Nickel nanostructures were synthesized onto the surface of glassy carbon microspheres (10-20 microm) with the aid of ultrasounds to produce bulk quantities of nickel micro and nanostructure surface-modified carbon microspheres (Ni-CMs). This new composite material was characterized by means of scanning electron microscopy (SEM), X-ray diffraction (XRD) and cyclic voltammetry (CV). The synthesized Ni micro and nanostructures on the glassy carbon microspheres were found to possess a large proportion of Ni (111) planes. The material was proved to be of interest for electrochemical ethanol sensing in particular. An optimized limit of detection of 1.3 ppm was obtained for ethanol in aqueous solution.