Hydrazide sol–gel process: A novel approach, for synthesizing nanostructured titanium nitride

A novel hydrazide sol–gel process has been developed to synthesize nanocrystalline titanium nitride. The process involves the reaction of titanium isopropoxide with anhydrous hydrazine in the presence of anhydrous acetonitrile to yield a solid precursor. Gas chromatography supported by chemical analysis shows that ≈80% of the isopropoxy groups are replaced by hydrazine. Nanostructured TiN is seen to evolve when the as-prepared precursor is pyrolyzed in ultra high purity (UHP) N2, UHP-Ar and NH3 at a temperature as low as 600 °C. However, fully crystallized single phase TiN is detected by X-ray diffraction at a temperature of 800 °C. Transmission electron microscopy and specific surface area analyses revealed that TiN obtained after pyrolysis in UHP-N2 is nanocrystalline (<100 nm) exhibiting a high specific surface area (≅250 m2 g−1).