Abstract
Gas phase nitridation of nc-TiO2 was carried out for obtaining nc-TiN. The nc-TiO2 precursor itself was derived from a Ti(OH)x precipitate formed through hydrolysis of titanium nitrate solution by aqueous ammonia reagent. Calcination of titanium hydroxide at 1000 °C yielded nc-TiO2 powder with an average particle size of ∼5 nm. Both nc-Ti(OH)x as well as nc-TiO2 were separately nitrided in an environment of argon and ammonia for synthesizing nc-TiN. A home-built thermogravimetric analysis-mass spectrometer apparatus was used for the nitridation experiment. The nanocrystalline phases of Ti(OH)x, TiO2 and TiN were characterized by XRD, TEM, IR and XPS techniques. The powders' XRD patterns indicated the formation of nanocrystalline TiN by ammonia bases nitridation of nc-TiO2. These studies also revealed sequential crystallo-chemical transformation of the intermediate precursor. FTIR studies revealed the existence of IR active modes in nc-TiO2 and the formation of a chemically pure TiN phase. The TEM image of TiN powder depicted the formation of nanocrystalline phase. Ti(2p3/2) photoelectron spectra indicated complete conversion of nc-TiO2 to nc-TiN.
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