Recent advances in the operando structural and interface characterisation of electrocatalysts

Using multiple operando characterisation techniques to elucidate the structure-reactivity correlations of electrocatalytic systems is becoming more desirable. In this review article, we primarily employed the electrocatalytic CO₂ reduction reaction over nanocatalysts as a model reaction to discuss the recent advances in the use of operando characterisation techniques. The synergy between various techniques can circumvent, to a great extent, the limitations of using one sole technique. For instance, the advances in using a combination of operando powder X-ray diffraction and Raman spectroscopy are discussed, which enables the complementary characterisation of nanocatalysts in both bulk and surface levels. Under operando conditions, the adsorbate and intermediate species, as well as the structural parameters of the catalyst can be simultaneously tracked for an extensive understanding of the reaction mechanisms.