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Figure 5.6: a) Thermodynamic free energy diagram for electrochemical N2 reduction to NH3 at the equilibrium potential. On the ideal catalyst, the pathway is completely planar. On Au(211), the most uphill step is *N2H formation, while on Re(111), the most uphill step is *NH2 formation. b) Linear scaling relationship for closely packed transition metal surfaces between the free energies for *NH2 formation and *N2H formation. Also indicated via contours is the theoretical limiting potential, the maximum of which is shown to lie far from the transition-metal surfaces. Reproduced with permission from [17]. protocols for ammonia testing based on 15N2 isotope labelling [8]. On the basis of the established protocols, previous positive reports of N2 electroreduction need to be reappraised. Mechanistic insight into the most promising materials Those materials identified as promising from the benchmarking activity described should be sub- jected to detailed investigation, with experiment and theory in synergy. There should be a particular focus on: • The structure, dimensionality, and composition of the electrode, electrolytes, reaction interme- diates, interfaces, and interphases, bridging information between multiple length scales and domains, especially under reaction conditions. From an experimental perspective, this in- cludes x-ray absorption spectroscopy (XAS) and x-ray emission spectroscopy (XES) both in the hard x-ray regime to probe metal sites and soft x-rays for detection of N species. The recent development of high-pressure x-ray photoelectron spectroscopy (HPXPS) (currently up to 2 bar, but potentially 10-30 bar in the future) has enabled probing of the thermal process with high surface sensitivity, and involving electrochemical cells allows detection of electrode oxidation state and species at the solid-liquid interface. Surface-Enhanced Infrared Absorption Spectroscopy (SEIRAS), Surface Enhanced Raman Spectroscopy (SERS) and Sum Frequency Generation (SFG) allow detection of molecular species through N-N and N-H stretches. The utilization of optical and x-ray lasers for ultrafast measurements can provide avenues to probe transient intermediates and transition states. Many of the techniques are 56PDF Image | sustainable production of fuels and chemicals
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