In-situ synthesis of zirconium oxycarbide by electroreduction of ZrO2/C in molten salt

Homogenous ZrC x O y powders have been successfully synthesized by in-situ electro-reduction of solid ZrO 2 –C composite precursors in molten CaCl 2 . The effect of applied cell voltage and molar ratio of ZrO 2 to C on preparation of ZrC x O y were investigated. The reduction pathway of the composite electrode was studied based on the analysis of intermediate products using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results show that ZrO 2 is firstly converted to CaZrO 3 . The resulting CaZrO 3 is then reduced to ZrC x O y . The ZrC x O y formation is dramatically influenced by electrolysis voltage and molar ratio of ZrO 2 to C: a higher cell voltage and lower molar ratio of the ZrO 2 to C are more preferable for the formation of ZrC x O y powder. Homogenous ZrC x O y powders with particle size of ~100 nm are synthesized by ZrO 2 /C starting elemental powders in CaCl 2 molten salt at 1123 K for more than 3 h, when the cell voltage is 3.0 V and the molar ratio of the ZrO 2 to carbon starting materials is 1:1.0.