Electrochemical Flow Reactor Design Allows Tunable Mass Transport Conditions for Operando Surface Enhanced Infrared Absorption Spectroscopy

Avilés Acosta, Jaime E.; Lin, John C.; Un Lee, Dong; Jaramillo, Thomas F.; Hahn, Christopher

doi:10.1002/cctc.202300520

Electrochemical Flow Reactor Design Allows Tunable Mass Transport Conditions for Operando Surface Enhanced Infrared Absorption Spectroscopy

Journal Article · Mon Jul 03 00:00:00 EDT 2023 · ChemCatChem

DOI:https://doi.org/10.1002/cctc.202300520· OSTI ID:1994586

^[1]; Lin, John C. ^[2]; ^[2]; ^[2]; ^[3]

SUNCAT Center for Interface Science and Catalysis SLAC National Accelerator Laboratory Menlo Park CA-94025 USA, Department of Materials Science and Engineering Stanford University Stanford CA-94305 USA
SUNCAT Center for Interface Science and Catalysis SLAC National Accelerator Laboratory Menlo Park CA-94025 USA, Department of Chemical Engineering Stanford University Stanford CA-94305 USA
Materials Science Division Lawrence Livermore National Laboratory Livermore CA-94550 USA

Abstract

In situ attenuated total reflection surface enhanced infrared absorption spectroscopy (ATR‐SEIRAS) is often used to investigate the near‐surface electrocatalytic reaction environment. However, there is a gap in directly correlating the near‐surface reaction environment with electrocatalytic reaction rates. To that end, we designed an electrochemical flow reactor for operando electrochemical ATR‐SEIRAS and demonstrate its capability with the CO ₂ reduction reaction (CO ₂ RR). Roughened gold catalyst thin films are prepared on ATR silicon crystals as a model system to probe local species under CO ₂ RR conditions in 0.1 M KHCO ₃ . We measured changes in the interfacial CO ₂ concentration as a function of applied potential and electrolyte flow rate in operando , allowing us to correlate the changes in reaction rates with the observed CO ₂ concentration. Including the choice of the catalyst and electrolyte, coupling hydrodynamic control with ATR‐SEIRAS in this platform enables investigations of how the local microenvironment affects the activity and selectivity of electrochemical reactions.

View Accepted Manuscript (Publisher)

Sponsoring Organization:: USDOE

Grant/Contract Number:: SC0004993; SC0021266

OSTI ID:: 1994586

Alternate ID(s):: OSTI ID: 1998182

Journal Information:: ChemCatChem, Journal Name: ChemCatChem Journal Issue: 15 Vol. 15; ISSN 1867-3880

Publisher:: Wiley Blackwell (John Wiley & Sons)Copyright Statement

Country of Publication:: Germany

Language:: English

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Optical Constants of Water in the 200-nm to 200-μm Wavelength Region Hale, George M.; Querry, Marvin R. Applied Optics, Vol. 12, Issue 3 https://doi.org/10.1364/AO.12.000555	journal	January 1973
In-situ Spectroscopic Techniques as Critical Evaluation Tools for Electrochemical Carbon dioxide Reduction: A Mini Review Adarsh, K. S.; Chandrasekaran, Naveen; Chakrapani, Vidhya Frontiers in Chemistry, Vol. 8 https://doi.org/10.3389/fchem.2020.00137	journal	March 2020

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