Characterisation and testing of novel electrodes and electrolytes for efficient N2 reduction

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The current method for ammonia production, the Haber-Bosch process, consumes >1% of fossil fuels and emits vast quantities of greenhouse gas. Electrochemical ammonia synthesis, powered by renewable energy, could provide a green solution. However, there exist many significant contamination sources, complicating quantitative proof of synthesis. Additionally, any catalyst active for nitrogen reduction will preferentially evolve hydrogen [1].This project will build on the recent first quantitative proof of ammonia synthesis using a lithium mediated route and an organic electrolyte [2]. The aim is to understand the role of the electrode and electrolyte using cutting-edge characterisation techniques translated from battery science. A magnetron sputter deposition chamber directly attached to a glove box will be used to grow highly reactive thin film electrodes. These can be quickly transferred to an electrochemical cell, minimising deleterious oxidisation. The glove box will contain a hypersensitive mass spectrometer to measure gas evolution in-situ, never used before for non-aqueous electrochemistry, and an infrared spectrometer to probe intermediates. These operando techniques will be complemented by various ex-situ characterisation methods, including secondary ion mass spectrometry, nuclear magnetic resonance spectroscopy, Raman spectroscopy and electrochemical atomic force microscopy. The emergent molecular-scale picture will elucidate pathways towards efficient electrochemical ammonia synthesis.[1] Nilsson, A. & Stephens, I. E. L. "Sustainable N2 reduction" in Research needs towards sustainable production of fuels and chemicals (eds J.K. Norskov, A. Latimer, & C. F. Dickens) 49 (Energy-X, Brussels, Belgium, 2019)[2] Andersen, S. Z., Colic, V., Yang, S., Schwalbe, J. A., Nielander, A. C., McEnaney, J. M., Enemark-Rasmussen, K., Baker, J. G., Singh, A. R., Rohr, B. A., Statt, M. J., Blair, S. J., Mezzavilla, S., Kibsgaard, J., Vesborg, P. C. K., Cargnello, M., Bent, S. F., Jaramillo, T. F., Stephens, I. E. L., Norskov, J. K. & Chorkendorff, I. Nature 570, 504, (2019)