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

Ben J. Blackburn; Jared H. Crane; Caroline E. Knapp; Michael J. Powell; Peter Marchand; David Pugh; Joseph C. Bear; Ivan P. Parkin; Claire J. Carmalt

Materials & Design (Oct 2016)

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

Ben J. Blackburn,
Jared H. Crane,
Caroline E. Knapp,
Michael J. Powell,
Peter Marchand,
David Pugh,
Joseph C. Bear,
Ivan P. Parkin,
Claire J. Carmalt

Affiliations

Ben J. Blackburn: Materials Chemistry Centre, Department of Chemistry, University College London, 20 Gordon Street, London WC1H 0AJ, UK
Jared H. Crane: Materials Chemistry Centre, Department of Chemistry, University College London, 20 Gordon Street, London WC1H 0AJ, UK
Caroline E. Knapp: Materials Chemistry Centre, Department of Chemistry, University College London, 20 Gordon Street, London WC1H 0AJ, UK
Michael J. Powell: Materials Chemistry Centre, Department of Chemistry, University College London, 20 Gordon Street, London WC1H 0AJ, UK
Peter Marchand: Materials Chemistry Centre, Department of Chemistry, University College London, 20 Gordon Street, London WC1H 0AJ, UK
David Pugh: Department of Chemistry, University of Southampton, Highfield, Southampton SO17 1BJ, UK
Joseph C. Bear: Materials Chemistry Centre, Department of Chemistry, University College London, 20 Gordon Street, London WC1H 0AJ, UK
Ivan P. Parkin: Materials Chemistry Centre, Department of Chemistry, University College London, 20 Gordon Street, London WC1H 0AJ, UK
Claire J. Carmalt: Materials Chemistry Centre, Department of Chemistry, University College London, 20 Gordon Street, London WC1H 0AJ, UK; Corresponding author.

Journal volume & issue: Vol. 108
pp. 780 – 790

Abstract

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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. Keywords: Vanadium oxychloride, Precursors, Ester adducts, Vanadium carbide, Vanadium nitride, Hard materials

Published in Materials & Design

ISSN: 0264-1275 (Print); 1873-4197 (Online)
Publisher: Elsevier
Country of publisher: United Kingdom
LCC subjects: Technology: Electrical engineering. Electronics. Nuclear engineering: Materials of engineering and construction. Mechanics of materials
Website: https://www.journals.elsevier.com/materials-and-design

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