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Chloroantimonate electrochemistry in dichloromethane

Chloroantimonate electrochemistry in dichloromethane
Chloroantimonate electrochemistry in dichloromethane
Antimony is a technologically relevant element, which is present in many semiconductor materials. Electrodeposition of such materials offers a potential route for cheaper and less wasteful manufacturing, and is especially suited for micro- and nano-feature sizes with complex geometries. Previous work has shown the applicability of electrodeposition of p-block metals and metalloids from the weakly coordinating solvent dichloromethane, using halometallate precursors. Here we more thoroughly investigate the behaviour of the tetrabutylammonium chloroantimonate precursor, [TBA][SbCl4]. We use voltammetry at a stationary macroelectrode, rotating disc electrode and electrochemical quartz crystal microbalance, as well as microelectrodes and highlight the advantages of microelectrodes in this context. Using [TBA]Cl as a background electrolyte it is found that the diffusion coefficients calculated from the rotating disc electrode and microelectrodes are similar. Due to the possibility of mixed speciation with an excess of Cl−, tetrabutylammonium tetrafluoroborate, [TBA][TFB], is also used as a background electrolyte and it is found that the diffusion coefficient does not change. Using a modified form of the Stokes-Einstein equation, that takes into account the shape of the solute and the relative sizes of the solute and solvent, the diffusion coefficients of the antimony precursor and decamethylferrocene are consistent with their relative sizes. Electrodeposition onto large surface area platinum and titanium nitride substrates using either background electrolyte results in amorphous deposits of elemental antimony with similar morphology.
0013-4686
Reeves, Simon
121fe250-d3b8-4fd7-830b-deaa06385b9c
Noori, Yasir
704d0b70-1ea6-4e00-92ce-cc2543087a09
Zhang, Wenjian
1f80ac5e-d4c2-4720-b19e-be700cd411e7
Reid, Gillian
37d35b11-40ce-48c5-a68e-f6ce04cd4037
Bartlett, Philip N.
d99446db-a59d-4f89-96eb-f64b5d8bb075
Reeves, Simon
121fe250-d3b8-4fd7-830b-deaa06385b9c
Noori, Yasir
704d0b70-1ea6-4e00-92ce-cc2543087a09
Zhang, Wenjian
1f80ac5e-d4c2-4720-b19e-be700cd411e7
Reid, Gillian
37d35b11-40ce-48c5-a68e-f6ce04cd4037
Bartlett, Philip N.
d99446db-a59d-4f89-96eb-f64b5d8bb075

Reeves, Simon, Noori, Yasir, Zhang, Wenjian, Reid, Gillian and Bartlett, Philip N. (2020) Chloroantimonate electrochemistry in dichloromethane. Electrochimica Acta, 354, [136692]. (doi:10.1016/j.electacta.2020.136692).

Record type: Article

Abstract

Antimony is a technologically relevant element, which is present in many semiconductor materials. Electrodeposition of such materials offers a potential route for cheaper and less wasteful manufacturing, and is especially suited for micro- and nano-feature sizes with complex geometries. Previous work has shown the applicability of electrodeposition of p-block metals and metalloids from the weakly coordinating solvent dichloromethane, using halometallate precursors. Here we more thoroughly investigate the behaviour of the tetrabutylammonium chloroantimonate precursor, [TBA][SbCl4]. We use voltammetry at a stationary macroelectrode, rotating disc electrode and electrochemical quartz crystal microbalance, as well as microelectrodes and highlight the advantages of microelectrodes in this context. Using [TBA]Cl as a background electrolyte it is found that the diffusion coefficients calculated from the rotating disc electrode and microelectrodes are similar. Due to the possibility of mixed speciation with an excess of Cl−, tetrabutylammonium tetrafluoroborate, [TBA][TFB], is also used as a background electrolyte and it is found that the diffusion coefficient does not change. Using a modified form of the Stokes-Einstein equation, that takes into account the shape of the solute and the relative sizes of the solute and solvent, the diffusion coefficients of the antimony precursor and decamethylferrocene are consistent with their relative sizes. Electrodeposition onto large surface area platinum and titanium nitride substrates using either background electrolyte results in amorphous deposits of elemental antimony with similar morphology.

Text
Chloroantimonate Electrochemistry in Dichloromethane - Accepted Manuscript
Restricted to Repository staff only until 13 July 2021.
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More information

Accepted/In Press date: 26 June 2020
e-pub ahead of print date: 13 July 2020
Published date: 10 September 2020

Identifiers

Local EPrints ID: 442777
URI: http://eprints.soton.ac.uk/id/eprint/442777
ISSN: 0013-4686
PURE UUID: 10e9d127-d9ee-44dd-8465-f9aa5d0ee4ff
ORCID for Simon Reeves: ORCID iD orcid.org/0000-0001-5475-2484
ORCID for Yasir Noori: ORCID iD orcid.org/0000-0001-5285-8779
ORCID for Gillian Reid: ORCID iD orcid.org/0000-0001-5349-3468
ORCID for Philip N. Bartlett: ORCID iD orcid.org/0000-0002-7300-6900

Catalogue record

Date deposited: 27 Jul 2020 16:30
Last modified: 18 Feb 2021 17:37

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