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Hierarchical Structural Change in the Stress-Induced Phase Transition of Poly(tetramethylene terephthalate) As Studied by the Simultaneous Measurement of FTIR Spectra and 2D Synchrotron Undulator WAXD/SAXS Data
The simultaneous measurement of Fourier
transform infrared (FTIR)
transmission spectra and 2-dimensional wide-angle X-ray diffraction
(WAXD) and small-angle X-ray scattering (SAXS) patterns has been performed
successfully to investigate the hierarchical structure changes occurring
in the stress-induced phase transition phenomenon of uniaxially oriented
polyÂ(tetramethylene terephthalate) film. The molar fraction of the
β-crystal form, evaluated from the IR and WAXD data analyses,
increased steeply in the plateru region of the stress–strain
curve as already known well. The 2D SAXS data have revealed the remarkable
and reversible change in the stacked lamellar structure just after
the α-to-β phase transition was completed, where the tilting
angle of the stacked lamellae measured from the draw axis of the oriented
sample became zero, and the lamellar thickness increased due to the
inclusion of amorphous region located in the boundary part of the
crystalline lamellae. In parallel, the X-ray reflection spots in a
wider diffraction angle region became diffuse in the observed WAXD
pattern of the β form, indicating the packing disorder of the
mechanically stressed chains. In this way, the simultaneous combination
of the 3 different types of equipments has allowed us to deduce the
detailed structural change from the various levels: the stress-induced
α–β transition was found to occur not only with
the remarkable changes in the molecular chain conformation and chain
packing mode in the crystal lattice, but also with the large and reversible
change in the lamellar stacking structure. The stress-induced changes
in lamellar thickness and long period were simulated using a mechanical
model with these hierarchical structure changes taken into account,
giving relatively good reproduction of the observed data