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 A guanidinium-based iCOF interfacial membrane was directly grown over Zn anode to mitigate its limitations in aqueous batterie. The guanidinium moietie's functions include: 1) immobilizes water molecules through H-bond, effectively suppressing parasitic side reactions; 2) promotes Zn2+ dissociation and uniform Zn deposition through coulombic interactions with sulphate ion. Benefiting from the improved electrochemical stability of modified Zn anode, the assembled pouch cell delivers a reversible capacity of ~0.35 Ah g−1 with a 98.72% capacity retention over prolonged cycling. This work was collaborated with Prof. Jingyu Sun and published in Angew. Chem. as a Very Important Paper and featured as Editors' Choice: Spotlights.