Nickel Single‐Atom Intercalated MXene/Metal–Organic Framework Composite for Superior Lithium and Sodium Storage

The rapid growth of portable electronics continues to drive the demand for advanced lithium‐ion batteries (LIBs). In this study, we synthesized a nickel single‐atom intercalated Ti 3 C 2 T x /ZIF‐8 composite (Ni‐MXene/metal–organic framework (MOF)) to overcome the limitations of conventional anode materials. The local coordination environment and electronic structure of nickel atoms in the MXene/MOF composite were systematically investigated using synchrotron radiation–based X‐ray absorption fine structure (XAFS) spectroscopy. XAFS analysis provided a precise determination of the oxidation states and bonding configurations of Ni. The room temperature synthesis method used for the Ni‐MXene/MOF composite effectively preserved its layered structure. Comprehensive structural and electrochemical analysis revealed that incorporating nickel single atoms within the MXene/MOF framework improved conductivity, enhanced active sites, and ensured stable structural integrity during charge–discharge cycles. The Ni‐MXene/MOF composite electrodes demonstrated an outstanding initial discharge capacity of 1319 mA h g −1 at 0.1 A g −1 for LIBs, while delivering 573 mAh g −1 under the same conditions for sodium ion batteries. The novel structural design of Ni‐MXene/MOF demonstrated minimal capacity degradation even after extended cycling, underscoring the exceptional stability. These results suggest a promising approach for the rational design of high‐performance anode materials, emphasizing the synergistic role of metal intercalation in hybrid architectures for next‐generation lithium‐ and sodium‐storage systems.