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

Abstract

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)more » 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.« less

Authors:
ORCiD logo [1]; ORCiD logo [1]; ORCiD logo [1];  [1];  [2]; ORCiD logo [2]; ORCiD logo [3];  [3];  [3];  [2]; ORCiD logo [3]; ORCiD logo [1]
+ Show Author Affiliations
  1. Argonne National Lab. (ANL), Lemont, IL (United States)
  2. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
  3. Univ. of Delaware, Newark, DE (United States)
Publication Date:
Research Org.:
Energy Frontier Research Centers (EFRC) (United States). Fluid Interface Reactions, Structures and Transport Center (FIRST); Argonne National Lab. (ANL), Argonne, IL (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
OSTI Identifier:
1481745
Grant/Contract Number:  
AC02-06CH11357
Resource Type:
Accepted Manuscript
Journal Name:
ACS Catalysis
Additional Journal Information:
Journal Volume: 7; Journal Issue: 10; Journal ID: ISSN 2155-5435
Publisher:
American Chemical Society (ACS)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; EQCM; EXAFS; X-ray reflectivity; XANES; bismuth electrocatalyst; electrochemical CO2 reduction; electrode restructuring; ionic liquid

Citation Formats

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, and Fenter, Paul. Structural Dynamics and Evolution of Bismuth Film Electrodes during Electrochemical Reduction of CO2 in Imidazolium-Based Ionic Liquid Solutions. United States: N. p., 2017. Web. doi:10.1021/acscatal.7b01370.
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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. Structural Dynamics and Evolution of Bismuth Film Electrodes during Electrochemical Reduction of CO2 in Imidazolium-Based Ionic Liquid Solutions. United States. https://doi.org/10.1021/acscatal.7b01370
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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, and Fenter, Paul. Tue . "Structural Dynamics and Evolution of Bismuth Film Electrodes during Electrochemical Reduction of CO2 in Imidazolium-Based Ionic Liquid Solutions". United States. https://doi.org/10.1021/acscatal.7b01370. https://www.osti.gov/servlets/purl/1481745.
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@article{osti_1481745,
title = {Structural Dynamics and Evolution of Bismuth Film Electrodes during Electrochemical Reduction of CO2 in Imidazolium-Based Ionic Liquid Solutions},
author = {Medina-Ramos, Jonnathan and Lee, Sang Soo and Fister, Timothy T. and Hubaud, Aude A. and Sacci, Robert L. and Mullins, David R. and DiMeglio, John L. and Pupillo, Rachel C. and Velardo, Stephanie M. and Lutterman, Daniel A. and Rosenthal, Joel and Fenter, Paul},
abstractNote = {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.},
doi = {10.1021/acscatal.7b01370},
journal = {ACS Catalysis},
number = 10,
volume = 7,
place = {United States},
year = {Tue Sep 12 00:00:00 EDT 2017},
month = {Tue Sep 12 00:00:00 EDT 2017}
}
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https://doi.org/10.1021/acscatal.7b01370
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Figures / Tables:

Figure 1 Figure 1: Bi LIII-edge XANES spectra of Bi-CMEC films in acetonitrile-based solutions containing (a) TBAPF6 and (b) [BMIM]OTf. The electrode potential and the gas that was sparged through the electrolyte solutions are indicated in the legend; measurements were run sequentially in the order indicated in the figure’s legend from topmore » to bottom. For referencing purposes, the XANES for metallic Bi and Bi2O3 standards are shown as dotted black and dashed blue dotted lines, respectively.« less
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