Carbon-based materials have a broad range of applications. Among various carbon-based materials, reduced graphene oxide (rGO) is one of the facile options for supercapacitor (SCs) fabrication. The main reason is that it offers excellent conductance and enhanced surface redox reactivity. Therefore, there is a significant possibility that this material will boost the electrochemical efficiency of pseudocapacitive materials based on transition metals. Using the sonication route, we have synthesized NiO/CoFe2O4 composite and decorated it with rGO. After structural and morphological analysis, the prepared electrode materials were subjected to electrochemical energy storage efficiency studies. The obtained data showed that the NiO/CoFe2O4@rGO exhibited a higher specific capacitance of 911.25 Fg-1 as compared to other electrode materials (such as NiO/CoFe2O4, NiO, and CoFe2O4). Moreover, it was observed that NiO/CoFe2O4@rGO has low equivalence series resistance (ESR) as 0.29 Ω, in comparison to NiO/CoFe2O4, NiO, and CoFe2O4. The enhanced conductivity of rGO and the good crystallinity of NiO and CoFe2O4 are responsible for the excellent efficiency of the NiO/CoFe2O4@rGO electrode material. According to the obtained results, the NiO/CoFe2O4@rGO nanocomposite is an effective capacitive material for supercapacitors fabrication.