The operating voltage of aqueous hybrid capacitors are generally limited to 2 V due to the decomposition of water, which significantly impede the progress of energy density. Herein, the porous low-crystalline FeOx nanorod array on carbon cloth is prepared by the novel electrochemical Li+ pre-insertion method, and a 2.4 V high-voltage aqueous hybrid capacitor device is successfully obtained after matching with the nickel doped (Ni0.25Mn0.75)(3)O-4@PPy nanoprisms array. The low-crystalline structure of FeOx preserved during the first Li+ insertion and space created via the elimination of low-cry...