AbstractRecently, aqueous rechargeable zinc batteries (ARZBs) have become a hot topic in secondary batteries. Constant attention has witnessed the development of ARZBs, such as active materials, reaction mechanisms, and mass transport, and huge successes have been achieved. However, as the fundamental basis of battery monitoring in real‐time and the theories of ARZBs, the in situ characterization techniques are equally worth discussing but the relevant review remains missing. Herein, this review focuses on the in situ characterization techniques of visualization and spectroscopy characterizations for ARZBs. Typical research of the in situ techniques is comprehensively discussed, including the setup of the in situ cells, the working principle of characterizations, the application, and the analysis applied in ARZBs. With the help of in situ characterizations, the reaction dynamics, transport kinetics, and thermodynamics in ARZBs can be thoroughly researched. Finally, the current primary challenges and future opportunities faced by in situ techniques toward ARZBs are also summarized.