First studies on intercalation of graphite date back to the first half of the XX century. At first, the ability of graphite to spontaneously form intercalation compound (GIC) by the soaking in strong acids was studied. Only later, GIC were obtained by electrochemical route, highlighting the mechanism of formation of GIC in extremely ordered layered structure as HOPG [1,2]. Anodic electrochemical intercalation is typically performed in acidic aqueous solution, forming GIC by the insertion of anions as ClO4-, HSO4- and NO3- [3]. Anodic electrochemical intercalation is nowadays useful to obtain high quality Graphene Oxide (GO) thorough an easy and green route [4]. Studies on the formation of GIC by cathodic polarization opened to the understanding and exploitation of the reversible intercalation of alkali ions (Li+, Na+) that found the suitable application in Li battery technology [5]. However, up to now, studies have concentrated mainly on the electrochemical formation of GIC HOPG, but very few have investigated the GIC formation in nanoscaled graphitic material as graphene [6]. In this work, we provide a comprehensive understanding of the GIC formation by electrochemical route in few-layer graphene grown through atmospheric pressure chemical vapor deposition (ACVD) on metallic substrates. Anodic electrochemical intercalation of few layer graphene in acidic, organic-based and aqueous-based media has been investigated. A deeper understanding of intercalation and doping phenomena of few layer graphene has been performed in situ through Raman spectroscopy measurements. Preliminary results on cathodic intercalation of few layer graphene in aqueous and organic media will be also discussed.

References

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[2] F.Beck, H.Junge, H.Krohn, Electrochemical Acta, 26 (7), 1981, 799-809

[3] D.C. Alsmeyer, R. L. McCreery, Anal. Chem., 1992, 64 (14), 1528–153

[4] K. Parvez, Z. Wo, R. Li, X. Liu, R. Graf, X. Feng, K. Müllen J. Am. Chem. Soc., 2014, 136 (16), 6083–6091

[5] S.Basu, C.Zeller, P.J.Flanders, C.D.Fuerst, W.D.Johnson, J.E.Fischer, Materials Science and Engineering, 1979, 38 (3), 275-283

[6] E. Pollak, B. Geng, K. Jeon, I.T. Lucas, T. J, Richardson, F. Wang, R. Kostecki, Nano Lett., 2010, 10 (9), pp 3386–3388.