Nickel cobalt phosphate (NiCoP) nanoparticles were synthesized by a co-precipitation method at concentrations of 0.1 M, 0.2 M, 0.3 M, 0.4 M, and 0.5 M. Drop-casting method was utilized in depositing the nanoparticles on the substrate surface to ensure uniform distribution on the substrate surface. Various analytical techniques including XRD, SEM, EDX, Raman spectroscopy, and electrochemical measurements were employed to comprehensively understand the structural, morphological, elemental, vibrational, and electrochemical properties of the synthesized nanoparticles. Results indicate amorphous phases for all samples, with nanoflake-like morphology observed via SEM, and constituent elements confirmed through EDX analysis. Raman spectroscopy validates the composition, while electrochemical measurements demonstrate the NiCoP electrodes’ promising utility in energy storage, particularly with the 0.1 M electrode exhibiting a maximum specific capacitance of 91.2 F g−1 and stability over 3000 cycles. Overall, the findings highlight the potential applications of NiCoP nanoparticles in energy storage and electrochemical devices, providing valuable insights for researchers in the field.