| Summary: | Abstract Developing low‐cost and safe batteries with high energy density is promising for large‐scale energy storage applications. Currently, aqueous zinc ion batteries (AZIBs) using Zn metal as the anode have attracted tremendous research attention as the next generation of energy storage devices due to their advantages of high energy density, environmental friendliness, and natural Zn abundance. The utilization of synchrotron X‐ray analytical techniques for in situ/ex situ characterizations offers a comprehensive understanding of the atomic local structure, crystalline structure, chemical states, coordination environment, interface properties, morphologies, and other physicochemical properties of materials on a variety of temporal and length scales, providing valuable insights into the fundamental mechanisms of AZIBs. This review highlights the recent advances and accomplishments of various synchrotron X‐ray techniques, which have been employed to investigate different components of AZIBs and show great promise for battery research and development.
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