ABSTRACT Two‐dimensional (2D) transition‐metal compounds often suffer from the dissolution of active transition metals and structural collapse during electrochemical cycling. Herein, a sequential acid‐base regulation strategy is proposed to construct Zn and Al vacancies within layered double hydroxide (LDH) laminates, yielding a defect‐engineered NiZnFeAl‐V Zn V Al ‐Cl LDH. Benefiting from the synergistic effect of dual vacancies, LDH concurrently achieves “ion channel” and “ion locking” functio
