Ammonia leaching has been gained considerable attention for its ability to selectively extract nickel and cobalt from spent ternary cathode material. Despite its efficacy, the subsequent recovery of ammonia leachate remains challenging. Herein, a short-process and sustainable method for the synthesis of nickel-cobalt oxide via ammonia evaporation of ammonia leachate and heat treatment of the resultant precursor has been proposed. The ammonia evaporation process, conducted at an evaporation temperature of 130 °C with hydrazine hydrate as a reducing agent, facilitated the precipitation of ∼95% Ni and ∼99% Co as a precursor. Subsequently, the effect of precursor roasting temperature on electrode material synthesis was systematically studied. The precursor was roasted at 300 °C to successfully synthesize nickel-cobalt oxide. Physical and electrochemical characterizations revealed that the nickel-cobalt oxide possesses a significant specific surface area of 161.150 m2/g, and exhibits excellent oxygen evolution reaction performance, evidenced by an overpotential of 350.7 mV at 10 mA/cm2 and a Tafel slope of 159.8 mV/dec. Overall, the proposed method not only promotes the recycling and utilization of ammonia reagents and mother liquor, but also introduces an innovative approach for the synthesis of nickel-cobalt oxide as an electrode material.