Abstract
High-resolution 19F, 1H, 31P and 13C solid-state NMR methods were assessed to ascertain their suitability for studying the morphological behavior in the crystalline domain of phosphazene polymers with partially fluorinated side-chains. Poly[bis(trifluoroethoxy)phosphazene] (PBFP) was used as a sample system. Fast magic angle spinning (MAS), along with simultaneous 19F and 1H decoupling using the xy-16 sequence, were employed, as this has proven to greatly improve resolution in 13C spectra of perfluorinated materials. Information obtained from Discrimination Induced by Variable Amplitude Minipulses (DIVAM) nutation experiments and cross-polarization (CP) methods aided the deconvolution analysis used to identify all components in the 1H, 19F and 13C signals. DIVAM nutation experiments were also used to discriminate between signals from the amorphous and crystalline domain. The crystallinity in the solvent-cast PBFP was determined to be approximately 70%, which was seen to increase to approximately 80% in the heat-treated material, for all nuclei studied. A preliminary assignment was made for the crystalline signals in the 1H and 13C spectra to the α-, β- and γ-phases. Therefore, high-resolution 13C and 1H methods are valuable tools for morphological investigations into this class of polymer.
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