Nanoscale transition metal selenides are promising electrocatalytic materials for efficient energy conversion applications. Synthesis of NiRu0.3Se nanoparticles, in situ grown on reduced graphene oxide, for oxygen evolution reaction (OER) are reported here. The composite exhibited hexagonal and cubic phase structure corresponding to NiSe and RuSe2, having irregular morphology. NiRu0.3Se/rGO exhibited superior OER performance than NiSe/rGO requiring an overpotential of 290 mV to generate a benchmarked current density of 10 mA cm−2 in 0.1 M KOH.