Synergistic Dual‐Doping and Hollow Nanostructure Engineering in MoS ₂ Anode for Enhanced Lithium Storage

Abstract The development of high‐performance anode materials is critical to overcoming the limitations of conventional graphite in lithium‐ion batteries (LIBs), particularly its low theoretical capacity and sluggish kinetics. MoS 2 with high theoretical capacity and layered structure has emerged as a promising alternative, yet its practical application is hindered by poor conductivity, severe volume expansion, and nanosheet aggregation. While strategies such as heteroatom doping and nano‐structural engineering have been explored, challenges in scalability, interfacial stability, and synthesis complexity persist. Herein, a Ni/Co co‐doped MoS 2 hollow nanocubic anode designed to synergistically address these limitations is reported. The incorporation of Ni and Co atoms enhances electronic conductivity and introduces dual redox‐active sites, while the hollow architecture mitigates mechanical stress from volume changes and provides abundant active surfaces. This unique configuration enables efficient Li + diffusion, robust structural integrity, and reduced charge transfer resistance. The optimized material delivers a high reversible capacity of 1174.2 mAh g −1 at 0.1 A g −1 , exceptional rate capability (409.7 mAh g −1 at 2 A g −1 ), and cyclic cyclability with 64.2% capacity retention after 150 cycles.