Executed by In situ chemically oxidative route has been prepared PANI and doped Polyaniline (PANI/NiO) with weight percent of doping oxide. Oxidant agent as an Ammonium persulfate & HCL as a catalyst. Further these composites were characterized by XRD & SEM methods to investigate their structural and morphological studies. As a part of electrical studies DC conductivity was studied as a function of temperature and AC conductivity was studied as a function of frequency.