Preparation of graphene oxide and characterisation using electron spectroscopy

B. Lesiak, L. Stobinski, A. Malolepszy, M. Mazurkiewicz, L. Kövér, J. Tóth

Research output: Contribution to journalArticle

31 Citations (Scopus)


Graphene oxide was prepared from commercial graphene powder (G) platelets of 8 nm thickness by oxidation in ozone (G-O3) and low-energy (cold) glow air plasma in a pink region (G-PP). X-ray photoelectron spectroscopy (XPS) was applied for chemical characterisation of the atomic content and for obtaining quantitative information on C hybridisation. Reflection electron energy loss spectroscopy (REELS) was used for characterising the surface structure including the content of surface and bulk carbon atoms of sp2 and sp 3 hybridisation. The G-O3 and G-PP graphene oxide samples contain a low amount of C sp3 bonds and carbon-oxygen groups in comparison to graphene oxide prepared by the "wet" chemical methods. Oxidation of commercial graphene platelets powder, especially in air plasma, leads to increasing surface C sp3 and significantly bulk C sp3 contributions, indicating intercalation by oxygen groups. The intensity ratio of the REELS π + σ C sp2 bulk to the C sp2 surface energy loss peaks, decreasing in the order G>G-O3>G-PP, indicates exfoliation of layers in G-O3 and G-PP by oxygen functional groups and water with decreasing average number of layers in graphene oxide nanostructures due to oxidation. Although, the "wet" chemical methods are more effective for oxidation leading to a larger amount of C sp3 and oxygen groups, the proposed methods of oxidation by ozonation and in air plasma are inexpensive, safe, effective, environmentally friendly and do not result in toxic chemical waste products.

Original languageEnglish
Pages (from-to)92-99
Number of pages8
JournalJournal of Electron Spectroscopy and Related Phenomena
Publication statusPublished - Mar 2014


  • Graphene
  • Graphene oxidation
  • Graphene oxide
  • XPS

ASJC Scopus subject areas

  • Electronic, Optical and Magnetic Materials
  • Radiation
  • Atomic and Molecular Physics, and Optics
  • Condensed Matter Physics
  • Spectroscopy
  • Physical and Theoretical Chemistry

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