In this work, the co-precipitated bare Co3O4 and Fe-doped Co3O4 nanoparticles were prepared by incorporating 5 wt% and 10 wt% of iron. The structural analysis of the prepared samples reflected the cubic structure of Co3O4 with a reduction in crystallinity and an increase in Fe concentration. The synthesized nanocrystals had a crystallite size ranging from 7.15 to 16.58 nm. The F2g, Eg, and A1g vibrational modes of the micro-Raman spectrum reflect the phonon symmetries of Co2+ and Co3+ cations positioned at tetrahedral and octahedral sites in the Co3O4 cubic lattice. An agglomerated spherical morphology was observed for Fe-doped Co3O4 with 10 wt% Fe, and the elemental composition was analyzed using EDS analysis. From the electrochemical analysis (CV and GCD) the Fe-doped Co3O4 with 10 wt% Fe produced a better specific capacitance value of 54.06 Fg−1 at 1Ag−1.