To increase specific surface property of activated carbon fiber(ACF), chemical activation(CA) using alkali metals and surface treatment(ST) using oxidant was widely used. The CA and ST process developed micro-pore on the surface of ACF by chemical reaction of the alkali metals and oxidative of oxidant, respectively. To improve the efficiency of CA process for developing micro-pores on the surface of ACF, the ST process was adopted as an pre-treatment method. After treatment of ST process, ACF properties was investigated depending on the ST pre-treatment process. FT-IR, TG and elemental analysis of the ACF are carried out, and an adsorption property of ACF was also evaluated using toluene(which in typical volatile organic matter). Once the single CA process is used, the surface area and adsorption capacity of ACF were increased from 1,483 to 1,988 $m^2/g$ and from 0.22 to 0.27 $g_{-Tol.}/g_{-ACF}$, respectively. On the other hands, once the ST and CA processes are used successively, the surface area and adsorption capacity of ACF are greatly increase(where the surface area is 2,743 $m^2/g$ and the adsorption capacity is 0.37 $g_{-Tol.}/g_{-ACF}$). It indicates that the combined process of ST and CA can improve the surface process properties of ACF.