Superfine graphite powder was prepared by ball‐milling exfoliated graphite containing anhydrous CuCI2 in planetary ball milling systems. Nano‐scale CuCl2 graphite intercalation compounds were synthesized by heating a mixture of anhydrous CuCl2 and graphite nanosheets. Scanning electron microscopy, energy‐dispersive X‐ray spectroscopy and high‐resolution transmission electron microscopy were performed to characterize the microstructures of stage‐1 nano‐scale CuCI2 graphite intercalation compounds. The structure and components of the domain wall and core in the nano‐scale CuCl2 graphite intercalation compounds are described. The results show that the content of CuCl2 in the mixture plays a crucial role in the size of the nano‐scale CuCl2 graphite intercalation compound.
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