The complexes MCl3(THF)3 (M = Ti, V, Cr, Mo, etc.) were used as precursors for early transition metal nitrides, and solid solutions of these isomorphous complexes MxM’1-xCl3(THF)3 were prepared by co-crystallization. Heating the precursor under NH3 flow from 800-950 °C produced powders of the nitride MN, and solid solutions of these precursors produced alloys of the nitrides. Nanomaterials were synthesized by two methods: (1) reaction of a MCl3(THF)3 solution with 3 eq of KNH2 in THF in the presence (or absence) of oleylamine (OA), followed by nitridation under NH3 flow at 650-950 °C and (2) loading a porous catalyst support such as pelletized Al2O3 with the MCl3(THF)3 complex, followed by similar heat treatment. The materials were characterized by powder X-ray diffraction, elemental analysis, BET, SEM, and optical spectroscopy. Diffuse reflectance and UV-Vis-NIR spectroscopy showed the plasmonic resonances, and these were compared to theoretical calculations. The plasmon resonances of TiN nanoparticles made with oleylamine were redshifted compared to those made without, and from commercial nanomaterials. The figures below shows the XRD patterns of some example materials and diffuse reflectance of nanomaterial in porous Al2O3 support. Preliminary results show TiN nanoparticles have some activity in the photodegradation of the CWA simulant DEMETON-S.

Synthesis and plasmonic properties of early transition metal nitride powders and nanomaterials

254th National Meeting (2017)

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