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Thermal analysis of the improved Hummers’ synthesis of graphene oxide

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Abstract

The improved Hummers’ synthesis of graphene oxide (GO) from graphite is investigated to monitor how the functional groups form during the synthesis steps. To achieve these, samples are taken after every preparation step and analyzed with TG–DTA/MS, FTIR, XRD and SEM–EDX techniques. It was found that the main characteristic mass loss step of GO was around 200 °C, where at first the carboxyl and lactone groups were released, and the evolution of sulfonyl groups followed them right away in a partially overlapping step. It became clear that in the as-prepared acidic GO sample the presence of H2SO4 originating from the reaction solution was still dominant. The functional groups were formed only after washing the as-prepared GO with HCl. The consecutive washing step with distilled water did not alter the functional groups or the thermal properties significantly; however, it made the GO structure more ordered. The reduction of the GO structure back to reduced GO resulted in the loss of the functional groups, and a graphitic material was obtained back.

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Acknowledgements

I. M. Szilágyi thanks for a János Bolyai Research Fellowship of the Hungarian Academy of Sciences, an ÚNKP-17-4-IV-BME-188 and an OTKA PD-109129 Grant. Financial support from the National Scientific Research Fund (OTKA) through NN110209 and K109558 is acknowledged. Financial support from VEKOP-2.3.2-16-2017-00013 and K124212 grants are thanked. K. László extends her thanks to K. Katsumi for the graphite material. The help of Virág Bérczes (Budapest University of Technology and Economics, Department of Physical Chemistry and Materials Science) in the synthesis steps is acknowledged.

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Authors and Affiliations

  1. Department of Inorganic and Analytical Chemistry, Budapest University of Technology and Economics, Szt. Gellért tér 4., Budapest, 1111, Hungary

    Nóra Justh & Imre Miklós Szilágyi

  2. Department of Physical Chemistry and Materials Science, Budapest University of Technology and Economics, P.O. Box 92, Budapest, 1521, Hungary

    Barbara Berke & Krisztina László

  3. MTA-BME Research Group of Technical Analytical Chemistry, Szt. Gellért tér 4., Budapest, 1111, Hungary

    Imre Miklós Szilágyi

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  1. Nóra Justh
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  4. Imre Miklós Szilágyi
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Correspondence to Imre Miklós Szilágyi.

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Justh, N., Berke, B., László, K. et al. Thermal analysis of the improved Hummers’ synthesis of graphene oxide. J Therm Anal Calorim 131, 2267–2272 (2018). https://doi.org/10.1007/s10973-017-6697-2

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  • DOI: https://doi.org/10.1007/s10973-017-6697-2

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