Publication date: 15th December 2025
The electrochemical CO2 reduction reaction (CO2RR) is one of the chemists’ tools for contributing to environmental remediation through low-impact methods. Its complexity relies on the stability of the CO2 molecule and the multiple potential products derived from this reaction [1]. There is a necessity to develop new CO2RR electrocatalysts due to the lack of selectivity of the current solutions. Recently, the potential of Cu-nitrogen-doped carbon composites has been demonstrated to be effective for the selective conversion of CO2 [2]. Similarly, our research group has been able to demonstrate that the addition of a second heteroatom (P), contributes to improving the efficiency of these nanocomposites for obtaining C2+ compounds, especially ethylene [3]. However, little changes in the synthetic procedure showed us unexpected behaviours, allowing us to modulate the electrocatalyst activity from a hydrogen evolution predominance to the obtention of more than 50% C2+ products passing through catalysts capable of transforming CO2 into methane with an efficiency of around 30%.
This contribution approaches the preparation of N, P-doped carbon-Cu nanocomposites by solvothermal characterization and its optimization for the obtainment of ethylene. During this process, it was possible to observe that slight variations in synthesis parameters led to remarkable differences in electrocatalytic activity. In order to find a justification for this change in behaviour, a complete physicochemical characterization was carried out to gain a deeper understanding of the environment and transformations of catalytic centers before, during, and after the electrochemical reaction. STEM studies revealed a change in the dispersion of metal when the heteroatom presence or the pyrolytic treatment is modified. In situ XAS experiments demonstrated a change in the oxidation state under catalytic conditions, a modification that only occurs for the catalysts with the presence of P in their structure. Thus, it is fair to affirm that this synthetic procedure allows us to control the selectivity of CO2RR through the fitting of these little changes.
Authors acknowledge the COREC2MAS project funded by CSIC COCRE24026 and PID2024-158477OB-I00 funded by MICIU/ AEI / 10.13039/501100011033/ FEDER, UE. The authors would like to thank Diamond Light Source for providing beamtime (NT28356). Authors express their gratitude to the node CNME of ICTS “ELECMI” for the use of instrumentation as well as the technical advice provided during the electronic microscopy studies.
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