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Spectroscopic Characterization of Mixed Fe–Ni Oxide Electrocatalysts for the Oxygen Evolution Reaction in Alkaline Electrolytes

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U.S.-DOE National Energy Technology Laboratory, Pittsburgh, Pennsylvania 15236, United States
Department of Chemical Engineering, Carnegie Mellon University, Pittsburgh Pennsylvania 15213, United States
§ Operando Molecular Spectroscopy & Catalysis Lab, Department of Chemical Engineering, Lehigh University, Bethlehem, Pennsylvania 18015, United States
Yeshiva University, 245 Lexington Avenue, New York, New York 10016, United States
Cite this: ACS Catal. 2012, 2, 8, 1793–1801
Publication Date (Web):July 24, 2012
https://doi.org/10.1021/cs3002644
Copyright © 2012 American Chemical Society
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Abstract

Mixed Fe–Ni oxide electrocatalysts for the oxygen evolution reaction in alkaline electrolytes were synthesized using three different approaches: evaporation induced self-assembly, hard templating, and dip-coating. For each synthesis method, a peak in oxygen evolution activity was observed near 10 mol % Fe content, where the mixed metal oxide was substantially more active than the parent metal oxide electrocatalysts. X-ray diffraction (XRD) analysis showed the formation of a mixed NiO/NiFe2O4 phase at low Fe concentrations, and formation of Fe2O3 at compositions above 25 mol % Fe. Raman vibrational spectroscopy confirmed the formation of NiFe2O4, and did not detect Fe2O3 in the electrocatalysts containing up to 20 mol % Fe. X-ray absorption near edge structure (XANES) showed the Fe in the mixed oxides to be predominantly in the +3 oxidation state. Extended X-ray absorption fine structure (EXAFS) showed changes in the Fe coordination shells under electrochemical oxygen evolution conditions. Temperature programmed reaction spectroscopy showed the mixed oxide surfaces also have superior oxidation activity for methanol oxidation, and that the reactivity of the mixed oxide surface is substantially different than that of the parent metal oxide surfaces. Overall, the NiFe2O4 phase is implicated in having a significant role in improving the oxygen evolution activity of the mixed metal oxide systems.

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