The solution combustion synthesis is a simple, cost-effective, and versatile method for electrocatalyst preparation. The present work reports combustion synthesis of nickel vanadium oxide nanoparticles utilizing two distinct fuels, namely citric acid (sample NV1) and glycine (sample NV2), as the oxide electrocatalyst. These nanoparticles (NPs) were subsequently dispersed in ethanol and drop-cast onto porous Toray carbon sheets to fabricate electrodes for electrochemical investigations relevant to supercapacitor applications. The scanning electron micrographs of the nanoparticles (NPs) confirm the presence of relatively smaller, uniform, and well-dispersed particles of dimensions approximately 21.1 nm. This is in contrast to the aggregates of polyhedral-shaped, bigger particles of average size approximately 39.5 nm observed for the NV2 sample. Energy dispersive X-ray analysis revealed the existence of oxygen (O), nickel (Ni), and vanadium (V) species in the prepared nanoparticles (NPs). The FTIR results confirm the presence of bending and stretching vibrations of V=O, O–H, C–H, and CH2 groups in the sample. The nanoparticles prepared using citric acid (NV1) and glycine (NV2) exhibit high specific capacitances of 886.49 and 787.12 F/g, respectively. The presented results highlight the essential role of citric acid as fuel in nanoparticle synthesis to improve the structural and electrochemical properties of the electrocatalyst for supercapacitor applications.