In this work, polyvinylidene fluoride (PVDF) aerogels with a tailorable phase composition
were prepared by following the crystallization-induced gelation principle. A series of PVDF wet gels
(5 to 12 wt.%) were prepared from either PVDF–DMF solutions or a mixture of DMF and ethanol
as non-solvent. The effects of the non-solvent concentration on the crystalline composition of the
PVDF aerogels were thoroughly investigated. It was found that the nucleating role of ethanol can be
adjusted to produce low-density PVDF aerogels, whereas the changes in composition by the addition
of small amounts of water to the solution promote the stabilization of the valuable β and γ phases.
These phases of the aerogels were monitored by FTIR and Raman spectroscopies. Furthermore, the
crystallization process was followed by in-time and in situ ATR–FTIR spectroscopy. The obtained
aerogels displayed specific surface areas > 150 m2 g−1, with variable particle morphologies that are
dependent on the non-solvent composition, as observed by using SEM and Synchrotron Radiation
Computed micro-Tomography (SR-μCT
