In situ Raman investigation to electrochemical synthesis of ammonia on Pd nanocrystals

Abstract Nitrate and nitrite are widely present in industrial wastewater and domestic sewage, so electrocatalytic reduction of both nitrate and nitrite to ammonia synthesis is considered to be a sustainable development approach. Pd nanostructures have attracted much attention because of their high activity in catalyzing the nitrate electrochemical reduction reaction. Here we prepare Pd nanocube and octahedron for the electrochemical reduction of nitrate and nitrite. It is found that Pd octahedron shows slightly higher activity toward nitrate reduction than Pd nanocube, while for nitrite reduction, Pd octahedron shows much higher activity than Pd nanocube. The ammonia yield rate is more potential–dependent. In situ Raman characterization further confirms the existence of adsorbed ammonia on the surface of nanocube and octahedron, indicating similar reduction pathways on (111)–facet octahedron and (100)–facet nanocube.