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Nickel hydroxide nanoflakes (Ni(OH)-NF) were prepared by chemical deposition and in situ exfoliation of nickel hydroxide layers confined in the aqueous domain of the liquid crystalline hexagonal template of Brij®78 surfactant. Using excess of sodium borohydride as a reducing agent generates concurrent excessive dynamic hydrogen bubbles which exfoliated and fragmented the nickel hydroxide layers precipitated within the soft hexagonal template. The physicochemical characterizations of Ni(OH)-NF by using surface area analyser, X-ray diffraction (XRD), XPS and transmission electron microscope (TEM) showed the formation of α-Ni(OH) nanoflakes with thickness of 2-3 nm and have about 450 m g surface area which is 20 times higher than that for bare nickel (bare-Ni) deposited without surfactant template. The electrocatalytic activity of the Ni(OH)-NF catalyst for urea electrolysis was studied by cyclic voltammetry and chronoamperometry techniques. The Ni(OH)-NF has shown a superior activity for the electrochemical oxidation of urea in alkaline solution and exhibits more than tenfold increase in activity in comparison with the bare-Ni deposit. The enhancement of urea electrooxidation activity was related to the superficial enhancement in the electroactive surface area of Ni(OH)-NF. This new approach of deposition and in situ exfoliation by using liquid crystal template and hydrogen bubbles offers a new platform to nanostructuring wide range of catalysts with better catalytic performance. [ABSTRACT FROM AUTHOR]