Zirconium carbide (ZrC) was synthesized by solution-based processing using versatile starting reagents including zirconium oxychloride octahydrate (ZrOCl2·8H2O, ZOC), acetylacetone (Hacac), and phenolic resin. Polyzirconoxane (PZO), obtained by chelation of Hacac to zirconium, was used to combine with phenolic resin to form a precursor for ZrC. It generated ZrC at a relatively low temperature (1550°C) and in a low C/Zr molar ratio of 2 assuming that phenolic resin was the only carbon source. As a comparison, synthesis of ZrC only using ZOC and phenolic resin was also conducted. Besides, the pyrolysis of PZO was carried out and the transformation mechanism during the pyrolysis was studied, during which ZrC was obtained at 1550°C in flowing argon. The conversions from as-synthesized preceramic precursors to ceramics were studied by means of FTIR, DSC-TG, SEM, EDS, and XRD.