CHARACTERISTICS OF STRAIN-INDUCED CRYSTALLIZATION IN NATURAL RUBBER DURING FATIGUE TESTING: IN SITU WIDE-ANGLE X-RAY DIFFRACTION MEASUREMENTS USING SYNCHROTRON RADIATION

Strain-induced crystallization of carbon black-filled natural rubber is investigated by wide-angle X-ray diffraction (WAXD) during in situ fatigue tests using synchrotron radiation. Thanks to an original experimental method, we measure the evolution with the number of cycles of: (i) the index of crystallinity, both (ii) size and (iii) orientation of the crystallites, and finally (iv) the lattice parameters. It is shown that when the minimum stretch ratio of the fatigue test is lower than the onset of melting of the crystallites, then the index of crystallinity and the size of the crystallites decrease, whereas they increase when the minimum stretch ratio is higher than the onset of melting. For all the fatigue tests, the misorientation of the crystallites slightly decreases and the lattice parameters remain constant with the number of cycles.