High quality nano-sized zirconium carbide (ZrC) powders were successfully fabricated via a developed chemical active dilution self-propagating high-temperature synthesis (SHS) method assisted by ball milling pretreatment process using traditional cheap zirconium dioxide powder (ZrO 2 ), magnesium powder (Mg) and sucrose (C 12 H 22 O 11 ) as raw materials. FSEM, TEM, HRTEM, SAED, XRD, FTIR and Raman, ICP-AES, laser particle size analyzer, oxygen and nitrogen analyzer, carbon/sulfur determinator and TG-DSC were employed for the characterization of the morphology, structure, chemical composition and thermal stability of the as-synthesized ZrC samples. The as-synthesized samples demonstrated high purity, low oxygen content and evenly distributed ZrC nano-powders with an average particle size of 50nm. In addition, the effects of endothermic rate and the possible chemical reaction mechanism were also discussed.