Composite catalysts Fe0.3Co0.7-doped carbon aerogel have been in situ synthesized by chemical reduction method and successfully employed in the hydrolysis of NH3BH3 (AB) at room temperature. The mass percent of the doped Fe0.3Co0.7 alloys can reach to the maximum value of 40 wt%. The prepared catalysts exhibit excellent catalytic activity, especially for the specimen of 40 wt% Fe0.3Co0.7/C, which shows high catalytic activity and long durability. Its maximum hydrogen generation rate is as high as 13,695.6 ml min(-1) g(-1) at 298 K and the activation energy is only 20.83 kJ mol(-1). Besides, this catalyst possesses preferable cycling stability at room temperature. The low cost, high catalytic activity and enhanced cycling stability can make it have a bright future in the application field of fuel chemistry. Copyright (C) 2012, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.