Skip to main content
Log in

An NMR Study of the Occupation of C60 Interstitial Sites by Oxygen Molecules

  • Published:
MRS Online Proceedings Library Aims and scope

Abstract

The 13C NMR of FCC C60 under magic angle spinning (MAS) conditionsyields linewidths on the order of 1 Hz at fields of 4.7 T. The spectrum consists of a primary resonance at 143.7 ppm and a minor peak shifted 0.7 ppm downfield. The intensity of the minor resonance relative to the primary resonance was found to vary from 0.6 to 5.5 % depending on the sample history. The downfield shift obeys Curie's law and isattributed to the Fermi contact coupling interaction between paramagnetic oxygen molecules and all 60 carbon atoms of rapidly rotating adjacent C60 molecules. Exposure of the sample to 1 kbar oxygen for 1 3/4 hours resulted in a spectrum of 7 evenly spaced resonances corresponding to 0 to 6 of the adjacent octahedral interstitial sites being filled with oxygen molecules. At ambient pressure, the oxygen diffused out of the lattice on time scales ranging from hours to days.

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

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Similar content being viewed by others

References

  1. H. W. Kroto, J. R. Heath, S. C. O'Brien, R. F. Curl, R. E. Smalley, Nature318, 162 (1985).

    Article  CAS  Google Scholar 

  2. W. Kratschmer, L. D. Lamb, K. Fostiropoulos, D. R. Huffman, Nature347, 354 (1990).

    Article  Google Scholar 

  3. (A) The sample was purified by chromatography ( P.-M. Allemand et al., J. Am. Chem. Soc.113, 1050 (1991)) from toluene soluble soot purchased from Texas Fullerene Corp, Houston, TX. This material was then annealed for 2 hrs at 225 C. Annealing sharpened the x-ray powder diffraction lines and removed the stacking faults and defects contributing to the “foot” character of the (111) line. (B) Additional material was purchased as 99.5 % pure C60 from Texas Fullerene Corp. This sample as-received showed broad x-ray lines which became sharp upon annealing at 225 C with no evidence of a “foot” on the (111) line. Identical NMR results were obtained with this material.

    Article  Google Scholar 

  4. K. M. Creegan et al., poster presented at the MRS Fall Meeting, Boston, MA, 2–6 December 1991.

  5. J. P. Jesson in The Paramagnetic Shift, G. N. La Mar, W. DeW. HorrocksJr., and R. H. Holm, Eds. (Academic Press, New York, 1973) pp. 1–52.

  6. R. Tycko et al., J. Phys. Chem.95, 518 (1991); C. S. Yannoni, R. D. Johnson, G. Meijer, D. S. Bethune, J. R. Salem, J. Phys. Chem. 95, 9 (1991).

    Article  CAS  Google Scholar 

  7. R. Tycko et al., Phys. Rev. Lett.67, 1886 (1991).

    Article  CAS  Google Scholar 

  8. P. Heiney et al., Phys. Rev. Lett.66, 2911 (1991); S. Liu, Y. Lu, M. M. Kappes, J. A. Ibers, Science 254, 408 (1991); W. I. F. David et al., Nature 353, 147 (1991).

    Article  CAS  Google Scholar 

  9. L. Pauling, The Nature of the Chemical Bond (Cornell University Press, 1960) pp. 259–64.

    Google Scholar 

  10. R. A. Assink, J. E. Schirber, Douglas A. Loy, B. Morosin and G. A. Carlson, J. Mater. Res., accepted for publication.

Download references

Acknowledgement

This work was supported by the U.S. Dept. of Energy under contract DE-AC04-76DP00789.

Author information

Authors and Affiliations

Authors

Rights and permissions

Reprints and permissions

About this article

Cite this article

Assink, R.A., Loy, D.A., Schirber, J.E. et al. An NMR Study of the Occupation of C60 Interstitial Sites by Oxygen Molecules. MRS Online Proceedings Library 270, 255–260 (1992). https://doi.org/10.1557/PROC-270-255

Download citation

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1557/PROC-270-255

Navigation