A kind of promising hydrogen storage material-hydrazine bisborane (N(2)H(4)(BH(3))(2), HBB) is synthesized by a typical chemical method. HBB exhibits relatively low dehydrogenation temperature (around 100 degrees C), effective prevention of any unwanted gaseous products, such as ammonia, diborane, confirming a very high hydrogen release purity of >99%. The activation energy (E(a)) of the first-step dehydrogenation of HBB is calculated to be 106.4 kJ/mol using Kissinger's method. According to the (11)B NMR and FT-IR results, the thermal decomposition of HBB was determined to produce [HBN(2)BH](2) dimers, in which the coordination environment of B atoms located in the formation of HBN(2). Copyright (C) 2011, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.