The AUREX cell: a versatile operando electrochemical cell for studying catalytic materials using X-ray diffraction, total scattering and X-ray absorption spectroscopy under working conditions

Frank, S.; Ceccato, M.; Jeppesen, H.S.; Marks, M.J.; Nielsen, M.L.N.; Lu, R.; Gammelgaard, J.J.; Quinson, J.; Sharma, R.; Jensen, J.S.; Hjelme, S.; Friberg Klysner, C.; Billinge, S.J.L.; Just, J.; Gjørup, F.H.; Catalano, J.; Lock, N.

doi:10.1107/S1600576724007817

Figure 5
Multimodal XAS–XRD experiment performed under the operando conditions of prolonged anodic etching (45 min at 1.25 V_RHE) and a subsequent cathodic pulse (15 min at 0.85 V_RHE). Ten sample positions were probed repeatably. (a) Contour map over the time evolution of the normalized XANES data. (b) PCC matrix between the time-resolved XAS data, indicating structurally distinct regions. The color scale goes from blue, which represents the most dissimilar areas with a PCC of 0.999, to yellow, corresponding to a PCC of 1. (c) Time evolution of the XRD data recorded simultaneously with the XAS. (d) Pulsed potential profile. (e) Two internal reference spectra recorded during the operando experiment, used in the LCA. Comp 0 (black) is the starting structure, while Comp 1 (orange) is the most oxidized spectrum. (f) Evolution of the LCA components. The vertical black line (at 1 min) represents the position of Comp 0 in the data series, while the vertical orange line (at 37 min) shows the position of Comp 1. The shaded lavender region indicates the region where the anodic potential of 1.25 V_RHE is applied, and the pale-orange region indicates the change to the cathodic potential of 0.85 V_RHE.

JOURNAL OF
APPLIED
CRYSTALLOGRAPHY

ISSN: 1600-5767

Volume 57| Part 5| October 2024| Pages 1489-1502

https://doi.org/10.1107/S1600576724007817

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