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A study was made of the yield and crystallinity of graphite fluoride using a vertical vibrating reactor, which made it possible to prepare much graphite fluoride. The yield of graphite fluoride decreased beyond 500 °C for natural graphite and petroleum coke heat-treated at 2800 °C, and beyond 300 °C for calcined petroleum coke. The crystallinity of graphite fluoride was improved through the decomposition and refluorination process in these temperature ranges where the yield decreased. It was found that a sublimative solid by-product was formed together with gaseous fluorocarbons. It was a white solid fluorocarbon with 5–9 cyclohexane rings.