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Real‐time FTIR and WAXS studies of drawing behavior of poly(ethylene terephthalate) films
Author(s) -
Middleton A. C.,
Duckett R. A.,
Ward I. M.,
Mahendrasingam A.,
Martin C.
Publication year - 2001
Publication title -
journal of applied polymer science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.575
H-Index - 166
eISSN - 1097-4628
pISSN - 0021-8995
DOI - 10.1002/1097-4628(20010307)79:10<1825::aid-app110>3.0.co;2-s
Subject(s) - materials science , crystallite , annealing (glass) , crystallization , crystallography , fourier transform infrared spectroscopy , attenuated total reflection , composite material , anisotropy , ethylene , analytical chemistry (journal) , optics , chemistry , organic chemistry , physics , metallurgy , catalysis
The development of molecular orientation and crystallization was studied during uniaxial drawing of poly(ethylene terephthalate) (PET) films, which was immediately followed by subsequent taut annealing at the drawing temperature. The behavior was monitored in real time throughout the drawing and annealing using dynamic FTIR spectroscopy and in situ WAXS measurements using the Daresbury Synchrotron Radiation Source. Films were drawn at 80 and 85°C at varying strain rates (0.001–0.7 s −1 ). The true stress–strain behavior was determined at each of the drawing conditions and the density and optical anisotropy of unloaded samples was measured. The IR spectra were analyzed using curve reconstruction procedures developed previously, and they showed that orientation of the phenylene groups and the trans glycol conformers occurred before significant gauche–trans conformational changes could be seen. The onset of crystallization, defined as the point that the crystalline 1 05 reflection could be first observed using WAXS, was not found to correlate with any specific change in the proportions of trans and gauche isomers nor with any feature on the stress–strain curve. However, it was clear that, for these comparatively low strain rates, crystallization occurred during the drawing process while the crosshead was moving and the draw ratio was increasing. The orientation of the crystallites was calculated from the 1 05 reflection observed in a tilted film, transmission geometry. The crystallites were found to form at a draw ratio of about 2.5 with high orientation values (P 2 > 0.8) that increased during drawing and annealing to P 2 values of 0.95, irrespective of the drawing conditions. Semiquantitative measurements of crystallinity showed that the fraction of crystalline material that developed during drawing decreased with increasing strain rate. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 79: 1825–1837, 2001