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Surface-enhanced spectroscopy techniques are the method-of-choice tocharacterize adsorbed intermediates occurring during electrochemical reactions,which are crucial in realizing a green sustainable future. Characterizingspecies with low coverages or short lifetimes have so far been limited by lowsignal enhancement. Recently, metasurface-driven surface-enhanced infraredabsorption spectroscopy (SEIRAS) has been pioneered as a promising narrowbandtechnology to study single vibrational modes of electrochemical interfacesduring CO oxidation. However, many reactions involve several species orconfigurations of adsorption that need to be monitored simultaneously requiringreproducible and broadband sensing platforms to provide a clear understandingof the underlying electrochemical processes. Here, we experimentally realizemulti-band metasurface-driven SEIRAS for the in-situ study of electrochemicalCO2 reduction on a Pt surface. We develop an easily reproducible andspectrally-tunable platinum nano-slot metasurface. Two CO adsorptionconfigurations at 2030 cm-1 and 1840 cm-1 are locally enhanced as a proof ofconcept that can be extended to more vibrational bands. Our platform provides a41-fold enhancement in the detection of characteristic absorption signalscompared to conventional broadband electrochemically roughened platinum films.A straightforward methodology is outlined starting by baselining our system inCO saturated environment and clearly detecting both configurations ofadsorption, in particular the hitherto hardly detectable CO bridgeconfiguration. Then, thanks to the signal enhancement provided by our platform,we find that the CO bridge configuration on platinum does not play asignificant role during CO2 reduction in an alkaline environment. We anticipatethat our technology will guide researchers in developing similar sensingplatforms.

Multi-band metasurface-driven surface-enhanced infrared absorption spectroscopy for improved characterization of in-situ electrochemical reactions