3-D periodic mesoporous nickel oxide (NiO) particles with crystalline walls have been synthesized through the microwave-assisted hard template route toward the KIT-6 silica. It was investigated as a nonenzymatic amperometric sensor for the detection of uric acid. 3-D periodic nickel oxide matrix has been obtained by the hard template route from the KIT-6 silica template. The crystalline nickel oxide belonged to the Ia3d space group, and its structure was characterized by X-ray diffraction (XRD), N-2 adsorption-desorption, and transmission electron microscopy (TEM). The analysis results showed that the microwave-assisted mesoporous NiO materials were more appropriate to be electrochemical sensors than the traditional mesoporous NiO. Cyclic voltammetry (CV) revealed that 3-D periodic NiO exhibited a direct electrocatalytic activity for the oxidation of uric acid in sodium hydroxide solution. The enzymeless amperometric sensor used in the detection of uric acid with detection limit of 0.005 mu M (S/N = 3) over wide linear detection ranges up to 0.374 mM and with a high sensitivity of 756.26 mu A mM(-1) cm(-2), and a possible mechanism was also given in the paper. (C) 2015 Elsevier B.V. All rights reserved.