Polyaniline-NiO nanocomposites were prepared by employing interfacial polymerization using ammonium persulphate as an oxidizing agent. The formations of regular nanocomposite materials were studied by Fourier transform infrared (FTIR) spectroscopy and XRD techniques. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images were conducted to characterize the morphology. Thermo gravimetric (TG) analysis was carried out study the thermal stability of the resulting composites. Formation of conducting emeraldine salt form was concluded by electrical conductivity.