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Stage 2 FeCl3-graphite intercalation compound (GIC) was chemically reduced with lithium-naphthalene complex in THF and 1-MB. The GIC was also reduced electrochemically in THF, PC and EC+DEC, containing 1 mol/dm3 of LiClO4. When the reduction was performed in THF chemically or electrochemically, fine iron particles were obtained in the graphite matrix. The mean diameter of the particles is in the range of 11-13nm in this case, while 4nm for 1-MB. For PC and EC+DEC, no iron particle was observed in the product. The difference would be related to the co-intercalation of the solvent. In the reduction process, THF is incorporated together with lithium in the interlayer spacing of FeCl3-GIC. The co-intercalated THF molecules facilitate the reduction of FeCl3 by lithium in the graphite gallery probably because FeCl3 is soluble in THF, and relatively large iron particles are obtained.

Solvent effect in the reduction of FeCl3-GIC