Water pollution caused by pharmaceutical wastewater is becoming increasingly serious. Diclofenac (DCF), a pharmaceutical compound widely used in many medicines, is an organic pollutant that poses potential risks to ecosystems and human health. In this study, a morphologically modified NiCo 2 O 4 (NCO) catalyst was synthesized via a hydrothermal method and employed to activate peroxymonosulfate (PMS) for DCF degradation. As a result, 99.9 % of the DCF was successfully degraded within 10 min. It also succeeded in mineralizing 97.2 % of DCF after 10 min. Moreover, the NCO/PMS system was effective over a wide pH range. The degradation pathways involved both radical and non-radical mechanisms, with 1 O 2 , SO 4 •– , and • OH identified as the primary active species. In addition, the surface hydroxyl groups on the NCO are likely to play a significant role in the degradation process. This paper presents the development of a highly efficient catalyst for the degradation of organic pollutants using PMS. • A morphologically modified NCO catalyst was prepared via hydrothermal method. • The optimized NCO/PMS could degrade 99.9 % and mineralize 97.2 % of DCF in 10 min. • 1 O 2 , SO 4 •– , and •OH were the main reactive species in the degradation reaction. • Surface hydroxyl groups on NCO were important for the formation of SO 4 •– and 1 O 2 . • Stable redox couple ratios in NCO indicate good redox cycles during the reaction.