Magnetic nanoparticles of NiFe2O4 were successfully prepared by utilizing the sol–gel techniques. The prepared samples were investigated through various techniques such as X-ray diffraction (XRD), transmission electron microscopy (TEM), dielectric spectroscopy, DC magnetization and electrochemical measurements. XRD data analysed using Rietveld refinement procedure inferred that NiFe2O4 nanoparticles displayed a single-phase nature with face-centred cubic crystallinity with space group Fd-3m. Average crystallite size estimated using the XRD patterns was observed to be ~10 nm. The ring pattern observed in the selected area electron diffraction pattern (SAED) also confirmed the single-phase formation in NiFe2O4 nanoparticles. TEM micrographs confirmed the uniformly distributed nanoparticles with spherical shape and an average particle size of 9.7 nm. Raman spectroscopy showed characteristic bands corresponding to NiFe2O4 with a shift of the A1g mode, which may be due to possible development of oxygen vacancies. Dielectric constant, measured at different temperatures, increased with temperature and decreased with increase in frequency at all temperatures. The Havrilliak–Negami model used to study the dielectric spectroscopy indicated that a NiFe2O4 nanoparticles display non-Debye type relaxation. Jonscher’s power law was utilized for the calculation of the exponent and DC conductivity. The exponent values clearly demonstrated the non-ohmic behaviour of NiFe2O4 nanoparticles. The dielectric constant of the nanoparticles was found to be >300, showing a normal dispersive behaviour. AC conductivity showed an increase with the rise in temperature with the highest value of 3.4 × 10−9 S/cm at 323 K. The M-H curves revealed the ferromagnetic behaviour of a NiFe2O4 nanoparticle. The ZFC and FC studies suggested a blocking temperature of ~64 K. The saturation of magnetization determined using the law of approach to saturation was ~61.4 emu/g at 10 K, corresponding to the magnetic anisotropy ~2.9 × 104 erg/cm3 . Electrochemical studies showed that a specific capacitance of ~600 F g−1 was observed from the cyclic voltammetry and galvanostatic charge–discharge, which suggested its utilization as a potential electrode for supercapacitor applications.