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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Journal of sol gel science and technology 2 (1994), S. 239-244 
    ISSN: 1573-4846
    Keywords: thermoporometry ; permeability ; texture of gels
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The textures of silica gels made by two-step acid/base and acid/acid catalysis of TEOS have been examined by thermoporometry (TPM) and NMR, and their permeabilities (D) have been measured by a thermal expansion technique. Using the pore size distribution given by TPM, which includes a large proportion of macropores (≥30 nm), calculated values of D are seriously overestimated. We conclude that, consistent with a theoretical prediction, compliant materials such as gels undergo contraction during freezing in the calorimeter, so that most of the macropore volume reported by TPM is actually extracted from mesopores. The mesopore radius reported by TPM is underestimated by only ∼20%, even if 50% of the pore liquid is drained during crystallization, assuming that the change in pore radius is related to the cube root of the volume change. NMR does not distinguish macropores, because of diffusional averaging, but provides an apparent distribution that permits an accurate estimate of the permeability.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 887-898 
    ISSN: 1572-8943
    Keywords: calorimetric analysis ; liquid-solid phase transformation ; porous materials
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Kalorimetrische Analyse zeigt eine Reihe von Umwandlungen inner- und außerhalb von Poren, wobei die Charakteristik der Umformungen von der Konzentration der Lösung sowie von der Menge des anwesenden porösen Körpers abhängt. Bei einem gegebenen porösen Körper verändert sich die Konzentration des Kapillarkondensates unabhängig von der Ausgangskonzentration systematisch immer in Richtung der eutektischen Konzentration, auch wenn die Salzkonzentration zu Beginn über der eutektischen Konzentration liegt. Man muß bemerken, daß diese Erscheinung je nach Ausgangskonzentration auf Migration von Wasser oder Kaliumjodid außerhalb der Poren hinweist. Für verschiedene Proben mit abnehmender Porengröße findet bei sinkender Temperatur ein nacheinanderfolgendes Erstarren von getrenntem Wasser und Eutektikum statt. Die Gefrierpunktserniedrigung von Wasser in derartig getrennten KI-Lösungen scheint nicht eine Funktion der Salzkonzentration zu sein sondern hauptsächlich vom Separierungseffekt abzuhängen. Für unterteilte Eutektika konnte ein annähernd linearer Zusammenhang zwischen dem Porenradius und dem Reziproken der Temperaturerniedrigung festgestellt werden.
    Notes: Abstract Calorimetric analysis shows a succession of transformations inside and outside the pores, whose characteristics depend on the concentration of the solution and the amount of porous body present. For a given porous body, whatever the initial concentration of the solution, the capillary condensate concentration evolves systematically, during cooling, towards the eutectic concentration even if the initial salt concentration is higher than the eutectic one. It should be noted that this phenomenon indicates migration outside the pores of water or potassium iodide according to the initial concentration. For various samples whose pore size is decreasing, successive solidification of divided water and eutectic occurs at decreasing temperatures. The freezing temperature depression of water in divided KI solutions does not seem to be a function of the salt concentration but is dependent mainly on the division effect. A nearly linear relationship between pore radius and the reciprocal of temperature depression may experimentally be established for divided eutectic.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Journal of sol gel science and technology 2 (1994), S. 277-281 
    ISSN: 1573-4846
    Keywords: thermoporometry ; densification of aerogels ; PDA: Partially densified aerogels ; impregnation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The evolution of the texture of silica aerogels during sintering is studied by thermoporometry for both neutral and base catalysed materials. During the densification the macroporous volume drops and the analysis of the mesopore size distribution evolution shows that the collapse of the smallest mesopores is responsible for the macropore volume transformation. However, corrections of the measured volumes are necessary to characterize the most compliant materials.
    Type of Medium: Electronic Resource
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