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The geometrically multiplied development of 2D MXenes has already promoted the prosperity of various fields of scientific researches especially but not limited in energy storage and conversion. Notably, cation intercalation can improve the interlayer spacing of MXenes resulting in tunable physical and chemical properties. Moreover, the synchrotron radiation X-ray characterizations have also shown high potential on exploring the property and structure of cation intercalated MXenes. This review is mainly focused on the recent achievements of cation intercalated MXenes through different methods on energy storage systems. Synchrotron-based X-ray absorption spectroscopic characterizations are emphasized to probe the local coordination and electronic structure in intercalated MXenes. The outlook of cation intercalation on MXenes and their applications are also discussed.