Spectroscopic Studies of Nanoparticulate Thin Films of a Cobalt-Based Oxygen Evolution Catalyst

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Department of Chemistry and Chemical Biology, Harvard University, 12 Oxford Street, Cambridge, Massachusetts 02138, United States
*E-mail: [email protected]. Tel: 1-617-495-8904.
Cite this: J. Phys. Chem. C 2014, 118, 30, 17060–17066
Publication Date (Web):March 28, 2014
https://doi.org/10.1021/jp5008347
Copyright © 2014 American Chemical Society
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Abstract

Nanoparticle (NP) cobalt–phosphate (Co-Pi) water oxidation catalysts are prepared as thin films by anodic electrodeposition from solutions of Co2+ dissolved in proton-accepting electrolytes. Compositional and structural insight into the nature of the catalyst film is provided from advanced spectroscopy. Infrared spectra demonstrate that counteranions incorporate into the Co-Pi thin films and that the phosphate ion, among various anion electrolytes, exhibits the highest binding affinity to the cobalt centers. Atomic force microscopy images show a highly porous morphology of the thin film that is composed of Co-Pi NPs. Whereas conventional X-ray powder diffraction technique shows catalyst films to be amorphous, synchrotron-based X-ray grazing incidence diffraction reveals well-defined diffraction patterns that are indicative of long-range ordering within the film. Azimuthal scans imply that as-prepared films possess a highly preferred orientation and texture on the electrode surface.

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Co 2p3/2 XPS spectra of different Co-X films, various Co-X thin-film formation conditions, FTIR spectra of recovery experiment, and SEM and AFM images of Co-Pi on Au and Pt electrodes. This material is available free of charge via the Internet at http://pubs.acs.org.

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