In this study, niobium nitride (NbN) is prepared via the urea-glass route by annealing a mixture of NbCl5 and urea at 650 °C under a flow of N2, and is used as a catalyst for the electrochemical nitrogen reduction reaction (NRR). The as-prepared NbN exhibits a maximum production rate of 5.46 × 10-10 mol s-1 cm-2 at -0.6 V vs. RHE, along with an apparent FE of 16.33% at -0.3 V vs. RHE. In addition, the leaching of NbN is confirmed by ICP-OES, where the leached amount of Nb is almost identical to the amount of N measured by UV-vis. Moreover, 1H NMR experiments are performed using 15N2 as the feeder gas; the dominant detection of 14NH4+ peaks strongly suggests that the produced NH3 originates from the leaching of NbN rather than via an electrocatalytic process. Hence, for a comprehensive understanding of NH3 generation, especially when utilizing transition metal nitride (TMN)-based NRR catalysts, a thorough investigation employing multiple analytical methods is imperative.
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