Urea as an energy generation and storage fuel has attracted increased attention for its stability, non-toxicity, and availability. Urea possesses 10.1 wt.% of hydrogen. Nevertheless, its electrochemical oxidation is generally sluggish and inefficient. Nibased catalysts which showed efficient activity towards urea electrooxidation in the alkaline medium were studied for Direct Urea Fuel Cell (DUFC) anodes. In the present study, we investigated urea oxidation on a novel three-dimensional mixed oxide catalyst, NiCo 2 O 4 . Mn-doped NiCo 2 O 4 catalyst exhibited urea oxidation activity of 45.88 mA cm À 2 (at 1.30 V vs SHE), fifteen times higher than NiO and Co 3 O 4 and twice that of bare NiCo 2 O 4 spinel. Chronoamperometry curves of the Mn-doped NiCo 2 O 4 catalyst demonstrated stable urea oxidation for over 3 hours. The significantly higher mass activity of Mn-doped NiCo 2 O 4 catalyst is attributed to the least nano-crystallite size, better dispersion of Ni nuclei onto the spinel crystal matrix, enhanced Ni electrochemical active surface area, and lower bandgap.