Operando NRIXS and XAFS Investigation of Segregation Phenomena in Fe-Cu and Fe-Ag Nanoparticle Catalysts during CO2 Electroreduction

Kunze, Sebastian; Grosse, Philipp; Bernal Lopez, Miguel; Sinev, Ilya; Zegkinoglou, Ioannis; Mistry, Hemma; Timoshenko, Janis; Hu, Michael Y.; Zhao, Jiyong; Alp, Ercan E.; Chee, See Wee; Roldan Cuenya, Beatriz

doi:10.1002/anie.202010535

Title: Operando NRIXS and XAFS Investigation of Segregation Phenomena in Fe-Cu and Fe-Ag Nanoparticle Catalysts during CO₂ Electroreduction

Abstract

Operando nuclear resonant inelastic X-ray scattering (NRIXS) and X-ray absorption fine-structure spectroscopy (XAFS) measurements were used to gain insight into the structure and surface composition of FeCu and FeAg nanoparticles (NPs) during the electrochemical CO₂ reduction (CO₂RR) and to extract correlations with their catalytic activity and selectivity. The formation of a core–shell structure during CO₂RR for FeAg NPs was inferred from the analysis of the operando NRIXS data (phonon density of states, PDOS) and XAFS measurements. Electrochemical analysis of the FeAg NPs revealed a faradaic selectivity of 36 % for CO in 0.1 M KHCO₃ at -1.1 V vs. RHE, similar to that of pure Ag NPs. In contrast, a predominant selectivity towards H₂ evolution is obtained in the case of the FeCu NPs, analogous to the results obtained for pure Fe NPs, although small Cu NPs have also been shown to favor H₂ production.

Authors:

^[1];

^[2]; Sinev, Ilya ^[2];

^[2]; Mistry, Hemma ^[2];

^[3]; Hu, Michael Y. ^[4]; Zhao, Jiyong ^[4]; Alp, Ercan E. ^[4];

^[3];

^[3]

Ruhr Univ., Bochum (Germany); Fritz-Haber Institute of the Max Planck Society, Berlin (Germany)
Ruhr Univ., Bochum (Germany)
Fritz-Haber Institute of the Max Planck Society, Berlin (Germany)
Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS)

Publication Date:: Tue Oct 06 00:00:00 EDT 2020

Research Org.:: Argonne National Lab. (ANL), Argonne, IL (United States)

Sponsoring Org.:: European Research Council (ERC); German Research Foundation (DFG); USDOE Office of Science (SC), Basic Energy Sciences (BES)

OSTI Identifier:: 1785375

Grant/Contract Number:: AC02-06CH11357

Resource Type:: Accepted Manuscript

Journal Name:: Angewandte Chemie (International Edition)

Additional Journal Information:: Journal Name: Angewandte Chemie (International Edition); Journal Volume: 59; Journal Issue: 50; Journal ID: ISSN 1433-7851

Publisher:: Wiley

Country of Publication:: United States

Language:: English

Subject:: 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; CO(2)electroreduction; NRIXS; XAFS; nanoparticles; operando measurements

Citation Formats


                    Kunze, Sebastian, Grosse, Philipp, Bernal Lopez, Miguel, Sinev, Ilya, Zegkinoglou, Ioannis, Mistry, Hemma, Timoshenko, Janis, Hu, Michael Y., Zhao, Jiyong, Alp, Ercan E., Chee, See Wee, and Roldan Cuenya, Beatriz. Operando NRIXS and XAFS Investigation of Segregation Phenomena in Fe-Cu and Fe-Ag Nanoparticle Catalysts during CO2 Electroreduction.  United States: N. p., 2020. 
Web.  doi:10.1002/anie.202010535.

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                    Kunze, Sebastian, Grosse, Philipp, Bernal Lopez, Miguel, Sinev, Ilya, Zegkinoglou, Ioannis, Mistry, Hemma, Timoshenko, Janis, Hu, Michael Y., Zhao, Jiyong, Alp, Ercan E., Chee, See Wee, & Roldan Cuenya, Beatriz. Operando NRIXS and XAFS Investigation of Segregation Phenomena in Fe-Cu and Fe-Ag Nanoparticle Catalysts during CO2 Electroreduction.  United States.  https://doi.org/10.1002/anie.202010535

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                    Kunze, Sebastian, Grosse, Philipp, Bernal Lopez, Miguel, Sinev, Ilya, Zegkinoglou, Ioannis, Mistry, Hemma, Timoshenko, Janis, Hu, Michael Y., Zhao, Jiyong, Alp, Ercan E., Chee, See Wee, and Roldan Cuenya, Beatriz. Tue .  
"Operando NRIXS and XAFS Investigation of Segregation Phenomena in Fe-Cu and Fe-Ag Nanoparticle Catalysts during CO2 Electroreduction".  United States.  https://doi.org/10.1002/anie.202010535.  https://www.osti.gov/servlets/purl/1785375.

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@article{osti_1785375,

  title        = {Operando NRIXS and XAFS Investigation of Segregation Phenomena in Fe-Cu and Fe-Ag Nanoparticle Catalysts during CO2 Electroreduction},

  author       = {Kunze, Sebastian and Grosse, Philipp and Bernal Lopez, Miguel and Sinev, Ilya and Zegkinoglou, Ioannis and Mistry, Hemma and Timoshenko, Janis and Hu, Michael Y. and Zhao, Jiyong and Alp, Ercan E. and Chee, See Wee and Roldan Cuenya, Beatriz},

  abstractNote = {Operando nuclear resonant inelastic X-ray scattering (NRIXS) and X-ray absorption fine-structure spectroscopy (XAFS) measurements were used to gain insight into the structure and surface composition of FeCu and FeAg nanoparticles (NPs) during the electrochemical CO2 reduction (CO2RR) and to extract correlations with their catalytic activity and selectivity. The formation of a core–shell structure during CO2RR for FeAg NPs was inferred from the analysis of the operando NRIXS data (phonon density of states, PDOS) and XAFS measurements. Electrochemical analysis of the FeAg NPs revealed a faradaic selectivity of 36 % for CO in 0.1 M KHCO3 at -1.1 V vs. RHE, similar to that of pure Ag NPs. In contrast, a predominant selectivity towards H2 evolution is obtained in the case of the FeCu NPs, analogous to the results obtained for pure Fe NPs, although small Cu NPs have also been shown to favor H2 production.},

  doi          = {10.1002/anie.202010535},

  journal      = {Angewandte Chemie (International Edition)},

  number       = 50,

  volume       = 59,

  place        = {United States},

  year         = {Tue Oct 06 00:00:00 EDT 2020},

  month        = {Tue Oct 06 00:00:00 EDT 2020}

}

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Title: Operando NRIXS and XAFS Investigation of Segregation Phenomena in Fe-Cu and Fe-Ag Nanoparticle Catalysts during CO2 Electroreduction

Abstract

Citation Formats

Applications of extended X-ray absorption fine-structure spectroscopy to studies of bimetallic nanoparticle catalysts journal, January 2012

Adsorbate-Induced Surface Segregation for Core-Shell Nanocatalysts journal, April 2009

ATHENA , ARTEMIS , HEPHAESTUS : data analysis for X-ray absorption spectroscopy using IFEFFIT journal, June 2005

Surface energy of arbitrary crystal plane of bcc and fcc metals journal, August 2000

Surface Segregation in CuNi Nanoparticle Catalysts During CO 2 Hydrogenation: The Role of CO in the Reactant Mixture journal, October 2018

Local atomic environment in silver chlorobromides from exafs journal, March 1993

Operando Phonon Studies of the Protonation Mechanism in Highly Active Hydrogen Evolution Reaction Pentlandite Catalysts journal, October 2017

Exceptional Size-Dependent Activity Enhancement in the Electroreduction of CO 2 over Au Nanoparticles journal, November 2014

Determination of Néel Temperatures in fcc Iron journal, August 1963

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

Characterization of Metal-Oxide Catalysts in Operando Conditions by Combining X-ray Absorption and Raman Spectroscopies in the Same Experiment journal, May 2013

Influence of interfaces on the phonon density of states of nanoscale metallic multilayers: Phonon confinement and localization journal, July 2018

New insights into working nanostructured electrocatalysts through operando spectroscopy and microscopy journal, February 2017

Synchrotron Techniques for In Situ Catalytic Studies: Capabilities, Challenges, and Opportunities journal, September 2012

Operando methodology: combination of in situ spectroscopy and simultaneous activity measurements under catalytic reaction conditions journal, February 2005

High-energy phonon confinement in nanoscale metallic multilayers journal, April 2008

Particle Size Effects in the Catalytic Electroreduction of CO 2 on Cu Nanoparticles journal, May 2014

Subnanometer Substructures in Nanoassemblies Formed from Clusters under a Reactive Atmosphere Revealed Using Machine Learning journal, August 2018

Phonon Density of States Measured by Inelastic Nuclear Resonant Scattering journal, May 1995

Kern-Schale-Nanokatalysatoren durch adsorbatinduzierte Oberflächensegregation journal, April 2009

Circularly polarized light detection with hot electrons in chiral plasmonic metamaterials journal, September 2015

Identification of carbon-encapsulated iron nanoparticles as active species in non-precious metal oxygen reduction catalysts journal, August 2016

The surface energy of metals journal, August 1998

Developments in operando studies and in situ characterization of heterogeneous catalysts journal, May 2003

Extended X-ray Absorption Fine Structure (EXAFS) Studies of Hydroxo(oxo)iron Aggregates and Minerals, and a Critique of their Use as Models for Ferritin journal, June 1996

Size-dependent evolution of the atomic vibrational density of states and thermodynamic properties of isolated Fe nanoparticles journal, October 2012

Silver clusters shape determination from in-situ XANES data journal, November 2018

Understanding heterogeneous electrocatalytic carbon dioxide reduction through operando techniques journal, December 2018

Operando Evolution of the Structure and Oxidation State of Size-Controlled Zn Nanoparticles during CO 2 Electroreduction journal, July 2018

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Determining the active site in a catalytic process: Operando spectroscopy is more than a buzzword journal, January 2003

Title: Operando NRIXS and XAFS Investigation of Segregation Phenomena in Fe-Cu and Fe-Ag Nanoparticle Catalysts during CO₂ Electroreduction

Applications of extended X-ray absorption fine-structure spectroscopy to studies of bimetallic nanoparticle catalysts
journal, January 2012

Adsorbate-Induced Surface Segregation for Core-Shell Nanocatalysts
journal, April 2009

ATHENA , ARTEMIS , HEPHAESTUS : data analysis for X-ray absorption spectroscopy using IFEFFIT
journal, June 2005

Surface energy of arbitrary crystal plane of bcc and fcc metals
journal, August 2000

Surface Segregation in CuNi Nanoparticle Catalysts During CO 2 Hydrogenation: The Role of CO in the Reactant Mixture
journal, October 2018

Local atomic environment in silver chlorobromides from exafs
journal, March 1993

Operando Phonon Studies of the Protonation Mechanism in Highly Active Hydrogen Evolution Reaction Pentlandite Catalysts
journal, October 2017

Exceptional Size-Dependent Activity Enhancement in the Electroreduction of CO ₂ over Au Nanoparticles
journal, November 2014

Determination of Néel Temperatures in fcc Iron
journal, August 1963

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

Characterization of Metal-Oxide Catalysts in Operando Conditions by Combining X-ray Absorption and Raman Spectroscopies in the Same Experiment
journal, May 2013

Influence of interfaces on the phonon density of states of nanoscale metallic multilayers: Phonon confinement and localization
journal, July 2018

New insights into working nanostructured electrocatalysts through operando spectroscopy and microscopy
journal, February 2017

Synchrotron Techniques for In Situ Catalytic Studies: Capabilities, Challenges, and Opportunities
journal, September 2012

Operando methodology: combination of in situ spectroscopy and simultaneous activity measurements under catalytic reaction conditions
journal, February 2005

High-energy phonon confinement in nanoscale metallic multilayers
journal, April 2008

Particle Size Effects in the Catalytic Electroreduction of CO ₂ on Cu Nanoparticles
journal, May 2014

Subnanometer Substructures in Nanoassemblies Formed from Clusters under a Reactive Atmosphere Revealed Using Machine Learning
journal, August 2018

Phonon Density of States Measured by Inelastic Nuclear Resonant Scattering
journal, May 1995

Kern-Schale-Nanokatalysatoren durch adsorbatinduzierte Oberflächensegregation
journal, April 2009

Circularly polarized light detection with hot electrons in chiral plasmonic metamaterials
journal, September 2015

Identification of carbon-encapsulated iron nanoparticles as active species in non-precious metal oxygen reduction catalysts
journal, August 2016

The surface energy of metals
journal, August 1998

Developments in operando studies and in situ characterization of heterogeneous catalysts
journal, May 2003

Extended X-ray Absorption Fine Structure (EXAFS) Studies of Hydroxo(oxo)iron Aggregates and Minerals, and a Critique of their Use as Models for Ferritin
journal, June 1996

Size-dependent evolution of the atomic vibrational density of states and thermodynamic properties of isolated Fe nanoparticles
journal, October 2012

Silver clusters shape determination from in-situ XANES data
journal, November 2018

Understanding heterogeneous electrocatalytic carbon dioxide reduction through operando techniques
journal, December 2018

Operando Evolution of the Structure and Oxidation State of Size-Controlled Zn Nanoparticles during CO ₂ Electroreduction
journal, July 2018

Electrochemical Reduction of CO ₂ Catalyzed by Fe-N-C Materials: A Structure–Selectivity Study
journal, January 2017

The interaction of Cu(100)Fe surfaces with oxygen studied by X-ray photoelectron spectroscopy
journal, October 1994

Nuclear resonant spectroscopy
journal, January 2004

Determining the active site in a catalytic process: Operando spectroscopy is more than a buzzword
journal, January 2003