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In situ XRD investigation of the evolution of surface layers on Pb-alloy anodes

Published online by Cambridge University Press:  22 August 2017

Marie Clancy ,
Mark J. Styles ,
Colleen J. Bettles ,
Nick Birbilis ,
Justin A. Kimpton  and
Nathan A. S. Webster
Marie Clancy
Affiliation:
Department of Materials Science and Engineering, Monash University, Clayton, VIC 3800, Australia
Mark J. Styles
Affiliation:
CSIRO Manufacturing, Private Bag 10, Clayton, VIC 3169, Australia
Colleen J. Bettles
Affiliation:
Department of Materials Science and Engineering, Monash University, Clayton, VIC 3800, Australia
Nick Birbilis
Affiliation:
Department of Materials Science and Engineering, Monash University, Clayton, VIC 3800, Australia
Justin A. Kimpton
Affiliation:
Australian Synchrotron, 800 Blackburn Rd, Clayton, VIC 3168, Australia
Nathan A. S. Webster*
Affiliation:
CSIRO Mineral Resources, Private Bag 10, Clayton South, VIC 3169, Australia
*
a)Author to whom correspondence should be addressed. Electronic mail: nathan.webster@csiro.au
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Abstract

The electrochemical behaviour of a number of Pb-based anode alloys, under simulated electrowinning conditions, in a 1.6 M H2SO4 electrolyte at 45 °C was studied. Namely, the evolution of PbO2 and PbSO4 surface layers was investigated by quantitative in situ synchrotron X-ray diffraction (S-XRD) and subsequent Rietveld-based quantitative phase analysis (QPA). In the context of seeking new anode alloys, this research shows that the industry standard Pb-0.08Ca-1.52Sn (wt%) anode, when exposed to a galvanostatic current and intermittent power interruptions, exhibited poor electrochemical performance relative to select custom Pb-based binary alloys; Pb–0.73Mg, Pb–5.05Ag, Pb–0.07Rh, and Pb–1.4Zn (wt%). The in situ S-XRD measurements and subsequent QPA indicated that this was linked to a lower proportion of β-PbO2, relative to PbSO4, on the Pb-0.08Ca-1.52Sn alloy at all stages of the electrochemical cycling. The best performing alloy, in terms of minimisation of overpotential during normal electrowinning operation and minimising the deleterious effects of repeated power interruptions – both of which are significant factors in energy consumption – was determined to be Pb–0.07Rh.

Keywords

copper electrowinningpower interruptionPbO2 and PbSO4 surface layersin situ synchrotron X-ray diffractionquantitative phase analysis
Type
Technical Articles
Information
Powder Diffraction , Volume 32 , Supplement S2 , December 2017 , pp. S54 - S60
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Copyright
Copyright © International Centre for Diffraction Data 2017 

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