Publication date: 21st July 2025
Electrochemical conversion of small molecules into value-added products is one of the most promising approaches to decarbonize the chemical industry. Improving the efficiency and stability of many of these reactions relies on a molecular-level understanding of the reaction mechanisms. Operando characterizations play a critical role in this regard. Nuclear magnetic resonance (NMR) is an element-specific, quantitative, and non-destructive spectroscopic technique, making it ideal for operando and in situ characterizations.
In this talk, I will showcase how we develop and apply operando NMR to understand chemical and physical processes in the electrolyte and at the electrode in a working electrochemical reactor.[1,2] In the first half of my talk, I will focus on CO₂ reduction, highlighting the coupling of a benchtop NMR system with a gas diffusion electrolyzer, real-time quantification of electrolyte carbonation, water crossover, and their link to device failure.[3] In the second half, focusing on lithium-mediated ammonia synthesis, I will present the development of new in situ NMR techniques for the direct observation of key reaction steps, including the plating of metallic lithium and its concurrent corrosion, nitrogen splitting on lithium metal, and protonolysis of lithium nitride. Informed by these observations, we have developed a new reaction cycle.[4]
By the end of this talk, I hope to demonstrate the versatility and rich informational content that operando NMR can offer in the field of electrochemical conversion, and how it can be used to track reaction stability and guide the design of new reactions.
References
1. Luo R et al. “A parallel line probe for spatially selective electrochemical NMR spectroscopy” J. Magn. Reson. 2024, 361, 107666 (Front cover; Special Issue: New Voices in Magnetic Resonance; Invited).
2. Zhu Z et al. “Operando NMR methods for studying electrocatalysis” Magnetic Resonance Letters, 2024, 4, 100096 (invited).
3. Zhu Z et al. “Operando NMR quantifies liquid product, water crossover and carbonates for electrochemical CO2 reduction” ACS Catalysis, 2025, in press.
4. Luo R et al. “Direct in situ NMR observation of lithium plating, corrosion, nitridation and protonolysis for ammonia synthesis” ChemRxiv, DOI 10.26434/chemrxiv-2024-cpf4.
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