Pursuing of straightforward and cost-effective methods for synthesizing high-performance anode materials for lithium-ion batteries is a topic of significant interest. This study elucidates a one-step synthesis approach for a conversion composite using glow discharge in a nickel formate solution, yielding a composite precursor comprising metallic nickel, nickel hydroxide, and basic nickel salts. Subsequent annealing of the precursor facilitated the formation of the Ni@NiO composite, exhibiting exceptional electrochemical properties as anode material in Li-ion batteries: a capacity of approximately 1000 mAh g−1, cyclic stability exceeding 100 cycles, and favorable rate performance (200 mAh g−1 at 10 A g