The electrochemical synthesis of hydrogen peroxide through the two-electron oxygen reduction (2e⁻ ORR) pathway represents a promising and environmentally friendly technique. The development of efficient electrocatalyst is crucial to enable this process. In this work, a nickel, nitrogen and oxygen co-doped nanocatalyst (Ni–N/C_ox) was prepared and its oxygen reduction performance was assessed using linear sweep voltammetry experiments. The results revealed excellent 2e⁻ ORR activity of the catalyst under alkaline condition with a remarkable selectivity for hydrogen peroxide of up to 96%. Comprehensive characterization techniques including SEM, TEM, XPS, XRD and FT-IR were employed. These analyses indicated that the surface of the Ni–N/C_ox catalyst contained abundant oxygen-containing functional groups and active nitrogen species, with the Ni element uniformly dispersed on the surface of the carbon substrates. Based on our findings, we propose that the excellent 2e⁻ ORR activity and selectivity of the catalyst stem from the formation of Ni–N₂O₂ active centers on the carbon surface. Additionally, the presence of abundant oxygen functional groups and active nitrogen species on the carbon surface further enhanced the catalytic performance of bulk carbon materials. This study presents a new avenue for the development of efficient and cost-effective 2e⁻ ORR catalysts, with potential implications for various electrochemical applications.