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Abstract With the aim of developing fuel cell applications that are capable of generating efficient electrical energy, much of the attention should be given to exploring new catalysts that could be less costly and more abundant than the most commonly used catalyst, platinum. This work explores nickel-based layered double hydroxide (Ni-LDH) as a fuel cell’s affordable catalyst for Oxygen Reduction Reaction (ORR). Ni-LDH was prepared and drop coated onto a Glassy Carbon Electrode (GCE) to conduct a 3-way electrode cyclic voltammetry using an oxygen-saturated aqueous sodium hydroxide (NaOH) solution as electrolyte. The electroanalytical study of the GCE-modified Ni-LDH working electrode showed an enhancement of both anodic and cathodic peaks because of the presence of oxygen at low temperatures. Data obtained from this experiment will serve as a reference for fuel cell systems in which Ni-LDH modified working electrodes are scaled up for comparison of area-specific properties.