In the present manuscript we describe the sonoelectrochemical synthesis of nanocomposites formed by nickel and cobalt hydroxide. The modified electrodes were characterized by electrochemical techniques such as Cyclic Voltammetry (CV) and Electrochemical Impedance Spectroscopy (EIS). In order to study the electrocatalytic properties of the electrodes aiming the development of electrochemical sensors, glucose was employed as electrochemical probe. The nanocomposites electrode showed an excellent sensitivity and the kinetic parameters were evaluated by using Rotating Disk Electrode (RDE) measurements. Both RDE and EIS results indicated that the interfacial properties play the most important role on the electrocatalytic reaction where the surfaces of the modified electrodes were analyzed by using Scanning Electronic Microscopies (SEM). By this way, our findings contribute in the sensor technology on the achievement of unique nanostructured electrocatalytic surfaces, synthesized in a single step with the influence of the ultrasonic radiation. (C) 2016 Elsevier Ltd. All rights reserved.