Direct Solvothermal Synthesis of Early Transition Metal Nitrides
Baishakhi Mazumder (2413546)Pietro Chirico (2413549)Andrew L. Hector (1290588)
Abstract
Solvothermal reactions of TaCl<sub>5</sub> with LiNH<sub>2</sub> in benzene result in nanocrystalline Ta<sub>3</sub>N<sub>5</sub> at 500 or 550 °C. The ∼25 nm Ta<sub>3</sub>N<sub>5</sub> particles have a band gap of 2.08−2.10 eV. The same reactions in mesitylene resulted in a higher crystallization temperature and large amounts of carbon incorporation due to solvent decomposition. Reactions of Ta(NMe<sub>2</sub>)<sub>5</sub> with LiNH<sub>2</sub> under the same conditions resulted in TaN. Rocksalt-type MN phases are obtained for Zr, Hf, or Nb when their chlorides (ZrCl<sub>4</sub>, HfCl<sub>4</sub>, or NbCl<sub>5</sub>) or dialkylamides (M(NEtMe)<sub>4</sub>, M = Zr, Hf) are reacted with LiNH<sub>2</sub> under similar conditions. With the amides, there is some evidence for nitrogen-rich compositions (HfN<sub>>1</sub>), and carbon is incorporated into the products through pyrolysis of the dialkylamide groups.
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