Publication date: 28th August 2024
Resolving the distribution of ionic species at the electrode-electrolyte interface is of key importance for all electrochemical processes. Specifically, the configuration of cations [1], anions [2], and solvent molecules [3] in the double-layer region governs the binding of surface adsorbates and the accompanying electron transfers at the electrochemical interface. Characterization techniques with such interfacial sensitivity are however limited. While vibrational spectroscopy methods can provide useful insights into this regime under electrochemical conditions, their lack of element specificity (relies on chemical bond vibrations) calls for complementary techniques. In the presented work, we introduce a combination of in situ X-ray spectroscopy techniques applied to the investigation of the electrical double layer (EDL) formed at the metal electrode-aqueous electrolyte interface. We will discuss how the combination of X-ray spectroscopic technique with the dip-and-pull geometry (Fig. 1) can satisfy both conditions necessary to monitor the EDL in situ: (1) an ultrathin electrolyte film and (2) an electrochemically connected system. We will demonstrate how X-ray photoelectron spectroscopy (XPS) with the dip-and-pull and geometry can yield information about the potential dependent distribution of K+ cations across the EDL. We present a study of how such potential dependence near a Au surface might be affected by non-adsorbing compared to specifically adsorbing ions. Furthermore, we report how total electron yield X-ray absorption spectroscopy (TEY-XAS) combined with the dip-and-pull geometry can simultaneously indicate changes in the coordination of K+ cations at a metal-aqueous electrolyte interface (Fig. 1). Through these case studies, we will highlight the challenges and prospects of the dip-and-pull geometry combined with X-ray spectroscopy for the study of electrocatalytic interfaces. The chemical universality of this approach makes it compatible with various electrolyte compositions and thus, with a broad range of heterogeneous electrocatalytic reactions. In light of the development of the dip-an-pull approach, we will discuss the outlook of applying it to more complex electrocatalytic systems like the alkaline hydrogen evolution reaction (HER) or the CO2 reduction reaction (CO2RR).
The presented work received funding from the 2022 HORIZON-MSCA-PF program under grant agreement No 101109314.
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