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Quantification of passivation layer growth in inert anodes for molten salt electrochemistry by in situ energy-dispersive diffraction

DOI: 10.1107/S0021889811044104 DOI Help

Authors: Matthew Rowles (CSIRO Process Science and Engineering; CSIRO Future Manufacturing Flagship; University of Melbourne) , Mark Styles (University of Melbourne) , Ian Madsen (CSIRO Process Science and Engineering; CSIRO Future Manufacturing Flagship) , Nicola Scarlett (CSIRO Process Science and Engineering; CSIRO Future Manufacturing Flagship) , Katherine Mcgregor (CSIRO Process Science and Engineering; CSIRO Future Manufacturing Flagship) , Daniel Riley (University of Melbourne) , Graeme Snook (CSIRO Process Science and Engineering; CSIRO Future Manufacturing Flagship) , Andrew Urban (CSIRO Process Science and Engineering; CSIRO Future Manufacturing Flagship) , Thomas Connolley (Diamond Light Source) , Christina Reinhard (Diamond Light Source)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Journal Of Applied Crystallography , VOL 45 (1) , PAGES 28-37

State: Published (Approved)
Published: January 2012
Diamond Proposal Number(s): 3171

Abstract: An in situ energy-dispersive X-ray diffraction experiment was undertaken on operational titanium electrowinning cells to observe the formation of rutile (TiO2) passivation layers on Magnéli-phase (TinO2n-1; n = 4-6) anodes and thus determine the relationship between passivation layer formation and electrolysis time. Quantitative phase analysis of the energy-dispersive data was undertaken using a crystal-structure-based Rietveld refinement. Layer formation was successfully observed and it was found that the rate of increase in layer thickness decreased with time, rather than remaining constant as observed in previous studies. The limiting step in rutile formation is thought to be the rate of solid-state diffusion of oxygen within the anode structure.

Journal Keywords: Rietveld Refinement; In Situ Energy-Dispersive Diffraction; Electrolysis

Subject Areas: Technique Development, Chemistry


Instruments: I12-JEEP: Joint Engineering, Environmental and Processing