Skip to main content
SpringerLink
Log in

Electron crystallography of linear polymers

  • Chapter
Characterization of Solid Polymers

Abstract

As a tool for the qualitative description of morphology, the electron microscope has enjoyed a long use in polymer science, as can be appreciated by examination of a recent monograph [1]. Similarly, the selected area electron diffraction mode of the electron microscope has been frequently employed for the determination of unit cell constants and symmetry for thin lamellar crystals [2]. This exploits the enhanced scattering cross-section of matter for electrons which enables these thin lamellar plates to be examined as single crystals [3]. What is not generally appreciated is that the electron microscope can also be employed as an instrument for the quantitative determination of linear polymer crystal structures [4].

This is a preview of subscription content, log in via an institution to check access.

Access this chapter

Log in via an institution
Chapter
USD 29.95
Price excludes VAT (USA)
  • Available as PDF
  • Read on any device
  • Instant download
  • Own it forever
eBook
USD 169.00
Price excludes VAT (USA)
  • Available as PDF
  • Read on any device
  • Instant download
  • Own it forever
Softcover Book
USD 219.99
Price excludes VAT (USA)
  • Compact, lightweight edition
  • Dispatched in 3 to 5 business days
  • Free shipping worldwide - see info
Hardcover Book
USD 219.99
Price excludes VAT (USA)
  • Durable hardcover edition
  • Dispatched in 3 to 5 business days
  • Free shipping worldwide - see info

Tax calculation will be finalised at checkout

Purchases are for personal use only

Institutional subscriptions

Preview

Unable to display preview. Download preview PDF.

Unable to display preview. Download preview PDF.

References

  1. Woodward, A.E. (1988) Atlas of Polymer Morphology, Hanser, Munich.

    Google Scholar 

  2. Geil, P.H. (1973) Polymer Single Crystals, Krieger, Huntington, NY.

    Google Scholar 

  3. Vainshtein, B.K. (1964) Structure Analysis by Electron Diffraction, Pergamon, Oxford, pp. 3–4.

    Google Scholar 

  4. Dorset, D.L. (1989) Electron diffraction from crystalline polymers, in Comprehensive Polymer Science, Vol. 1 Polymer Characterization, (eds C. Booth and C. Price), Pergamon, Oxford, pp. 651–68.

    Google Scholar 

  5. Fryer, J.R. and Dorset, D.L. (eds) (1991) Electron Crystallography of Organic Molecules, Kluwer, Dordrecht.

    Google Scholar 

  6. Cowley, J.M. (1981) Diffraction Physics, 2nd edn, North-Holland, Amsterdam.

    Google Scholar 

  7. Jap, B.K. and Glaeser, R.M. (1980) The scattering of high energy electrons. II Quantitative validity domains of the single-scattering approximations for organic crystals. Acta Crystallogr. A36 57–67.

    CAS  Google Scholar 

  8. Cowley, J.M., Rees, A.L.G. and Spink, J.A. (1951) Secondary electron scattering in electron diffraction. Proc. Phys. Soc. (London), A64, 609–19.

    Google Scholar 

  9. Cowley, J.M. (1961) Diffraction intensities from bent crystals. Acta Crystallogr., 14, 920–7.

    Article  CAS  Google Scholar 

  10. Moss, B. and Dorset, D.L. (1982) Refinement of linear polymer crystal structures determined from electron diffraction data. J. Polym. Sci. Polym. Phys. Ed. 20,1789–804.

    Article  CAS  Google Scholar 

  11. Dorset, D.L. (1980) Electron diffraction intensities from bent molecular organic crystals. Acta Crystallogr. A36, 592–600.

    CAS  Google Scholar 

  12. Moss, B. and Dorset, D.L. (1983) Dynamical electron diffraction from elastically bent organic crystals. Acta Crystallogr. A39, 609–15.

    CAS  Google Scholar 

  13. Wittmann, J.C., Hodge, A.M. and Lotz, B. (1983) Epitaxial crystallization of polymers onto benzoic acid: polyethylene and paraffins, aliphatic polyesters, and polyamides. J. Polym. Sci.-Polym. Phys. Ed. 21, 2495–509.

    Article  CAS  Google Scholar 

  14. Zeitler, E. (1991) Radiation damage in electron crystallography, in Electron Crystallography of Organic Molecules, (eds J.R. Fryer and D.L. Dorset), Kluwer, Dordrecht, pp. 355–60.

    Chapter  Google Scholar 

  15. Glaeser, R.M. (1975) Radiation damage and biological electron microscopy, in Physical Aspects of Electron Microscopy and Microbeam Analysis, (eds B.M. Siegel and D.R. Beaman), Wiley, New York, pp. 205–29.

    Google Scholar 

  16. Zemlin, F., Reuber, E., Beckmann, E. et al. (1985) Molecular resolution electron micrographs of monolamellar paraffin crystals. Science, 229, 461–2.

    Article  CAS  Google Scholar 

  17. Revol, J.F. and Manley, R. St. J. (1986) Lattice imaging in polyethylene single crystals. J. Mater. Sci. Lett. 5, 249–51.

    Article  CAS  Google Scholar 

  18. Downing, K.H. and Glaeser, R.M. (1986) Improvement in high resolution image quality of radiation-sensitive specimens with reduced spot size of the electron beam. Ultramicroscopy, 20, 269–78.

    Article  CAS  Google Scholar 

  19. Fujiyoshi, Y., Kobayashi, T., Ishizuka, K. et al. (1980) A new method for optimal-resolution electron microscopy of radiation-sensitive specimens. Ultramicroscopy, 5, 459–68.

    CAS  Google Scholar 

  20. Misell, D.L. (1978) Image Analysis Enhancement and Interpretation, North-Holland, Amsterdam, pp. 142–7.

    Google Scholar 

  21. Heel, M.V. and Keegshra, W. (1981) IMAGIC: a fast, flexible and friendly image analysis software system. Ultramicroscopy, 7,113–30.

    Article  Google Scholar 

  22. Frank, J. (1980) The role of correlation techniques in computer image processing, in Computer Processing of Electron Microscope Images, (ed. P.W. Hawkes), Springer, Berlin, pp. 187–222.

    Google Scholar 

  23. Buerger, M.J. (1959) Vector Space and Its Application in Crystal-Structure Investigation, Wiley, New York.

    Google Scholar 

  24. Brisse, F. (1989) Electron diffraction of synthetic polymers; The model compound approach to polymer structure. J. Electron Microsc. Techn. 11, 272–9.

    Article  CAS  Google Scholar 

  25. Perez, S. and Chanzy, H. (1989) Electron crystallography of polysaccharides. J. Electron Microsc. Techn. 11, 280–5.

    Article  CAS  Google Scholar 

  26. Hamilton, W.C. (1964) Statistics in Physical Science. Estimation, Hypothesis Testing and Least-Squares, Ronald, New York, pp. 157–60.

    Google Scholar 

  27. Dorset, D.L. Is electron crystallography possible? The direct determination of organic crystal structures. Ultramicroscopy, 38, 23–40.

    Google Scholar 

  28. Hauptman, H.A. (1972) Crystal Structure Determination. The Role of the Cosine Seminvariants, Plenum, New York.

    Google Scholar 

  29. Tsuji, M. (1989) Electron microscopy, in Comprehensive Polymer Science. Vol. 1 Polymer Characterization, (eds C. Booth and C. Price), Pergamon, Oxford, pp. 785–840.

    Google Scholar 

  30. Dorset, D.L., Hanlon, J., McConnell, C.H. et al. (1990) Why do polyethylene crystals have sectors? Proc. Natl. Acad. Sci. U.S.A. 87, 1696–700.

    Article  CAS  Google Scholar 

  31. Isoda, S., Tsuji, M., Ohara, M. et al. (1983) Direct observation of dislocation in polymer single crystals. Makromol. Chem. Rapid Commun. 4, 141–4.

    Article  CAS  Google Scholar 

  32. Kawaguchi, A., Isoda, S., Petermann, J. and Katayama, K. (1984) High resolution electron microscopy of (SN) x . Colloid Polym. Sci. 262, 429–34.

    Article  CAS  Google Scholar 

  33. Isoda, S., Tsuji, M., Ohara, M. et al. (1983) Structural analysis of β-form poly(p-xylylene) starting from a high-resolution image. Polymer 24,1155.

    Article  CAS  Google Scholar 

  34. Voigt-Martin, I.G. and Durst, H. (1987) Direct observation of smectic layers in side chain liquid crystal polymer films. Liquid Crystals, 2, 601–10.

    Article  CAS  Google Scholar 

  35. Vainshtein, B.K. and Tatarinova, L.I. (1967) Electron-diffraction studies of synthetic polypeptides, in Conformation of Biopolymers Vol. 2, (ed. G.N. Ramachandran), Academic, New York, pp. 569–82.

    Google Scholar 

  36. Dorset, D.L. (1991) Electron crystallography of linear polymers: direct structure analysis of poly(ε-caprolactone). Proc. Natl. Acad. Sci. U.S.A. 88, 5499–502.

    Article  CAS  Google Scholar 

  37. Chatani, Y., Okita, Y., Tadokoro, H. and Yamashita, Y. (1970) Structural studies of polyesters III. Crystal structure of poly-ε-caprolactone. Polym. J., 1, 555–62.

    Article  CAS  Google Scholar 

  38. Dorset, D.L., Hu, H. and Jäger, J. Continuous diffuse scattering from polymethylene chains — an electron diffraction study of crystalline disorder. Acta Crystallogr. A47, 543–49.

    Google Scholar 

  39. Dorset, D.L. and Zemlin, F. (1990) Direct phase determination in electron crystallography. The crystal structure of an n-paraffin. Ultramicroscopy, 33, 227–36.

    Article  CAS  Google Scholar 

  40. Dorset, D.L., Tivol, W.F. and Turner, J.N. Electron crystallography at atomic resolution — ab initio structure analysis of copper perchlorophthalocyanine. Ultramicroscopy, 38, 41–5.

    Google Scholar 

  41. Uyeda, N., Kobayashi, T., Ishizuka, K. and Fujiyoshi, Y. (1978) High voltage electron microscopy for image discrimination of constituent atoms in crystals and molecules. Chem. Scripta, 14, 47–61.

    Google Scholar 

  42. Chanzy, H., Folda, T., Smith, P., Gardner, K.H. and Revol, J.F. (1986) Lattice imaging in polytetrafluoroethylene single crystals. J. Mater. Sci. Lett. 5, 1045–7.

    Article  CAS  Google Scholar 

  43. Pradere, P., Revol, J.F., Nguyea, L. and Manley, R. St. J. (1988) Lattice imaging of poly-4-methyl-pentene-1 single crystals: use and misuse of Fourier averaging techniques. Ultramicroscopy 25 69–80.

    Article  CAS  Google Scholar 

  44. Revol, J.F., Chanzy, H.D., Deslaudes, Y. and Marchessault, R.H. (1989) High resolution electron microscopy of poly(β-hydroxybutyrate). Polymer, 30, 1973–6.

    Article  Google Scholar 

  45. Revol, J.-F. (1989) Lattice resolution in α-chitin. Int. J. Biol. Macromol. 11, 233–5.

    Article  CAS  Google Scholar 

  46. Revol, J.-F. and Chanzy, H. (1986) High-resolution electron microscopy of β-chitin microfirils. Biopolymers, 25,1599–1607.

    Article  Google Scholar 

  47. Sugiyama, J., Harada, H. and Saihi, H. (1987) Crystalline morphology of Valonia macrophysa cellulose I revealed by direct lattice imaging. Int. J. Biol. Macromol. 9, 122–30.

    Article  CAS  Google Scholar 

  48. Tsuji, M., Isoda, S., Ohara, M., Kawaguchi, A. et al. (1982) Direct imaging of molecular chains in a poly(ρ-xylylene) single crystal. Polymer, 23, 1568–74.

    Article  CAS  Google Scholar 

  49. Tsuji, M., Roy, S.K. and Manley, R. St. J. (1984) Direct lattice imaging in single crystals of isotactic polystyrene. Polymer 25, 1573–6.

    Article  CAS  Google Scholar 

  50. Tsuji, M., Ohara, M., Isoda, S., Kawaguchi, A. et al. (1989) Direct imaging of the molecular arrangement in a radiation-sensitive polymer single crystal; poly(tetramethyl-ρ-silphenylene siloxane). Phil. Mag. B54, 393–403.

    Article  Google Scholar 

  51. Uemura, A., Tsuji, M., Kawaguchi, A. and Katayama, K. (1988) High-resolution electron microscopy of solution-grown crystals of poly(p-phenylene sulphide). J. Mater. Sci. 23, 1506–9.

    Article  CAS  Google Scholar 

  52. Dorset, D.L. (1977) Perfluoroalkane. A model for the hexagonal methylene subcell? Chem. Phys. Lipids, 20, 13–19.

    Article  CAS  Google Scholar 

  53. Day, E. and Lando, J.B. (1980) Structure determination of a poly(diacetylene) monolayer. Macromolecules, 13, 1483–7.

    Article  CAS  Google Scholar 

  54. Shimamura, K., Karasz, F.E., Hirsch, J.A. and Chien, J.C.W. (1981) Crystal structure of trans-polyacetylene. Makromol. Sci. Rapid Commun. 2, 473–80.

    Article  CAS  Google Scholar 

  55. Hasegawa, H., Claffey, W. and Geil, P.H. (1977) Analysis of the crystal structure of poly (ethylene sulfide) by electron diffraction. J. Macromol. Sci.-Phys. B13, 89–100.

    CAS  Google Scholar 

  56. Moss, B. and Dorset, D.C. (1983) Polyethylene sulfide): re-evaluation of the electron diffraction structure analysis. J. Macromol. Sci.-Phys. B22, 69–77.

    CAS  Google Scholar 

  57. Claffey, W., Gardner, K., Blackwell, J., Lando, J. et al. (1974) Structure analysis of polymer single crystals by electron diffraction. Phil. Mag. 30, 1223–32.

    Article  CAS  Google Scholar 

  58. Roche, E., Chanzy, H., Boudeulle, M., Marchessault, R.H. et al. (1978) Three-dimensional crystalline structure of cellulose triacetate II. Macromolecules, 11, 86–94.

    Article  CAS  Google Scholar 

  59. Perez, S., Roux, M., Revol, J.F. and Marchessault, R.H. (1979) Dehydration of nigeran crystal: crystal structure and morphological aspects. J. Mol. Biol. 129, 113–33.

    Article  CAS  Google Scholar 

  60. Poulin-Dandurand, S., Perez, S., Revol, J.F. and Brisse, F. (1974) The crystal structure of poly(trimethylene terephthalate) by X-ray and electron diffraction. Polymer, 20, 419–26.

    Article  Google Scholar 

  61. Brisse, F., Palmer, A., Moss, B., Dorset, D. et al. (1984) Poly(hexamethylene terephthalate) Part II: the crystal structure of Form I and Form II from electron and X-ray diffraction and packing analyses. Eur. Polym. J. 20, 791–7.

    Article  CAS  Google Scholar 

  62. Thakur, M. and Lando, J.B. (1983) Structure determination of the macro-monomer poly(1,11-dodecadiyne) and its cross-linked product. Macromolecules, 16, 143–6.

    Article  Google Scholar 

  63. Tatarinova, L.I. and Vainshtein, B.K. (1962) Issledovanie poli-γ-metil-l-glutamata v α-forme metodom difraktsii elektronov. Visokomolek. Soed, 4, 261–9.

    Google Scholar 

  64. Vainshtein, B.K. and Tatarinova, L.I. (1967) The β-form of poly-γ-methyl-l-glutamate. Sov. Phys. Crystallogr. 11, 494–8.

    Google Scholar 

  65. Guizard, C., Chanzy, H. and Sarko, A. (1985) The molecular and crystal structure of dextrans: a combined electron and X-ray diffraction study II. Low temperature, hydrated polymorph. J. Mol. Biol. 183, 397–408.

    Article  CAS  Google Scholar 

  66. Guizard, C., Chanzy, H. and Sarko, A. (1984) Molecular and crystal structure dextrans: a combined electron and X-ray diffraction study. 1. The anhydrous high-temperature polymorph. Macromolecules, 17,100–7.

    Article  CAS  Google Scholar 

  67. Hu, H. and Dorset, D.L. (1989) Three-dimensional electron diffraction structure analysis of polyethylene. Acta Crystallogr. B45, 283–90.

    CAS  Google Scholar 

  68. Dorset, D.L. (1991) Electron diffraction structure analysis of polyethylene. A direct phase determination. Macromolecules, 24, 1175–8.

    Article  CAS  Google Scholar 

  69. Hu, H. and Dorset, D.L. (1990) Crystal structure of poly(ε caprolactone). Macromolecules 23, 4604–7.

    Article  CAS  Google Scholar 

  70. Boudeulle, M. (1975) β-poly(sulfur-nitride) (SN) x . Cryst. Struct. Commun. 4, 9–12.

    CAS  Google Scholar 

  71. Chien, J.C.W., Karasz, F.E. and Shimamura, K. (1982) Crystal structure of pristane and iodine-doped cis-polyacetylene. Macromolecules, 15, 1012–7.

    Article  CAS  Google Scholar 

  72. Claffey, W. and Blackwell, J. (1976) Electron diffraction of Valonia cellulose. A quantitative interpretation. Biopolymers, 15, 1903–15.

    Article  CAS  Google Scholar 

  73. Chanzy, H., Perez, S., Miller, D.P. et al. (1987) An electron diffraction study of mannan I. Crystal and molecular structure. Macromolecules, 20, 2407–13.

    Article  CAS  Google Scholar 

  74. Brisson, J., Chanzy, H. and Winter, W.T. (1991) The crystal and molecular structure of VH amylase by electron diffraction analysis. Int. J. Biol. Macromol. 13, 31–9.

    Article  CAS  Google Scholar 

  75. Brisse, F., Rémillard, B. and Chanzy, H. (1984) Pory(l,4-trans-cyclohexane diyl dimethylene succinate): A structural determination using X-ray and electron diffraction. Macromolecules 17, 1980–7.

    Article  CAS  Google Scholar 

  76. Meille, S.V., Brückner, S. and Lando, J.B. (1989) The structure of γ-poly-pivalolactone: a combined analysis of single-crystal electron diffraction data and powder X-ray diffraction profiles with the Rietveld method. Polymer, 30, 786–92.

    Article  CAS  Google Scholar 

  77. Bricogne, G. (1984) Maximum entropy and the foundations of direct methods. Acta Crystallogr. A40, 410–45.

    CAS  Google Scholar 

  78. Dong, W., Baird, T., Fryer, J.R., Gilmore, G.J. et al. (1992) Extension of electron microscope resolution to 1 Å by entropy maximisation and likelihood estimation. Nature, 355, 605–9.

    Article  CAS  Google Scholar 

Download references

Authors
  1. D. L. Dorset
    View author publications

    You can also search for this author in PubMed Google Scholar

Editor information

Editors and Affiliations

  1. Division of Applied Physics, School of Science, Sheffield Hallam University, Sheffield, S1 1WB, UK

    S. J. Spells

Rights and permissions

Reprints and permissions

Copyright information

© 1994 Springer Science+Business Media Dordrecht

About this chapter

Cite this chapter

Dorset, D.L. (1994). Electron crystallography of linear polymers. In: Spells, S.J. (eds) Characterization of Solid Polymers. Springer, Dordrecht. https://doi.org/10.1007/978-94-011-1262-8_1

Download citation

  • DOI: https://doi.org/10.1007/978-94-011-1262-8_1

  • Publisher Name: Springer, Dordrecht

  • Print ISBN: 978-94-010-4550-6

  • Online ISBN: 978-94-011-1262-8

  • eBook Packages: Springer Book Archive

Publish with us

Policies and ethics

Search

Navigation