Ir. Herbert et al., NMR AND X-RAY STUDIES ON THE MORPHOLOGY OF THERMOREVERSIBLE POLYACRYLONITRILE GELS, Journal of polymer science. Part B, Polymer physics, 31(11), 1993, pp. 1459-1470
The morphology of thermoreversible polyacrylonitrile-propylene carbona
te (PAN-PC) gels was examined using solid-state carbon-13 nuclear magn
etic resonance (NMR) spectroscopy and x-ray diffraction. Following com
plete dissolution of the polymer at elevated temperature and cooling o
f the concentrated PAN-PC solutions, a gel was formed. The PAN-PC gels
consisted of regions of mobile polymer chains, rich in PC, ''cross-li
nked'' by regions of rigid polymer. The mobile regions of the gels sho
wed solution-type NMR spectra with resolution of tacticity effects. Th
e rigid component detected by NMR would correspond to the crystallites
detected previously by x-ray diffraction. Wide-angle x-ray diffractog
rams of the gels showed different peaks when compared with the dry pol
ymer powder. After solvent extraction and drying of the gel, the diffr
actogram reverted to that of the original dry powder. This new result
is the strongest evidence to support the view advanced earlier that th
e new peaks found in the diffraction pattern of the wet gels arises fr
om solvated polymer crystallites rather than from ordinary polymer cry
stallites. (C) 1993 John Wiley & Sons, Inc.