Tantalum hafnium carbide (Ta₄HfC₅) ultra pure and fine powders were fabricated by the pyrolysis of ceramic precursor. By co-hydrolysis with tantalum alkoxide and hafnium alkoxide as starting materials, blending phenolic resin (PF) as carbon source, the precursor PHT was successfully prepared as transparent stable light brown solution in xylene solvent. After the precursor was cured and mineralized, ceramic products were obtained at various pyrolysis conditions. Crystalline phase of the ceramic products was studied by XRD and SEM. Pure Ta₄HfC₅ solid solution was obtained when 3.25 wt% PF (weight ratio 100 % PHT supposed) was used and the sample was calcinated at 1450 ℃ for 1.5 h. Morphology, element and particle size analysis were conducted by SEM, TEM, ICP and laser particle analyzer. Particle size of the powder was 25 to 50 nm, and uniform fine particles were obtained with narrow size distribution, 100-200 nm with Dv(50)=136 nm. Viscosity of the PHT samples changed little after 3 months duration at atmospheric temperature with light avoided, which is favorable for the precursor impregnation pyrolysis manufacturing process.