Publication date: 15th December 2025
In the last decades Cu has attracted considerable attention over other pure metals catalysts for its exceptional performance of the electrocatalytic reduction of CO2 (CO2RR) into valuable hydrocarbons and alcohols [1]. However, the low selectivity and stability of this catalyst remain significant challenges. Consequently, understanding and controlling the dynamics of electronic properties at the solid-liquid interface during CO2RR using operando techniques is essential.
Soft X-ray Absorption Spectroscopy (XAS) offers unique access to the L-edges of transition metals and the K-edges of light elements. At BACH beamline (Elettra Sincrotrone) a microfluidic electrochemical cell for operando XAS has been developed [2], enabling a detailed characterization of oxidation states and electronic structure directly at the catalyst - electrolyte interface. The microfluidic electrochemical cell (ME-cell) features inlet and outlet channels, which allow for the renewal of the electrolyte, and a three-electrode system, comprising an Ag/AgCl leakless as reference electrode (RE), a Pt wire as counter electrode (CE) and a working electrode (WE) made of an Au-coated Si3N4 membrane onto which the catalytic material is deposited.
Our study revealed that while Nafion polymer binder enhances the catalyst stability, it also alters significantly the chemical state of the electrochemically deposited copper nanoparticles. Operando soft-XAS measurements revealed the formation Nafion-Cu interaction that induces a persistent copper (II) oxide state under catalytic conditions during CO2RR. These results were corroborated with ex-situ Cu K-edge measurements of the catalyst before and after the reaction. The effect of Cu catalyst selectivity as a function of the Nafion polymer incorporation method (spin-coating vs. drop-casting) was also investigated.
To the best of our knowledge, this is the first report highlighting the oxidative effect of Nafion on Cu-based catalytic materials. Complementary techniques, such as Raman and IR spectroscopy, will help in elucidating the chemical interaction between Cu and the Nafion polymer structure. In addition, investigating the influence of alternative ionomers (e.g., Fumion or Sustenion) on Cu catalysts during CO₂RR will provide further insights into ionomer–catalyst interactions.
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