The University of Southampton
University of Southampton Institutional Repository

The characterisation of PbO2–coated electrodes prepared from aqueous methanesulfonic acid under controlled deposition conditions

Sirés, I., Low, C.T.J, Ponce de Leon, C. and Walsh, F.C (2010) The characterisation of PbO2–coated electrodes prepared from aqueous methanesulfonic acid under controlled deposition conditions Electrochimica Acta, 55, (6), pp. 2163-2172. (doi:10.1016/j.electacta.2009.11.051).

Record type: Article


A series of PbO2 coatings on planar carbon substrates has been prepared by anodic deposition in aqueous methanesulfonic acid (MSA) under galvanostatic conditions. The effect of four experimental parameters, i.e., lead(II) methanesulfonate and MSA concentrations, current density, and temperature was analysed. Surface characterisation by XRD, SEM-EDX, and AFM has provided information about the structural (phase distribution, degree of crystallinity, and crystallite size), morphological (crystallite shape, degree of porosity), and tribological (surface roughness) properties of the PbO2 coatings, respectively. Electrochemical studies based on linear and cyclic voltammetry allowed comparison between electrodes prepared in MSA and classical electrodes prepared in HNO3. Pure ?- or ?-PbO2 and ? + ? mixtures were obtained depending on the conditions, being temperature the most influential deposition parameter. A temperature rise caused a transition to pure ?-PbO2 and led to a higher degree of crystallinity with a progressive increase of crystallite size, always within the range of 10–30 nm, as well as to a remarkably higher roughness, from smooth (35–50 nm rms) to rough (up to 500 nm rms) surfaces. Low MSA and high lead(II) methanesulfonate concentrations were required to avoid the formation of excessively porous powdery coatings, as well as cracks, pits, and holes. Most of the coatings obtained in MSA were uniform, nanocrystalline, and moderately rough. Their electrocatalytic behaviour was comparable to that of the electrodes prepared in HNO3, showing an O2-overpotential of +0.66 V in 0.05 M Na2SO4 at pH 3.0. Such coatings can then be envisaged as suitable anodes for energy and water treatment applications. Prolonged electrolysis has shown their stability against leaching.

PDF The_characterisation_of_PbO2.pdf - Version of Record
Restricted to Repository staff only
Download (3MB)

More information

e-pub ahead of print date: 22 November 2009
Published date: 15 February 2010
Keywords: electrochemical advanced oxidation processes, electrodeposition, lead dioxide, methanesulfonic acid, surface characterisation
Organisations: Engineering Mats & Surface Engineerg Gp


Local EPrints ID: 69890
ISSN: 0013-4686
PURE UUID: 068fec9f-2d38-46ad-827e-481e0ec1009a

Catalogue record

Date deposited: 09 Dec 2009
Last modified: 19 Jul 2017 00:05

Export record



Author: I. Sirés
Author: C.T.J Low
Author: F.C Walsh

University divisions

Download statistics

Downloads from ePrints over the past year. Other digital versions may also be available to download e.g. from the publisher's website.

View more statistics

Atom RSS 1.0 RSS 2.0

Contact ePrints Soton:

ePrints Soton supports OAI 2.0 with a base URL of

This repository has been built using EPrints software, developed at the University of Southampton, but available to everyone to use.

We use cookies to ensure that we give you the best experience on our website. If you continue without changing your settings, we will assume that you are happy to receive cookies on the University of Southampton website.