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Figure 3
Electrochemical behavior over time of the thin-film Mo cathode in the electrochemical cell is presented in (a). The electrolyte consisted of N2-saturated THF with 0.5 M LiClO4. Current density is normalized by the geometric surface area of the working electrode (1.75 cm2). Potentials were measured versus a leakless PEEK Ag/AgCl reference electrode. The measured uncompensated resistance of the cell was 1233.5 Ω and was corrected using standard methods (see the SI). XRD measurements performed during the electrochemical measurements shown in (a) are presented in (b), with each diffractogram labeled with the quantity of charge passed at the time of measurement. These timepoints are indicated in corresponding colors in (a). Purified N2 was sparged into the electrolyte continuously while the electrolyte was pumped back and forth through the cell.

Journal logoJOURNAL OF
SYNCHROTRON
RADIATION
ISSN: 1600-5775
Volume 30| Part 5| September 2023| Pages 917-922
https://doi.org/10.1107/S1600577523006331
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