Q. Deng et al., NOVEL NAFION(R) ORMOSIL HYBRIDS VIA IPL SITU SOL-GEL-REACTIONS .2. PROBE OF ORMOSIL PHASE NANOSTRUCTURE BY SI-29 SOLID-STATE NMR-SPECTROSCOPY/, JOURNAL OF SOL-GEL SCIENCE AND TECHNOLOGY, 7(3), 1996, pp. 177-190
[Perfluorosulfonic Acid (PFSA)]/[Organically-Modified Silicon Oxide (O
RMOSIL)] hybrids were formulated via sol-gel reactions of mixtures of
tetraethoxysilane (TEOS) and diethoxydimethylsilane (DEDMS) in the nan
ophase-separated morphology of a PFSA membrane (Nafion(R)). The molecu
lar structures of the ORMOSIL phases were investigated by Si-29 solid
state NMR spectroscopy and the spectra compared with those of correspo
nding bulk ORMOSILs. PFSA-in situ ORMOSIL composition can be tailored
by manipulating TEOS/DEDMS source solution composition and quantified
by Si-29 solid state NMR spectroscopy. Copolymerization of TEOS and DE
DMS monomers, rather than block formation, occurs within the PFSA as w
ell as in the bulk. As DEDMS feed concentration increases, ORMOSIL nan
ostructures are more hydrophobic and more flexible. Dimethylsiloxane r
ings are dominant in PFSAs in which hydrolysis + condensation of pure
DEDMS occurs.