O-17 and SI-29 Solid- State NMR-Study of Atomic- Scale Structure in SOL-GEL-Prepared TIO2-SIO2 Materials

Dirken, Peter J. and Smith, Mark E. and Whitfield, Harold J. (1995) O-17 and SI-29 Solid- State NMR-Study of Atomic- Scale Structure in SOL-GEL-Prepared TIO2-SIO2 Materials. Journal of Physical Chemistry, 99 (1). pp. 395-401. ISSN 0022-3654. (The full text of this publication is not currently available from this repository. You may be able to access a copy if URLs are provided)

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Solid state O-17 and Si-29 magic angle spinning (MAS) NMR spectroscopy has been applied to the study of the structure of three Ti-Si mixed oxides and their gel precursors. Gels were prepared by the hydrolysis of tetraethyl orthosilicate (TEOS) and titanium isopropoxide (Ti(OPrn)4). Both one-stage (addition of the Ti(OPrn)4 to the TEOS) and two-stage (partial hydrolysis of the TEOS before addition of the Ti(OPrn)4) procedures were used. Si-29 MAS NMR spectra hardly show any differences between the one- and two-stage gels. All consist of Q(2), Q(3), and Q(4) SiO4 species becoming Q(4) after heat treatment at 600 degrees C. This study shows that O-17 MAS NMR is a valuable tool in the characterization of amorphous oxides and that it is much more informative than Si-29 MAS NMR. O-17 MAS NMR shows that titanium is incorporated only as Ti-O-Si bonds in a two-stage gel, whilst samples that show phase separation alsb have Ti-O-Ti bonds. Ti-O-Si linkages persist until 600 degrees C and in conjunction with the Si-29 NMR data indicate that titanium enters the silica network. The assignment of the Ti-O-Si resonance is confirmed by studying the mineral fresnoite (Ba2TiSi2O8).

Item Type: Article
Subjects: Q Science > QD Chemistry
Divisions: Faculties > Science Technology and Medical Studies > School of Engineering and Digital Arts
Depositing User: P. Ogbuji
Date Deposited: 03 Jun 2009 08:39
Last Modified: 09 Jun 2014 10:33
Resource URI: https://kar.kent.ac.uk/id/eprint/19492 (The current URI for this page, for reference purposes)
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