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Scalable production of large quantities of defect-free few-layer graphene by shear exfoliation in liquids

Nature Materials volume 13, pages 624–630 (2014)Cite this article

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Abstract

To progress from the laboratory to commercial applications, it will be necessary to develop industrially scalable methods to produce large quantities of defect-free graphene. Here we show that high-shear mixing of graphite in suitable stabilizing liquids results in large-scale exfoliation to give dispersions of graphene nanosheets. X-ray photoelectron spectroscopy and Raman spectroscopy show the exfoliated flakes to be unoxidized and free of basal-plane defects. We have developed a simple model that shows exfoliation to occur once the local shear rate exceeds 104 s−1. By fully characterizing the scaling behaviour of the graphene production rate, we show that exfoliation can be achieved in liquid volumes from hundreds of millilitres up to hundreds of litres and beyond. The graphene produced by this method performs well in applications from composites to conductive coatings. This method can be applied to exfoliate BN, MoS2 and a range of other layered crystals.

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Figure 1: Production of graphene by shear mixing.
Figure 2: Characterization of the exfoliation mechanism.
Figure 3: Scaling of graphene production using a shear mixer.
Figure 4: Scaling of graphene production using a shear mixer.
Figure 5: Applications of mixer-exfoliated graphene.

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Acknowledgements

We thank Science Foundation Ireland (11/PI/1087), the European Research Council (SEMANTICS and 2DNanoCaps), the Graphene Flagship Project (no. 604391) and Thomas Swan for financial support. We acknowledge SuperSTEM and the CRANN Advanced Microscopy Laboratory for technical support.

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Authors and Affiliations

  1. Centre for Research on Adaptive Nanostructures and Nanodevices (CRANN), Trinity College Dublin, Dublin 2, Ireland

    Keith R. Paton, Eswaraiah Varrla, Claudia Backes, Ronan J. Smith, Umar Khan, Arlene O’Neill, Conor Boland, Mustafa Lotya, Oana M. Istrate, Paul King, Tom Higgins, Sebastian Barwich, Peter May, Pawel Puczkarski, Henrik Pettersson, Edmund Long, João Coelho, Sean E. O’Brien, Eva K. McGuire, Beatriz Mendoza Sanchez, Georg S. Duesberg, Niall McEvoy, Clive Downing, Valeria Nicolosi & Jonathan N. Coleman

  2. Thomas Swan and Company Limited, Rotary Way Consett DH8 7ND, UK,

    Keith R. Paton

  3. School of Physics, Trinity College Dublin, Dublin 2, Ireland

    Eswaraiah Varrla, Claudia Backes, Ronan J. Smith, Umar Khan, Arlene O’Neill, Conor Boland, Mustafa Lotya, Oana M. Istrate, Paul King, Tom Higgins, Sebastian Barwich, Peter May, Pawel Puczkarski, Iftikhar Ahmed, Matthias Moebius, Henrik Pettersson, Edmund Long, Sean E. O’Brien, Eva K. McGuire, Valeria Nicolosi & Jonathan N. Coleman

  4. School of Chemistry, Trinity College Dublin, Dublin 2, Ireland

    João Coelho, Beatriz Mendoza Sanchez, Georg S. Duesberg, Niall McEvoy & Valeria Nicolosi

  5. SuperSTEM, STFC Daresbury Laboratories, Keckwick Lane Warrington WA4 4AD, UK,

    Timothy J. Pennycook

  6. Department of Materials, University of Oxford, Parks Road Oxford OX1 3PH, UK,

    Timothy J. Pennycook & Alison Crossley

Authors
  1. Keith R. Paton
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  29. Jonathan N. Coleman
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Contributions

K.R.P., E.V. and P.P. performed the shear mixing and other experiments. A.O’N., M.L., P.M., R.J.S., H.P., E.L., J.C., S.E.O’B., B.M.S., E.Mc.G., T.J.P. and V.N. performed electron microscopy characterization and analysis. C.D. and A.C. performed XPS characterization and analysis. U.K., C. Boland, O.M.I., P.K., T.H. and I.A. performed applications measurements. C. Backes, N.Mc.E. and G.S.D. performed Raman and AFM analysis. S.B. and M.M. performed rheological characterization and analysis. J.N.C. designed the experiments, derived the models and wrote the paper.

Corresponding author

Correspondence to Jonathan N. Coleman.

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The authors declare no competing financial interests.

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Paton, K., Varrla, E., Backes, C. et al. Scalable production of large quantities of defect-free few-layer graphene by shear exfoliation in liquids. Nature Mater 13, 624–630 (2014). https://doi.org/10.1038/nmat3944

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