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nBu2Sn(SnBu)2 and nBu3SnEnBu (E = S or Se) - effective single source precursors for the CVD of SnS and SnSe thermoelectric thin films

nBu2Sn(SnBu)2 and nBu3SnEnBu (E = S or Se) - effective single source precursors for the CVD of SnS and SnSe thermoelectric thin films
nBu2Sn(SnBu)2 and nBu3SnEnBu (E = S or Se) - effective single source precursors for the CVD of SnS and SnSe thermoelectric thin films
The use of single source precursors offers a convenient option for the chemical vapour deposition of thin film semiconductor materials with good stoichiometric control and precursor efficiency. Here we show that reaction of nBu3SnCl with NaSnBu or LiSenBu, or nBu2SnCl2 with 2 mol equiv. of NaSnBu, gives the molecular alkyltin chalcogenolate precursors, nBu3SnEnBu (E = S (1), Se (3)) and nBu2Sn(SnBu)2 (2), respectively, in good yield as colourless (S) or yellow/orange (Se) oils. These were characterised by 1H, 13C{1H}, 77Se{1H} and 119Sn{1H} NMR spectroscopy, microanalysis and thermogravimetric analysis. Low pressure CVD experiments using these precursors showed that (1) gave S-deficient SnS thin films, whereas using (2) and implementing short deposition times and low precursor loadings, gave stoichiometric SnS films. Stoichiometric SnSe films were also obtained using (3) and confirmed by grazing incidence XRD analysis, which revealed the films adopt the orthorhombic Pnma structure. SEM and EDX analysis, together with Raman spectroscopic data, were also used to identify the films deposited and to correlate with the deposition conditions employed. Variable temperature Seebeck and Hall effect characterisation confirm that the stoichiometric SnS and SnSe films are semiconducting and highly resistive, giving large positive Seebeck coefficients, with the overall power factor ranging from 0.017 at 300 K to 0.049 μW cm−1 K−2 at 450 K for SnS and increasing from 0.06 at 300 K to 0.4 μW cm−1 K−2 at 425 K for SnSe.
2633-5409
Robinson, Fred
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Curran, Peter J.
cd6b4464-ed48-47a4-a68a-cb8244378680
De Groot, Kees
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Hardie, Duncan
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Hector, Andrew L.
f19a8f31-b37f-4474-b32a-b7cf05b9f0e5
Holloway, Katherine
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Huang, Ruomeng
c6187811-ef2f-4437-8333-595c0d6ac978
Newbrook, Daniel, William
380b603a-3de2-40d3-b008-2fa079341513
Reid, Gillian
37d35b11-40ce-48c5-a68e-f6ce04cd4037
Robinson, Fred
8fc7b408-097f-4550-b189-5b6e3a49bf93
Curran, Peter J.
cd6b4464-ed48-47a4-a68a-cb8244378680
De Groot, Kees
92cd2e02-fcc4-43da-8816-c86f966be90c
Hardie, Duncan
aad06fc3-41b6-4d76-a63e-f619dc856ff5
Hector, Andrew L.
f19a8f31-b37f-4474-b32a-b7cf05b9f0e5
Holloway, Katherine
64a3b0c0-8710-403b-a57e-eba76ae53be4
Huang, Ruomeng
c6187811-ef2f-4437-8333-595c0d6ac978
Newbrook, Daniel, William
380b603a-3de2-40d3-b008-2fa079341513
Reid, Gillian
37d35b11-40ce-48c5-a68e-f6ce04cd4037

Robinson, Fred, Curran, Peter J., De Groot, Kees, Hardie, Duncan, Hector, Andrew L., Holloway, Katherine, Huang, Ruomeng, Newbrook, Daniel, William and Reid, Gillian (2021) nBu2Sn(SnBu)2 and nBu3SnEnBu (E = S or Se) - effective single source precursors for the CVD of SnS and SnSe thermoelectric thin films. Materials Advances. (doi:10.1039/D1MA00331C).

Record type: Article

Abstract

The use of single source precursors offers a convenient option for the chemical vapour deposition of thin film semiconductor materials with good stoichiometric control and precursor efficiency. Here we show that reaction of nBu3SnCl with NaSnBu or LiSenBu, or nBu2SnCl2 with 2 mol equiv. of NaSnBu, gives the molecular alkyltin chalcogenolate precursors, nBu3SnEnBu (E = S (1), Se (3)) and nBu2Sn(SnBu)2 (2), respectively, in good yield as colourless (S) or yellow/orange (Se) oils. These were characterised by 1H, 13C{1H}, 77Se{1H} and 119Sn{1H} NMR spectroscopy, microanalysis and thermogravimetric analysis. Low pressure CVD experiments using these precursors showed that (1) gave S-deficient SnS thin films, whereas using (2) and implementing short deposition times and low precursor loadings, gave stoichiometric SnS films. Stoichiometric SnSe films were also obtained using (3) and confirmed by grazing incidence XRD analysis, which revealed the films adopt the orthorhombic Pnma structure. SEM and EDX analysis, together with Raman spectroscopic data, were also used to identify the films deposited and to correlate with the deposition conditions employed. Variable temperature Seebeck and Hall effect characterisation confirm that the stoichiometric SnS and SnSe films are semiconducting and highly resistive, giving large positive Seebeck coefficients, with the overall power factor ranging from 0.017 at 300 K to 0.049 μW cm−1 K−2 at 450 K for SnS and increasing from 0.06 at 300 K to 0.4 μW cm−1 K−2 at 425 K for SnSe.

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Accepted/In Press date: 16 June 2021
e-pub ahead of print date: 17 June 2021

Identifiers

Local EPrints ID: 450138
URI: http://eprints.soton.ac.uk/id/eprint/450138
ISSN: 2633-5409
PURE UUID: 7b0ec0e6-7401-4a99-b81e-2083c2b14b87
ORCID for Kees De Groot: ORCID iD orcid.org/0000-0002-3850-7101
ORCID for Andrew L. Hector: ORCID iD orcid.org/0000-0002-9964-2163
ORCID for Daniel, William Newbrook: ORCID iD orcid.org/0000-0002-5047-6168
ORCID for Gillian Reid: ORCID iD orcid.org/0000-0001-5349-3468

Catalogue record

Date deposited: 13 Jul 2021 16:31
Last modified: 14 Jul 2021 01:54

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Contributors

Author: Fred Robinson
Author: Peter J. Curran
Author: Kees De Groot ORCID iD
Author: Duncan Hardie
Author: Katherine Holloway
Author: Ruomeng Huang
Author: Daniel, William Newbrook ORCID iD
Author: Gillian Reid ORCID iD

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