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Energetically efficient and electrochemically tuneable exfoliation of graphite: process monitoring and product characterization

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Abstract

In this work, graphene oxide was prepared by electrochemical exfoliation of graphite in sodium dodecyl sulphate and sodium dodecylbenzene sulphonate aqueous solution. Two different working electrodes were investigated: an electrode prepared from natural graphite flakes and a commercial natural graphite rod. The working electrode was polarized in a two-electrode system by using platinum counter electrode and by a multistep change of polarity or by single anodic and cathodic polarization. The voltage value ranged from 2.5 to 3.2 V. By monitoring the current transients and the colour of the resultant solutions, it was shown that the exfoliation process depends on the type of working electrode, surfactants and applied voltage value. The multistep change of polarity was more effective compared to single polarization. The ultraviolet–visible spectrophotometry and Raman spectroscopy indicated the presence of defects within the graphene structure, while FTIR spectroscopy indicated the presence of oxygen functional groups, which is characteristic of graphene oxide (GO). Dynamic light scattering revealed that the solutions obtained in this work contained GO sheets within the size of 10–600 nm. Atomic force microscopy measurements proved that the obtained product contains multilayer sheets. The energy consumption for the process carried out in this work ranges from 0.084–0.038 kWh g−1, and therefore this process is considered to be a low-energy and cost-effective process.

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Acknowledgement

The authors are grateful to the “Croatian Science Foundation” for the financial support of the project ˝High power−high energy electrochemical supercapacitor for hybrid electrical vehicles˝, IP-2013-11-8825. The financial support of the Foundation of the Croatian Academy of Sciences and Arts for projects “Electrochemical exfoliation of graphite in surfactant solution” is gratefully acknowledged. Davor Čapeta and Iva Šrut Rakić acknowledge financial support by the Center of Excellence for Advanced Materials and Sensing Devices (ERDF Grant No. KK.01.1.1.01.0001). The authors would like to thank Professor Tajana Preočanin (Department of Chemistry, Faculty of Science, University of Zagreb) for dynamic light scattering measurements.

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Authors and Affiliations

  1. Faculty of Mining, Geology and Petroleum Engineering, University of Zagreb, Pierottijeva 6, 10000, Zagreb, Croatia

    Gabrijela Ljubek

  2. Center for Excellence for Advanced Materials and Sensing Devices, Institute of Physics, Bijenička 46, 10000, Zagreb, Croatia

    Davor Čapeta & Iva Šrut Rakić

  3. Faculty of Chemical Engineering and Technology, University of Zagreb, Marulićev trg 19, 10000, Zagreb, Croatia

    Marijana Kraljić Roković

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  1. Gabrijela Ljubek
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Ljubek, G., Čapeta, D., Šrut Rakić, I. et al. Energetically efficient and electrochemically tuneable exfoliation of graphite: process monitoring and product characterization. J Mater Sci 56, 10859–10875 (2021). https://doi.org/10.1007/s10853-021-05989-w

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