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TMDSC and Atomic Force Microscopy Studies of Morphology and Recrystallization in Polyesters Including Oriented Films

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Abstract

The thermal and crystal morphological properties of poly[ethylene teraphthalate] (PET) and poly(ethylene-2,6-naphthalenedicarboxylate) (PEN) biaxially oriented films were compared to amorphous and other isotropic semi-crystalline samples. Crystal melting as a function of temperature was characterized by temperature modulated DSC (TMDSC) and found to begin just above the glass transition for both oriented films. About 75°C above the glass transitions, substantial exothermic recrystallization begins and continues through the final melting region in oriented films. The maximum in the non-reversing TMDSC signal for the oriented films signifies the maximum recrystallization exothermic activity with peaks at 248°C and 258°C for PET and PEN, respectively. The final melting endotherm detected was 260°C and 270°C for PET and PEN, and is shown by the TMDSC data and by independent rapid heating rate melting point determinations to be due to the melting of species recrystallized during the heating scan. The results are compared with TMDSC data for initially amorphous and melt crystallized samples. The volume fraction of rigid species (Frigid=total crystal fraction plus ‘rigid amorphous or non-crystalline species’) were measured by TMDSC glass transition data, and contrasted with the area fraction of rigid species at the oriented film surface characterized with very high resolution atomic force microscopy (AFM) phase data. The data suggest that the 11 nm wide hard domains in PET, and 21 nm wide domains in PEN film detected by AFM consist of both crystal and high stiffness interphase species.

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References

  1. J. M. Schultz and S. Fakirov, ‘Solid State Behavior of Linear Polyesters and Polyamides’, Prentice Hall, Inc. Englewood Cliffs, New York 1990.

    Google Scholar 

  2. B. Wunderlich, Macromolecular Physics, Volume 3, Academic Press, New York 1980.

    Google Scholar 

  3. M. Reading, Trends Polym. Sci., 8 (1993) 248. M. Reading, D. Elliot and V. L. Hill, J. Thermal Anal., 40 (1993) 949.

    Google Scholar 

  4. I. Okazaki and B. Wunderlich, J. Polym. Sci., Polym. Phys., 34 (1996) 2941.

    Google Scholar 

  5. I. Okazaki and B. Wunderlich, Macromol. Rapid Commun., 18 (1997) 313.

    Google Scholar 

  6. I. Okazaki and B. Wunderlich, Macromolecules, 30 (1997) 1758.

    Google Scholar 

  7. H. G. Zachmann and H. A. Stuart, Makromol. Chem., 8 (1960) 131.

    Google Scholar 

  8. P. J. Holdsworth and A. Turner-Jones, Polymer, 12 (1971) 195.

    Google Scholar 

  9. G. Groeninckx, H. Reynaers, H. Berghmans and G. Smets, J. Polym. Sci., Polym. Phys., 18 (1980) 1311.

    Google Scholar 

  10. C. Zhou and S. B. Clough, Polym. Eng. Sci., 28 (1988) 65.

    Google Scholar 

  11. S. Buchner, D. Wiswe and H. G. Zachmann, Polymer, 30 (1989) 480.

    Google Scholar 

  12. S. Z. D. Cheng, M.-Y. Cao and B. Wunderlich, Macromolecules, 21 (1988) 789.

    Google Scholar 

  13. F. J. Medellin-Rodriguez, P. J. Phillips and J. S. Lin, Macromolecules, 29 (1996) 7491.

    Google Scholar 

  14. Z. G. Wang, B. S. Hsiao, B. B. Sauer and W. G. Kampert, Polymer, 40 (1999) 4615.

    Google Scholar 

  15. B. B. Sauer, W. G. Kampert, E. N. Blanchard, S. A. Threefoot and B. S. Hsiao, Polymer, 41 (2000) 1099.

    Google Scholar 

  16. C. Fougnies, P. Damman, M. Dosiere and M. H. Koch, J. Macromolecules, 30 (1997) 1392.

    Google Scholar 

  17. G. Qiu, Z.-L. Tang, N.-X. Huang and L. Gerking, J. Appl. Polym. Sci., 69 (1998) 729.

    Google Scholar 

  18. S. Z. D. Cheng, J. J. Janimak, A. Zhang, J. Guan and A.-L. Chu, Polymer Bulletin, 20 (1988) 449.

    Google Scholar 

  19. S. N. Maganov and M.-H. Whangbo, ‘Surface Analysis with STM and AFM VCH’, VCH Publishers, Weinheim 1996.

    Google Scholar 

  20. R. S. McLean and B. B. Sauer, Macromolecules, 30 (1997) 8314.

    Google Scholar 

  21. S. Magonov and Y. Godovsky, Amer. Lab., 31 (1999) 52.

    Google Scholar 

  22. S. A. C. Gould, D. A. Schiraldi and M. L. Occelli, J. Appl. Polym. Sci., 65 (1997) 1237.

    Google Scholar 

  23. J. S. G. Ling and G. Leggett, J. Amer. Chem. Soc. Polym. Preprints, 38(1) (1997) 1061.

    Google Scholar 

  24. D. J. Blundell and B. N. Osborn, Polymer, 24 (1983) 953.

    Google Scholar 

  25. P. Zoller, T. A. Kehl, H. W. Starkweather and G. A. Jones, J. Polym. Sci., Polym. Phys., 27 (1989) 993.

    Google Scholar 

  26. J. N. Hay, J. I. Langford and J. R. Lloyd, Polymer, 30 (1989) 489.

    Google Scholar 

  27. H. W. Starkweather, P. Zoller and G. A. Jones, J. Polym. Sci., Polym. Phys., 21 (1983) 295.

    Google Scholar 

  28. B. Wunderlich, in ‘Thermal Analysis’, Academic Press, New York 1990.

    Google Scholar 

  29. L. C. Thomas and S. R. Aubuchon, to be published, 1999. Software provided by T.A. Instruments, Inc. 109 Lukens Drive, New Castle, DE 19720.

  30. K. Ishikiriyama and B. Wunderlich, Macromolecules, 30 (1997) 4126.

    Google Scholar 

  31. Q. Zhong, D. Inniss, K. Kjoller and V. B. Elings, Surface Sci. Lett., 290 (1993) L688.

    Google Scholar 

  32. G. Bar, Y. Thomann and M.-H. Whangbo, Langmuir, 14 (1998) 1219.

    Google Scholar 

  33. R. S. McLean and B. B. Sauer, J. Polym. Sci., Polym. Phys., 37 (1999) 859.

    Google Scholar 

  34. S. Z. D. Cheng, M.-Y. Cao and B. Wunderlich, Macromolecules, 19 (1986) 1868.

    Google Scholar 

  35. B. B. Sauer and B. S. Hsiao, Proceedings of the Amer. Chem. Society, Division of P.M.S.E., 69 (1993) 35.

    Google Scholar 

  36. B. B. Sauer and B. S. Hsiao, Polymer, 35 (1995) 2553.

    Google Scholar 

  37. E. J. Donth, Non-Cryst. Solids, 53 (1982) 325.

    Google Scholar 

  38. C. Santa Cruz, N. Stribeck, H. G. Zachmann and F. J. Balta Calleja, Macromolecules, 24 (1991) 5980.

    Google Scholar 

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Authors and Affiliations

  1. DuPont Central Research & Development, Experimental Station, Wilmington, DE, 19880-0356, USA

    B. B. Sauer, W. G. Kampert, R. S. McLean & P. F. Carcia

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  1. B. B. Sauer
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  2. W. G. Kampert
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  3. R. S. McLean
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  4. P. F. Carcia
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Sauer, B.B., Kampert, W.G., McLean, R.S. et al. TMDSC and Atomic Force Microscopy Studies of Morphology and Recrystallization in Polyesters Including Oriented Films. Journal of Thermal Analysis and Calorimetry 59, 227–243 (2000). https://doi.org/10.1023/A:1010148331705

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