<p>Here, we reported the successful synthesis of nano-scale ZnCo₂O₄ materials via a polymer network gel method. The homogeneous fine ZnCo₂O₄ particles (20–50&#xa0;nm) exhibited excellent electrochemical properties. The initial discharge capacity reached 1076.7 mAh·g⁻¹, and the first coulombic efficiency was 61.6%. After 250 cycles at 0.2 A·g⁻¹, the coulomb efficiency remained 25.1% and the discharge capacity was 262.5 mAh·g⁻¹. Meanwhile, the capacity was maintained at 226.4 mAh·g⁻¹ after 300 cycles at 0.5 A·g⁻¹, and the electrode sheet retained a flat structure after cycling, demonstrating excellent cycle stability. The superior electrochemical performance of ZnCo₂O₄ can be attributed to the fact that the gel formed by polymerization prevented the components in the solution from direct contact, enabling the prepared material to possess advantages of good dispersion and small particle size, thereby reducing charge transfer resistance and enhancing lithium ion transport capability.</p>