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materials Article Development and Up-Scaling of Electrochemical Production and Mild Thermal Reduction of Graphene Oxide Markus Ostermann 1,*,† , Peter Velicsanyi 1,†,‡, Pierluigi Bilotto 1,* , Juergen Schodl 1, Markus Nadlinger 1, Guenter Fafilek 2, Peter A. Lieberzeit 3 and Markus Valtiner 1,4 Citation: Ostermann, M.; Velicsanyi, P.; Bilotto, P.; Schodl, J.; Nadlinger, M.; Fafilek, G.; Lieberzeit, P.A.; Valtiner, M. Development and Up-Scaling of Electrochemical Production and Mild Thermal Reduction of Graphene Oxide. Materials 2022, 15, 4639. https://doi.org/10.3390/ ma15134639 Academic Editors: Federico Cesano and Julia A. Baimova Received: 19 May 2022 Accepted: 27 June 2022 Published: 1 July 2022 Publisher’s Note: MDPI stays neutral with regard to jurisdictional claims in published maps and institutional affil- iations. Copyright: © 2022 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https:// creativecommons.org/licenses/by/ 4.0/). 1 2 3 4 Abstract: To reduce the global emissions of CO2, the aviation industry largely relies on new light weight materials, which require multifunctional coatings. Graphene and its derivatives are partic- ularly promising for combining light weight applications with functional coatings. Although they have proven to have outstanding properties, graphene and its precursor graphene oxide (GO) remain far from application at the industrial scale since a comprehensive protocol for mass production is still lacking. In this work, we develop and systematically describe a sustainable up-scaling process for the production of GO based on a three-step electrochemical exfoliation method. Surface characterization techniques (XRD, XPS and Raman) allow the understanding of the fast exfoliation rates obtained, and of high conductivities that are up to four orders of magnitude higher compared to GO produced via the commonly used modified Hummers method. Furthermore, we show that a newly developed mild thermal reduction at 250 °C is sufficient to increase conductivity by another order of magnitude, while limiting energy requirements. The proposed GO powder protocol suggests an up-scaling linear relation between the amount of educt surface and volume of electrolyte. This may support the mass production of GO-based coatings for the aviation industry, and address challenges such as low weight, fire, de-icing and lightning strike protection. Keywords: graphene oxide; reduced graphene oxide; up-scaling; thermal reduction; aeronautical application; polymer filler 1. Introduction At the end of 2019 the European Union presented the European Green Deal as a counteraction to the ramping climate crisis [1]. The document addressed the challenges for the aviation industry in the CORSIA (Carbon Offsetting and Reduction Scheme for International Aviation) program [2]. In order to reduce their CO2 emissions, aviation industries started to explore novel light composite materials. Eventually, it became clear that the composites require fillers and coatings to enhance the adaptability of the aircraft parts to external factors. For instance, while being light, the composite parts need to show resistance to corrosion, to water uptake and to fire, and sufficient conductivity for lightning strike protection. At the same time, it would be ideal to implement thermoelectrical de-icing properties in these composites to avoid the formation of ice clusters on the wing, which may compromise flight safety. Novel materials, e.g., graphene, offer possibilities to obtain such functionalities and preserve the advantage of low composite mass [3]. Centre for Electrochemical Surface Technology, CEST GmbH, A-2700 Wiener Neustadt, Austria; pv@zitt.at (P.V.); juergen.schodl@cest.at (J.S.); markus.nadlinger@cest.at (M.N.); markus.valtiner@cest.at (M.V.) Institute of Chemical Technologies and Analytics, Vienna University of Technology, A-1040 Vienna, Austria; guenter.fafilek@tuwien.ac.at Institute of Physical Chemistry, University of Vienna, A-1090 Vienna, Austria; peter.lieberzeit@univie.ac.at Applied Interface Physics, Vienna University of Technology, A-1040 Vienna, Austria * Correspondence: markus.ostermann@cest.at (M.O.); pierluigi.bilotto@cest.at (P.B.) † These authors contributed equally to this work. ‡ Current address: Zitt GmbH & Co., KG, D-81379 München, Germany. Materials 2022, 15, 4639. https://doi.org/10.3390/ma15134639 https://www.mdpi.com/journal/materialsPDF Image | Electrochemical Production Thermal Reduction Graphene Oxide
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