Nanostructural characterization of poly (vinylidene fluoride)-clay nanocomposites prepared by a one-step reactive extrusion process

Poly (vinylidene fluoride) (PVDF)-untreated clay nanocomposites were successfully prepared using an innovative one-step reactive melt extrusion process. Through specific temperature and shear conditions, the chemical reactions took place between the polymer matrix, the inorganic clay particles, and three main reactive agents: an organic peroxide, sulfur, and a specific activator led finally to the PVDF-clay nanocomposites. The materials were formulated with various amounts of clay in order to identify the best conditions, enabling to obtain the optimal particle exfoliation in the polymer matrix at the nanometric scale. The microstructure and nanostructure modifications were characterized by Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry (DSC), and wide-and small-angle X-ray scattering (WAXS and SAXS). The relationship between nanostructure and mechanical behavior was investigated by tensile experiments, impact tests, and microhardness measurements. The FTIR results suggest that there is a chemical interaction between the clay and the polymer. Furthermore, the WAXS study shows that no intercalation step takes place in any composition. In addition to this, the sample with 2.5 wt.% clay could present a total exfoliation of the clay particles. The PVDF matrix is found to be exclusively of the a-form in all compositions. The final microhardness slightly increases with both nanoclay content and degree of crystallinity.