Due to poor mechanical properties and antioxidation properties, etc of single phase ultrahigh-temperature ceramics (UHTCs), the second phase such as SiC was usually introduced for improving those properties. Herein, a novel stratagem for synthesis of binary HfC-SiC ceramics has been presented. A Hf-O-Hf polymer as a HfO 2 precursor has been synthesized for preparing soluble HfC-SiC precursors with high solid content and low viscosity solutions without additional organic solvents. The structure of PHO was characterized by FTIR and 1 H-NMR, the crystalline behavior and morphologies of polymer-derived ceramics were identified by XRD, SEM-EDS, and TEM. It was shown that PHO firstly transformed into HfO 2 , and then reacted with in situ carbon derived from DVB and PCS thus producing cubic HfC through carbothermal reduction. In addition, the obtained HfC-SiC nanopowders exhibited spherical morphology with a diameter less than 100 nm, while the Hf, Si, and C are homogeneously distributed.