Abstract: Graphite oxide is of great importance in preparing graphene, the average layer of graphene depends on that of graphene oxide in some extent. In this paper, we prepared graphite oxide via H3PO4/H2SO4mixed acid, then which were dried by vacuum drying in a freezer dryer and drying oven respectively, the graphite oxide powder and thin film were obtained correspondingly. After dispersing the above two forms of graphite oxide in water by shaking, stirring or supersonic wave, they were reduced in the same condition. According to the XRD, AFM results, vacuum freeze-drying was inclined to gain few-lay graphene.