Reactivity of vanadium oxytrichloride with β-diketones and diesters as precursors for vanadium nitride and carbide

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Abstract

Vanadium(V) oxytrichloride was reacted with 2,4-pentanedione, diethyl malonate, and diethyl succinate under inert conditions, forming compounds: dichloro(oxo)(2,4-pentanedione) vanadium(V) [1], dichloro(oxo)(diethyl malonate) vanadium(IV) [2] and dichloro(oxo)(diethyl succinate) vanadium(IV) [3]. Compounds 1–3 are coordinated to the vanadium centre through the two carbonyl oxygen atoms of the bidentate ligand. It was determined by X-ray crystallography that the structures of the resulting complexes were significantly different, resulting in a monomeric complex (1), a tetrameric ring (2) and a 1D coordination polymer (3). Following the synthesis and isolation of 1–3, they were tested as precursors for vanadium nitride and vanadium carbide by annealing under nitrogen and argon respectively at 1200 °C for 24 h. The resulting materials were characterised by: XRD, EDS, XPS and TEM.

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Blackburn, B. J., Crane, J. H., Knapp, C. E., Powell, M. J., Marchand, P., Pugh, D., … Carmalt, C. J. (2016). Reactivity of vanadium oxytrichloride with β-diketones and diesters as precursors for vanadium nitride and carbide. Materials and Design, 108, 780–790. https://doi.org/10.1016/j.matdes.2016.06.029

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