Abstract
The structural evolution of carbon nanofibers submitted to high-temperature (1800, 2300, and 2800 °C) heat treatments has been investigated at the nanometric and atomic scales by means of scanning tunneling microscopy (STM). To complement the local STM observations, X-ray diffraction and Raman spectroscopy characterization of the samples were also carried out. On the nanometer scale, the as-grown nanofibers displayed an isotropic platelet morphology that developed into striped arrangements of increasing width at 1800 and 2300 °C, and into large, atomically flat terraces at 2800 °C. On the atomic scale, the starting nanofibers were characterized by tiny (≲2 nm) crystallites. The crystallites were observed to coalesce at 1800 °C into appreciably larger (∼3–4 nm) although still defective units. Atomic structures evidencing truly graphitic ordering (i.e. the typical STM triangular pattern with a periodicity of 0.25 nm) started to develop at 2300 °C. At this temperature, a segregation of graphitic domains and highly defective areas was noticed and attributed mainly to the mobility and subsequent aggregation of point defects (atomic vacancies). Long-range atomic-scale order was generally established in the nanofibers heat treated at 2800 °C, where only some incompletely graphitized, fragmentary graphenes were left on the surface.
Similar content being viewed by others
References
R.T.K. Baker, M.A. Barber, R.J. Waite, P.S. Harris, F.S. Feates: J. Catal. 26, 51 (1972)
R.T.K. Baker, P.S. Harris, R.B. Thomas, R.J. Waite: J. Catal. 30, 86 (1973)
R.T.K. Baker, P.S. Harris, S. Terry: Nature 253, 37 (1975)
R.T.K. Baker, R.J. Waite: J. Catal. 37, 101 (1975)
M. Audier, J. Guinot, M. Coulon, L. Bonnetain: Carbon 19, 99 (1981)
M. Audier, A. Oberlin, M. Oberlin, M. Coulon, L. Bonnetain: Carbon 19, 217 (1981)
L.P. Biró, C.A. Bernardo, G.G. Tibbetts, P. Lambin (Eds.): Carbon Filaments and Nanotubes: Common Origins, Differing Applications? (Kluwer, Dordrecht 2001)
S. Helveg, C. López-Cartes, J. Sehested, P.L. Hansen, B.S. Clausen, J.R. Rostrup-Nielsen, F. Abild-Pedersen, J.K. Nørskov: Nature 427, 426 (2004)
B.O. Boskovic, V. Stolojan, R.U.A. Khan, S. Haq, S.R.P. Silva: Nat. Mater. 1, 165 (2002)
S. Kumar, H. Doshi, M. Srinivasarao, J.O. Park, D.A. Schiraldi: Polymer 43, 1701 (2002)
D. Shi, J. Lian, P. He, L.M. Wang, F. Xiao, L. Yang, M.J. Schulz, D.B. Mast: Appl. Phys. Lett. 83, 5301 (2003)
D.J. Browning, M.L. Gerrard, J.B. Lakeman, I.M. Mellor, R.J. Mortimer, M.C. Turpin: Nano Lett. 2, 201 (2002)
A.D. Lueking, R.T. Yang, N.M. Rodriguez, R.T.K. Baker: Langmuir 20, 714 (2004)
N.M. Rodriguez, M.-S. Kim, R.T.K. Baker: J. Phys. Chem. 98, 13108 (1994)
T.G. Ros, A.J. van Dillen, J.W. Geus, D.C. Koningsberger: Chem. Eur. J. 8, 2868 (2002)
T.G. Ros, D.E. Keller, A.J. van Dillen, J.W. Geus, D.C. Koningsberger: J. Catal. 211, 85 (2002)
E.S. Steigerwalt, G.A. Deluga, C.M. Lukehart: J. Phys. Chem. B 106, 760 (2002)
R. Vieira, C. Pham-Huu, N. Keller, M.J. Ledoux: Chem. Commun. 954 (2002)
S.-H. Yoon, C.-W. Park, H. Yang, Y. Korai, I. Mochida, R.T.K. Baker, N.M. Rodriguez: Carbon 42, 21 (2004)
M. Endo, K. Nishimura, Y.A. Kim, K. Hakamada, T. Matushita, M.S. Dresselhaus, G. Dresselhaus: J. Mater. Res. 14, 4474 (1999)
G.-B. Zheng, H. Sano, Y. Uchiyama: Carbon 41, 853 (2003)
M. Endo, Y.A. Kim, T. Hayashi, T. Yanagisawa, H. Muramatsu, M. Ezaka, H. Terrones, M. Terrones, M.S. Dresselhaus: Carbon 41, 1941 (2003)
H. Saadaoui, J.C. Roux, S. Flandrois, B. Nysten: Carbon 31, 481 (1993)
B. Nysten, J.-C. Roux, S. Flandrois, C. Daulan, H. Saadaoui: Phys. Rev. B 48, 12527 (1993)
H.N. Lei, A. Métrot, M. Troyon: Carbon 32, 79 (1994)
S.N. Magonov, M.-H. Whangbo: Surface Analysis with STM and AFM (VCH, Weinheim 1996)
J.R. Hahn, H. Kang, S. Song, I.C. Jeon: Phys. Rev. B 53, R1725 (1996)
J.I. Paredes, A. Martínez-Alonso, J.M.D. Tascón: Langmuir 18, 4314 (2002)
J.I. Paredes, A. Martínez-Alonso, J.M.D. Tascón: Carbon 39, 1575 (2001)
J.I. Paredes, A. Martínez-Alonso, J.M.D. Tascón: Carbon 40, 1101 (2002)
Y.A. Kim, T. Matusita, T. Hayashi, M. Endo, M.S. Dresselhaus: Carbon 39, 1747 (2001)
I.C. Finegan, G.G. Tibbetts: J. Mater. Res. 16, 1668 (2001)
G.G. Tibbetts, D.W. Gorkiewicz, R.L. Alig: Carbon 31, 809 (1993)
G.G. Tibbetts, G.L. Doll, D.W. Gorkiewicz, J.J. Moleski, T.A. Perry, C.J. Dasch, M.J. Balogh: Carbon 31, 1039 (1993)
T.C. Chieu, M.S. Dresselhaus, M. Endo: Phys. Rev. B 26, 5867 (1982)
A.M. Rao, E. Richter, S. Bandow, B. Chase, P.C. Eklund, K.A. Williams, S. Fang, K.R. Subbaswamy, M. Menon, A. Thess, R.E. Smalley, G. Dresselhaus, M.S. Dresselhaus: Science 275, 187 (1997)
M.S. Dresselhaus, G. Dresselhaus, A. Jorio, A.G. Souza Filho, M.A. Pimenta, R. Saito: Acc. Chem. Res. 35, 1070 (2002)
H. Jantoljak, J.-P. Salvetat, L. Forró, C. Thomsen: Appl. Phys. A 67, 113 (1998)
X. Zhao, Y. Ando, L.-C. Qin, H. Kataura, Y. Maniwa, R. Saito: Chem. Phys. Lett. 361, 169 (2002)
J.M. Benoit, J.P. Buisson, O. Chauvet, C. Godon, S. Lefrant: Phys. Rev. B 66, 073417 (2002)
D. Roy, M. Chhowalla, H. Wang, N. Sano, I. Alexandrou, T.W. Clyne, G.A.J. Amaratunga: Chem. Phys. Lett. 373, 52 (2003)
M. Endo, K. Takeuchi, K. Kobori, K. Takahashi, H.W. Kroto, A. Sarkar: Carbon 33, 873 (1995)
N. Jiang, R. Koie, T. Inaoka, Y. Shintani, K. Nishimura, A. Hiraki: Appl. Phys. Lett. 81, 526 (2002)
H. Chang, A.J. Bard: J. Am. Chem. Soc. 113, 5588 (1991)
J.R. Hahn, H. Kang: Phys. Rev. B 60, 6007 (1999)
P.L. Giunta, S.P. Kelty: J. Chem. Phys. 114, 1807 (2001)
P. Samorí, N. Severin, C.D. Simpson, K. Müllen, J.P. Rabe: J. Am. Chem. Soc. 124, 9454 (2002)
K.H. Lee, H.M. Lee, H.M. Eun, W.R. Lee, S. Kim, D. Kim: Surf. Sci. 321, 267 (1994)
B. An, S. Fukuyama, K. Yokogawa, M. Yoshimura: J. Appl. Phys. 92, 2317 (2002)
K. Sattler: Carbon 33, 915 (1995)
J.I. Paredes, F. Suárez-García, S. Villar-Rodil, A. Martínez-Alonso, J.M.D. Tascón, E.J. Bottani: J. Phys. Chem. B 107, 8905 (2003)
Author information
Authors and Affiliations
Corresponding author
Additional information
PACS
81.07.-b; 81.40.Ef; 68.37.Ef
Rights and permissions
About this article
Cite this article
Paredes, J., Burghard, M., Martínez-Alonso, A. et al. Graphitization of carbon nanofibers: visualizing the structural evolution on the nanometer and atomic scales by scanning tunneling microscopy. Appl. Phys. A 80, 675–682 (2005). https://doi.org/10.1007/s00339-004-3109-9
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s00339-004-3109-9