In this study, we successfully synthesized NiCo(HPO4) as an electrode material for supercapacitors using a one-step solvothermal method. Water, ethanol, and glycerol were employed as solvents, while phosphoric acid solution served as a phosphate agent. The synthesized NiCo(HPO4) was characterized using Fourier transform infrared (FT-IR) spectroscopy and X-ray diffraction (XRD) analysis confirming its phase and chemical properties. Scanning electron microscopy (SEM) was utilized to examine the surface morphology, revealing the mixture of nanoparticle and plate like particle of NiCo(HPO4). In terms of electrochemical performance, NiCo(HPO4) demonstrated a specific capacitance of 641 Fg−1 at 0.5 A g−1 in a three-electrode configuration using a 2 M KOH electrolyte. These results indicate that NiCo(HPO4) exhibits excellent capacitance and offers promise for the development of stable and high-performance electrodes in supercapacitor devices. [ABSTRACT FROM AUTHOR]