Melting behavior of polymorphic crystals of poly(trimethylene 2,6-naphthalate) studied by simultaneous synchrotron X-ray scattering and thermal analysis

作者:Chuang Wei Tsung; Hong Po Da*; Chen Chih Hua; Sheu Hwo Shuenn; Jeng U Ser
来源:Journal of Applied Crystallography, 2007, 40: S637-S641.
DOI:10.1107/S002188980700461X

摘要

The polymorphic crystallization and melting behavior of poly(trimethylene 2,6-naphthalate) (PTN) have been investigated using small-angle X-ray scattering and simultaneous wide-angle X-ray scattering (WAXS) and differential scanning calorimetry (DSC). The alpha-crystal, the beta-crystal and the coexistence of both crystal forms of PTN develop at an isothermal temperature below 393 K, above 453 K and between these two temperatures, respectively. The simultaneous WAXS/DSC measurement provides a good way to identify the origin of multiple melting peaks and to get equilibrium melting temperatures. During the PTN melting process, the thermal evolutions of crystallinities, Bragg diffraction intensities and DSC thermograms reveal that the alpha -> beta phase transformation and primary and secondary crystallizations arise to generate the multiple melting peaks. The beta-crystal with high equilibrium melting temperature (T-m(,beta)0 = 510 K) is a structurally stable phase while the beta-crystal with low equilibrium melting temperature (T-m(0),(beta)= 488 K) is a metastable phase. The temperature-dependent structural parameters such as the long period, lamellar thickness and amorphous thickness were extracted from the interface distribution function. Two-step changes in the lamellar thickness and the invariant during the subsequent melting of PTN crystallized at 383 K are consistent with the alpha -> beta transformation obtained by WAXS/DSC. The alpha -> beta transformation, a typical melting-recrystallization, proceeds firstly via surface melting of alpha-lamellae, and then the PTN chains near the boundaries of surviving alpha-lamellae modify their conformation to form the beta-crystal resulting in thickening lamellae.

  • 出版日期2007-4