Temperature-resolved SAXS studies of morphological changes in melt-crystallized poly(hexamethylene terephthalate) and its melting upon heating

Temperature-resolved small-angle X-ray scattering (SAXS) on poly(hexamethylene terephthalate) (PHT) samples crystallized from the melt yields direct information about the morphological changes in lamellar crystals and interlamellar amorphous layers upon melt-crystallization and subsequent heating to melting. Absolute intensities of these SAXS patterns were further analyzed via one-dimensional correlation and interface distribution functions. These analyses indicate that melt-crystallization at low temperature produces lamellar crystals having diverse thicknesses whereas crystallization at high temperature tends to favor growth of thick lamellar crystals with a nearly uniform distribution of thickness. When heating the PHT samples in the melting temperature region, the melting of the lamellar crystals was found to correlate well with the sequential-melting features. When these crystals are heated to higher temperatures, structural alterations from stacked lamellae to isolated lamellar crystals evolve with increasing extent of sequential melting, but, upon re-crystallization during extended annealing, the isolated lamellar crystals can pass through a reversible transition back to stacked lamellae.