Journal
ZEITSCHRIFT FUR KRISTALLOGRAPHIE
Volume 222, Issue 11, Pages 656-662Publisher
OLDENBOURG VERLAG
DOI: 10.1524/zkri.2007.222.11.656
Keywords
sol-gel synthesis; polysilsesquioxane; polysiloxane; silica; higher-ordered nanostructure
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Rodlike polysilsesquioxanes forming regular higher-ordered nanostructure such as hexagonal phase were prepared by sol-gel reaction of organotrimethoxysilanes having amino groups in aqueous solutions of inorganic strong acids. The XRD profiles of the resulting polysilsesquioxanes showed three peaks with the d-value ratio of 1 : 1/root 3 : 1/2, indicating that these polysilsesquioxanes have hexagonal phase. The diffraction peaks shifted by changing the humidity. In addition, the d-values of diffraction peaks increased by ion-exchange reaction with organic compounds such as fatty acid salt and anionic polymer. Therefore, this hexagonal phase originated from the stacking of rodlike polysilsesquioxanes with Si-O-Si framework at the core and ammonium groups extruding outside. This Si-O-Si framework probably formed a ladder or ladder-related structure, which was characterized by solid-state Si-29 NMR and IR spectrometries.
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