Proceedings of MATSUS Spring 2025 Conference (MATSUSSpring25)
Publication date: 16th December 2024
The photoelectrochemical N2 reduction reaction (PEC-N2RR) is a pathway for solar light-assisted ammonia (NH3) synthesis under ambient conditions. However, in addition to activating the highly stable N2 molecule, aqueous PEC-N2RR faces other major challenges. The low solubility of N2 in water and the competing H2 evolution reaction (HER) result in generally low NH3 yields. These low yields elevate the risk of contamination-induced spurious results. In addition to ambient NH3 and NOx species, cell compartment separator membranes used to prevent ammonium (NH4+) crossover during PEC-N2RR can interfere with NH3 quantification. In this work, we report a simple yet effective cleaning process for a microporous separator membrane. We found that the as-cleaned microporous membrane surpasses commonly used proton and anion exchange membranes in terms of chemical inertness, electrochemical ion transport, and structural stability in an alkaline aqueous environment. These findings supplement efforts to establish a contamination-free workstation for PEC-N2RR catalyst evaluation. After thoroughly assessing background contaminations (NH3, N2H4, and NOx) in a homebuilt workstation and ensuring high purity, we examined the activity of three promising Cu-based semiconductors – CuO, Cu2O, and CuBi2O4 – for PEC-N2RR. The Cu-oxide electrodes were synthesized using electrodeposition methods, and alkaline aqueous electrolyte was used to investigate their PEC-N2RR performance. Despite all three materials exhibiting photoactivity, no NH3 production was observed. All materials rapidly lost photoactivity due to photocorrosion, with CuBi2O4 showing improved stability but overall reduced photocurrent density. These results indicate that in spite of favorable p-type semiconducting properties, moderate bandgaps, and suitable band edge positions Cu-based oxides are ineffective for N2 to NH3 conversion under aqueous photoelectrochemical conditions.
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