ZrB2 were synthesized by a Pechini-type route, wherein a precursor solution of citric acid, glycerol, boric acid, and metal ions was prepared.The precursors were gelled at 150 ℃ and then heat treated at high temperatures to form the diboride powders.Submicrometer (200-800 nm) ZrB2 were obtained at 1400 ℃ with 2.5 B/metal molar ratios.The final products also contained a little amount of carbide phase, indicating that the boride formation may concern the intermediary phase of carbide.The HfB2 and temary diboride powders were also synthesized by the same method and had a submicrometer size, moreover, the ternary boride Hf0.5Zr0.5B2 showed a single phase of AlB2-type.