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Synthesis and properties of MoCl4 complexes with thio- and seleno-ethers and their use for chemical vapour deposition of MoSe2 and MoS2 films

Synthesis and properties of MoCl4 complexes with thio- and seleno-ethers and their use for chemical vapour deposition of MoSe2 and MoS2 films
Synthesis and properties of MoCl4 complexes with thio- and seleno-ethers and their use for chemical vapour deposition of MoSe2 and MoS2 films
Treatment of trans-[MoCl4(MeCN)2] with L (L = Me2S, Me2Se, THT, ½ MeSCH2CH2SMe) in CH2Cl2 solution, or reaction of MoCl5 with excess L’ (L’ = nBu2S, nBu2Se, ½ MeSCH2CH2SMe, ½ iPrSCH2CH2SiPr, ½ MeSCH2CH2CH2SMe, ½ MeSeCH2CH2CH2SeMe) in MeCN, produces the Mo(IV) complexes, [MoCl4(L)2] and [MoCl4(L’)2], respectively, in good yield. The new complexes have been characterised by IR and UV-vis spectroscopy, elemental analysis and magnetic measurements, whilst crystal structure analyses of trans-[MoCl4(Me2S)2], cis-[MoCl4{RS(CH2)2SR}] (R = Me, iPr) and cis-[MoCl4{MeS(CH2)3SMe}] confirmed their identities and distorted octahedral geometries. The potential of [MoCl4(nBu2E)2] (E = S, Se) as the first examples of molybdenum halide derived single source CVD precursors for the growth of MoE2 thin films was first probed by TGA, which showed multi-step decomposition processes, with the masses of the final residues consistent with MoSe2 and MoCl4 (from E = S; see discussion), respectively. Low pressure CVD experiments conducted at 750 C (E = S) and 525 C (E = Se) gave silvery and golden yellow films, respectively. Grazing incidence and in plane XRD data confirmed these to be 2H-MoE2, whilst the texture of the MoSe2 was investigated using pole figure measurements. SEM and EDX data, optical and Raman data on the films are also reported.
0300-9246
2406-2414
Chang, Yao-Pang
9516eba3-1424-411c-8f13-c564cae63407
Hector, Andrew L.
f19a8f31-b37f-4474-b32a-b7cf05b9f0e5
Levason, William
e7f6d7c7-643c-49f5-8b57-0ebbe1bb52cd
Reid, Gillian
37d35b11-40ce-48c5-a68e-f6ce04cd4037
Whittam, Joshua
9793bbc2-ee36-4f64-a585-22f18ccef85a
Chang, Yao-Pang
9516eba3-1424-411c-8f13-c564cae63407
Hector, Andrew L.
f19a8f31-b37f-4474-b32a-b7cf05b9f0e5
Levason, William
e7f6d7c7-643c-49f5-8b57-0ebbe1bb52cd
Reid, Gillian
37d35b11-40ce-48c5-a68e-f6ce04cd4037
Whittam, Joshua
9793bbc2-ee36-4f64-a585-22f18ccef85a

Chang, Yao-Pang, Hector, Andrew L., Levason, William, Reid, Gillian and Whittam, Joshua (2018) Synthesis and properties of MoCl4 complexes with thio- and seleno-ethers and their use for chemical vapour deposition of MoSe2 and MoS2 films. Dalton Transactions, 47 (7), 2406-2414. (doi:10.1039/C7DT04352J).

Record type: Article

Abstract

Treatment of trans-[MoCl4(MeCN)2] with L (L = Me2S, Me2Se, THT, ½ MeSCH2CH2SMe) in CH2Cl2 solution, or reaction of MoCl5 with excess L’ (L’ = nBu2S, nBu2Se, ½ MeSCH2CH2SMe, ½ iPrSCH2CH2SiPr, ½ MeSCH2CH2CH2SMe, ½ MeSeCH2CH2CH2SeMe) in MeCN, produces the Mo(IV) complexes, [MoCl4(L)2] and [MoCl4(L’)2], respectively, in good yield. The new complexes have been characterised by IR and UV-vis spectroscopy, elemental analysis and magnetic measurements, whilst crystal structure analyses of trans-[MoCl4(Me2S)2], cis-[MoCl4{RS(CH2)2SR}] (R = Me, iPr) and cis-[MoCl4{MeS(CH2)3SMe}] confirmed their identities and distorted octahedral geometries. The potential of [MoCl4(nBu2E)2] (E = S, Se) as the first examples of molybdenum halide derived single source CVD precursors for the growth of MoE2 thin films was first probed by TGA, which showed multi-step decomposition processes, with the masses of the final residues consistent with MoSe2 and MoCl4 (from E = S; see discussion), respectively. Low pressure CVD experiments conducted at 750 C (E = S) and 525 C (E = Se) gave silvery and golden yellow films, respectively. Grazing incidence and in plane XRD data confirmed these to be 2H-MoE2, whilst the texture of the MoSe2 was investigated using pole figure measurements. SEM and EDX data, optical and Raman data on the films are also reported.

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MoCl4 ms Dalton final 10_12_2017 - revised - Accepted Manuscript
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Accepted/In Press date: 15 December 2017
e-pub ahead of print date: 29 January 2018
Published date: 2018

Identifiers

Local EPrints ID: 417216
URI: https://eprints.soton.ac.uk/id/eprint/417216
ISSN: 0300-9246
PURE UUID: 161c8643-4511-4caa-a45a-6892f532596e
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: 25 Jan 2018 17:30
Last modified: 15 Oct 2019 04:32

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