Synthesis of Uniform Titanium Nitride Nanocrystalline Powders via a Reduction–Hydrogenation–Dehydrogenation–Nitridation Route

A novel reaction of TiCl₄ and NaNH₂ at 450°–500°C for 12–24 h was performed for the preparation of TiN nanocrystalline powders. Powder XRD patterns indicated that the as-synthesized powder was cubic-phase TiN with a lattice constant a =4.225 Å. Transmission electron microscopy images showed that the TiN powders consisted of uniform particles with an average diameter of 10–20 nm. The binding energies of Ti2p_3/2 and N1s core levels at the position of 455.50 and 396.96 eV, respectively, were detected by X-ray photoelectron spectra. Four peaks, related to transverse acoustic, longitudinal acoustic, second-order acoustic, and transverse optical (TO) modes of TiN, respectively, were observed in the Raman spectra of TiN particles. A very reasonable formation mechanism of TiN nanocrystalline powders was proposed.