Crystallization effects on autoclave foaming of polycarbonate using supercritical carbon dioxide

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AbstractIn this study, the conditions leading to the formation of cells and to the onset of crystallization of polycarbonate were examined with the use of supercritical carbon dioxide for the production of foams from preforms. Small plaques cut from extruded sheets were treated with supercritical carbon dioxide in an autoclave at temperatures varying from 60 to 200°C and from 4.5 to 30 MPa pressure. Visual observations and stereoscan electron microscopy examination revealed that penetration of supercritical carbon dioxide takes place via the advancing layer mechanism and that, for the particular grade of polycarbonate used in this study, the nucleation of the cells can take place at temperatures as low as 60°C. It requires, however, long treatment times and high pressures, and the growth of foam cells is severely restricted. Nucleation and growth of cells occurred much more readily at somewhat higher temperatures. With treatments at around 80°C, the onset of crystallization started to impose considerable hindrance to the formation of uniform and evenly distributed cells. This becomes increasingly evident at higher temperatures, between 100 and 180°C, owing to the formation of large spherulitic crystalline domains. A very effective nucleation and growth mechanism for the formation of cells was obtained, on the other hand, with treatments at 200°C due to the absence of crystallization phenomena. The degree of crystallinity increased with increasing treatment temperature, and the resulting morphology gave rise to two broad melting peaks. These are displaced to higher temperatures and become closer, merging into one peak with a low‐temperature shoulder. These events were monitored by thermal analysis and wide‐angle X‐ray diffraction examinations. © 2007 Wiley Periodicals, Inc. Adv Polym Techn 25:225–235, 2006; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/adv.20075