The Ni(OH) 2 /NiOOH nanoparticles (NPs) electrodeposited on a glassy carbon electrode (GCE) in Ni(NO 3) 2 and NH 3 •H 2 O aqueous solution for the electrode materials. Then the nickel hydroxide/oxyhydroxide acetate was formed in acetate solution. The effects of deposition conditions such as the concentration of Ni(NO 3) 2 solution, the number of sedimentary cycles, the concentration of acetate in the soaking liquid and the soaking time are discussed in detail. The electrochemical properties of the material have been investigated by cyclic voltammetry, Tafel curve, EIS and amperometric it curve techniques. The result displays excellent electrocatalytic activity towards the electrocatalytic oxidation of urea in alkaline solution. Furthermore, the modified electrode for oxidation reaction has the advantages of simple preparation, good electrochemical properties and stabilisation.