Publication date: 15th December 2025
This contribution will showcase how lab-based in situ and operando methods can be extended from photoelectrodes to polymer membranes to unravel coupled processes in solar-driven photoelectrochemical (PEC) energy conversion.
On the photoelectrode side, I will present a time-resolved operando Raman spectroscopy (RS) strategy tailored to realistic PEC operation, including broadband-like excitation and complex chemistries such as biomass reforming. In tandem and multi-junction architectures, different absorbers harvest distinct portions of the solar spectrum, so relying on a single monochromatic bias wavelength can be misleading. To address the strong spectral overlap between broadband illumination and Raman probe light, we employ a pulsed-bias approach: the sample is periodically exposed to a controlled light pulse, while Raman spectra are recorded in the subsequent “dark” window. By synchronously triggering the bias light, Raman laser, and detector, we track transient spectral changes relative to a well-defined reference state, resolving reaction intermediates, local pH shifts, and photocorrosion processes over timescales from ∼10 ms to hours [1].
Complementarily, I will discuss a four-terminal electrochemical impedance spectroscopy (EIS) platform for ion-exchange membranes in (photo)electrolyzer-relevant environments. The membrane is mounted between independently addressable flow chambers, and a Kelvin-type configuration enables accurate DC resistance, broadband (1 MHz–1 mHz) impedance spectra, and voltage-loss analysis under galvanostatic operation, free from lead and contact artefacts [2, 3].
Together, these PEC and membrane case studies demonstrate how transient operando spectroscopy and precision impedance diagnostics can be combined to probe dynamic structure–function relationships across interfaces in integrated energy-conversion devices.
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