CHARACTERIZATION OF TITANIA GELS BY O-17 NUCLEAR-MAGNETIC-RESONANCE AND ELECTRON-DIFFRACTION

被引:63
作者
BASTOW, TJ
MOODIE, AF
SMITH, ME
WHITFIELD, HJ
机构
[1] CSIRO,DIV MAT SCI & TECHNOL,LOCKED BAG 33,CLAYTON,VIC 3168,AUSTRALIA
[2] ROYAL MELBOURNE INST TECHNOL,DEPT APPL PHYS,MELBOURNE,VIC 3001,AUSTRALIA
[3] UNIV KENT,PHYS LAB,CANTERBURY CT2 7NR,ENGLAND
关键词
SOL GEL PROCESSING; TITANIA; O-17 MAS NMR; ELECTRON DIFFRACTION;
D O I
10.1039/jm9930300697
中图分类号
O64 [物理化学(理论化学)、化学物理学];
学科分类号
070304 ; 081704 ;
摘要
The reaction of O-17-labelled water with titanium n-propoxide [Ti(OPrn)4] proceeds rapidly to produce OTi3 and OTi4 environments that can be clearly identified from O-17 magic-angle spinning NMR spectra. The gel structure is highly disordered but the quadrupolar interaction is shown to be small throughout (quadrupolar coupling constant, C(q) < 1.5 MHz). Organic fragments, which can be monitored by C-13 NMR, remain right up until crystallisation of anatase at 300-degrees-C.Crystallisation is confirmed by electron diffraction, and electron microscopy determines the crystallite size to be ca. 3 nm. O-17 NMR and electron diffraction are also used to follow the conversion of anatase to rutile.
引用
收藏
页码:697 / 702
页数:6
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