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

Lobaccaro, Peter; Singh, Meenesh R.; Clark, Ezra Lee; Kwon, Youngkook; Bell, Alexis T.; Ager, Joel W.

doi:10.1039/c6cp05287h

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

Journal Article · Tue Sep 06 00:00:00 EDT 2016 · Physical Chemistry Chemical Physics. PCCP

DOI:https://doi.org/10.1039/c6cp05287h· OSTI ID:1398394

Lobaccaro, Peter ^[1];

^[1]; Clark, Ezra Lee ^[1]; Kwon, Youngkook ^[2]; Bell, Alexis T. ^[1];

^[3]

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
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
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

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.

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

Grant/Contract Number:: AC02-05CH11231; SC0004993

OSTI ID:: 1398394

Alternate ID(s):: OSTI ID: 1497011

Journal Information:: Physical Chemistry Chemical Physics. PCCP, Vol. 18, Issue 38; ISSN 1463-9076

Publisher:: Royal Society of ChemistryCopyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 97 works

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Mechanistic insights into electrochemical reduction of CO ₂ over Ag using density functional theory and transport models Singh, Meenesh R.; Goodpaster, Jason D.; Weber, Adam Z. Proceedings of the National Academy of Sciences, Vol. 114, Issue 42 https://doi.org/10.1073/pnas.1713164114	journal	October 2017
Current achievements and the future direction of electrochemical CO 2 reduction: A short review Lee, Mi-Young; Park, Ki Tae; Lee, Wonhee Critical Reviews in Environmental Science and Technology https://doi.org/10.1080/10643389.2019.1631991	journal	June 2019
Towards Higher Rate Electrochemical CO2 Conversion: From Liquid-Phase to Gas-Phase Systems Song, Jun; Song, Hakhyeon; Kim, Beomil Catalysts, Vol. 9, Issue 3 https://doi.org/10.3390/catal9030224	journal	March 2019
Atomic‐Scale Spacing between Copper Facets for the Electrochemical Reduction of Carbon Dioxide Jeong, Hyung Mo; Kwon, Youngkook; Won, Jong Ho Advanced Energy Materials, Vol. 10, Issue 10 https://doi.org/10.1002/aenm.201903423	journal	March 2020
Nanocrystal/Metal–Organic Framework Hybrids as Electrocatalytic Platforms for CO ₂ Conversion Guntern, Yannick T.; Pankhurst, James R.; Vávra, Jan Angewandte Chemie, Vol. 131, Issue 36 https://doi.org/10.1002/ange.201905172	journal	July 2019

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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