Graphite intercalation compounds are often prepared by flake graphite, oxidants, inorganic acids, organic acids and intercalated ions which are usually hydrogen protons between the graphene planes. They are also known as the acid-treated graphite intercalation compounds. In this work, alkaline graphite intercalation compounds were prepared by flake graphite, K2Cr2O7, concentrated H2SO4 and NaOH, and the morphology and structure were characterized by Electron microscopy and X-ray techniques. The results display that the combination of neutralisation heat and oxidation capability produced by K2Cr2O7 can break the bonds to produce the spaces between the graphene planes and hydroxyl ions also intercalate into the graphene planes to form alkaline graphite intercalation compounds in alkali solution. The morphology and structure of alkaline graphite intercalation compounds are analogous to the ones of the acid-treated graphite intercalation compounds, but the intercalated ions and the expansion volume are different. The results show that the method is an innovation.