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Title: Effects of temperature and gas–liquid mass transfer on the operation of small electrochemical cells for the quantitative evaluation of CO2 reduction electrocatalysts

Abstract

In the last few years, there has been increased interest in electrochemical CO2 reduction (CO2R). Many experimental studies employ a membrane separated, electrochemical cell with a mini H-cell geometry to characterize CO2R catalysts in aqueous solution. This type of electrochemical cell is a mini-chemical reactor and it is important to monitor the reaction conditions within the reactor to ensure that they are constant throughout the study. Here we show that operating cells with high catalyst surface area to electrolyte volume ratios (S/V) at high current densities can have subtle consequences due to the complexity of the physical phenomena taking place on electrode surfaces during CO2R, particularly as they relate to the cell temperature and bulk electrolyte CO2 concentration. Both effects were evaluated quantitatively in high S/V cells using Cu electrodes and a bicarbonate buffer electrolyte. Electrolyte temperature is a function of the current/total voltage passed through the cell and the cell geometry. Even at a very high current density, 20 mA cm -2 , the temperature increase was less than 4 °C and a decrease of < 10% in the dissolved CO2 concentration is predicted. In contrast, limits on the CO2 gas-liquid mass transfer into the cells produce much largermore » effects. By using the pH in the cell to measure the CO2 concentration, significant undersaturation of CO2 is observed in the bulk electrolyte, even at more modest current densities of 10 mA cm -2 . Undersaturation of CO2 produces large changes in the faradaic efficiency observed on Cu electrodes, with H2 production becoming increasingly favored. Finally, we show that the size of the CO2 bubbles being introduced into the cell is critical for maintaining the equilibrium CO2 concentration in the electrolyte, and we have designed a high S/V cell that is able to maintain the near-equilibrium CO2 concentration at current densities up to 15 mA cm-2.« less

Authors:
 [1]; ORCiD logo [1];  [1];  [2];  [1]; ORCiD logo [3]
  1. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Joint Center for Artificial Photosynthesis; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Chemical Sciences Division; Univ. of California, Berkeley, CA (United States). Dept. of Chemical and Biomolecular Engineering
  2. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Joint Center for Artificial Photosynthesis; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Chemical Sciences Division
  3. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Joint Center for Artificial Photosynthesis; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Materials Sciences Division; Univ. of California, Berkeley, CA (United States). Dept. of Materials Science and Engineering
Publication Date:
Research Org.:
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); California Institute of Technology (CalTech), Pasadena, CA (United States). Joint Center for Artificial Photosynthesis (JCAP)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
OSTI Identifier:
1398394
Alternate Identifier(s):
OSTI ID: 1497011
Grant/Contract Number:  
AC02-05CH11231; SC0004993
Resource Type:
Accepted Manuscript
Journal Name:
Physical Chemistry Chemical Physics. PCCP
Additional Journal Information:
Journal Volume: 18; Journal Issue: 38; Journal ID: ISSN 1463-9076
Publisher:
Royal Society of Chemistry
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Citation Formats

Lobaccaro, Peter, Singh, Meenesh R., Clark, Ezra Lee, Kwon, Youngkook, Bell, Alexis T., and Ager, Joel W.. Effects of temperature and gas–liquid mass transfer on the operation of small electrochemical cells for the quantitative evaluation of CO2 reduction electrocatalysts. United States: N. p., 2016. Web. https://doi.org/10.1039/c6cp05287h.
Lobaccaro, Peter, Singh, Meenesh R., Clark, Ezra Lee, Kwon, Youngkook, Bell, Alexis T., & Ager, Joel W.. Effects of temperature and gas–liquid mass transfer on the operation of small electrochemical cells for the quantitative evaluation of CO2 reduction electrocatalysts. United States. https://doi.org/10.1039/c6cp05287h
Lobaccaro, Peter, Singh, Meenesh R., Clark, Ezra Lee, Kwon, Youngkook, Bell, Alexis T., and Ager, Joel W.. Tue . "Effects of temperature and gas–liquid mass transfer on the operation of small electrochemical cells for the quantitative evaluation of CO2 reduction electrocatalysts". United States. https://doi.org/10.1039/c6cp05287h. https://www.osti.gov/servlets/purl/1398394.
@article{osti_1398394,
title = {Effects of temperature and gas–liquid mass transfer on the operation of small electrochemical cells for the quantitative evaluation of CO2 reduction electrocatalysts},
author = {Lobaccaro, Peter and Singh, Meenesh R. and Clark, Ezra Lee and Kwon, Youngkook and Bell, Alexis T. and Ager, Joel W.},
abstractNote = {In the last few years, there has been increased interest in electrochemical CO2 reduction (CO2R). Many experimental studies employ a membrane separated, electrochemical cell with a mini H-cell geometry to characterize CO2R catalysts in aqueous solution. This type of electrochemical cell is a mini-chemical reactor and it is important to monitor the reaction conditions within the reactor to ensure that they are constant throughout the study. Here we show that operating cells with high catalyst surface area to electrolyte volume ratios (S/V) at high current densities can have subtle consequences due to the complexity of the physical phenomena taking place on electrode surfaces during CO2R, particularly as they relate to the cell temperature and bulk electrolyte CO2 concentration. Both effects were evaluated quantitatively in high S/V cells using Cu electrodes and a bicarbonate buffer electrolyte. Electrolyte temperature is a function of the current/total voltage passed through the cell and the cell geometry. Even at a very high current density, 20 mA cm -2 , the temperature increase was less than 4 °C and a decrease of < 10% in the dissolved CO2 concentration is predicted. In contrast, limits on the CO2 gas-liquid mass transfer into the cells produce much larger effects. By using the pH in the cell to measure the CO2 concentration, significant undersaturation of CO2 is observed in the bulk electrolyte, even at more modest current densities of 10 mA cm -2 . Undersaturation of CO2 produces large changes in the faradaic efficiency observed on Cu electrodes, with H2 production becoming increasingly favored. Finally, we show that the size of the CO2 bubbles being introduced into the cell is critical for maintaining the equilibrium CO2 concentration in the electrolyte, and we have designed a high S/V cell that is able to maintain the near-equilibrium CO2 concentration at current densities up to 15 mA cm-2.},
doi = {10.1039/c6cp05287h},
journal = {Physical Chemistry Chemical Physics. PCCP},
number = 38,
volume = 18,
place = {United States},
year = {2016},
month = {9}
}

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    Current achievements and the future direction of electrochemical CO 2 reduction: A short review
    journal, June 2019


    Towards Higher Rate Electrochemical CO2 Conversion: From Liquid-Phase to Gas-Phase Systems
    journal, March 2019


    Atomic‐Scale Spacing between Copper Facets for the Electrochemical Reduction of Carbon Dioxide
    journal, March 2020

    • Jeong, Hyung Mo; Kwon, Youngkook; Won, Jong Ho
    • Advanced Energy Materials, Vol. 10, Issue 10
    • DOI: 10.1002/aenm.201903423

    Nanocrystal/Metal–Organic Framework Hybrids as Electrocatalytic Platforms for CO 2 Conversion
    journal, July 2019

    • Guntern, Yannick T.; Pankhurst, James R.; Vávra, Jan
    • Angewandte Chemie, Vol. 131, Issue 36
    • DOI: 10.1002/ange.201905172