Two types of nano composite were obtained by in situ chemical method in polyaniline (PANI)/dodecylbenzenesulfonic acid (DBSA) system depending on the use of either ammonium persulfate (APS) or ferric chloride (FeCl 3 ) as the oxidant. In order to study the difference of the two composites in the surface characteristics, thermal stability, and electric properties, the composite films were studied by transmission electron microscopy (TEM), Xray diffraction (XRD), thermogravimetric analysis (TGA), and temperature dependent DC electrical conductivity. The results revealed a large difference in the surface morphology, thermal stability, and the microstructure properties between the two composites, and these differences were considered responsible for the molecular order and conductivity.