Carbon microbead-encapsulated ZnO (CM-ZnO) particles have been synthesized from the spent coffee ground (SCG) by chemical activation with ZnCl 2 followed by calcination at 700 ℃ in N 2 environment. Interestingly, ZnCl 2 can act as an activating agent as well as a precursor for ZnO particles. The structure of the core and shell of the CM-ZnO was investigated by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) techniques. Moreover, X-ray diffraction (XRD) and energy-dispersive spectroscopy (EDS) studies confirmed the presence of the encapsulated ZnO particles. The Brunauer-Emmett-Teller (BET) and Barrett-Joyner-Halenda (BJH) plots showed a well-developed porous structure with a specific surface area of 210 m 2 /g, average pore volume of 1.12 cm 3 /g, and an average pore radius of 31.7 Å. The electrooxidation behavior of ethanol toward the synthesized CM-ZnO was then studied using cyclic voltammetry (CV) technique. For comparison, two types of modified electrodes were prepared: the first one with the non-activated SCG and the second one with the CM-ZnO. The electrochemical measurements of the prepared CM-ZnO demonstrated higher electrocatalytic activity with a current density of ~ 35 mA/cm 2 at 0.4 V vs. Ag/AgCl for ethanol electrooxidation in an alkaline medium. The electrochemical measurements specified that the presence of ZnO particles and the high surface area of the activated sample have a significant influence on electrooxidation activity. Therefore, the introduced CM-ZnO particles could be an alternative and effective non-precious electrocatalyst for ethanol electrooxidation.