The two-stage aerosol-assisted synthesis technique was first used to prepare titanium containing raw aerosol powders with spherical particle morphology from aqueous and methanol solutions of selected oxygen-bearing titanium precursors and from neat titanium(IV) i-propoxide. The aerosol powders were subsequently pyrolyzed under ammonia at 1000, 1100, and 1200 °C, giving, in some favorable cases, compositions ranging from titanium oxynitride TiO x N y to titanium nitride TiN with average crystallite sizes of 32-38 nm and a residual oxygen content in the latter below 2 wt %. The intermediate and final products were characterized by SEM, XRD, FT-IR, and XPS analytical methods. For selected materials, oxygen content, helium density, and BET surface area were also determined.
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