This study intended to synthesize Nickel-doped Cerium oxide (Ni-CeO2 NPs) nanoparticles using Pedalium Murex leaf extract. X-ray diffraction (XRD) was used to investigate the structure of the Ni-CeO2 NPs. The XRD measurements showed that the Ni-CeO2 NPs crystallized into the face-centered cubic system. The Ni(1%)-CeO2 and Ni(3%)-CeO2 NP’s crystallite sizes were between 47[Formula: see text]nm and 59[Formula: see text]nm. FTIR and Raman spectral studies were conducted to investigate the sample’s atomic vibrations and chemical bonding. Energy-dispersive X-ray study and field-emission scanning electron microscopy were performed to examine the surface texture and chemical assembly of the Ni-CeO2 NPs. UV–Vis DRS spectrum study was performed to ascertain the reflectance characteristics and bandgap of Ni-CeO2 NPs. The Ni(1%)-CeO2 and Ni(3%)-CeO2 NPs were found to have bandgaps of 2.73[Formula: see text]eV and 2.82[Formula: see text]eV, respectively. Electrochemical impedance spectroscopy and cyclic voltammetry were employed to explore the electrochemical nature of Ni-CeO2 NPs and their capacitive properties at various scanning rates. Using the agar well-diffusion technique, the antifungal activities of Ni-CeO2 NPs were assessed. The experimental findings illustrate the utility of Ni-CeO2 NPs for supercapacitor electrode material and healthcare applications.