Nano-sized ZrB2 powders were synthesised using the high energy ball milling with ZrO2 and B2O3 as raw materials and Mg as the reducing agent. The resulting powders were characterised by X-ray diffraction, scanning electron microscopy, laser particle size analysis, transmission electron microscopy, energy dispersive spectrometry, and X-ray photoelectron spectroscopy. The influence of the synthesis parameters, including the ratios of ZrO2 to B2O3, milling medium, and reaction time, on the synthetic course of the ZrB2 nanopowders were studied systematically. The mechanisms by which these parameters influence the synthetic course of and the resulting product quality are determined. Ultimately, the diameter of the resulting particles is about 200–400 nm, which are an agglomeration composed of many individual small particles with an average diameter of ∼50 nm. In addition, the oxidation of ZrB2 powders has also been studied.
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