Dense bulk ZrB2 ceramic was synthesized by mechanical alloying (MA) and followed spark plasma sintering (SPS) using zirconium and boron as initial materials. It was found that MA process was effective to fragment the coarse metal zirconium particles from 45 μm to less than 1 ?m within 20 hours. In comparison with the commercial ZrB2 powder, the as-obtained zirconium and boron mixture powders showed higher sinterability. When the sintering was carried out at 1800°C, the relative density of synthesized ZrB2 samples using mixture powder was above 95%, higher than that of ZrB2 sample prepared using commercial powder (73%). Vickers hardness of those ZrB2 samples was at the same level of 15 GPa. However, the fracture toughness of ZrB2 samples seemed to depend on the heating rate of the SPS process. Corresponding to the heating rates of 10, 50, and 100°C/min, the fracture toughness of as-prepared ZrB2 samples were 3.83, 3.19, and 2.74 MPa·m1/2, respectively.