In this talk, I will present the recent work in my group on developing various electrochemical Raman spectroscopy for in-situ and operando studies of electrochemical systems at the limits of time and spatial resolution and sensitivity<br/>With the help of the plasmonic enhancement at the tip of a plasmonic material, electrochemical tip-enhanced Raman spectroscopy (EC-TERS) offers itself as the only nanospectroscopy for investigating the electrochemical interface with unprecedent spatial resolution and explicit chemical fingerprint information. We developed the electrochemical TERS both based on STM and AFM using the water immersion objective and homemade optical instrument. EC-TERS was applied to obtain the molecular fingerprint information of surface adsorption and electrochemical reaction on single crystal surfaces and monitor the plasmon-driven reaction at the nanoscale.<br/>Aiming at addressing the challenge of monitoring the highly dynamic changing electrochemical interfaces under potential control and presence of the electrolyte, a transient electrochemical surface-enhanced Raman spectroscopy (TEC-SERS) was developed to monitor the structural evolution of surface species at a time resolution that equals the transient electrochemical methods (e.g. cyclic voltammetry and chronoamperometry), allowing the precise correlation of Raman signal with the molecular signature information and the electrochemical current signal. A wide-field Raman imaging system was developed to offer a high imaging speed to monitor the spatial and temporal change at every point over the whole electrode surface simultaneously. The heterogeneity of electrocatalytic reaction on the electrode surface was observed. This technique offers the possibility to spatially correlate electrochemical behavior and the particular surface sites where the reaction happens.<br/>A high-sensitive setup based on water immersion objectives for electrochemical dark field scattering technique was developed to observe the deposition of submonolayer atoms on single nanocrystal (NC) surfaces for the first time. The “cyclic voltammogram (CV)” of every individual NCs was reconstructed using the peak position or peak intensity of the potential-dependent scattering spectra. These optical “CV”s provide more accurate potential and narrow band width of the UPD peak of each NC and on different facets of single NC, which cannot be obtained by conventional electrochemical technique.

Electrochemical raman spectroscopy for in-situ and operando studies at limits of time and spatial resolution and sensitivity

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