NDLI: A structural study of (TiO2)x(SiO2)1–x (x=0.18, 0.30 and 0.41) xerogels prepared using acetylacetone

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A structural study of (TiO₂)_x(SiO₂)_1–x (x=0.18, 0.30 and 0.41) xerogels prepared using acetylacetone

Content Provider	Royal Society of Chemistry (RSC)
Author	Anderson, Ruth Newport, Robert J. Cole, Jacqui M. Wallidge, Graham W. Smith, Mark E. Mountjoy, Gavin Pickup, David M.
Copyright Year	1999
Abstract	A combination of 29 Si and 17 O MAS NMR, EXAFS and FTIR spectroscopy have been used to study the atomic structure of (TiO 2 ) x (SiO 2 ) 1–x (x=0.18, 0.30 and 0.41) xerogels prepared using an acetylacetone stabilised Ti(OPr i ) 4 precursor. In the as-prepared materials, Ti is present in a distorted octahedral coordination with a significant proportion still complexed by acetylacetone. For the first time in such an amorphous solid, a 17 O NMR resonance has been observed at 110 ppm which is attributed to (O 5 )Ti-O-Si groups. Heat treatment of these xerogels tends to convert TiO 6 into TiO 4 where the Ti is substituted into the silica network. Our results are in accord with previous work which suggests that the upper limit for solubility of TiO 2 in SiO 2 is ca. 15 mol%. Clear evidence of some phase separation in the (TiO 2 ) 0.41 (SiO 2 ) 0.59 sample after heat treatment to 750 °C is presented, although the 17 O MAS NMR results show that the use of acetylacetone significantly increases the amount of Ti-O-Si bonding at this composition compared to samples prepared without it.
Starting Page	1299
Ending Page	1305
Page Count	7
File Format	PDF
ISSN	09599428
Volume Number	9
Issue Number	6
Journal	Journal of Materials Chemistry
DOI	10.1039/a809810g
Language	English
Publisher	Royal Society of Chemistry
Access Restriction	Open
Subject Keyword	Ti Magic angle spinning Extended X-ray absorption fine structure Spectroscopy Acetylacetone Amorphous solid Nuclear magnetic resonance Silicon dioxide
Content Type	Text
Resource Type	Article
Subject	Chemistry Materials Chemistry

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