In situ/operando X-ray spectroscopy applied to electrocatalytic CO2 reduction: Status and perspectives

In Situ/Operando Characterization Techniques of Electrochemical CO2 Reduction

“…In situ/operando techniques can shed light on different issues during the CO 2 electrochemical reduction (12)(13)(14), such as (a) surface morphology, reconstruction, state, and stability; (b) determination of active sites; (c) the electrode-electrolyte interface; and (d) identification of reaction intermediates and products. As summarized in Figure 1, widely used in situ/operando techniques include surface-enhanced Raman spectroscopy (SERS) (15,16), surface-enhanced infrared absorption spectroscopy (SEIRAS) (17,18), mass spectrometry (MS) (19), X-ray absorption spectroscopy (XAS) (20,21), X-ray diffraction (XRD) (22), transmission electron microscopy (TEM) (23), and atomic force microscopy (AFM) (24).…”

Multiscale effects in tandem CO2 electrolysis to C2+ products

“…68,69 Additionally, due to the reversible nature of common dynamic alterations, operando spectroscopic techniques should be used when possible to elucidate the active structure. 70,71 Fig. 3 This article is licensed under a Creative Commons Attribution 3.0 Unported Licence.…”

Controlled Potential Electrolysis: Transition from Fast to Slow Regimes in Homogeneous Molecular Catalysis. Application to the Electroreduction of CO2 Catalyzed by Iron Porphyrin

“…The goal might be to identify the product formed during electrolysis or/and to follow the time evolution of the various catalyst forms with the aim to detect intermediates or transformation or degradation of the catalyst. SEC has thus been used as a tool to investigate molecular catalytic processes for a long time [10] and many developments have been made [11] including recent ones regarding the use of XAS spectroscopy [12] . Even considering only CPE, the outcome of a SEC experience is sensitive to the experimental conditions for molecular catalysis in solution due to inherent inhomogeneous concentrations in an electrolysis cell.…”

“…SEC has thus been used as a tool to investigate molecular catalytic processes for a long time [10] and many developments have been made [11] including recent ones regarding the use of XAS spectroscopy. [12] Even considering only CPE, the outcome of a SEC experience is sensitive to the experimental conditions for molecular catalysis in solution due to inherent inhomogeneous concentrations in an electrolysis cell. Despite several formal descriptions of SEC experiments for molecular catalytic systems considering various configurations (light beam normal or parallel to the electrode surface; thinlayer or larger cells) being available, [13] reports on experimental SEC do not always pay attention to it in the data analysis and interpretation.…”