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

A novel reaction of TiCl 4 and NaNH 2 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.