The initial stage of fiber structure development in the continuous neck-drawing of amorphous poly(ethylene terephthalate) fibers was analyzed by in-situ wide-angle x-ray diffraction, small-angle x-ray scattering, and temperature measurements. The time error of the measurements (< 600 μs) was obtained by synchrotron x-ray source and laser irradiation heating. A highly ordered fibrillar-shaped two-dimensional (smectic-like) structure was found to be formed less than 1 ms after necking. By analyzing its (001') and (002') diffractions, the length of the structure 60-70 nm were obtained. A three-dimensionally ordered triclinic crystal began to form with the vanishing of the structure around 1 ms after necking. The amount and size of the crystal were almost saturated within several milliseconds of necking, during which time a mainly exothermic heat of crystallization was also observed.
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