4.5 Article

Polymer crystallization studies under processing-relevant conditions at the SAXS/WAXS DUBBLE beamline at the ESRF

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JOURNAL OF APPLIED CRYSTALLOGRAPHY
卷 46, 期 -, 页码 1681-1689

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INT UNION CRYSTALLOGRAPHY
DOI: 10.1107/S0021889813027076

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  1. Dutch Polymer Institute (DPI)

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Recent developments on the experimental infrastructure and the acquisition of new detectors on the Dutch-Belgian beamline BM26B at the ESRF offer novel and promising possibilities for synchrotron X-ray experiments in the field of polymer crystallization under processing-relevant conditions. In this contribution, some of the most recent experiments mimicking conditions similar to those relevant for the plastics processing industry are discussed. Simultaneous thermal analysis and wide-angle X-ray scattering (WAXS) experiments, at the millisecond time-frame level, on beta-nucleated isotactic polypropylene (i-PP) samples subjected to ballistic cooling up to 230 K s(-1), show that the efficiency of the nucleating agent can be suppressed when quenched cooling rates higher than 130 K s(-1) are used. In situ WAXS experiments using small-scale industrial equipment during a real film blowing process reveal the dependence of the onset of crystallinity (the so-called freeze line) and the crystal orientation as a function of different take-up and blow-up ratios. In situ small-angle X-ray scattering (SAXS) experiments during high-flow fields reveal the formation of shish and kebab structures in i-PP as a function of the imposed stress. Quantitative analysis of i-PP flow-induced structures is presented. The beamline specifications required to obtain high quality and industrially relevant results are also briefly reported.

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