Silicothermic synthesis of phase-pure HfB2 fine powder

Phase pure and nano-sized hafnium diboride (HfB 2 ) fine powder was prepared via a novel sustainable silicothermic route at 1100°C from inexpensive raw materials HfO 2 , Na 2 B 4 O 7 and Si. By introducing sodium oxysalts as source of Na 2 O into the batch mixtures, the SiO 2 / Na 2 O modulus in the melt were reduced from 5:1 to 2:1, and the original water-insoluble byproduct SiO 2 was taken by the melt at test temperature and converted into water soluble sodium silicate (Na 2 Si 2 O 5 ) which was easily removed from the reacted mass via simple hot water washing. Consequently, the aqua sodium silicate could be readily recycled and used as a precursor for preparing many other valuable materials due to absence of foreign salts (eg halides, especially in the molten salt-assisted synthesis process) in the synthesis process, and the relevant environmental concerns could be alleviated. Using excessive amount of 20 wt% Si and 15 wt% Na 2 B 4 O 7 as compensation for the evaporation loss of silicon, in the form of SiO (g), and B 2 O 3 in the reduction process, a high reaction extent was achieved and HfO 2 and Na 2 B 4 O 7 were completely converted into HfB 2 at 1100°C.