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A mechanically induced self-sustaining reaction (MSR) was used to synthesize hafnium diboride nanoparticles. Along this route, magnesium was selected as a robust reducing agent for co-reduction in boron and hafnium oxides in a combustive manner. Combustion occurred after a short milling period of 12 minutes. The hafnium diboride nanoparticles had a polygonal faceted morphology and were 50-250 nm in diameter. The assessment of the processing mechanism revealed that the initial combustive reduction in BO to elemental B by Mg was the major step for progressing the overall reaction. After that, HfO can be reduced to elemental Hf, followed by the synthesis of HfB phase.

A ZrSiO4/B2O3/Mg/C system was used to synthesize a ZrB2-based composite through a high-energy ball milling process. As a result of the milling process, a mechanically induced self-sustaining reaction (MSR) was achieved in this system. A composite powder of ZrB2–SiC–ZrC was prepared in situ by a magnesiothermic reduction with an ignition time of approximately 6 min. The mechanism for the formation of the product was investigated by studying the relevant subreactions, the stoichiometric amount of B2O3, and thermal analysis.