Chemical and electrochemical syntheses of a graphite fluoro-tris(pentafluoroethyl)borate intercalation compound

Graphite intercalation compounds (GICs) of composition Cx[FB(C2F5)3] · δF are prepared for the first time by the intercalation of fluoro-tris(pentafluoroethyl)borate anion, [FB(C2F5)3]−, under ambient conditions in 48% hydrofluoric acid containing the oxidant K2[MnF6]. Powder XRD data indicate that products are of mixed stages 2 and 3 after reactions for 1–20 h, with a gallery height of 0.87 nm. The intercalate orientation is modeled using an energy-minimized anion structure. Microwave digestion followed by B and F elemental analyses, along with thermogravimetric analyses provide compositional x and δ parameters for the GICs obtained. In addition, Cx[FB(C2F5)3] · δCH3NO2 with stage 2 is prepared by electrochemical oxidation of graphite in a nitromethane solution and characterized as above.