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Liquid phase exfoliation of few‐layer phosphorene (FL‐P) is extensively explored in recent years. Nevertheless, their deficiencies such as ultralong sonication time, limited flake size distribution, and uncontrollable thicknesses are major hurdles for the development of phosphorene‐based materials. Herein, electrochemical cationic intercalation has been introduced to prepare phosphorene, through which large‐area FL‐P without surface functional groups can be efficiently attained (less than 1 h). More importantly, its layer number (from 2 to 11 layers) can be manipulated by changing the applied potential. The as‐obtained phosphorene delivers superior sodium‐storage performances when directly utilized as an anode material in sodium‐ion batteries. This electrochemical cation insertion method to prepare phosphorene should greatly facilitate the development of phosphorene‐based technologies. Moreover, this …