Operando Raman spectroscopy uncovers hydroxide and CO species enhance ethanol selectivity during pulsed CO<sub>2</sub> electroreduction.

Herzog, Antonia; Lopez Luna, Mauricio; Jeon, Hyo Sang; Rettenmaier, Clara; Grosse, Philipp; Bergmann, Arno; Roldan Cuenya, Beatriz · Nat Commun · 2024

basic_science · Level V

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Abstract

Pulsed CO<sub>2</sub> electroreduction (CO<sub>2</sub>RR) has recently emerged as a facile way to in situ tune the product selectivity, in particular toward ethanol, without re-designing the catalytic system. However, in-depth mechanistic understanding requires comprehensive operando time-resolved studies to identify the kinetics and dynamics of the electrocatalytic interface. Here, we track the adsorbates and the catalyst state of pre-reduced Cu<sub>2</sub>O nanocubes ( ~ 30 nm) during pulsed CO<sub>2</sub>RR using sub-second time-resolved operando Raman spectroscopy. By screening a variety of product-steering pulse length conditions, we unravel the critical role of co-adsorbed OH and CO on the Cu surface next to the oxidative formation of Cu-O<sub>ad</sub> or CuO<sub>x</sub>/(OH)<sub>y</sub> species, impacting the kinetics of CO adsorption and boosting the ethanol selectivity. However, a too low OH<sub>ad</sub> coverage following the formation of bulk-like Cu<sub>2</sub>O induces a significant increase in the C<sub>1</sub> selectivity, while a too high OH<sub>ad</sub> coverage poisons the surface for C-C coupling. Thus, we unveil the importance of co-adsorbed OH on the alcohol formation under CO<sub>2</sub>RR conditions and thereby, pave the way for improved catalyst design and operating conditions.