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Polyaniline (PANI)/polysulfone (PSF) composite films are successfully prepared by phase separation and one-step in-situ polymerization.It is found that the head-on face (in contact with solution) of the films is green while the back face is white.The chemical component and the surface morphology of both surfaces of the films are characterized by FT-IR spectra and SEM,respectively.The effect of the polymerization temperature,time and concentration of the reactants on the electrical properties of the films are discussed in details.The thermo-oxidative degradation of the films is studied by thermogravimetric analysis (TGA).The results indicate that the thermal stability of the PANI/PSF films is higher than that of the pure PSF film.