Based on the charge intercalation mechanism, an optimized regulation of the interlayer spacing and micromorphology is crucial to achieving promoted Zn2+ storage performance for the affordable layered vanadium oxides. Herein, an original chrysanthemum-like organic conductive polyaniline (PANI) intercalated hybridized cathode (PANI0.22·V2O5·0.88H2O) is developed by preintercalation of the aniline monomer and subsequently in situ polymerization within the oxide interlayers. Profiting from the “pillars” effects as well as the unique π-conjugated structure of PANI, the electrostatic interactions between the Zn2+ and the V–O layer can be effectively weakened. More importantly, the conjugated conductive guest polymer could inherently induce electron transfer to lower the valence of vanadium, which is beneficial for enhancing electronic conductivity. Moreover, the 3D micromorphology guarantees abundant active sites for Zn2+ transfer and intimate contact with electrolytes. Accordingly, the chrysanthemum-like PANI-intercalated V2O5 exhibits a high specific capacity of 447 mA h g–1 at 0.1 A g–1 and state-of-the-art cycling stability at 92% capacity retention after 3000 cycles. Also, the meticulous charge storage mechanism of this hybrid cathode is investigated systematically through a series of in-depth analyses. Our findings provide a pathway for tuning the interlayer spacing and microstructure toward advanced multivalent ion storage applications.

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