Publication date: 21st July 2025
Solute transport underpins the functionality of many modern electrochemical devices involved in energy generation and storage. In solar fuel generation, mass transport limits the efficiency of product generation, and CO2 reduction intermediaries can cause cell degradation and may further limit efficiency. Despite its immense importance, there are no demonstrations of direct solute imaging of solar fuel generation that could reveal such structure–property relationships and the role of intermediates, limiting rational design. We therefore developed and fabricated a three-electrode microfluidic electrochemical cell that is compatible with a high resolution microscope. By imaging the cell in operando using interference reflection microscopy (IRM), we measure the evolution of voltage-induced spatiotemporal concentration profiles through their changes to the local refractive index in order to extract transport coefficients.
I will discuss imaging of two partial reactions involved in CO2 reduction. First, to investigate replacing the slow, high-overpotential oxygen evolution reaction at the anode, we image the lower-overpotential oxalic acid oxidation. Second, to overcome the conversion efficiency limitations arising from the low solubility of CO2 in water, we image catalyst-assisted bicarbonate dehydration to increase the supply of CO2 to the cathode for enhanced product generation. Probing these reactions with spatiotemporal imaging has allowed us to measure transport and reaction dynamics, identify limitations on the rate of reaction, separate identify time scales on which different steps of the reactions occur, and measure reactant usage and product generation.
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