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Inducing defects in metal oxide materials via doping with transition metal ions is a well-established strategy to enhance the electrochemical performance of supercapacitors. In this study, we synthesized manganese (Mn)-doped zinc oxide (ZnO) and evaluated its potential as an electrode material for supercapacitor applications. A comprehensive analysis of the defect environment in both undoped and Mn-doped ZnO was conducted using electron paramagnetic resonance (EPR) and photoluminescence (PL) spectroscopy. These techniques revealed the evolution of defect centers as a function of Mn doping concentration, offering insights into their role in electrochemical performance. Among the synthesized samples, ZnO doped with 0.6% Mn exhibited the highest specific capacitance of 163 F/g at a scan rate of 10 mV/s, along with excellent cyclic stability, retaining 95% of its initial capacitance after 500 cycles. This study highlights the significance of defect engineering in metal oxides for energy storage applications and underscores Mn-doped ZnO as a promising candidate for high-performance supercapacitors.