The development of inexpensive, highly active and non-noble catalysts for the methanol oxidation reaction is extremely desirable for the practical use of direct-methanol fuel cells. Here, we have developed a template-free hydrothermal synthesis followed by calcination to produce highly active hybrid material of reduced graphene oxide (rGO) supported NiCo 2 O 4 (NiCo 2 O 4 /rGO) nano-rods as a non-expensive electro-catalyst for methanol oxidation. The electrochemical performance of the prepared NiCo 2 O 4 /rGO spinel catalyst was investigated by cyclic voltammetry (CV), chronoamperometry (CA) and electrochemical impedance spectroscopy (EIS) techniques. Impressively, the NiCo 2 O 4 /rGO showed greater electrocatalytic activity (78 mA/ cm 2 ) and stability during methanol oxidation in comparison to that of the commercial Pt/C catalyst, which was 3.11 folds higher than the commercial Pt/C (25.08 mA/cm 2 ). The NiCo 2 O 4 / rGO electrode also maintained its remarkable catalytic stability even after consecutive 500 cycles, which was~50 times higher than that of the commercial Pt/C. The overall electroactivity of NiCo 2 O 4 /rGO was remarkably enhanced by the synergistic effect between NiCo 2 O 4 and rGO. This may be due to the formation of mixed-valence cations of Ni 2 + and Co 3 + from the octahedral sites and high electron-transfer conductivity of rGO as well.[a] N.