in quench depth on a timescale similar to that of the growth of concentration fluctuations. In the following stage, the coarsened domain structure was frozen-in by the sol-gel transition as the permanent morphology.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 2
    Digitale Medien
    Digitale Medien
    Springer
    Journal of sol gel science and technology 8 (1997), S. 71-76 
    ISSN: 1573-4846
    Schlagwort(e): silica-zirconia ; poly(ethylene oxide) ; spinodal decomposition ; light scattering
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Abstract Gels with interconnected domain morphologies in the micrometer-range have been prepared in the silica-zirconia system. The domain formation kinetics in the gelling solution have been examined. Growth of an ordered structure on the length scale of micrometers, for which the kinetics are interpreted as spinodal decomposition, was observed by time-resolved light scattering measurements. The remarkable feature of the silica-zirconia system was that a time-dependent decrease of the wavelength of compositional fluctuations was observed. This occurred in the early stage, probably because the fast condensation reaction which was induced by the addition of zirconia, lead to a substantial change in quench depth on a timescale similar to that of the growth of concentration fluctuations. In the following stage, the coarsened domain structure was frozen-in by the sol-gel transition as the permanent morphology.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 3
    Digitale Medien
    Digitale Medien
    Springer
    Journal of sol gel science and technology 17 (2000), S. 191-210 
    ISSN: 1573-4846
    Schlagwort(e): silica ; phase separation ; pore structure ; mesopores ; chromatography columns
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: 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.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 4
    Digitale Medien
    Digitale Medien
    Springer
    Journal of sol gel science and technology 19 (2000), S. 65-70 
    ISSN: 1573-4846
    Schlagwort(e): porous material ; phase separation ; microporous crystals ; chromatography
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Abstract Recent progress in the sol-gel science concerning the porous gels made by phase separation has been reviewed. Based on the principle and technique explored for monoliths, the material shape has been extended to a macroporous thick film and a macroporous gel in a confined space such as capillary, both of which are expected to find useful applications in the chromatography. The modifiable size range of the additional porosity within the micrometer-sized gel skeleton has been broadened from micropores by zeolite, mesopores by surfactant templates to macropores by intensive hydrothermal treatments. A detailed investigation of 3D interfacial structure in real space has been performed using the laser scanning confocal microscope, which enabled quantitative comparison of the structure with those of other phase-separating systems.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 5
    Digitale Medien
    Digitale Medien
    Springer
    Journal of sol gel science and technology 19 (2000), S. 769-773 
    ISSN: 1573-4846
    Schlagwort(e): silica ; macropores ; deposition ; silicalite-1 ; microporous crystals
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: 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.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 6
    Digitale Medien
    Digitale Medien
    Springer
    Journal of sol gel science and technology 19 (2000), S. 371-375 
    ISSN: 1573-4846
    Schlagwort(e): phase separation ; silica ; capillary column ; HPLC ; CEC
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: 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.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 7
    ISSN: 1573-4846
    Schlagwort(e): silica ; poly(ethylene oxide) ; light scattering ; spinodal decomposition ; initial stage
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: 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.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 8
    Digitale Medien
    Digitale Medien
    Springer
    Journal of porous materials 5 (1998), S. 103-110 
    ISSN: 1573-4854
    Schlagwort(e): silica ; sol-gel ; phase separation ; solvent exchange ; surfactant
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie , Maschinenbau
    Notizen: 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.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 9
    Digitale Medien
    Digitale Medien
    Springer
    Journal of porous materials 4 (1997), S. 67-112 
    ISSN: 1573-4854
    Schlagwort(e): pore structure control ; silica gels ; phase separation ; spinodal decomposition ; chromatography ; sol-gel
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie , Maschinenbau
    Notizen: Abstract In the alkoxy-derived sol-gel system, various macroporous morphologies can be obtained by inducing the phase separation parallel to the sol-gel transition. This principle of macroporous morphology control can be best applied to pure silica and silica-based multicomponent oxide systems. The earlier the phase separation takes place than the sol-gel transition, the larger the characteristic sizes of pores and gel skeletons become. The time resolved light scattering measurements revealed that the morphology formation process exhibits the features of spinodal decomposition and that the final gel morphology is determined by the competitive kinetics between the domain coarsening and the structure freezing by sol-gel transition. The mesopore structure of such macroporous gel skeletons could be easily tailored by the solvent exchange procedures. Silica gels with controlled macropores and mesopores were successfully applied as a material for the continuous rod type column for high performance liquid chromatography.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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