Publication date: 15th December 2025
The IPCC (Intergovernmental Panel for Climate Change) defines climate change mitigation as “human intervention to [...] enhance the sinks of greenhouse gases”. Amongst these greenhouse gases, CO2 represents 75% of global emissions. Faced with this, the electrochemical CO2 reduction reaction (CO2RR) presents a promising opportunity for the removal of anthropogenic CO2 from the atmosphere whilst simultaneously yielding valuable chemicals. However, the CO2RR is limited by high cathodic overpotentials, unfavourably scarce metallic catalysts of Ag and Au, and low selectivity towards C2+ products on pristine Cu-based materials, the only metal capable of facilitating the C-C coupling. Metal Nitrogen-doped Carbon catalysts (MNCs) comprise an isolated metal atom coordinated in a conductive nitrogen-doped carbon matrix. These sustainable and bio-inspired materials present enhanced selectivity and activity towards CO2RR as a result of their heterogeneity and dipole-catalyst interactions. Nonetheless, previously reported single-atom catalysts (SACs) of this nature have typically been synthesised using a single step pyrolysis resulting in materials riddled with elemental metal aggregates and sites hindered by limited exposure. Via the implementation of a decoupled synthesis protocol allowing for the polymerisation of a Carbon-Nitrogen substrate and the subsequent coordination of a metallic centre, electrocatalytic materials with highly available active sites, can be characterised. This versatile approach enables the unequivocal synthesis of MNCs with myriad metallic centres. The research conducted as part of this project harnesses the advantages of dual-step SAC synthesis to gauge the true and unpolluted activity, selectivity and stability of metal-nitrogen doped carbon catalysts coordinated with a variety of metal centres by way of optimising CO2 reduction to CO at commercially relevant current densities. These materials are investigated via electrochemical measurements in a catholyte-bearing gas diffusion electrode cell, implementing gas chromatography by way of product quantification. These complementary techniques provide insight into the stability, activity and resistivity of the investigated set-ups and the yielded results will allow for the foundations of a fully optimised CO2 electrolyser.
I would like to thank my supervisors, Professor Maria-Magdalena Titirici and Dr Jesús Barrio-Hermida for their unwavering support and guidance.I am also very grateful to the members of the electrocatalysis team, in both the Titirici and Stephens group, who always make the time to help me. Furthermore, thanks go out to Saurav Chandra and Crina Corbos at Johnson Matthey. Their advice has allowed me to troubleshoot many issues, and I am grateful for their expertise and the time they take to share it with me
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