Ni–Co bimetallic phosphide catalyst toward electrocatalytic ammonia synthesis under ambient conditions

Electrocatalytic nitrate reduction reaction (NitRR) under ambient conditions is a promising sustainable and eco-friendly method for ammonia (NH₃) synthesis, which currently highly relies on the energy-consuming Haber-Bosch process with enormous CO₂ emissions. In this work, we report the synthesis of a Ni-Co bimetallic phosphide catalyst (NiCoP) using the traditional hydrothermal combined high-temperature phosphorization method. Compared with monometallic phosphides such as Ni₂P and CoP, the as-synthesized NiCoP catalyst with synergistic effects exhibits remarkable NitRR performance with the highest faradaic efficiency (FE) of 91.3 ± 4.4% at -1.2 V (<i>vs.</i> RHE) with the maximum NH₃ yield rate of 5553.4 ± 400.8 μg h^-1 cm^-2 at -1.4 V (<i>vs.</i> RHE). Further <i>in situ</i> different electrochemical mass spectrometry (DEMS) analysis is employed to identify the intermediate produced during the electrocatalytic NitRR process, confirming NiCoP as a promising electrocatalyst for NH₃ synthesis.