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A versatile precursor system for supercritical fluid electrodeposition of main-group materials

A versatile precursor system for supercritical fluid electrodeposition of main-group materials
A versatile precursor system for supercritical fluid electrodeposition of main-group materials
For the first time, a versatile electrolyte bath is described that can be used to electrodeposit a wide range of p-block elements from supercritical difluoromethane (scCH2F2). The bath comprises the tetrabutylammonium chlorometallate complex of the element in an electrolyte of 50×10?3?mol?dm?3 tetrabutylammonium chloride at 17.2?MPa and 358?K. Through the use of anionic ([GaCl4]?, [InCl4]?, [GeCl3]?, [SnCl3]?, [SbCl4]?, and [BiCl4]?) and dianionic ([SeCl6]2? and [TeCl6]2?) chlorometallate salts, the deposition of elemental Ga, In, Ge, Sn, Sb, Bi, Se, and Te is demonstrated. In all cases, with the exception of gallium, which is a liquid under the deposition conditions, the resulting deposits are characterised by SEM, energy-dispersive X-ray analysis, XRD and Raman spectroscopy. An advantage of this electrolyte system is that the reagents are all crystalline solids, reasonably easy to handle and not highly water or oxygen sensitive. The results presented herein significantly broaden the range of materials accessible by electrodeposition from supercritical fluid and open up the future possibility of utilising the full scope of these unique fluids to electrodeposit functional binary or ternary alloys and compounds of these elements.
electrochemistry, main-group elements, metal–metal interactions, supercritical fluids, surface chemistry
0947-6539
302-309
Bartlett, Philip N.
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Burt, Jennifer
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Cook, David A.
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Cummings, Charles Y.
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George, Michael W.
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Hector, Andrew
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Hasan, Mahboba
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Ke, Jie
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Levason, William
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Pugh, David
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Reid, Gillian
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Richardson, Peter W.
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Smith, David C.
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Spencer, Joe
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Suleiman, Norhidayah
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Zhang, Wenjian
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Bartlett, Philip N.
d99446db-a59d-4f89-96eb-f64b5d8bb075
Burt, Jennifer
4f8a0b68-2fb3-4136-98ff-70dfe1acba98
Cook, David A.
0fca0ffb-eef4-422f-b513-ce9a1f7de7cc
Cummings, Charles Y.
37ed515b-eb09-4c6b-9c66-61013c8c132a
George, Michael W.
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Hector, Andrew
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Hasan, Mahboba
fdb892ba-7f72-4e59-98c1-f070733840c9
Ke, Jie
e4b531d4-7642-4367-9a4e-d06f126c2599
Levason, William
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Pugh, David
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Reid, Gillian
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Richardson, Peter W.
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Smith, David C.
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Spencer, Joe
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Suleiman, Norhidayah
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Zhang, Wenjian
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Bartlett, Philip N., Burt, Jennifer, Cook, David A., Cummings, Charles Y., George, Michael W., Hector, Andrew, Hasan, Mahboba, Ke, Jie, Levason, William, Pugh, David, Reid, Gillian, Richardson, Peter W., Smith, David C., Spencer, Joe, Suleiman, Norhidayah and Zhang, Wenjian (2016) A versatile precursor system for supercritical fluid electrodeposition of main-group materials. Chemistry - A European Journal, 22 (1), 302-309. (doi:10.1002/chem.201503301).

Record type: Article

Abstract

For the first time, a versatile electrolyte bath is described that can be used to electrodeposit a wide range of p-block elements from supercritical difluoromethane (scCH2F2). The bath comprises the tetrabutylammonium chlorometallate complex of the element in an electrolyte of 50×10?3?mol?dm?3 tetrabutylammonium chloride at 17.2?MPa and 358?K. Through the use of anionic ([GaCl4]?, [InCl4]?, [GeCl3]?, [SnCl3]?, [SbCl4]?, and [BiCl4]?) and dianionic ([SeCl6]2? and [TeCl6]2?) chlorometallate salts, the deposition of elemental Ga, In, Ge, Sn, Sb, Bi, Se, and Te is demonstrated. In all cases, with the exception of gallium, which is a liquid under the deposition conditions, the resulting deposits are characterised by SEM, energy-dispersive X-ray analysis, XRD and Raman spectroscopy. An advantage of this electrolyte system is that the reagents are all crystalline solids, reasonably easy to handle and not highly water or oxygen sensitive. The results presented herein significantly broaden the range of materials accessible by electrodeposition from supercritical fluid and open up the future possibility of utilising the full scope of these unique fluids to electrodeposit functional binary or ternary alloys and compounds of these elements.

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CEJ p-block scfed1 revised.pdf - Accepted Manuscript
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Accepted/In Press date: 26 November 2015
e-pub ahead of print date: 26 November 2015
Published date: 4 January 2016
Keywords: electrochemistry, main-group elements, metal–metal interactions, supercritical fluids, surface chemistry
Organisations: Chemistry

Identifiers

Local EPrints ID: 385449
URI: https://eprints.soton.ac.uk/id/eprint/385449
ISSN: 0947-6539
PURE UUID: 0d601f5f-11cd-4189-a47e-ed3832432150
ORCID for Philip N. Bartlett: ORCID iD orcid.org/0000-0002-7300-6900
ORCID for Andrew 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 Jan 2016 09:08
Last modified: 17 Jul 2019 20:08

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Contributors

Author: Jennifer Burt
Author: David A. Cook
Author: Charles Y. Cummings
Author: Michael W. George
Author: Andrew Hector ORCID iD
Author: Mahboba Hasan
Author: Jie Ke
Author: William Levason ORCID iD
Author: David Pugh
Author: Gillian Reid ORCID iD
Author: Peter W. Richardson
Author: David C. Smith
Author: Joe Spencer
Author: Norhidayah Suleiman
Author: Wenjian Zhang

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