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ZrC powder was directly electrosynthesized from inexpensive ZrO2 and carbon black precursors in molten CaCl2-NaCl at 800 °C. Constant voltage electrolysis was applied at 3.1 V between a graphite anode and a cathode composed of a ZrO2/carbon mixture. The reaction pathway of the solid state reduction was investigated by characterizing the composition and microstructure of partially and fully reduced samples. The spontaneous formation of the intermediate compound CaZrO3 was studied by an immersion experiment and thermodynamic analysis. The results show that the as-synthesized ZrC was composed of spherical particles with an average particle size of roughly 50 nm. The reduction pathway started by converting m-ZrO2 to CaZrO3, ZrCxO1-x and t,c-ZrO2. The phases of t,c-ZrO2 and CaZrO3 were then reduced to ZrCxO1-x, which was subsequently reduced to ZrC by the removal of oxygen and in situ carbonization.

Low Temperature Electrochemical Synthesis of Nanostructured ZrC Powder in Molten Salt