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

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 e...

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Bibliographic Details
Main Authors: Rowles, Matthew, Styles, M., Madsen, I., Scarlett, N., McGregor, K., Riley, D., Snook, G., Urban, A., Connolley, T., Reinhard, C.
Format: Journal Article
Published: IUCr Journals 2012
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Online Access:http://hdl.handle.net/20.500.11937/25298
Description
Summary: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.