Industrial & Engineering Chemistry Research, Vol.59, No.10, 4459-4471, 2020
Flow-Induced Crystallization of Crosslinked Poly(vinylidene fluoride) at Elevated Temperatures: Formation and Evolution of the Electroactive beta-Phase
Flow-induced crystallization of poly(vinylidene fluoride) (PVDF) was investigated for a broad temperature range from 160 to 220 degrees C by in situ synchrotron wide-angle X-ray diffraction (WAXD) and small-angle X-ray scattering (SAXS). Unexpectedly, the electroactive beta-phase is obtained directly from the melt with an extensional flow at 160-200 degrees C, which is in contrary to the quiescent crystallization of generating the pure aphase. For 220 degrees C, the observation of an equatorial SAXS streak without WAXD signals indicates the generation of fibrillar shish. Second, within the isothermal process after flow, the evolution of the flow-induced structure exhibits a strong temperature dependence. The generated beta-phase triggers subsequent crystallite growth at 160-180 degrees C. However, at 190-220 degrees C, flow-induced fibrillar shish relaxes partially. Third, cooling triggers the crystallization of the a-phase, which competes with the beta-phase to determine the final phase constitute. This work reveals the detailed formation and evolution processes of the flow-induced beta-phase, which provides an effective approach to obtain the electroactive PVDF materials.