Haloplumbate salts as reagents for the non-aqueous electrodeposition of lead
| Autor: | William Levason, Gillian Reid, Peter W. Richardson, Andrew L. Hector, Jennifer S. Burt, Mahboba M. Hasan, Philip N. Bartlett |
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| Jazyk: | angličtina |
| Rok vydání: | 2016 |
| Předmět: |
Aqueous solution
Chemistry Supporting electrolyte General Chemical Engineering Inorganic chemistry Analytical chemistry chemistry.chemical_element 02 engineering and technology General Chemistry Electrolyte 010402 general chemistry 021001 nanoscience & nanotechnology 01 natural sciences 0104 chemical sciences Reagent Solubility Cyclic voltammetry 0210 nano-technology Tin Voltammetry |
| Popis: | 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. |
| Databáze: | OpenAIRE |
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