Nucleation and crystallization of low-crystallinity polypropylene followed in situ by hot stage atomic force microscopy

Macromolecules

Volumn 36, Issue 7, 2003, Pages 2412-2418

  Schönherr, Holger ^a,b,c   Waymouth, Robert M ^b   Frank, Curtis W ^a,b  

^a Stanford University   (United States)

^b STANFORD UNIVERSITY   (United States)

^c UNIVERSITY OF TWENTE   (Netherlands)

Author keywords

[No Author keywords available]

Indexed keywords

ATOMIC FORCE MICROSCOPY; CRYSTAL GROWTH; CRYSTALLIZATION; DIFFERENTIAL SCANNING CALORIMETRY; ELASTOMERS; ETHERS; ISOTHERMS; NUCLEATION; THERMAL EFFECTS; X RAY SCATTERING;

CROSSHATCHING; CRYSTALLINITY; HOT STAGE ATOMIC FORCE MICROSCOPY; ISOTHERMAL CRYSTALLIZATION; LAMELLAR CRYSTALS;

POLYPROPYLENES;

EID: 0037426520     PISSN: 00249297     EISSN: None     Source Type: Journal    
DOI: 10.1021/ma0208335     Document Type: Article

References (64)

1. Thermoplastic Elastomers, 2nd ed.; Holden, G., Legge, N. R., Quirk, R. P., Schroeder, H. E., Eds.; 1996.
2. Ho, T.; Martin, J. M. In Metallocene-Based Polyolefins; Scheirs, J., Kaminsky, W., Eds.; Wiley: Chichester, England, 2000; Vol. 2, pp 175-203.
3. For a morphological investigation of polyethylene copolymers, see: Bensason, S.; Minick, J.; Moet, A.; Chum, S.; Hiltner, A.; Baer, E. J. Polym. Sci., Part B: Polym. Phys. 1996, 34, 1301.
4. (a) Collette, J. W.; Tullock, C. W.; MacDonald, R. N.; Buck, W. H.; Su, A. C. L.; Harrel, J. R.; Mülhaupt, R.; Anderson, B. C. Macromolecules 1989, 22, 3851, 3858.
5. (b) Ittel, S. D. J. Macromol. Sci. Chem. 1990, A27, 9.
6. (a) Mallin, D. T.; Rausch, M. D.; Lin, Y. G.; Dong, S.; Chien, J. C. W. J. Am. Chem. Soc. 1990, 112, 2030.
7. (b) Bravakis, A. M.; Bailey, L. E.; Pigeon, M.; Collins, S. Macromolecules 1998, 31, 1000.
8. (c) Dietrich, U.; Hackmann, M.; Rieger, B.; Klinga, M.; Leskelae, M. J. Am. Chem. Soc. 1999, 121, 4348.
9. (d) Dreier, T.; Erker, G.; Frohlich, R.; Wibbeling, B. Organometallics 2000, 19, 4095.
10. (a) Coates, G. W.; Waymouth, R. M. Science 1995, 267, 217.
11. (b) Bruce, M. D.; Coates, G. W.; Hauptman, E.; Waymouth, R. M.; Ziller, J. W. J. Am. Chem. Soc. 1997, 119, 11174.
12. Ho, T.; Martin, J. M. in Metallocene-Based Polyolefins; Scheirs, J., Kaminsky, W., Eds.; Wiley: Chichester, England, 2000; Vol. 2, p 175.
13. (a) Carlson, E. D.; Krejchi, M. T.; Shah, C. D.; Terekawa, T.; Waymouth, R. M.; Fuller, G. G. Macromolecules 1998, 31, 5343.
14. (b) Hu, Y.; Carlson, E. D.; Waymouth, R. M.; Fuller, G. G. Macromolecules 1999, 32, 3334.
15. (c) Kravchenko, R.; Masood, A.; Waymouth, R. M.; Myers, C. L. J. Am. Chem. Soc. 1998, 120, 2039.
16. (d) Carlson, E. D.; Fuller, G. G.; Waymouth, R. M. Macromolecules 1999, 32, 8094.
17. Natta, G. J. Polym. Sci. 1959, 34, 531.
18. Schönherr, H.; Wiyatno, W.; Pople, J.; Frank, C. W.; Fuller G. G.; Gast, A. P.; Waymouth, R. M. Macromolecules 2002, 35, 2654.
19. (a) Pearce, R.; Vancso, G. J. Macromolecules 1997, 30, 5843.
20. (b) Pearce, R.; Vancso, G. J. Polymer 1998, 39, 1237.
21. Schultz, J. M.; Miles, M. J. J. Polym. Sci., Part B: Polym. Phys. 1998, 36, 2311.
22. For an overview see e.g.: (a) Wunderlich, B. Macromolecular Physics; Academic Press: New York, 1973, 1976, 1980; Vol. 1, Vol. 2, Vol. 3.
23. (b) Bassett, D. C. Principles of Polymer Morphology; Cambridge University Press: Cambridge, England, 1981.
24. (c) Strobl, G. Polym. Phys.; Springer: Heidelberg, Germany, 1997.
25. (d) Gedde, U. Polymer Physics, 1st ed.; Kluwer: Academic Publishers: Dordrecht, The Netherlands, 1995.
26. Studies on polymer crystallization close to room temperature (without active control of the specimen temperature) have been reported: (a) Hobbs, J. K.; McMaster, T. J.; Miles, M. J.; Barham, P. J. Polymer 1998, 39, 2437.
27. (b) McMaster, T. J.; Hobbs, J. K.; Barham, P. J.; Miles, M. J. Probe Microsc. 1997, 1, 43.
28. (c) Li, L.; Chan, C.-M.; Yeung, K. L.; Li, J.-X.; Ng, K.-M.; Lei, Y. Macromolecules 2001, 34, 316.
29. Kikkawa, Y.; Inoue, Y.; Abe, H.; Iwata, T.; Doi, Y. Polymer 2001, 42, 2707.
30. Basire, C.; Ivanov, D. A. Phys. Rev. Lett. 2000, 85, 5587.
31. Zhou, W.; Cheng, S. Z. D.; Putthanarat, S.; Eby, R. K.; Lotz, B.; Magonov, S. N.; Hsieh, E. T.; Geerts, R. G.; Palackal, S. J.; Hawley, G. R.; Welch, M. B. Macromolecules 2000, 33, 6861.
32. (a) Vancso, G. J.; Beekmans, L. G. M.; Pearce, R.; Trifonova, D.; Varga, J. J. Macromol. Sci. Phys. 1999, B 38, 491.
33. (b) Beekmans, L. G. M.; Vancso, G. J. Polymer 2000, 41, 8975.
34. (a) Hoobs, J. K.; Miles, M. J. Macromolecules 2001, 34, 353.
35. (b) Hobbs, J. K.; Humphris, A. D. L.; Miles, M. J. Macromolecules 2001, 34, 5508.
36. Schönherr, H.; Bailey, L. E.; Frank, C. W. Langmuir 2002, 18, 490.
37. (a) Schönherr, H.; Waymouth, R. M.; Hawker, C. J.; Frank, C. W. Polym. Mater. Sci. Eng. 2001, 84, 453.
38. (b) Schönherr, H.; Frank, C. W. Macromolecules 2003, 36, 1188-1198, 1199-1208.
39. Wiyatno, W.; Chen, Z.; Liu, Y.; Waymouth, R. M.; Brennan, K.; Krukonis, V. Macromolecules, submitted for publication.
40. We have previously shown that lamellar crystals of ES melt at temperatures of <120 °C.
41. The TM-AFM phase images are presented without absolute color scale. Since the magnitude of the signals is affected by various scan parameters, such as precise amplitude of the free vibrating cantilever, and the setpoint amplitude ratio, the values given by the AFM software can only be considered as relative values.
42. Information from Matweb database (http://www.matweb.com).
43. Perry's Chemical Engineers' Handbook, 6th ed.; Perry, R. H., Green, D., Eds.; McGraw-Hill: New York, 1984; pp 3-254.
44. Magonov, S. N.; Elings, V.; Whangbo, M.-H. Surf. Sci. 1997, 372, L385.
45. For a discussion of image contrast and its dependence on scanning conditions, see, e.g.: Bar, G.; Thomann, Y.; Brandsch, R.; Cantow, H.-J.; Whangbo, M.-H. Langmuir 1997, 13, 3807.
46. Lotz, B.; Wittmann, J. C. J. Polym. Sci., Polym. Phys. 1986, 24, 1541 and references cited therein.
47. (a) Bassett, D. C.; Olley, R. H. Polymer 1984, 25, 935.
48. (b) Olley, R. H.; Bassett, D. C. Polymer 1989, 30, 399.
49. Based on imaging of a calibration standard (Silicon grating GT01, Silicon MDT, Moscow, Russia), the radii of the tips used in our studies were estimated to be 5-15 nm.
50. The imaging conditions were noninvasive as can be concluded from the absence of an increased or decreased rate of nucleation (and growth) in the scanned area compared to previously unscanned areas.
51. ES of the ES fraction (1.73 MPa: Wiyatno, W.; Pople, J.; Gast, A. P.; Waymouth, R. M.; Fuller, G. G. Macromolecules 2002, 35, 8488, 8498)
52. iPP (1.0-1.7 GPa: Polymer Handbook, 4th ed.; Brandrup, J., Immergut, E. H., Eds.; Wiley: New York, 1989; pp V27), we can conclude a difference in modulus by 3 orders of magnitude. This difference is responsible for the pronounced contrast observed in the TM-AFM phase images.
53. In addition, tip convolution effects and the penetration of the AFM tip into the melt, which results in a sampling of a surface-near volume, lead to a significant overestimation of the surface area occupied by crystallites.
54. Lamellar thickness of 13-17 nm were reported for crystallization temperatures of 120 and 130 °C, see: (a) Ceres, B. V.; Schultz, J. M. J. Appl. Polym. Sci. 1984, 29, 4183.
55. Further comparable data can be found in: (b) Mezghani, K.; Campbell, R. A.; Philips, P. J. Macromolecules 1994, 27, 997.
56. We did not carry out a quantitative deconvolution of the AFM images since it is not a priori clear whether and to what extent these lamellar features protrude from the surface and since the information/penetration depths in our experiments are difficult to quantify.
57. In addition, the melting point of these lamellar features of ca. 100-120 °C, as determined by hot stage AFM, is consistent with a lamellar morphology rather than a simple fringed micellar morphology. The stepwise increase in temperature in increments of 5 °C and the subsequent stabilization period of several minutes resulted in an approximate mean heating rate of 0.6 °C/min.
58. Bartczak, Z.; Argon, A. S.; Cohen, R. E.; Kowalewski, T. Polymer 1999, 40, 2367 and references cited therein.
59. Lamberti, G.; Titomanilo, G. Polym. Bull. (Berlin) 2001, 46, 231.
60. Altenatively, the latter observation may indicate a transition from nucleation and growth to diffusion-controlled crystallization at later stages. A similar dendritic habit of crystals is well-known for a wide variety of materials.
61. Geil, P. H. Polymer Single Crystals; Wiley-Interscience: New York, 1963.
62. In a very recent paper, Lei et al. report on a similar observation of nuclei and embryonic crystals in poly(bisphenol A octane ether) observed by in situ AFM at room temperature (Lei, Y.-G.; Chan, C.-M.; Li, J.-X.; Ng, K.-M.; Wang, Y.; Jiang, Y.; Li, L. Macromolecules 2002, 35, 6751.).
63. Ivanov, D. A.; Amalou, Z.; Magonov, S. N. Macromolecules 2001, 34, 8944.
64. Sulchek, T.; Hsieh, R.; Adams, J. D.; Minne, S. C.; Quate, C. F.; Adderton, D. M. Rev. Sci. Instrum. 2000, 71, 2097.