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Figure 4
Operando XRD data (λ = 0.207 Å) measured during prolonged anodic etching (45 min at 1.25 VRHE) followed by reducing potentials (15 min at 0.85 VRHE). (a) Contour map of the time evolution of XRD data during the experiment. (b) PCC matrix between the time-resolved XRD data, indicating structurally distinct regions. The color scale goes from blue, which represents the most dissimilar areas with a PCC of 0.89, to yellow, corresponding to a PCC of 1. (c) Pulsed potential profile. (d) Weight fractions obtained from a three-phase sequential Rietveld refinement against Ag f.c.c. in black [ICSD 64706 (Swanson & Tatge, 1953BB75)], Ag2CO3/HT in green [ICSD 281043 (Norby et al., 2002BB57)] and Ag2CO3/RT in pink [ICSD 8011 (Masse et al., 1979BB48)]. The lavender and pale-orange background colors represent the regions biased at potentials of 1.25 and 0.85 VRHE, respectively. The error bars on the weight fractions are smaller than the width of the markers and therefore have not been included in this plot. (e) NMF mapping with four components performed on the same data. (f) Calculated diffraction patterns of the Ag f.c.c. phase, the two Ag2CO3 phases and the four NMF components determined from NMF mapping.

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