The temperature profiles associated with the passing of a self‐propagating wave in the combustion synthesis of zirconium boride were investigated. The use of these profiles in the determination of the kinetics of the associated synthesis reaction was investigated. From profile analysis an activation energy of 144.5 ± 15 kJ · mol−1was calculated and was found to agree very well with the corresponding value obtained from wave velocity measurements, 148.6 ± 12 kJ · mol−1. From these analyses, the thermal diffusivity of the reactants was also calculated. The thermal diffusivity decreased slightly with increasing combustion temperature, with the values ranging from 2.10 × 10−3to 1.79 × 10−3over the range of 2609 to 2909