Hafnium carbide ceramic powders were prepared by pyrolysis of a novel precursor, which was synthesized via one pot method using hafnium tetrachloride, acetylacetone, methanol, and hydroquinone as raw materials. The composition, morphology and microstructure of the pyrolysis products were characterized by XRD, FTIR, SEM/EDS, TEM, and SAED. The pyrolysis behavior of the obtained HfC precursor was investigated by TG-DSC and TG-MS. The results show that the ceramization of the HfC precursor starts at about 600℃, and the formation of HfC ceramics is initiated at about 1300℃. At temperature above 1500℃, the precursor completely transforms into HfC ceramics and free carbon. The as-obtained HfC phase has a single crystal structure and the size of the HfC particles ranges from 50 to 100 nm. Formation of the HfC ceramics can be attributed to the carbothermal reduction reaction of the HfO 2 , which is produced by pyrolysis of the precursor at a relative low temperature. The growth of the HfC crystals is retarded by free carbon formed during pyrolysis of the precursor.