In-situ X-ray deformation study of fluorinated multiwalled carbon nanotube and fluorinated ethylene-propylene nanocomposite fibers

A fluorinated multiwalled carbon nanotube (FMWNT) was prepared by reaction of 3-perfluoro-octylpropylamine with carboxylic acid groups on the oxidized carbon nanotube surface. The modification was confirmed by TGA, TEM, and solubility tests in a perfluorodecalin solvent. Nanocomposite fibers based on FMWNT and a fluoro-ethylene-propylene (FEP) copolymer were fabricated by melt blending and melt spinning. SEM examination indicated that the dispersion of FMWNT in FEP was significantly better than that of the as-received multiwalled carbon nanotube (MWNT) in FEP. Both yield strength and modulus of the melt-spun FMWNT/FEP nanocomposite fiber increased with increasing FMWNT content, but the elongation-to-break ratio decreased. In-situ small-angle X-ray scattering (SAXS) and wide-angle X-ray diffraction (WAXD) techniques were used to follow the structural changes during tensile deformation of melt-spun fibers. In pure FEP fibers, perpendicularly arranged lamellar stacks (with respect to the fiber axis) became tilted at small strains, while destruction of lamellae took place at high strains (>250%), resulting in the rapid decrease of crystallinity. Surprisingly, the tilting of lamellar stacks was not observed in FEP/FMWNT nanocomposite fibers during deformation. We hypothesize that the well-dispersed FMWNT particles form a fibrous network, which can carry a significant fraction of local stress, resulting in overall increases of yield strength and modulus. A possible mechanism to explain the effect of FMWNT on the lamellar structural change in FEP and corresponding mechanical behavior is presented.