Publication date: 22nd July 2026
Transient electrochemical intermediates often exist on timescales far shorter than the temporal resolution accessible to conventional operando spectroscopic techniques. As a result, many key steps of electrocatalytic reaction mechanisms remain experimentally inaccessible. While substantial progress has been made in the development of in situ and operando methods over the past decade, the typical time resolution of structural spectro-electrochemical techniques remains limited to approximately 0.1 s.
In this talk, I will present a general approach for extending operando spectroscopy into the sub-millisecond regime through synchronized electrochemical reaction activation and spectroscopic probing. First, I will demonstrate how a conventional Raman spectroscopy setup can be adapted to perform time-resolved investigations of electrochemically driven processes. The method enables direct observation of bond formation and bond breaking events with a time resolution of 0.2 ms, representing an improvement of nearly two orders of magnitude over conventional operando Raman measurements.
I will then show how the same concept can be translated to X-ray absorption spectroscopy through the development of a transient spectro-electrochemical Hard XAS setup implemented at the Balder beamline at MAX IV. The technique provides access to transient changes in the electronic and structural state of electrocatalysts on sub-millisecond timescales and is demonstrated using the oxygen evolution catalyst NiOOH. Finally, I will present our preliminary efforts to extend this methodology to the soft X-ray regime through the development of the first operando Soft X-ray flow cell capable of sustaining current densities up to 100 mA cm-2, tested at the Elettra Synchrotron. This new platform opens the way to time-resolved operando Soft X-ray spectroscopy under technologically relevant reaction conditions.
Together, these developments represent the first step towards a systematic resolving of short-lived reaction intermediates of electrocatalytic processes.
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