Operando Synthesis of Macroporous Molybdenum Diselenide Films for Electrocatalysis of the Hydrogen-Evolution Reaction

Saadi, Fadl H.; Carim, Azhar I.; Velazquez, Jesus M.; Baricuatro, Jack H.; McCrory, Charles C. L.; Soriaga, Manuel P.; Lewis, Nathan S.

doi:10.1021/cs500412u

Title: Operando Synthesis of Macroporous Molybdenum Diselenide Films for Electrocatalysis of the Hydrogen-Evolution Reaction

Journal Article · Thu Jul 17 00:00:00 EDT 2014 · ACS Catalysis

DOI:https://doi.org/10.1021/cs500412u· OSTI ID:1634224

Saadi, Fadl H. ^[1]; Carim, Azhar I. ^[1]; Velazquez, Jesus M. ^[1]; Baricuatro, Jack H. ^[1]; McCrory, Charles C. L. ^[1]; Soriaga, Manuel P. ^[2]; Lewis, Nathan S. ^[1]

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

The catalytically inactive components of a film have been converted, through an operando method of synthesis, to produce a catalyst for the reaction that the film is catalyzing. Specifically, thin films of molybdenum diselenide have been synthesized using a two-step wet-chemical method, in which excess sodium selenide was first added to a solution of ammonium heptamolydbate in aqueous sulfuric acid, resulting in the spontaneous formation of a black precipitate that contained molybdenum triselenide (MoSe₃), molybdenum trioxide (MoO₃), and elemental selenium. After purification and after the film had been drop cast onto a glassy carbon electrode, a reductive potential was applied to the precipitate-coated electrode. Hydrogen evolution occurred within the range of potentials applied to the electrode, but during the initial voltammetric cycle, an overpotential of ~400 mV was required to drive the hydrogen-evolution reaction at a benchmark current density of –10 mA cm^–2. The overpotential required to evolve hydrogen at the benchmark rate progressively decreased with subsequent voltammetry cycles, until a steady state was reached at which only ~250 mV of overpotential was required to pass –10 mA cm^–2 of current density. During the electrocatalysis, the catalytically inactive components in the as-prepared film were (reductively) converted to MoSe₂ through an operando method of synthesis of the hydrogen-evolution catalyst. The initial film prepared from the precipitate was smooth, but the converted film was completely covered with pores ~200 nm in diameter. In conclusion, the porous MoSe₂ film was stable while being assessed by cyclic voltammetry for 48 h, and the overpotential required to sustain 10 mA cm^–2 of hydrogen evolution increased by <50 mV over this period of operation.

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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:: 1634224

Journal Information:: ACS Catalysis, Vol. 4, Issue 9; ISSN 2155-5435

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 116 works

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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
hydrogen-evolution reaction
synthesis of molybdenum diselenide
wet-chemical synthesis of layered electrocatalysts
mesoporous catalysts
synthesis of group VI dichalcogenides