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In this work a novel bimetallic nickel oxide/copper oxide metal–organic framework (NiO/CuO MOF) has been developed by using two linkers: Benzene Dicarboxylic acid (BDC) and Pyrazine. The composites of NiO/CuO MOF with different amounts of reduced graphene oxide (rGO) were synthesized through a hydrothermal method and subsequently characterized by multiple significant techniques like XRD, SEM, EDX, FTIR and Raman IR for an investigation of their structural and morphological properties. The prepared series of material was later employed for electrochemical oxidation of methanol, tested by cyclic voltammetry (CV) in basic medium on a modified glassy carbon electrode (GCE). The electrochemical response depicts that increasing concentration of rGO enhances the electrocatalytic activity of the catalyst for methanol oxidation reaction (MOR). The catalyzed oxidation reaction of methanol by NiO/CuO MOF and rGO-NiO/CuO MOF composites give a superlative current density of 437. 28 mA/cm2 at 0.9 V potential at 50 mV/s scan rate. This activity makes it a promising catalytic material for electrolysis of methanol in direct methanol fuel cell (DMFC).