Nickel ferrite nanoparticles (NFNPs) were synthesized in an alkaline medium (pH ∼ 11) using a wet chemical co-precipitation technique. To probe the effect of surfactants on the surface morphology, particle size and size distribution of nanoparticles; two surfactants, namely, cetyl trimethyl ammonium bromide (CTAB) and sodium dodecyl sulphate (SDS), were applied. The native and surfactant-assisted nickel ferrite NPs were characterized using Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), dynamic light scattering (DLS) and transmission electron microscopy (TEM). The addition of surfactants (CTAB/SDS) effectively controlled the secondary growth of nickel ferrite particles and reduced their size, as examined by XRD, AFM, DLS, SEM and TEM. Characterization technique results affirmed that CTAB is a more optimistic surfactant to control the clustering, dispersion and particle size (∼22 nm) of NFNPs. To identify the impact of ferrite particle size on charge storage devices, their electrochemical properties were studied by using cyclic voltammetry (CV), galvanic charge-discharge (GCD) and electrochemical impedance spectroscopy (EIS) in 1 M KOH electrolyte through three-electrode assembly. NiFe2O4@CTAB showed a specific capacity of 267.1 C g-1, specific capacitance of 593.6 F g-1 and energy density of 16.69 W h kg-1, which was far better than the performances of other synthesized native NFNPs and NiFe2O4@SDS having larger surface areas.