Synthesis of Transition-Metal Nitrides from Nanoscale Metal Particles Prepared by Homogeneous Reduction of Metal Halides with an Alkalide

Transition-metal nitrides have been synthesized by heating nanoscale metal particles under flowing N 2 (g) or NH 3 (g). In some cases reaction temperatures are significantly lower than those required by conventional heating procedures. Nanoscale metal particles of Mo, Nb, Ta, Fe−Mo, Fe−Nb, and Cu−Nb were prepared by reduction of the respective metal chloride or mixture of chlorides with the sodide, [K + (15-crown-5) 2 ]Na -, in dimethyl ether solution. The previously characterized nitrides that were prepared (with synthesis conditions indicated) include γ-Mo 2 N (800 °C, N 2 ) and Mo 2 N (720 °C, N 2 ), Ta 3 N 5 (650 °C, NH 3 ), Fe 3 Mo 3 N (>650 °C, N 2 ), and a mixture of niobium nitride phases (800 °C, N 2 ). A previously unreported phase has been found in the Ba−Nb−N system.