Thickening process of polyethylene single crystals at an early stage of annealing

By the use of a position sensitive proportional counter, changes in small and wide angle X-ray scattering during annealing of polyethylene single crystal mats were measured from the start in successive spans of very short measuring time. At high temperatures, the long period relating to stacking of lamellae rapidly increased at an early stage, passed through a plateau, and thereafter again increased gradually. With a decrease in annealing temperature, the amount of its first rapid increase was reduced and the plateau changed into an ascending slope. At much lower annealing temperatures, the long period increased following the logt law after an induction time. The integral breadth of a peak corresponding to the long period first increased rapidly, simultaneously with the rapid increase in the long period, and thereafter decreased. Wide angle X-ray measurement showed that the integrated intensity of 110 reflection first decreased and then increased during annealing at high temperatures. This fall and rise process was more marked, when the annealing temperature is higher and the initial thickness of lamellae is smaller. From these observations, it was inferred that in the thickening process, stacking order of lamellae at first decreased because of rapid reorganization due to partial melting or melt-recrystallization and subsequently increased through increasing evenness of lamellar thickness.