S. Prabakar et al., IDENTIFICATION OF SELF-CONDENSATION AND CROSS-CONDENSATION PRODUCTS IN ORGANICALLY MODIFIED SILICA SOLS BY SI-29 AND O-17 NMR-SPECTROSCOPY, Journal of non-crystalline solids, 202(1-2), 1996, pp. 53-60
High resolution Si-29 and O-17 NMR spectroscopy has been used to ident
ify self- and cross-condensation products in sols prepared from tetrae
thoxysilane (TEOS) and organically modified triethoxysilanes (RTES, wh
ere R is a methyl, ethyl or phenyl group). The sols were prepared by t
he acid catalyzed hydrolysis of TEOS and RTES with H2O/Si mole ratios
of 0.15, 0.3 or 0.5, Resonance assignments were made by comparing the
positions and intensities of peaks in the spectra of single and multic
omponent systems as a function of reaction time. Both Si-29 and O-17 N
MR spectroscopy exhibit resonances which are uniquely attributed to sp
ecies formed by cross-condensation reactions between TEOS and RTES. Ap
proaches to improve the resolution of O-17 NMR spectra were only moder
ately successful because the resonance envelopes have substantial cont
ributions from inhomogeneous components.