Morphological Changes During Crystallization and Melting of Polyoxymethylene Studied by Synchrotron X-Ray Scattering and Modulated Differential Scanning Calorimetry
作者:
BRYANB. SAUER,
ROBERTS. MCLEAN,
J.DAVID LONDONO,
BENJAMINS. HSIAO,
期刊:
Journal of Macromolecular Science, Part B
(Taylor Available online 2000)
卷期:
Volume 39,
issue 4
页码: 519-543
ISSN:0022-2348
年代: 2000
DOI:10.1081/MB-100100402
出版商: Taylor & Francis Group
数据来源: Taylor
摘要:
Temperature scanning techniques, including synchrotron small-angle X-ray scattering (SAXS), wide-angle X-ray diffraction(WAXD), and temperature-modulated differential scanning calorimetry (TMDSC), were used to study melting recrystallization in semicrystalline polyoxymethylene (POM). The isothermal crystallization of POM was also studied by time-resolved SAXS. From SAXS profiles, several morphological variables were calculated, including the long periodL, lamellar thicknesslc, interlamellar amorphous thicknessla, and scattering invariantQ. The lamellar parameters were also obtained using tapping atomic force microscopy (AFM) for two thermal histories, and some lamellar-scale and larger-scale morphological changes were characterized before and after partial melting. These real-space images also provided support to interpretation of SAXS analysis in the interpretation of first- and second-order intensity maxima. During melting at constant heating rates,lafrom SAXS increased slowly starting at about 100°C, suggesting melting of thin inserted lamellae, and at about 150°C,lcbegan to increase combined with a more rapid increase inladue to further melting of inserted lamellae and some recrystallization into separate stacks of lamellae. The end of melting was about 182°C. TMDSC data also characterized the level of melting and recrystallization starting at low temperatures for a quenched sample. The DSC data provided the total extent of melting, and this was contrasted with the drop in SAXS and WAXD intensities. SAXS and TMDSC temperature scans on a quenched, but still highly crystalline, POM sample were compared with the data from a high-temperature (145°C) isothermally crystallized POM sample with a higher degree of crystal perfection.
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