Nickel oxide nanoparticles were formed on mesoporous carbon (NiO/MC) through precipitating nickel hydroxide species followed by post annealing treatment. The as-prepared electrocatalysts were physically characterized using XRD, Raman, EDX, SEM, TEM and HRTEM analysis techniques. Very fine nanoparticles were shown in TEM image and their chemical identity was proved in XRD pattern by three crystal indices of nickel oxide species as (111), (200) and (220). The electrocatalytic activity of NiO/MC electrocatalysts was investigated for oxidizing urea molecules in 0.5 M NaOH solution. Adding variable nickel oxide loading values during the electrocatalyst preparation method appreciably affected the obtained oxidation current density. Increasing the deposited oxide weight percentage would enhance the activity of formed nanocomposite to attain its optimum performance at the electrocatalyst containing 17.5 wt% NiO. The effect of altering urea concentration and scan rate during the oxidation process on the resultant electrocatalyst activity was studied. Chronoamperograms displayed improved steady state oxidation current density values after 1800 s revealing stable nanocatalysts. This promising electrocatalytic behavior of NiO/MC elects its application as an active component for urea electro-oxidation in many potential applications including hydrogen production, fuel cells and water purification. (C) 2018 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.