Abstract A new method was developed for quickly preparing a highemissivity silicon boride compound of SiBx (x = 3, 4, 5, 6) by highly exothermic Ti-TiO2-Si-Al chemical oven preheating. The SiBx combustion synthesis process and adiabatic combustion temperature were investigated. A large exothermic reaction occurred at the combustion temperature of 1 700 K. X-ray diffraction results indicate that an SiBx phase and a substantial amount of unreacted Si were identified in the products. By increasing the boron content until the Si-B ratio reached to 1 : 6, the diffraction peaks primarily indicated SiB6, SiB4, and Si11B33 in the final product. According to the spectra and quantitative results, the atomic chemical composition ratio of Si and B was close to the nominal composition. Thus, this method offers an efficient way to produce Si-B compounds with less time and energy consumption than current methods.