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Single stage electrochemical exfoliation method for the production of few-layer graphene via intercalation of tetraalkylammonium cations

Cooper, Adam J., Wilson, Neil R., Kinloch, Ian A., Dryfe, Robert A.W.
Carbon 2014 v.66 pp. 340-350
Raman spectroscopy, X-ray photoelectron spectroscopy, atomic force microscopy, cations, electrochemistry, electrodes, graphene, quaternary ammonium compounds, solvents, sonication, ultrasonic treatment
We present a non-oxidative production route to few layer graphene via the electrochemical intercalation of tetraalkylammonium cations into pristine graphite. Two forms of graphite have been studied as the source material with each yielding a slightly different result. Highly orientated pyrolytic graphite (HOPG) offers greater advantages in terms of the exfoliate size but the source electrode set up introduces difficulties to the procedure and requires the use of sonication. Using a graphite rod electrode, few layer graphene flakes (2nm thickness) are formed directly although the flake diameters from this source are typically small (ca. 100–200nm). Significantly, for a solvent based route, the graphite rod does not require ultrasonication or any secondary physical processing of the resulting dispersion. Flakes have been characterized using Raman spectroscopy, atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS).