The effects of fabrication process, namely, calcination temperature, electrode support, and quenching, on electrochemical nitrate reduction were investigated, exemplified by Pd0.09Sn0.91 electrode. The electrode was characterized by X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, energy-dispersive X-ray spectroscopy, and cyclic voltammetry. Results showed that electrode surface morphology, crystalline formation, and chemical composition, which were influenced by the electrode fabrication process, controlled nitrogen selectivity and nitrate reduction reactivity. The Pd0.09Sn0.91/SS electrodes were calcined at different temperatures (from 100 to 700 °C) for 3 h in air and the results showed that high calcination temperature rendered electrode oxidized, and decreased nitrogen selectivity and nitrate reduction capability. Electrode supports affected nitrate reduction following the order of Ni ≈SS > G > Ti. Quenching electrode in ice water decreased nitrate reduction capability. Porous surface with small oxygen content, less degree of metal oxidation (i.e., higher fraction of Pd0 and Sn0), and Sn crystals favored nitrogen selectivity and nitrate removal.
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