We designed and constructed an extensional rheometer for in situ small and wide angle x-ray study on flow-induced crystallization of polymer. Two rotating drums with an axis distance of 20 mm are employed to impose extensional deformation on the samples. With a constant angular velocity, the two drums generate a constant Henkcy strain rate as sample length for testing keeps constant during deformation. An ionic liquid is used as heating medium to prevent polymer melt from bending downward due to gravity, which is excellent in terms of high thermal stability, low viscosity, and relative low adsorption on x-ray. Flow-induced crystallization experiments are conducted with this apparatus on x-ray scattering station in Shanghai Synchrotron Radiation Facility (SSRF), which allows us to collect rheological and structural data simultaneously and may lead to a better understanding on flow-induced crystallization of polymer.
Strain-induced crystallization (SIC) of natural rubber (NR) samples with different strain rates at a fixed strain was investigated by synchrotron radiation X-ray diffraction measurements, which provided the evolution trends of crystal sizes and crystallinity during the SIC process. It was found that the Avrami index was about 1 during the crystallization of NR after the cessation of stretch, which demonstrated that sporadic nucleation occurred during SIC process. The increase of the crystallinity was attributed to the increase of the number of new crystallites rather than the growth of the crystal size. An unexpected relationship between the final crystallinity and the strain rates was observed. The increase of physical crosslink points originated from either entanglement or crystallite was considered as the reason that leads to the nonmonotonic variation of the final crystallinity with strain rates.
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