RF thermal plasma had been employed to prepare ZrB2 and ZrC ultra鄄fine powder materials based on thermodynamic calculation. The products were characterized by XRD, FESEM, and Hall flowmeter. Results revealed that high鄄purity ZrB2 and ZrC powders with an average diameter less than 100 nm could be obtained, and the apparent density of ZrB2 and ZrC was 0.71 g/ mL and 0.46 g/ mL. The production capability in the laboratory can reach 500 g/ h.