Nanocrystallized zirconium carbide (ZrC) powder was synthesized by an aqueous solution-based process using zirconium acetate and sucrose as starting reagents. Polyvinyl pyrrolidone (PVP) was used to combine the reactants to form a suitable precursor for ZrC. Through such a novel aqueous solutionbased process, fine-scale mixing of the reactants is achieved in an environmentally friendly manner. The formed precursor can be converted to ZrC by carbothermal reduction reaction at 1600-1650 C. Thanks to a limited amount of residual free carbon, the as-synthesized ZrC powder had an ultra-fine particle size (50-100 nm) and a low oxygen content less than 1.0 wt%. The conversion mechanisms from assynthesized pre-ceramic precursor to ZrC powder were investigated systematically and revealed by means of FTIR, TG-DSC, XRD, Raman, SEM and TEM.