Electrochemical synthesis of iron supported on exfoliated graphite

A graphite intercalation compound (GIC) of acceptor type with complexed transition metal (iron) has been selected as a catalyst precursor. Supported iron particles were prepared using an all-electrochemical method which overcomes most of the disadvantages of the other processes based on GIC precursors. In the first step, the 2nd stage CnFeCl4, 1.5 H2O, 0.5 HCl compound was prepared by anodic oxidation of graphite in a concentrated solution of FeCl3 in 12 M HCl, where the main species present in the solution are FeCl4- anions. The FeCl4--GIC was then submitted to cathodic reduction in the presence of LiClO4 in aprotic medium (mixture of ethylene carbonate and diethylcarbonate). When reduction proceeded, the graphite exfoliated, and at the end of the process, the solid phase was a mixture of graphite, 6th stage GIC, LiCl and Fe degrees. The co-intercalated solvent molecules are responsible both for the exfoliation and for the partial reduction in metallic iron. The method allows to obtain highly dispersed iron on exfoliated graphite at room temperature. Such a nanocomposite may have applications in catalytic reactions for which supported metals are required.