Soluble organometallic polymers containing zirconium and silicon were synthesized by a salt metathesis reaction. The molecular weight of the polymers was measured by GPC and the corresponding structures were identified by 13C NMR and FT-IR. After heat treatment of the polymers under argon at 1400 °C for 2 h, ZrC/SiC composites with different molar ratios of crystalline phases were obtained and characterized by XRD, elemental analysis, SEM and Raman spectroscopy. The crystalline size of the composites was approximately 100 nm–200 nm and the elements were well distributed at the different sites in the ceramics. The Raman results indicated that the ceramic residue could be considered as ZrC/SiC/C ternary composites.