Traditionally, ZrB2 powder was synthesized by various high temperature methods, such as the carbothermal reduction of ZrO2 and B4C (1400 °C) [3] and the mechano-chemistry treatment of a mixture of zirconia powder and amorphous boron followed by a relatively low temperature annealing (1100 °C) [4]. In addition, other methods have been developed to prepare zirconium diboride. Berthon et al. synthesized ZrB2 by CVD from a mixture of ZrCl4, BCl3 and H2[5]; Devyatkin researched electrosynthesis from cryolite-alumina melts containing zirconium and boron oxides [6]; Reich et al. prepared zirconium boride by plasma enhanced chemical vapor deposition [7]; and Andrievskii et al. obtained amorphous powder of ZrB2.76 with mean particle size 40 nm by thermolysis of Zr(BH4)4 at 573–623 °C [8].