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Haloplumbate salts as reagents for the non-aqueous electrodeposition of lead

Haloplumbate salts as reagents for the non-aqueous electrodeposition of lead
Haloplumbate salts as reagents for the non-aqueous electrodeposition of lead
Cyclic voltammetry experiments on the Pb(II) salts, [PPh4][PbX3] (X = Cl, Br, I) in CH2Cl2 solution ([PPh4]X supporting electrolyte) at a Pt disk electrode show reproducible nucleation and stripping features consistent with reduction to elemental Pb. The reduction potential shifts to less cathodic from Cl (?0.40 V) ? Br (?0.27 V) ? I (?0.19 V vs. Ag/AgCl), in line with the Pb–X bond strengths decreasing. Potentiostatic electrodeposition using [PPh4][PbCl3] in CH2Cl2 leads to growth of a thin film of crystalline Pb onto planar TiN electrodes, confirmed by SEM, EDX and XRD analysis. Electrodeposition under similar conditions onto a planar Au electrode leads to deposition of elemental Pb, accompanied by some alloying at the substrate/film interface, with XRD analysis confirming the formation of AuPb2 and AuPb3. Transferring the [PPh4][PbCl3] reagent into supercritical CH2F2 (17.5 MPa and 360 K) containing [PPh4]Cl led to very limited solubility of the Pb reagent; using [NnBu4]Cl as a supporting electrolyte caused an increase in solubility, although still lower than in liquid CH2Cl2. Cyclic voltammetry experiments (Pt disk) using this electrolyte also show voltammetry consistent with Pb deposition, however the low solubility of the lead salt in scCH2F2 meant that electrodeposition onto a planar TiN substrate was not possible.
2046-2069
73323-73330
Bartlett, Philip
d99446db-a59d-4f89-96eb-f64b5d8bb075
Burt, Jennifer
4f8a0b68-2fb3-4136-98ff-70dfe1acba98
Hasan, Mahboba
fdb892ba-7f72-4e59-98c1-f070733840c9
Hector, Andrew
f19a8f31-b37f-4474-b32a-b7cf05b9f0e5
Levason, William
e7f6d7c7-643c-49f5-8b57-0ebbe1bb52cd
Reid, Gill
37d35b11-40ce-48c5-a68e-f6ce04cd4037
Richardson, Peter
babd5d43-0ea3-4a27-b92f-820683acd781
Bartlett, Philip
d99446db-a59d-4f89-96eb-f64b5d8bb075
Burt, Jennifer
4f8a0b68-2fb3-4136-98ff-70dfe1acba98
Hasan, Mahboba
fdb892ba-7f72-4e59-98c1-f070733840c9
Hector, Andrew
f19a8f31-b37f-4474-b32a-b7cf05b9f0e5
Levason, William
e7f6d7c7-643c-49f5-8b57-0ebbe1bb52cd
Reid, Gill
37d35b11-40ce-48c5-a68e-f6ce04cd4037
Richardson, Peter
babd5d43-0ea3-4a27-b92f-820683acd781

Bartlett, Philip, Burt, Jennifer, Hasan, Mahboba, Hector, Andrew, Levason, William, Reid, Gill and Richardson, Peter (2016) Haloplumbate salts as reagents for the non-aqueous electrodeposition of lead. RSC Advances, 6 (77), 73323-73330. (doi:10.1039/C6RA12942K).

Record type: Article

Abstract

Cyclic voltammetry experiments on the Pb(II) salts, [PPh4][PbX3] (X = Cl, Br, I) in CH2Cl2 solution ([PPh4]X supporting electrolyte) at a Pt disk electrode show reproducible nucleation and stripping features consistent with reduction to elemental Pb. The reduction potential shifts to less cathodic from Cl (?0.40 V) ? Br (?0.27 V) ? I (?0.19 V vs. Ag/AgCl), in line with the Pb–X bond strengths decreasing. Potentiostatic electrodeposition using [PPh4][PbCl3] in CH2Cl2 leads to growth of a thin film of crystalline Pb onto planar TiN electrodes, confirmed by SEM, EDX and XRD analysis. Electrodeposition under similar conditions onto a planar Au electrode leads to deposition of elemental Pb, accompanied by some alloying at the substrate/film interface, with XRD analysis confirming the formation of AuPb2 and AuPb3. Transferring the [PPh4][PbCl3] reagent into supercritical CH2F2 (17.5 MPa and 360 K) containing [PPh4]Cl led to very limited solubility of the Pb reagent; using [NnBu4]Cl as a supporting electrolyte caused an increase in solubility, although still lower than in liquid CH2Cl2. Cyclic voltammetry experiments (Pt disk) using this electrolyte also show voltammetry consistent with Pb deposition, however the low solubility of the lead salt in scCH2F2 meant that electrodeposition onto a planar TiN substrate was not possible.

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Accepted/In Press date: 15 July 2016
e-pub ahead of print date: 25 July 2016
Organisations: Electrochemistry, Organic Chemistry: SCF

Identifiers

Local EPrints ID: 401724
URI: http://eprints.soton.ac.uk/id/eprint/401724
ISSN: 2046-2069
PURE UUID: cf4e99fb-79ac-487f-b841-d2f23ec0a2ee
ORCID for Philip 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 Gill Reid: ORCID iD orcid.org/0000-0001-5349-3468

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Date deposited: 20 Oct 2016 13:03
Last modified: 17 Dec 2019 06:35

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Contributors

Author: Philip Bartlett ORCID iD
Author: Jennifer Burt
Author: Mahboba Hasan
Author: Andrew Hector ORCID iD
Author: William Levason ORCID iD
Author: Gill Reid ORCID iD
Author: Peter Richardson

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