The world is expected to face an undeniable energy shortage in future due to the depletion of fossil fuel resources, increased energy demands, and the harmful environmental impacts of current energy resources [
1]. Therefore, significant research has been focused on the development of new, efficient, and cleaner energy resources to resolve energy and environmental issues [
2‐
4]. Fuel cells (FCs) could be a very good choice for a variety of applications due to the merits of zero-emission, ease of handling, low operating temperature, and high efficiency [
5,
6]. Fuel cells allow the direct conversion of the chemical energy contained in the hydrogen-enriched fuel and an oxidant into electrical energy through electrochemical oxidation with minimum power losses. Among the various types of fuel cells, direct alcohol fuel cells are promising options due to some unique characteristics such as low permeability in the proton exchange membrane (PEM), along with high energy and power densities [
7]. However, compared to direct methanol fuels (DMFCs), direct ethanol fuel cells (DEFCs) have been considered a more appealing candidate due to higher energy density, lower toxicity, volatility, and crossover rate [
8]. Moreover, ethanol could be produced from a wide variety of renewable sources [
9]. Despite these potential advantages, low electrocatalytic activity and the high cost of anode catalyst for ethanol oxidation are of great significance [
10]. Accordingly, considerable attention has been devoted to anode catalyst development and structure engineering perspectives to develop the catalyst that possesses high electrocatalytic activity and stability with the merits of low cost. There is no doubt that platinum (Pt) has been considered as an efficient electrocatalyst for ethanol oxidation reaction but the use of platinum is quite limited due to its high cost, the paucity of noble metals, and loss of activity through poisoning by reactive intermediates [
11‐
15]. Hence, to solve these problems, various Pt-based bimetallic alloys (PtRu, PtPd, and PtSn) have been used to enhance the catalytic activity and reduce the cost; on the other hand, these Pt-based bimetallic electrocatalysts seriously suffer from heavy aggregation [
16‐
18]. To address this problem, as an alternative to precious metals, to minimize the cost of the metal catalyst, and to reduce the catalyst poisoning, various carbon supports such as graphene [
19,
20], multiwall carbon nanotube [
21], activated carbon [
22], and carbon nanofibers [
23] have often been used as supporting materials for both precious and non-precious functional materials. However, as an alternative to the existing commercial activated carbon, a large number of natural sources such as nutshell, coconut shell, peanut, sugarcane bagasse, sawdust, rice husks have been used to synthesize activated carbon [
24‐
29]. In particular, spent coffee ground (SCG) is a suitable raw source for the synthesis of valuable carbonous materials, and it is one of the widely consumed beverages and most popular commodities all around the world. Further, it is grown in more than 80 territories and more than 6 million tons of SCG are produced annually [
30]. It is well known that the high surface area and porosity of the carbonous materials are the basic requirements in electrocatalysis. Typically, chemical activation or high-temperature steam activation processes are used to increase the surface area and porosity of the carbonous materials. Chemical activation generally involves two steps: carbonization and activation. Normally, the carbon precursor is soaked with a suitable activating agent such as zinc chloride (ZnCl
2), phosphoric acid (H
3PO
4), sulphuric acid (H
2SO
4), potassium hydroxide (KOH), sodium hydroxide (NaOH), and potassium carbonate K
2CO
3 before the carbonization step [
31‐
34]. Zinc chloride has been widely used for chemical activation due to its earth-abundance and unique properties. However, the main objective of this work was to synthesize relatively cheap and effective electrocatalyst from SCG for ethanol electrooxidation. Therefore, the activation of carbon derived from SCG was performed with ZnCl
2. Interestingly, ZnCl
2 acts as a pore-forming agent as well as a precursor for ZnO. In particular, ZnO-based nanocomposites as a low-cost alternative for noble metals are used in fuel cell applications [
35,
36]. Besides the semiconducting and piezoelectric properties, its d-orbital holes are easily valence, which may enhance its catalytic activity [
2]. In this work, carbon microbead-encapsulated ZnO particles (CM-ZnO) have been synthesized from SCG by simple approach, involving a chemical activation and subsequent calcination at 700 °C and used as an electrocatalyst for ethanol electrooxidation in the alkaline medium. The introduced CM-ZnO demonstrated distinct textural characteristics that resulted in an enhanced catalytic activity toward ethanol electrooxidation.