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

J. Appl. Cryst. (2012). 45, 28–37 (

[EDXRD] Accumulated EDXRD patterns of the inert anode as a function of electrolysis time. The main Magnéli (M) phases can be seen transforming into rutile (R).

Molten-salt electrochemistry takes place in a hot, aggressive environment. An inert anode operating within such an environment – calcium chloride at 950°C – has been studied using the high penetrating power of energy-dispersive X-ray diffraction (EDXRD). Methodology for performing quantitative crystal-structure-based Rietveld analysis of EDXRD has been developed and applied to this experiment, and has shown the mechanism of change in the phase chemistry of the anode in real time, and under realistic operating conditions. The analysis methodology is generally applicable to any EDXRD data.

M. R. Rowles, M. J. Styles, I. C. Madsen, N. V. Y. Scarlett, K. McGregor, D. P. Riley, G. A. Snook, A. J. Urban, T. Connolley and C. Reinhard