Operando spectroscopy study of the carbon dioxide electro-reduction by iron species on nitrogen-doped carbon

Chiara Genovese, Manfred E. Schuster, Emma K. Gibson, Diego Gianolio, Victor Posligua, Ricardo Grau-Crespo, Giannantonio Cibin, Peter P. Wells, Debi Garai, Vladyslav Solokha, Sandra Krick Calderon, Juan J. Velasco-Velez, Claudio Ampelli, Siglinda Perathoner, Georg Held, Gabriele Centi and Rosa Arrigo ()
Additional contact information
Chiara Genovese: University of Messina
Manfred E. Schuster: Johnson Matthey Technology Centre
Emma K. Gibson: UK Catalysis Hub, Research Complex at Harwell (RCaH)
Diego Gianolio: Diamond Light Source Ltd., Harwell Science and Innovation Campus
Victor Posligua: University of Reading
Ricardo Grau-Crespo: University of Reading
Giannantonio Cibin: Diamond Light Source Ltd., Harwell Science and Innovation Campus
Peter P. Wells: Diamond Light Source Ltd., Harwell Science and Innovation Campus
Debi Garai: Diamond Light Source Ltd., Harwell Science and Innovation Campus
Vladyslav Solokha: Diamond Light Source Ltd., Harwell Science and Innovation Campus
Sandra Krick Calderon: FAU Erlangen-Nürnberg
Juan J. Velasco-Velez: Max-Planck Institut für Chemische Energiekonversion
Claudio Ampelli: University of Messina
Siglinda Perathoner: University of Messina
Georg Held: Diamond Light Source Ltd., Harwell Science and Innovation Campus
Gabriele Centi: Computer, Physical and Earth Sciences - University of Messina, ERIC aisbl and CASPE/INSTM, V.le F. Stagno d’Alcontres 31
Rosa Arrigo: Diamond Light Source Ltd., Harwell Science and Innovation Campus

Nature Communications, 2018, vol. 9, issue 1, 1-12

Abstract: Abstract The carbon–carbon coupling via electrochemical reduction of carbon dioxide represents the biggest challenge for using this route as platform for chemicals synthesis. Here we show that nanostructured iron (III) oxyhydroxide on nitrogen-doped carbon enables high Faraday efficiency (97.4%) and selectivity to acetic acid (61%) at very-low potential (−0.5 V vs silver/silver chloride). Using a combination of electron microscopy, operando X-ray spectroscopy techniques and density functional theory simulations, we correlate the activity to acetic acid at this potential to the formation of nitrogen-coordinated iron (II) sites as single atoms or polyatomic species at the interface between iron oxyhydroxide and the nitrogen-doped carbon. The evolution of hydrogen is correlated to the formation of metallic iron and observed as dominant reaction path over iron oxyhydroxide on oxygen-doped carbon in the overall range of negative potential investigated, whereas over iron oxyhydroxide on nitrogen-doped carbon it becomes important only at more negative potentials.

Date: 2018
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DOI: 10.1038/s41467-018-03138-7

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