CoP as an Acid-Stable Active Electrocatalyst for the Hydrogen-Evolution Reaction: Electrochemical Synthesis, Interfacial Characterization and Performance Evaluation

Saadi, Fadl H.; Carim, Azhar I.; Verlage, Erik; Hemminger, John C.; Lewis, Nathan S.; Soriaga, Manuel P.

doi:10.1021/jp5054452

Title: CoP as an Acid-Stable Active Electrocatalyst for the Hydrogen-Evolution Reaction: Electrochemical Synthesis, Interfacial Characterization and Performance Evaluation

Journal Article · Sat Sep 27 00:00:00 EDT 2014 · Journal of Physical Chemistry. C

DOI:https://doi.org/10.1021/jp5054452· OSTI ID:1635017

Saadi, Fadl H. ^[1]; Carim, Azhar I. ^[1]; Verlage, Erik ^[1]; Hemminger, John C. ^[2]; Lewis, Nathan S. ^[1]; Soriaga, Manuel P. ^[3]

California Institute of Technology (CalTech), Pasadena, CA (United States)
California Institute of Technology (CalTech), Pasadena, CA (United States); Univ. of California, Irvine, CA (United States)
California Institute of Technology (CalTech), Pasadena, CA (United States); Texas A & M Univ., College Station, TX (United States)

Films of CoP have been electrochemically synthesized, characterized, and evaluated for performance as a catalyst for the hydrogen-evolution reaction (HER). The film was synthesized by cathodic deposition from a boric acid solution of Co²⁺ and H₂PO₂^– on copper substrates followed by operando remediation of exogenous contaminants. The films were characterized structurally and compositionally by scanning-electron microscopy, energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, and Raman spectrophotometry. The catalytic activity was evaluated by cyclic voltammetry and chronopotentiometry. Surface characterization prior to electrocatalysis indicated that the film consisted of micrometer-sized spherical clusters located randomly and loosely on a slightly roughened surface. The composition of both the clusters and surface consisted of cobalt in the metallic, phosphide, and amorphous-oxide forms (CoO·Co₂O₃) and of phosphorus as phosphide and orthophosphate. The orthophosphate species, produced by air-oxidation, were eliminated upon HER electrocatalysis in sulfuric acid. The operando film purification yielded a functional electrocatalyst with a Co:P stoichiometric ratio of 1:1. After the HER, the surface was densely packed with micrometer-sized, mesa-like particles whose tops were flat and smooth. The CoP eletrodeposit exhibited an 85 mV overvoltage (η) for the HER at a current density of 10 mA cm^–2 and was stable under operation in highly acidic solution, with an increase in η of 18 mV after 24 h of continuous operation. In conclusion, the comparative HER catalytic performance of CoP, film or nanoparticles, is as follows: ηPt < ηCoP film = ηCoP NP, ηNi₂P < ηCoSe₂ < ηMoS₂ < ηMoSe₂.

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Research Organization:: California Institute of Technology (CalTech), Pasadena, CA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: SC0004993

OSTI ID:: 1635017

Journal Information:: Journal of Physical Chemistry. C, Vol. 118, Issue 50; ISSN 1932-7447

Publisher:: American Chemical SocietyCopyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 196 works

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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
thin films
inorganic compounds
electrical properties
evolution reactions
cobalt