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

Vanadium selenoether and selenolate complexes, potential single-source precursors for CVD of VSe2 thin films
Vanadium selenoether and selenolate complexes, potential single-source precursors for CVD of VSe2 thin films
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.
1144-0546
641-645
Hector, Andrew L.
f19a8f31-b37f-4474-b32a-b7cf05b9f0e5
Jura, Marek
e4a8ae2b-5609-45bb-99d8-a2320b9c89b9
Levason, William
e7f6d7c7-643c-49f5-8b57-0ebbe1bb52cd
Reid, Stuart D.
50ffded0-cd9e-4565-b663-7fb5c5a7da45
Reid, Gillian
37d35b11-40ce-48c5-a68e-f6ce04cd4037
Hector, Andrew L.
f19a8f31-b37f-4474-b32a-b7cf05b9f0e5
Jura, Marek
e4a8ae2b-5609-45bb-99d8-a2320b9c89b9
Levason, William
e7f6d7c7-643c-49f5-8b57-0ebbe1bb52cd
Reid, Stuart D.
50ffded0-cd9e-4565-b663-7fb5c5a7da45
Reid, Gillian
37d35b11-40ce-48c5-a68e-f6ce04cd4037

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).

Record type: Article

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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Published date: 2009

Identifiers

Local EPrints ID: 146027
URI: http://eprints.soton.ac.uk/id/eprint/146027
ISSN: 1144-0546
PURE UUID: 8050ac89-babd-4b89-b7ad-562b52571bb4
ORCID for Andrew L. Hector: ORCID iD orcid.org/0000-0002-9964-2163
ORCID for William Levason: ORCID iD orcid.org/0000-0003-3540-0971
ORCID for Gillian Reid: ORCID iD orcid.org/0000-0001-5349-3468

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Date deposited: 20 Apr 2010 11:58
Last modified: 29 Oct 2019 02:11

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Contributors

Author: Marek Jura
Author: William Levason ORCID iD
Author: Stuart D. Reid
Author: Gillian Reid ORCID iD

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