Construction and performance of the millisecond-to-second QXAFS platform at SSRF BL11B for in situ dynamic characterization

Chen, Y.; Li, Y.; Gao, Q.; Gan, T.; Zhang, S.; Li, J.

doi:10.1107/S1600577526009781

Figure 10
In situ QXAFS characterization of β-CoMoO₄ under OER conditions. (a) Photograph of the operando electrochemical QXAFS setup at the BL11B beamline. (b) First-cycle CV curve of β-CoMoO₄ in 1 M KOH (pH = 13.5) with a potential window of 0.8–1.8 V versus RHE at a scan rate of 2.5 mV s⁻¹. (c) Operando time-resolved Co K-edge QXAFS spectra collected during the CV scanning. The upper and lower insets provide a magnified view of the k²-weighted EXAFS and the absorption-edge (XANES) regions, respectively. (d) 3D surface plot of the Fourier-transformed EXAFS spectra in R-space, illustrating the dynamic evolution of Co coordination structures as a function of the applied potential. (e) Selected XANES spectra extracted every 100 s (5 s per spectrum, 1000 spectra in total) under the pH = 12 condition. The spectra show no systematic edge shift or line-shape change within the observed variation, indicating no significant structural reconstruction within 5000 s.

JOURNAL OF
SYNCHROTRON
RADIATION

ISSN: 1600-5775

Volume 33| Part 6| November 2026|

https://doi.org/10.1107/S1600577526009781

Open

access