Structural Dynamics and Evolution of Bismuth Film Electrodes during Electrochemical Reduction of CO2 in Imidazolium-Based Ionic Liquid Solutions

Medina-Ramos, Jonnathan; Lee, Sang Soo; Fister, Timothy T.; Hubaud, Aude A.; Sacci, Robert L.; Mullins, David R.; DiMeglio, John L.; Pupillo, Rachel C.; Velardo, Stephanie M.; Lutterman, Daniel A.; Rosenthal, Joel; Fenter, Paul

doi:10.1021/acscatal.7b01370

Title: Structural Dynamics and Evolution of Bismuth Film Electrodes during Electrochemical Reduction of CO₂ in Imidazolium-Based Ionic Liquid Solutions

Journal Article · Tue Sep 12 00:00:00 EDT 2017 · ACS Catalysis

DOI:https://doi.org/10.1021/acscatal.7b01370· OSTI ID:1481745

^[1];

^[1]; Hubaud, Aude A. ^[1]; Sacci, Robert L. ^[2];

^[2];

^[3]; Pupillo, Rachel C. ^[3]; Velardo, Stephanie M. ^[3]; Lutterman, Daniel A. ^[2];

^[3];

^[1]

Argonne National Lab. (ANL), Lemont, IL (United States)
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Univ. of Delaware, Newark, DE (United States)

Real-time changes in the composition and structure of bismuth electrodes used for catalytic conversion of CO₂ into CO were examined via X-ray absorption spectroscopy (including XANES and EXAFS), electrochemical quartz crystal microbalance (EQCM) and in situ X-ray reflectivity (XR). Measurements were performed with bismuth electrodes immersed in acetonitrile (MeCN) solutions containing a 1-butyl-3-methylimidazolium ([BMIM]⁺) ionic liquid promoter or electrochemically inactive tetrabutylammonium supporting electrolytes (TBAPF₆ or TBAOTf). Altogether, these measurements show that bismuth electrodes are originally a mixture of bismuth oxides (including Bi₂O₃) and metallic bismuth (Bi⁰), and that the reduction of oxidized bismuth species to Bi⁰ is fully achieved under potentials at which CO₂ activation takes place. Furthermore, EQCM measurements conducted during cyclic voltammetry revealed that a bismuth-coated quartz crystal exhibits significant shifts in resistance (ΔR) prior to the onset of CO₂ reduction near -1.75 V vs. Ag/AgCl and pronounced hysteresis in frequency (Δf) and ΔR, which suggests significant changes in roughness or viscosity at the Bi/[BMIM]⁺ solution interface. In situ XR performed on rhombohedral Bi (001) oriented films indicates extensive restructuring of the bismuth film cathodes takes place upon polarization to potentials more negative than -1.6 V vs. Ag/AgCl, which is characterized by a decrease of the Bi (001) Bragg peak intensity of ≥50% in [BMIM]OTf solutions in the presence and absence of CO₂. Over 90% of the reflectivity is recovered during the anodic half-scan, suggesting that the structural changes are mostly reversible. By contrast, such a phenomenon is not observed for thin Bi (001) oriented films in solutions of tetrabutylammonium salts that do not promote CO₂ reduction. In conclusion, these results highlight that Bi electrodes undergo significant potential-dependent chemical and structural transformations in the presence of [BMIM]⁺ based electrolytes, including the reduction of bismuth oxide to bismuth metal, changes in roughness and near-surface viscosity.

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Research Organization:: Energy Frontier Research Centers (EFRC) (United States). Fluid Interface Reactions, Structures and Transport Center (FIRST); Argonne National Lab. (ANL), Argonne, IL (United States)

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

Grant/Contract Number:: AC02-06CH11357

OSTI ID:: 1481745

Journal Information:: ACS Catalysis, Vol. 7, Issue 10; ISSN 2155-5435

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 36 works

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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
EQCM
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Title: Structural Dynamics and Evolution of Bismuth Film Electrodes during Electrochemical Reduction of CO2 in Imidazolium-Based Ionic Liquid Solutions

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