Scanning Electrochemical Flow Cell with Online Mass Spectroscopy for Accelerated Screening of Carbon Dioxide Reduction Electrocatalysts

Lai, Yungchieh; Jones, Ryan J.  R.; Wang, Yu; Zhou, Lan; Gregoire, John M.

doi:10.1021/acscombsci.9b00130

Title: Scanning Electrochemical Flow Cell with Online Mass Spectroscopy for Accelerated Screening of Carbon Dioxide Reduction Electrocatalysts

Abstract

Electrochemical conversion of carbon dioxide into valuable chemicals or fuels is an increasingly important strategy for achieving carbon neutral technologies. The lack of a sufficiently active and selective electrocatalyst, particularly for synthesizing highly reduced products, motivates accelerated screening to evaluate new catalyst spaces. Traditional techniques, which couple electrocatalyst operation with analytical techniques to measure product distributions, enable screening throughput at 1–10 catalysts per day. In this paper, a combinatorial screening instrument is designed for MS detection of hydrogen, methane, and ethylene in quasi-real-time during catalyst operation experiments in an electrochemical flow cell. Coupled with experiment modeling, product detection during cyclic voltammetry (CV) enables modeling of the voltage-dependent partial current density for each detected product. Here, we demonstrate the technique by using the well-established thin film Cu catalysts and by screening a Pd–Zn composition library in carbonate-buffered aqueous electrolyte. The rapid product distribution characterization over a large range of overpotential makes the instrument uniquely suited for accelerating screening of electrocatalysts for the carbon dioxide reduction reaction.

Authors:

Lai, Yungchieh ^[1]; Jones, Ryan J. R. ^[1]; Wang, Yu ^[1]; Zhou, Lan ^[1];

^[2]

California Institute of Technology (CalTech), Pasadena, CA (United States). Joint Center for Artificial Photosynthesis (JCAP)
California Institute of Technology (CalTech), Pasadena, CA (United States). Joint Center for Artificial Photosynthesis (JCAP), and Division of Engineering and Applied Science

Publication Date:: Tue Aug 27 00:00:00 EDT 2019

Research Org.:: California Institute of Technology (CalTech), Pasadena, CA (United States)

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

OSTI Identifier:: 1606293

Grant/Contract Number:: SC0004993; AC02-76SF00515

Resource Type:: Accepted Manuscript

Journal Name:: ACS Combinatorial Science

Additional Journal Information:: Journal Volume: 21; Journal Issue: 10; Journal ID: ISSN 2156-8952

Publisher:: American Chemical Society (ACS)

Country of Publication:: United States

Language:: English

Subject:: 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; carbon dioxide reduction; catalyst discovery; electrocatalysis; high throughput experimentation; product detection

Citation Formats


                    Lai, Yungchieh, Jones, Ryan J.  R., Wang, Yu, Zhou, Lan, and Gregoire, John M. Scanning Electrochemical Flow Cell with Online Mass Spectroscopy for Accelerated Screening of Carbon Dioxide Reduction Electrocatalysts.  United States: N. p., 2019. 
Web.  doi:10.1021/acscombsci.9b00130.

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                    Lai, Yungchieh, Jones, Ryan J.  R., Wang, Yu, Zhou, Lan, & Gregoire, John M. Scanning Electrochemical Flow Cell with Online Mass Spectroscopy for Accelerated Screening of Carbon Dioxide Reduction Electrocatalysts.  United States.  https://doi.org/10.1021/acscombsci.9b00130

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                    Lai, Yungchieh, Jones, Ryan J.  R., Wang, Yu, Zhou, Lan, and Gregoire, John M. Tue .  
"Scanning Electrochemical Flow Cell with Online Mass Spectroscopy for Accelerated Screening of Carbon Dioxide Reduction Electrocatalysts".  United States.  https://doi.org/10.1021/acscombsci.9b00130.  https://www.osti.gov/servlets/purl/1606293.

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@article{osti_1606293,

  title        = {Scanning Electrochemical Flow Cell with Online Mass Spectroscopy for Accelerated Screening of Carbon Dioxide Reduction Electrocatalysts},

  author       = {Lai, Yungchieh and Jones, Ryan J.  R. and Wang, Yu and Zhou, Lan and Gregoire, John M.},

  abstractNote = {Electrochemical conversion of carbon dioxide into valuable chemicals or fuels is an increasingly important strategy for achieving carbon neutral technologies. The lack of a sufficiently active and selective electrocatalyst, particularly for synthesizing highly reduced products, motivates accelerated screening to evaluate new catalyst spaces. Traditional techniques, which couple electrocatalyst operation with analytical techniques to measure product distributions, enable screening throughput at 1–10 catalysts per day. In this paper, a combinatorial screening instrument is designed for MS detection of hydrogen, methane, and ethylene in quasi-real-time during catalyst operation experiments in an electrochemical flow cell. Coupled with experiment modeling, product detection during cyclic voltammetry (CV) enables modeling of the voltage-dependent partial current density for each detected product. Here, we demonstrate the technique by using the well-established thin film Cu catalysts and by screening a Pd–Zn composition library in carbonate-buffered aqueous electrolyte. The rapid product distribution characterization over a large range of overpotential makes the instrument uniquely suited for accelerating screening of electrocatalysts for the carbon dioxide reduction reaction.},

  doi          = {10.1021/acscombsci.9b00130},

  journal      = {ACS Combinatorial Science},

  number       = 10,

  volume       = 21,

  place        = {United States},

  year         = {Tue Aug 27 00:00:00 EDT 2019},

  month        = {Tue Aug 27 00:00:00 EDT 2019}

}

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Works referencing / citing this record:

The sensitivity of Cu for electrochemical carbon dioxide reduction to hydrocarbons as revealed by high throughput experiments
journal, January 2019

Lai, Yungchieh; Jones, Ryan J. R.; Wang, Yu
Journal of Materials Chemistry A, Vol. 7, Issue 47
DOI: 10.1039/c9ta10111j

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Title: Scanning Electrochemical Flow Cell with Online Mass Spectroscopy for Accelerated Screening of Carbon Dioxide Reduction Electrocatalysts

Abstract

Citation Formats

Photochemical and Photoelectrochemical Reduction of CO 2 journal, May 2012

Progress and Perspectives of Electrochemical CO 2 Reduction on Copper in Aqueous Electrolyte journal, April 2019

Electrocatalytic process of CO selectivity in electrochemical reduction of CO2 at metal electrodes in aqueous media journal, August 1994

New insights into the electrochemical reduction of carbon dioxide on metallic copper surfaces journal, January 2012

Combinatorial electrochemistry – Processing and characterization for materials discovery journal, January 2015

Reactor design and integration with product detection to accelerate screening of electrocatalysts for carbon dioxide reduction journal, December 2018

Screening of material libraries for electrochemical CO2 reduction catalysts – Improving selectivity of Cu by mixing with Co journal, November 2016

Measuring Electrocatalytic Activity on a Local Scale with Scanning Differential Electrochemical Mass Spectrometry journal, January 2003

A Multielectrode Electrochemical and Scanning Differential Electrochemical Mass Spectrometry Study of Methanol Oxidation on Electrodeposited Pt x Ru y journal, March 2004

Differential electrochemical mass spectrometry journal, December 2004

Direct Observation of the Local Reaction Environment during the Electrochemical Reduction of CO 2 journal, April 2018

Differential Electrochemical Mass Spectroscopy (DEMS) - a New Method for the Study of Electrode Processes journal, January 1984

Differential electrochemical mass spectrometry using smooth electrodes: adsorption and hydrogen/deuterium exchange reactions of benzene on platinum journal, May 1990

A New Approach for Simultaneous DEMS and EQCM: Electro-oxidation of Adsorbed CO on Pt and Pt-Ru journal, January 1999

On-line mass spectrometry system for measurements at single-crystal electrodes in hanging meniscus configuration journal, August 2006

An exchangeable-tip scanning probe instrument for the analysis of combinatorial libraries of electrocatalysts journal, February 2013

Scanning droplet cell for high throughput electrochemical and photoelectrochemical measurements journal, February 2013

Coupling of a high throughput microelectrochemical cell with online multielemental trace analysis by ICP-MS journal, December 2011

Coupling of a scanning flow cell with online electrochemical mass spectrometry for screening of reaction selectivity journal, October 2014

Electrochemical Real-Time Mass Spectrometry (EC-RTMS): Monitoring Electrochemical Reaction Products in Real Time journal, April 2019

Differential Electrochemical Mass Spectrometer Cell Design for Online Quantification of Products Produced during Electrochemical Reduction of CO 2 journal, July 2015

Combinatorial thin film composition mapping using three dimensional deposition profiles journal, March 2015

High-throughput synchrotron X-ray diffraction for combinatorial phase mapping journal, October 2014

Electrochemical reduction of carbon dioxide on hydrogen-storing materials. journal, April 1993

Synthesis of thin film AuPd alloys and their investigation for electrocatalytic CO 2 reduction journal, January 2015

Palladium–gold catalyst for the electrochemical reduction of CO 2 to C 1 –C 5 hydrocarbons journal, January 2016

Exclusive Formation of Formic Acid from CO 2 Electroreduction by a Tunable Pd-Sn Alloy journal, August 2017

High performance RuPd catalysts for CO2 reduction at gas-diffusion electrodes journal, June 1997

Doping palladium with tellurium for the highly selective electrocatalytic reduction of aqueous CO 2 to CO journal, January 2018

Pd-Containing Nanostructures for Electrochemical CO 2 Reduction Reaction journal, January 2018

Electrodeposited Zn Dendrites with Enhanced CO Selectivity for Electrocatalytic CO 2 Reduction journal, July 2015

Active learning across intermetallics to guide discovery of electrocatalysts for CO2 reduction and H2 evolution journal, September 2018

The sensitivity of Cu for electrochemical carbon dioxide reduction to hydrocarbons as revealed by high throughput experiments journal, January 2019

Photochemical and Photoelectrochemical Reduction of CO ₂
journal, May 2012

Progress and Perspectives of Electrochemical CO ₂ Reduction on Copper in Aqueous Electrolyte
journal, April 2019

Electrocatalytic process of CO selectivity in electrochemical reduction of CO₂ at metal electrodes in aqueous media
journal, August 1994

New insights into the electrochemical reduction of carbon dioxide on metallic copper surfaces
journal, January 2012

Combinatorial electrochemistry – Processing and characterization for materials discovery
journal, January 2015

Reactor design and integration with product detection to accelerate screening of electrocatalysts for carbon dioxide reduction
journal, December 2018

Screening of material libraries for electrochemical CO2 reduction catalysts – Improving selectivity of Cu by mixing with Co
journal, November 2016

Measuring Electrocatalytic Activity on a Local Scale with Scanning Differential Electrochemical Mass Spectrometry
journal, January 2003

A Multielectrode Electrochemical and Scanning Differential Electrochemical Mass Spectrometry Study of Methanol Oxidation on Electrodeposited Pt _x Ru _y
journal, March 2004

Differential electrochemical mass spectrometry
journal, December 2004

Direct Observation of the Local Reaction Environment during the Electrochemical Reduction of CO ₂
journal, April 2018

Differential Electrochemical Mass Spectroscopy (DEMS) - a New Method for the Study of Electrode Processes
journal, January 1984

Differential electrochemical mass spectrometry using smooth electrodes: adsorption and hydrogen/deuterium exchange reactions of benzene on platinum
journal, May 1990

A New Approach for Simultaneous DEMS and EQCM: Electro-oxidation of Adsorbed CO on Pt and Pt-Ru
journal, January 1999

On-line mass spectrometry system for measurements at single-crystal electrodes in hanging meniscus configuration
journal, August 2006

An exchangeable-tip scanning probe instrument for the analysis of combinatorial libraries of electrocatalysts
journal, February 2013

Scanning droplet cell for high throughput electrochemical and photoelectrochemical measurements
journal, February 2013

Coupling of a high throughput microelectrochemical cell with online multielemental trace analysis by ICP-MS
journal, December 2011

Coupling of a scanning flow cell with online electrochemical mass spectrometry for screening of reaction selectivity
journal, October 2014

Electrochemical Real-Time Mass Spectrometry (EC-RTMS): Monitoring Electrochemical Reaction Products in Real Time
journal, April 2019

Differential Electrochemical Mass Spectrometer Cell Design for Online Quantification of Products Produced during Electrochemical Reduction of CO ₂
journal, July 2015

Combinatorial thin film composition mapping using three dimensional deposition profiles
journal, March 2015

High-throughput synchrotron X-ray diffraction for combinatorial phase mapping
journal, October 2014

Electrochemical reduction of carbon dioxide on hydrogen-storing materials.
journal, April 1993

Synthesis of thin film AuPd alloys and their investigation for electrocatalytic CO ₂ reduction
journal, January 2015

Palladium–gold catalyst for the electrochemical reduction of CO ₂ to C ₁ –C ₅ hydrocarbons
journal, January 2016

Exclusive Formation of Formic Acid from CO ₂ Electroreduction by a Tunable Pd-Sn Alloy
journal, August 2017

High performance RuPd catalysts for CO₂ reduction at gas-diffusion electrodes
journal, June 1997

Doping palladium with tellurium for the highly selective electrocatalytic reduction of aqueous CO ₂ to CO
journal, January 2018

Pd-Containing Nanostructures for Electrochemical CO ₂ Reduction Reaction
journal, January 2018

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journal, September 2018

The sensitivity of Cu for electrochemical carbon dioxide reduction to hydrocarbons as revealed by high throughput experiments
journal, January 2019