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Electrocatalytic water splitting is a promising solution to resolve the global energy crisis. Tuning the morphology and particle size is a crucial aspect in designing a highly efficient nanomaterials-based electrocatalyst for water splitting. Herein, green synthesis of nickel oxide nanoparticles using phytochemicals from three different sources was employed to synthesize nickel oxide nanoparticles (NiOx NPs). Nickel (II) acetate tetrahydrate was reacted in presence of aloe vera leaves extract, papaya peel extract and dragon fruit peel extract, respectively, and the physicochemical properties of the biosynthesized NPs were compared to sodium hydroxide (NaOH)-mediated NiOx. Based on the average particle size calculation from Scherrer’s equation, using X-ray diffractograms and field-emission scanning electron microscope analysis revealed that all three biosynthesized NiOx NPs have smaller particle size than that synthesized using the base. Aloe-vera-mediated NiOx NPs exhibited the best electrocatalytic performance with an overpotential of 413 mV at 10 mA cm−2 and a Tafel slope of 95 mV dec−1. Electrochemical surface area (ECSA) measurement and electrochemical impedance spectroscopic analysis verified that the high surface area, efficient charge-transfer kinetics and higher conductivity of aloe-vera-mediated NiOx NPs contribute to its low overpotential values.