Zirconium diboride toughened by silicon carbide and zirconia fiber (ZrB2SiCZrO2f) was prepared by using planetary ball mill and the effect of milling time was investigated. The results showed that both the length of fiber and particle size of ZrB2SiC-matrix were reduced as the ball milling time increased. When milling time varied from 8 h to 12 h, the accumulated fibers and agglomerated particles were observed. The production of a homogeneous ceramic could be successfully achieved by using a combination of 20 h milling time and hot-pressing at 1850 °C for 60 min under a uniaxial load of 30 MPa. The optimal flexural strength and fracture toughness of the hot-pressed ZrB2SiCZrO2f ceramics reached 1084 MPa and 6.8 MPa m1/2, respectively. The main toughening mechanisms were fiber debonding, fiber pull-out and transformation toughening. The results indicated that the ball milling technique was proposed as a potential and simple method to obtain usable quantities of ZrB2SiCZrO2f ceramic.