Homogenous ZrC
xO
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
xO
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
xO
y. The ZrC
xO
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
xO
y powder. Homogenous ZrC
xO
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.
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