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.
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
2018
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), , [7].
(doi:10.1039/C7DT04352J).
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.
Text
MoCl4 ms Dalton final 10_12_2017 - revised
- Accepted Manuscript
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c7dt04352j
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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: http://eprints.soton.ac.uk/id/eprint/417216
ISSN: 0300-9246
PURE UUID: 161c8643-4511-4caa-a45a-6892f532596e
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Date deposited: 25 Jan 2018 17:30
Last modified: 16 Mar 2024 06:08
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Author:
Yao-Pang Chang
Author:
Joshua Whittam
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