Journal of Polymer Science Part B: Polymer Physics, Vol.34, No.16, 2783-2804, 1996
An Experimental-Method for Studying Nonisothermal Crystallization of Polymers at Very High Cooling Rates
A new technique based on light depolarizing microscopy was developed for studying non-isothermal crystallization of polymers at average cooling rates up to about 5000 degrees C/min. The polymer is cooled down by a gaseous cooling medium supplied at a constant temperature. The temperature of polymer is measured by a thermocouple imbedded directly in the sample. A heat transfer analysis was used to establish appropriate sample geometry to assure that, under the applied cooling condition, the temperature distribution along the sample thickness can be neglected. A light-scattering effect, which occurs when crystallization is carried out under high cooling rates, was observed. This required the development of a method to correct the depolarized light intensity for the effect of light scattering. An appropriate correction method was developed based on both a theoretical and an experimental analysis of the light intensity measurement. This provided a means to measure the overall crystallization kinetics. Examples of such measurements for iPP, HDPE, and LDPE are presented. In addition to the overall crystallization kinetics, the developed technique includes a video camera and VCR system used for measurements of spherulite growth rates during crystallization under high cooling rates. Constant spherulite growth rates were observed for isotactic polypropylene crystallized under very non-isothermal conditions.
Keywords:POLYPROPYLENE