The thermal decomposition of 3,4-bis(4'-aminofurazano-3') furoxan (BAFF) was studied by DSC, TG, the combination technique of in situ thermolysis cell with rapid-scan Fourier transform infrared spectroscopy (thermolysis/RSFT-IR) and the fast thermolysis probe with rapid-scan Fourier transform infrared spectroscopy (fast thermolysis/RSFT-IR). The result shows that the melting point of BAFF is 168.4 degrees C, the peak temperatures of the two exothermic peaks are respectively 260.4 degrees C and 338.8 degrees C on DSC curve. The apparent activation energy Ea and the pre-exponential factor A are respectively 122.21 kJ mol(-1) and 10(9.89) s(-1) for major exothermic decomposition process of BAFF. The kinetic equation of major exothermic decomposition for BAFF is d alpha/dt =10(10.07)exp(-1.46993 x 10(4)/T)(1 - alpha) [-ln (1 - alpha)](1/3). The thermal decomposition gaseous products of BAFF consist of CO2, NO2, N2O and NO. The BAFF is shown by IR spectroscopy to convert to ammonium dicyanamide (NR4[N(CN)(2)]), cyclic azine residues (melamine or melamine-like). (C) 2009 Elsevier B.V. All rights reserved.