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.
Akhtar et al. (Wed,) studied this question.