Henequen fiber was air-stabilized, carbonized, and steam-activated to obtain high surface area activated henequen fiber (AHF). Thermal behavior of henequen fibers has been studied by TGA. The structural morphology and characteristics were observed by SEM and BET surface area measurement. The yield of AHF from natural henequen was in the range of 20~25 wt%. Mesopores (2~2.5 nm) were developed on the AHF as the activation temperature was raised up to 700℃, and the band of mesopore size distribution moved to 15~30 nm when the activation were carried out at 900℃ for 30 min. The specific surface area and the total pore volume were about 1394 m2/g and 1.30 cm3/g, respectively at this activation conditions.