The ceramic precursor for HfB2/HfC/SiC/C was prepared via solution-based processing of polyhafnoxanesal, linear phenolic resin, boric acid and poly[(methylsilylene)acetylene)]. The obtained precursor could be cured at 250°C and subsequently heat treated at relative lower temperature (1500°C) to form HfB2/HfC/SiC/C ceramic powders. The ceramic powders were characterized by element analysis, thermal gravimetric analysis, X-ray diffraction, Raman spectroscopy, and Scanning electron microscopy. The results indicated that the ceramic powders with particle size of 200~500 nm were consisted of pure phase HfB2, HfC, and SiC along with free carbon as fourth phase with low crystallinity.