A new microwave‐based strategy for shock exfoliation of fluorinated graphite into few‐layer, partially fluorinated graphene has been developed. This method is simple and ultrafast, which will be attractive for rapid preparation of fluorine‐containing graphene and its derivatives. The excellent electrochemical performance of the fluorinated graphene for potassium ion batteries and oxygen reduction reactions is demonstrated. Abstract An unprecedented microwave‐based strategy is developed to facilitate solid‐phase, instantaneous delamination and decomposition of graphite fluoride (GF) into few‐layer, partially fluorinated graphene. The shock reaction occurs (and completes in few seconds) under microwave irradiation upon exposing GF to either “microwave‐induced plasma” generated in vacuum or “catalyst effect” caused by intense sparking of graphite at ambient conditions. A detailed analysis of the structural and compositional transformations in these processes indicates that the GF experiences considerable exfoliation and defluorination, during which sp2‐bonded carbon is partially recovered despite significant structural defects being introduced. The exfoliated fluorinated graphene shows excellent electrochemical performance as anode materials in potassium ion batteries and as catalysts for the conversion of O2 to H2O2. This simple and scalable method requires minimal energy input and does not involve the use of other chemicals, which is attractive for extensive research in fluorine‐containing graphene and its derivatives in laboratories and industrial applications.

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