The porous Ni/beta-Ni(OH)2 superstructures have been successfully prepared via a simple, fast one-pot solvothermal route in the presence of cetyltrimethyl ammonium bromide (CTAB), using NiCl2 center dot 6H(2)O and NaBH4 as the original reactants. The reaction was carried out in ethylene glycol at 170 C for I h. The morphology of the obtained product could be controlled by adjusting the reaction time and the surfactant. The products were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectrometry (EDS), Infrared (IR) spectrometry, and Brunauer-Emmett-Teller (BET). The electrochemical property of the as-obtained superstructures was investigated through the cyclic voltammogram (CV) measurements. It was found that the as-obtained porous Ni/beta-Ni(OH)(2) superstructures exhibited good electrochemical properties and could be used as electrochemical sensors for the detection of some organic small molecules such as hydrochinone, pyrocatechol, and glucose. (c) 2013 Elsevier Inc. All rights reserved.