Benchmarking Heterogeneous Electrocatalysts for the Oxygen Evolution Reaction

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§Joint Center for Artificial Photosynthesis and Division of Chemistry and Chemical Engineering, California Institute of Technology, Pasadena, California 91125, United States
Department of Chemical Engineering, Stanford University, Stanford, California 94305, United States
Cite this: J. Am. Chem. Soc. 2013, 135, 45, 16977–16987
Publication Date (Web):October 30, 2013
Copyright © 2013 American Chemical Society
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Objective evaluation of the activity of electrocatalysts for water oxidation is of fundamental importance for the development of promising energy conversion technologies including integrated solar water-splitting devices, water electrolyzers, and Li-air batteries. However, current methods employed to evaluate oxygen-evolving catalysts are not standardized, making it difficult to compare the activity and stability of these materials. We report a protocol for evaluating the activity, stability, and Faradaic efficiency of electrodeposited oxygen-evolving electrocatalysts. In particular, we focus on methods for determining electrochemically active surface area and measuring electrocatalytic activity and stability under conditions relevant to an integrated solar water-splitting device. Our primary figure of merit is the overpotential required to achieve a current density of 10 mA cm–2 per geometric area, approximately the current density expected for a 10% efficient solar-to-fuels conversion device. Utilizing the aforementioned surface area measurements, one can determine electrocatalyst turnover frequencies. The reported protocol was used to examine the oxygen-evolution activity of the following systems in acidic and alkaline solutions: CoOx, CoPi, CoFeOx, NiOx, NiCeOx, NiCoOx, NiCuOx, NiFeOx, and NiLaOx. The oxygen-evolving activity of an electrodeposited IrOx catalyst was also investigated for comparison. Two general observations are made from comparing the catalytic performance of the OER catalysts investigated: (1) in alkaline solution, every non-noble metal system achieved 10 mA cm–2 current densities at similar operating overpotentials between 0.35 and 0.43 V, and (2) every system but IrOx was unstable under oxidative conditions in acidic solutions.

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X-ray photoelectron spectra; discussion of choice of specific capacitance values; rotating disk voltammograms, chronopotentiometric steps and chronoamperometric steps for electrodeposited catalyts; OER activity and stability measurements for NiCeOx on Ni electrodes; confirmation of 2 e reduction of O2 on Pt ring electrodes at 0.7 V vs SCE and 1600 rpm rotation rate in 1 M NaOH; rotating disk voltammograms, chronopotentiometric steps and chronoamperometric steps for sputtered Ni and commercial Ni disks; discussion regarding the use of Tafel plots for comparing electrocatalysts and benchmarking intermediate pH solutions. This material is available free of charge via the Internet at

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