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The nickel sulphide (NiS) nanoparticles were synthesised by microwave-assisted-solvothermal method, pure Polyaniline (PANI) and Polyaniline with NiS (NiS–PANI) were synthesized at various weight percentages of NiS such as 1%, 5% and 15% by the oxidation polymerization method. The XRD pattern of NiS nanoparticles confirmed the formation of hexagonal structure, and its particle size was estimated by the Debye–Scherrer formula as 19 nm. The UV–visible absorption spectra recorded 200–1200 nm wavelength region and the bandgap was calculated from Tauc Plot. The morphology of PANI and NiS–PANI composites were observed as non-homogenous and agglomerated by field emission scanning electron microscope (FESEM). The FTIR spectra confirm the functional groups of the synthesized materials. The LCZ parameters were measured with the frequency of (1 Hz (hertz)–1 MHz (megahertz)) at room temperature was carried out, and the dielectric loss, dielectric constant, modulus plot and AC conductivity parameters were calculated for synthesized materials.