Reactions between zirconium powder 10–15 μm in particle size and microcrystalline boron 10–20 μm in particle size in an Na 2 B 4 O 7 ionic melt have been studied at temperatures from 600 to 850°C and reaction times from 5 to 10 h. The results demonstrate that ZrB 2 forms starting at 750°C. According to scanning electron microscopy data, the ZrB 2 powder consists of particles 90–95 nm in average size. The crystallite size evaluated from X-ray diffraction data is 85 nm.