Two types of supercapacitor electrode materials have been synthesized: AC/PANI, activated carbon composites polyaniline by in-situ polymerization of aniline on the surface of activated carbon, and Ni-AC/PANI, the AC/PANI composite dopes with nickel. The microstructure of composites has been examined by scanning electron microscope (SEM). Fourier transform infrared spectroscopy (FI-IR) has been used to determine the molecular structure and chemical bond of the composites. The nickel content has been measured by atomic absorption spectrometry (AAS). The electrochemical performance of the composite has been characterized by cyclic voltammery and galvanostatic charge-discharge in 6mol•L-1 KOH solution using Hg/HgO as reference electrode. Due to the doping of nickel salt, Ni-AC/PANI shows desired microstructure, good high-current charge-discharge performance and good electrochemical behavior with an capacitance of 535F•g-1, 38.2% higher than that of AC/PANI.