Simultaneous Anodic and Cathodic Exfoliation of Graphite Electrodes in an Aqueous Solution of Inorganic Salt

Abstract Electrochemical exfoliation of graphite offers a scalable and efficient approach to synthesise graphene nanomaterials. This process is commonly performed either anodically or cathodically, whereas simultaneous dual processes offer an attractive energy efficient means to produce graphene materials with tuneable properties. Here, we demonstrate a simple electro synthetic approach to produce graphene simultaneously from both a graphite anode and a graphite cathode in K 2 SO 4 aqueous solution. Graphite exfoliation was facilitated by employing 0.5 M K 2 SO 4 as an electrolyte at 10 V, where efficient exfoliation simultaneously occurs at graphite foils serving as both anode and cathode. The anodically exfoliated graphene has a high defect density ( I D / I G =0.58) and higher degree of oxidation (C/O=11.36), in comparison to graphene produced at cathode having a lower defect density ( I D / I G =0.06) and a low oxidation degree (C/O=31.68). The usage of aqueous solution for scalable and efficient concurrent‐dual electrochemical exfoliation of graphite electrodes will facilitate the development of large‐scale production of graphene.