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Intercalation of molecular species into the interstitial sites of fullerene

Published online by Cambridge University Press:  31 January 2011

Roger A. Assink ,
James E. Schirber ,
Douglas A. Loy ,
Bruno Morosin  and
Gary A. Carlson
Roger A. Assink*
Affiliation:
Sandia National Laboratories, Albuquerque, New Mexico 87185
James E. Schirber
Affiliation:
Sandia National Laboratories, Albuquerque, New Mexico 87185
Douglas A. Loy
Affiliation:
Sandia National Laboratories, Albuquerque, New Mexico 87185
Bruno Morosin
Affiliation:
Sandia National Laboratories, Albuquerque, New Mexico 87185
Gary A. Carlson
Affiliation:
Sandia National Laboratories, Albuquerque, New Mexico 87185
*
a)Author to whom correspondence should be addressed.
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Abstract

Molecular species were found to diffuse readily into the octahedral interstitial sites of the fcc lattice of C60. The 13C NMR spectrum of C60 under magic angle spinning (MAS) conditions consisted of a primary resonance at 143.7 ppm and a minor peak shifted 0.7 ppm downfield. The downfield shift obeys Curie's law and is attributed to the Fermi-contact interaction between paramagnetic oxygen molecules and all 60 carbon atoms of rapidly rotating adjacent C60 molecules. Exposure of C60 to 1 kbar oxygen for 1.75 h at room temperature resulted in a spectrum of seven evenly spaced resonances corresponding to the filling of 0 to 6 of the adjacent octahedral interstitial sites with oxygen molecules. The distribution of site occupancies about a C60 molecule provided evidence that the intercalation process is controlled by diffusion kinetics. Exposure to 0.14 kbar hydrogen gas at room temperature for 16 h filled a substantial fraction of the interstitial sites of C60 and C70 with hydrogen molecules.

Type
Articles
Information
Journal of Materials Research , Volume 7 , Issue 8 , August 1992 , pp. 2136 - 2143
Copyright
Copyright © Materials Research Society 1992

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References

1.Kioto, H. W., Heath, J. R., O'Brien, S. C., Curl, R. F., and Smalley, R. E., Nature 318, 162 (1985).Google Scholar
2.Kratschmer, W., Lamb, L. D., Fostiropoulos, K., and Huffman, D. R., Nature 347, 354 (1990).CrossRefGoogle Scholar
3.Haddon, R. C.et al., Nature 350, 320 (1990); A. F. Hebard et al., Nature 350, 600 (1991); Z. Zhang, C. Chen, S. Kelty, H. Dai, and C M. Lieber, Nature 353, 333 (1991) and references therein.CrossRefGoogle Scholar
4.Hawkins, J. M.et al., J. Org. Chem. 55, 6250 (1990); P. J. Fagan, J. C. Calabrese, and B. Malone, Science 252, 1160 (1991); A. L. Balch, V. J. Catalano, J. W. Lee, M. M. Olmstead, and S. R. Parkin, J. Am. Chem. Soc. 113, 8953 (1991); R. S. Koefod, M. F. Hudgens, and J. R. Shaply, J. Am. Chem. Soc. 113, 8957 (1991); F. Wudl, Large Carbon Clusters, ACS Symposium, Atlanta, GA, July 1991; H. Selig et al., J. Am. Chem. Soc. 113, 5907 (1991); J. W. Bausch et al., J. Am. Chem. Soc. 113, 3205 (1991); P. J. Krusic etal, J. Am. Chem. Soc.113, 6274 (1991); P. J. Krusic, E.Wasserman, P. N. Keizer, J. R. Morton, and K. F. Preston, Science 54, 1183 (1991); P-M. Allemand et al., J. Am. Chem. Soc. 113, 1050 (1991).Google Scholar
5.Fleming, R. M.et al., Phys. Rev. B 44, 888 (1991); untwinned crystals have been shown to be orthorhombic a = 10.34, b = 31.53, c = 10.18 Å, Cmcm with buckyballs centered at 0.0, 0.1396, 1/4 on 4-fold mm sites and toluene disordered on similar sites on the ab and be planes at z — 1/4 with carbon positions of y = 0.36 to 0.51 (B. Morosin, X. D. Xiang, and A. Zettl, unpublished).Google Scholar
6.Morosin, B.et al., Physica C 184, 21 (1991).CrossRefGoogle Scholar
7. (A) The sample was purified by chromatography [Allemand, P-M.et al., J. Am. Chem. Soc. 113, 1050 (1991)] from toluene soluble soot purchased from Texas Fullerene Corp., Houston, TX. The starting material was annealed for 2 h at 225 °C and this step sharpened the x-ray powder diffraction lines appreciably as well as annealed and removed the stacking faults and defects contributing to the “foot” character of the (111) line. (B) The sample was purchased as 99.5% pure 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 (11) line.Google Scholar
8.Creegan, K. M.et al., poster presented at the MRS Fall Meeting, Boston, MA, 2–6 December 1991.Google Scholar
9.Jesson, J. P., in The Paramagnetic Shift, edited by Mar, G. N. La, Horrocks, W. De W., Jr., and Holm, R. H. (Academic Press, New York, 1973), pp. 1–52.Google Scholar
10.Tycko, R.et al. J. Phys. Chem. 95, 518 (1991); C. S. Yannoni, R. D. Johnson, G. Meijer, D. S. Bethune, and J. R. Salem, J. Phys. Chem. 95, 9 (1991).CrossRefGoogle Scholar
11.Tycko, R.et al., Phys. Rev. Lett. 67, 1886 (1991).CrossRefGoogle Scholar
12.Devreux, F., Boilot, J. P., Chaput, F., and Sapoval, B., Phys. Rev. Lett. 65, 614 (1990).CrossRefGoogle Scholar
13.Haeberlin, U. and Waugh, J. S., Phys. Rev. 185, 420 (1969).CrossRefGoogle Scholar
14.Heiney, P.et al., Phys. Rev. Lett. 66, 2911 (1991); S. Liu, Y. Lu, M. M. Kappes, and J. A. Ibers, Science 254, 408 (1991); W. I. F. David et al., Nature 353, 147 (1991).CrossRefGoogle Scholar
15.Pauling, L., The Nature of the Chemical Bond (Cornell University Press, 1960), pp. 259–264.Google Scholar
16. To be published.Google Scholar
17. The molecular mechanics calculations were performed using the Dreiding II force field model [Mayo, S. L., Olafson, B. D., and Goddard, W. A., J. Phys. Chem. 94, 8897 (1990)] implemented on Biograf software, Molecular Simulations, Inc., Sunnyvale, CA.CrossRefGoogle Scholar