Ceramics-Silikáty 55, (4) 343 - 354 (2011) |
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STRUCTURAL STABILITY OF ALUMINOSILICATE INORGANIC POLYMERS: INFLUENCE OF THE PREPARATION PROCEDURE |
Kobera Libor 1, Slavík Roman 2, Koloušek David 3,
Urbanová Martina 1,
Kotek Jiří 1,
Brus Jiří 1 |
1 Institute of Macromolecular Chemistry, Academy of Sciences of the Czech Republic,
Heyrovsky sq. 2, 162 06 Prague, Czech Republic
2 Faculty of Technology, Tomas Bata University in Zlin,
sq. T. G. Masaryka 275, 762 72 Zlin, Czech Republic
3 Institute of Chemical Technology Prague, Technicka 5, 166 08 Prague, Czech Republic
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Keywords: Aluminosilicate inorganic polymers, Solid-state NMR, Phase transformation |
The stability of amorphous aluminosilicate inorganic polymer (AIP) systems with regard to the structural role of water
molecules incorporated in inorganic matrix is discussed. Innovative approach to preparation of amorphous AIP systems with
identical chemical composition but differing in structural and mechanical behavior is introduced. It is shown that even small
changes in the manufacture dramatically affect mechanical properties and the overall structural stability of AIP systems.
If the required quantity of water is admixed to the reaction mixture during the initial step of AIPs synthesis the resulting
amorphous aluminosilicate matrix undergoes extensive crystallization (zeolitization). On the other hand, if the amount of
water is added to the reaction mixture during the last step of the preparation procedure, the inorganic matrix exhibits
long-term stability without any structural defects. To find the structural reasons of the observed behavior a combination
of traditional solid state NMR (¹H and ²⁹Si MAS NMR, ²⁹Si CP/MAS NMR, ²⁹Si inverse-T1-filtered NMR), XRPD and TGA
measurements were used. The applied experiments revealed that the structural stability of AIPs can be attributed to the tight
binding of water molecules into the inorganic matrix. The structural stability of the prepared amorphous AIP systems thus
seems to be affected by the extent of hydration i.e. the strength of binding water into the inorganic framework.
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