Aqueous zinc ion batteries (ZIBs) are promising energy storage devices due to the high ionic conductivity of the aqueous electrolyte as well as the safety, eco‐friendliness, and low cost. Vanadium oxide‐based materials are attractive cathode materials for aqueous ZIBs because of their high capacity from their layered structure and multiple valences. However, it is difficult to achieve high cycle stability and rate capability due to the low electrical conductivity and trapping of diffused electrolyte cations within the crystal structure, limiting the commercialization of aqueous ZIBs. In this study, the authors propose a facile sonochemical method for controlling the interlayer of the vanadate nanofiber crystal structure using poly(3,4‐ethylene dioxythiophene) (PEDOT) to overcome the shortcomings of vanadium oxide‐based materials. In addition, the electrochemical correlation between the interplanar distance of the expanded vanadate layers by the insertion of PEDOT and the behavior of Zn2+ ions is investigated. As a result, the intercalation of the conducting polymer increases the electron pathway and extends the distance of the vanadate layers, which helps to increase the number of active sites inside the vanadate and accelerate the zinc ion intercalation/de‐intercalation process. Their findings may guide research on the next generation of ZIBs that can replace lithium ion batteries.
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