Vanadium selenoether and selenolate complexes, potential single-source precursors for CVD of VSe2 thin films

Hector, Andrew L., Jura, Marek, Levason, William, Reid, Stuart D. and Reid, Gillian (2009) Vanadium selenoether and selenolate complexes, potential single-source precursors for CVD of VSe2 thin films. New Journal of Chemistry, 33 (3), 641-645. (doi:10.1039/b817903d).

Abstract

Reactions of VCl4 with one mol equiv. of L–L (L–L = MeSe(CH2)2SeMe, MeSe(CH2)3SeMe, nBuSe(CH2)2SenBu) in anhydrous CH2Cl2 solution at room temperature give [VCl4(L–L)] as very moisture-sensitive dark purple solids. Using VCl4 and excess selenoether in gently refluxing CH2Cl2 leads to reduction to [VCl3(L–L)] (L–L as above and o-C6H4(CH2SeMe)2), while VCl4 reacts with excess SeMe2 at room temperature to give [VCl3(SeMe2)2].

All new complexes were characterised by microanalysis, IR and UV/visible spectroscopy and magnetic measurements. Reaction of [(Cp)2VCl2] with two mol equiv. of LiSetBu in anhydrous thf gives the VIV selenolate complex [(Cp)2V(SetBu)2] as a very moisture-sensitive brown solid. The new complexes have been investigated as possible reagents for deposition of vanadium selenide. While low pressure chemical vapour deposition (LPCVD) experiments showed that the diselenoether complexes were not sufficiently volatile for VSe2 deposition, [VCl3(SeMe2)2] gives very thin deposits of VSe2. LPCVD studies on [(Cp)2V(SetBu)2] at 600 °C produce thicker black films of VSe2. In all cases EDX measurements show that the films are Se deficient.

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Contributors

Author: Andrew L. Hector

Author: William Levason

Author: Gillian Reid

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