Thiourea Plasma‐Assisted Fabrication of N,S Co‐Doped Nickel Oxide Arrays on Hyphae Carbon for Enhanced Lithium Sulfur Batteries

Lithium‐Sulfur batteries (LSBs) face challenges like the polysulfide shuttle effect and sluggish kinetics. To address the above issues, we develop a novel composite cathode (NS‐NiO@HyC) via a bio‐inspired approach. Using hyphae‐derived carbon (HyC) as a conductive framework, NiO arrays are grown through chemical bath deposition of a Ni(OH) 2 precursor followed by annealing. The material is further treated with thiourea plasma to introduce N/S co‐doping and create Ni/O vacancies. The resulting NS‐NiO@HyC exhibits a high specific surface area (351.3 m 2 g −1 ), abundant defects, and strong polysulfide anchoring. In LSBs, it delivers a high initial capacity of 1355.3 mAh g −1 at 0.1 C, with 66.8% capacity retention after 260 cycles, and a low decay rate of 0.064% per cycle over 650 cycles at 0.5 C. In situ characterizations confirm suppressed shuttle effect and enhanced redox kinetics. This work demonstrates an effective strategy for designing high‐performance sulfur hosts by integrating biomass carbon with vacancy‐engineered metal oxides.