Application of the laser pyrolysis to the synthesis of SiC, TiC and ZrC pre-ceramics nano-powders

Refractory carbide nano-structured ceramics appear to be promising materials for high temperature applications requiring hard materials such as nuclear energy industry. Such carbide materials are usually obtained with micrometric sizes from the high temperature carbo-reduction of an oxide phase in a raw mixture of C black and titania or zirconia. TiC and ZrC nano-powders were produced from an intimate mixture of oxide nano-grains with free C synthesized by laser pyrolysis from the decomposition of a liquid precursor. The temperature and the duration of the thermal treatment leading to the carburization were decreased, allowing the preservation of the nano-scaled size of the starting grains. A solution of titanium iso-prop-oxide was laser-pyrolyzed with ethylene as sensitizer in order to synthesize Ti/C/O powders. These powders were composed of crystalline TiO2 nano-grains mixed with C. Annealing under argon enabled the formation of TiC through the carburization of TiO2 by free C. The final TiC mean grain size was about 80 nm. Zr/O/C powders were prepared from a solution of zirconium butoxide and were composed of ZrO2 crystalline nano-grains and free C. The same thermal treatment as for TiC, but at higher temperature, showed the formation of crystalline ZrC with a final mean grain size of about 40 nm. These two liquid routes of nano-particles synthesis are also compared to the very efficient gaseous route of SiC nano-powders synthesis from a mixture of silane and acetylene. (authors)