A Ni/Ni 3 Se 2 metal-semiconductor heterojunction catalyst with a sphere structure was prepared by a hydrothermal and hydrogen reduction method. The results showed that the heterostructure Ni/Ni 3 Se 2 exhibits better performance than Ni 3 Se 2 and Ni counterparts for electrochemical oxidation reactions. During electrocatalytic water oxidation, the overpotential is 340 mV to reach a catalytic current density of 10 mA cm À 2 in 1.0 M KOH solution. The heterogeneous interface formed between the metal Ni and Ni 3 Se 2 in the Ni/Ni 3 Se 2 catalyst can accelerate the electron transfer in the electrochemical oxidation process. Moreover, the asprepared material is also applied for sulfonamide degradation, with the aid from hydroxyl radicals generated during water oxidation. This application is meaningful since the product from water oxidation is not desired in hydrogen production from water electrolysis. The material with heterojunctions delivered degradation efficiency up to 80% of sulfonamide antibiotics within 2 h. Therefore, the Ni/Ni 3 Se 2 material might have application prospects in electrochemical sustainability research.