A new process was investigated which combines both fast pyrolysis carbonization and CS activated carbons with H3PO4 activation (CSAC). ACs were obtained as by-product from the preparation process of bio-oil with fast pyrolysis under different temperatures (T=727–973 K), in which the reaction ended in a very short duration. A two-step process of reaction is proposed to govern carbonization and activation: firstly fast pyrolysis reaction removing disorganized material was associated with considerable weight loss but with low generation of porosity, pyrolysis/carbonization under the flow of N2 is suggested to ensure fluidization of CS powders and bed material, enhance decomposition of raw material, initiates controlled gasification at different temperatures. Then H3PO4 activation process dominated at 573 K, which leads to considerable evolution of porosity. In this research, the adsorption characteristics were determined from N2 adsorption isotherms and subsequent analysised by the BET-and BJH-methods. As a result, the iodine adsorption number of AC was 1310 mg/g and the SSA of AC was 1421.38 m2/g .