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Experimental evaluation of eco-friendly exfoliation strategies for tour-method graphene oxide
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  • Published: 16 March 2026

Experimental evaluation of eco-friendly exfoliation strategies for tour-method graphene oxide

  • Hanna Bukovska1,
  • M. Belén Gómez-Mancebo1,
  • Fernando García-Pérez1,
  • Manuel Fernández1,
  • Sergio Fernández-Carretero2,
  • Susana Fernández3 &
  • …
  • Isabel Rucandio1 

Scientific Reports , Article number:  (2026) Cite this article

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We are providing an unedited version of this manuscript to give early access to its findings. Before final publication, the manuscript will undergo further editing. Please note there may be errors present which affect the content, and all legal disclaimers apply.

Subjects

  • Chemistry
  • Energy science and technology
  • Engineering
  • Environmental sciences
  • Materials science

Abstract

The exfoliation of graphite oxide (GrO) represents a critical stage prior to processes such as the reduction or functionalisation of graphene oxide (GO), directly affecting its final properties. In particular, GO synthesised by the Tour method, which offers advantages over conventional methods such as the Hummers method (higher safety, better oxidation degree and homogeneity of the material), has been scarcely studied in terms of the control of its specific surface area (SSA), a fundamental parameter for its performance in technological applications. In this work, the optimisation of the exfoliation process of GO prepared by the Tour method is proposed through the systematic comparison of different ecofriendly techniques: ultrasonic bath, ultrasonic probe, ball mill grinding and glucose-assisted grinding. A rigorous experimental design and a comprehensive statistical analysis were carried out, using carbon content, C (%), and SSA as main responses. In addition, complementary characterisations by X-ray diffraction (XRD, for number of stacked layers (n) and diffraction peak position, 2θ) were performed to deepen the structural analysis. The results reveal that ball milling without additives achieved the highest SSA (~ 71 m² g−1), followed by glucose-assisted milling (~ 54 m² g−1), while ultrasonic techniques offered significantly lower values (6–30 m² g−1). This study provides a solid and rigorous basis for understanding and optimizing the properties of GO according to the requirements of the specific applications for which it is intended and a study of the differences between ball milling and ultrasonic exfoliation in GO normally applied in graphite exfoliation.

Data availability

Data is provided within the manuscript.

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Acknowledgements

This research was supported by REGRAP-2D, Grants PID2020-114234RB-C21 and SOLENGRAFPID2023-146988OB-C21 funded by MCIN/AEI/10.13039/501100011033.

Funding

This research was supported by REGRAP-2D, Grants PID2020-114234RB-C21 funded by MCIN/AEI/https://doi.org/10.13039/501100011033. During the preparation of this work the author(s) used “DeepL“in order to check the grammar. After using this tool/service, the authors reviewed and edited the content as needed and take full responsibility for the content of the publication.

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Authors and Affiliations

  1. Chemistry Division, Technology Department, CIEMAT (Centro de Investigaciones Energéticas, Medioambientales y Tecnológicas), 28040, Madrid, Spain

    Hanna Bukovska, M. Belén Gómez-Mancebo, Fernando García-Pérez, Manuel Fernández & Isabel Rucandio

  2. Nuclear Fission Unit, CIEMAT (Centro de Investigaciones Energéticas, Medioambientales y Tecnológicas), 28040, Madrid, Spain

    Sergio Fernández-Carretero

  3. Energy Department, CIEMAT (Centro de Investigaciones Energéticas, Medioambientales y Tecnológicas), 28040, Madrid, Spain

    Susana Fernández

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“Conceptualization, Hanna Bukovska and M. Belén Gómez-Mancebo; methodology, Hanna Bukovska; software, Hanna Bukovska; formal analysis Hanna Bukovska, Fernando García Perez, Susana Fernández, Iván Sánchez, Manuel Fernández; investigation, Hanna Bukovska and M. Belén Gómez-Mancebo; resources, Javier Martínez, Isabel Rucandio and M. Belén Gómez Mancebo; writing—original draft preparation, Hanna Bukovska.; writing—review and editing, Hanna Bukovska, M. Belén Gómez-Mancebo and Isabel Rucandio; supervision, M. Belén Gómez Mancebo; project administration, M. Belén Gómez Mancebo, Javier Martínez and Isabel Rucandio. All authors have read and agreed to the published version of the manuscript.”

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Bukovska, H., Gómez-Mancebo, M.B., García-Pérez, F. et al. Experimental evaluation of eco-friendly exfoliation strategies for tour-method graphene oxide. Sci Rep (2026). https://doi.org/10.1038/s41598-026-42185-9

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  • Received: 23 July 2025

  • Accepted: 24 February 2026

  • Published: 16 March 2026

  • DOI: https://doi.org/10.1038/s41598-026-42185-9

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Keywords

  • Exfoliation
  • Graphite oxide
  • Ultrasound
  • Ball mill
  • Experimental design
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