화학공학소재연구정보센터
Thermochimica Acta, Vol.563, 33-37, 2013
Microfocus wide-angle X-ray scattering of polymers crystallized in a fast scanning chip calorimeter
Microfocus wide-angle X-ray scattering (WAXS) has been applied for analysis of the polymorphism of isotactic polypropylene and polyamide 6 prepared in a fast scanning chip calorimeter (FSC). Samples with a typical mass of few hundred nanograms, and lateral dimension and thickness of about 100 mu m and 20 mu m, respectively, were exposed to a defined thermal history in the FSC and subsequently analyzed regarding the X-ray structure at ambient temperature using an intense synchrotron microfocused X-ray beam. The relaxed melt of isotactic polypropylene was cooled at rates of 40 K s(-1) 200 K s(-1) which allowed formation of alpha-crystals or mesophase, respectively. Polyamide 6 was isothermally crystallized at 95 degrees C and 180 degrees C which led to formation of gamma-mesophase and alpha-crystals, respectively. This study demonstrated, for the first time, that FSC polymer crystallization experiments could be completed and expanded by subsequent in situ structure analysis by X-ray scattering. (C). 2013 Elsevier B.V. All rights reserved.