Facet-dependent active sites of a single Cu2O particle photocatalyst for CO2 reduction to methanol

Wu, Yimin A.; McNulty, Ian; Liu, Cong; Lau, Kah Chun; Liu, Qi; Paulikas, Arvydas P.; Sun, Cheng-Jun; Cai, Zhonghou; Guest, Jeffrey R.; Ren, Yang; Stamenkovic, Vojislav; Curtiss, Larry A.; Liu, Yuzi; Rajh, Tijana

doi:10.1038/s41560-019-0490-3

Title: Facet-dependent active sites of a single Cu₂O particle photocatalyst for CO₂ reduction to methanol

Abstract

Atomic level understanding of the active sites and transformation mechanisms under realistic working conditions are pre-requisites for rational design of high performance photocatalysts. By using correlated scanning fluorescence x-ray microscopy and environmental transmission electron microscopy at atmospheric pressure, in operando, we directly observed that the (110) facet of a single Cu₂O photocatalyst particle is photocatalytically active for CO₂ reduction to methanol while the (100) facet is inert. The oxidation state of the active sites changed from Cu(I) towards Cu(II) due to CO₂ and H₂O coadsorption and changed back to Cu+ after CO₂ conversion under visible light illumination. The Cu₂O photocatalyst oxidized water as it reduced CO₂. At the same time, the crystal lattice expanded due to CO₂ adsorption then reverted after CO₂ conversion. The internal quantum yield for unassisted wireless photocatalytic reduction of CO₂ to methanol using Cu₂O crystals is ~ 72% with 10% solar to fuel efficiency.

Authors:

Wu, Yimin A. ^[1]; McNulty, Ian ^[2];

^[3]; Lau, Kah Chun ^[4]; Liu, Qi ^[5]; Paulikas, Arvydas P. ^[6]; Sun, Cheng-Jun ^[7]; Cai, Zhonghou ^[7]; Guest, Jeffrey R. ^[2]; Ren, Yang ^[7]; Stamenkovic, Vojislav ^[6]; Curtiss, Larry A. ^[6];

^[2];

^[2]

Argonne National Lab. (ANL), Argonne, IL (United States); Univ. of Waterloo, ON (Canada)
Argonne National Lab. (ANL), Argonne, IL (United States)
Argonne National Lab. (ANL), Argonne, IL (United States). Chemical Sciences and Engineering Division
Argonne National Lab. (ANL), Argonne, IL (United States). Materials Science Division; Univ. of California, Northridge, CA (United States). Dept. of Physics and Astronomy
Hong Kong Univ. (Hong Kong). Dept. of Physics
Argonne National Lab. (ANL), Argonne, IL (United States). Materials Science Division
Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS)

Publication Date:: 2019-11-22

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

Sponsoring Org.:: USDOE Laboratory Directed Research and Development (LDRD) Program; USDOE Office of Science (SC), Basic Energy Sciences (BES)

OSTI Identifier:: 1600936

Grant/Contract Number:: AC02-06CH11357

Resource Type:: Accepted Manuscript

Journal Name:: Nature Energy

Additional Journal Information:: Journal Volume: 4; Journal Issue: 11; Journal ID: ISSN 2058-7546

Publisher:: Nature Publishing Group

Country of Publication:: United States

Language:: English

Subject:: 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; carbon dioxide reduction; methanol; active sites; cuprous oxide; X-ray nanoprobe; electron microscopy; EPR

Citation Formats


                    Wu, Yimin A., McNulty, Ian, Liu, Cong, Lau, Kah Chun, Liu, Qi, Paulikas, Arvydas P., Sun, Cheng-Jun, Cai, Zhonghou, Guest, Jeffrey R., Ren, Yang, Stamenkovic, Vojislav, Curtiss, Larry A., Liu, Yuzi, and Rajh, Tijana. Facet-dependent active sites of a single Cu2O particle photocatalyst for CO2 reduction to methanol.  United States: N. p., 2019. 
        Web.  doi:10.1038/s41560-019-0490-3.

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                    Wu, Yimin A., McNulty, Ian, Liu, Cong, Lau, Kah Chun, Liu, Qi, Paulikas, Arvydas P., Sun, Cheng-Jun, Cai, Zhonghou, Guest, Jeffrey R., Ren, Yang, Stamenkovic, Vojislav, Curtiss, Larry A., Liu, Yuzi, & Rajh, Tijana. Facet-dependent active sites of a single Cu2O particle photocatalyst for CO2 reduction to methanol.  United States.  doi:https://doi.org/10.1038/s41560-019-0490-3

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                    Wu, Yimin A., McNulty, Ian, Liu, Cong, Lau, Kah Chun, Liu, Qi, Paulikas, Arvydas P., Sun, Cheng-Jun, Cai, Zhonghou, Guest, Jeffrey R., Ren, Yang, Stamenkovic, Vojislav, Curtiss, Larry A., Liu, Yuzi, and Rajh, Tijana. Fri .  
        "Facet-dependent active sites of a single Cu2O particle photocatalyst for CO2 reduction to methanol".  United States.  doi:https://doi.org/10.1038/s41560-019-0490-3.  https://www.osti.gov/servlets/purl/1600936.

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@article{osti_1600936,

  title        = {Facet-dependent active sites of a single Cu2O particle photocatalyst for CO2 reduction to methanol},

  author       = {Wu, Yimin A. and McNulty, Ian and Liu, Cong and Lau, Kah Chun and Liu, Qi and Paulikas, Arvydas P. and Sun, Cheng-Jun and Cai, Zhonghou and Guest, Jeffrey R. and Ren, Yang and Stamenkovic, Vojislav and Curtiss, Larry A. and Liu, Yuzi and Rajh, Tijana},

  abstractNote = {Atomic level understanding of the active sites and transformation mechanisms under realistic working conditions are pre-requisites for rational design of high performance photocatalysts. By using correlated scanning fluorescence x-ray microscopy and environmental transmission electron microscopy at atmospheric pressure, in operando, we directly observed that the (110) facet of a single Cu2O photocatalyst particle is photocatalytically active for CO2 reduction to methanol while the (100) facet is inert. The oxidation state of the active sites changed from Cu(I) towards Cu(II) due to CO2 and H2O coadsorption and changed back to Cu+ after CO2 conversion under visible light illumination. The Cu2O photocatalyst oxidized water as it reduced CO2. At the same time, the crystal lattice expanded due to CO2 adsorption then reverted after CO2 conversion. The internal quantum yield for unassisted wireless photocatalytic reduction of CO2 to methanol using Cu2O crystals is ~ 72% with 10% solar to fuel efficiency.},

  doi          = {10.1038/s41560-019-0490-3},

  journal      = {Nature Energy},

  number       = 11,

  volume       = 4,

  place        = {United States},

  year         = {2019},

  month        = {11}

}

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DOI: https://doi.org/10.1038/s41560-019-0490-3

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Mechanistic Study of CO ₂ Photoreduction with H ₂ O on Cu/TiO ₂ Nanocomposites by in Situ X-ray Absorption and Infrared Spectroscopies

Journal Article Liu, Lianjun ; Zhao, Cunyu ; Miller, Jeffrey T. ; ... - Journal of Physical Chemistry. C

Cu/TiO2 composites are extensively studied for photocatalytic reduction of CO2 with H2O, but the roles of Cu species (Cu2+, Cu+, or Cu0) is not well understood, and the photocatalyst deactivation mechanism is seldom addressed. In this work, we have employed in situ techniques, i.e., X-ray absorption spectroscopy (XAS) and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), to explore the surface chemistry of Cu/TiO2 composites under CO2 photoreduction environment. We found that the air-calcined Cu/TiO2 (Cu/Ti(air)) surface was dominated by isolated Cu2+ sites, while the one post-treated with H2 at 200 °C (Cu/Ti(H2)) was rich in Cu+ and oxygen vacancy (VO).more »« less
DOI: https://doi.org/10.1021/acs.jpcc.6b10835

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CO2 Reduction at Low Overpotential on Cu Electrodes Resulting from the Reduction of Thick Cu2O Films journal, April 2012

Highly active oxide photocathode for photoelectrochemical water reduction journal, May 2011

New Developments in Transmission Electron Microscopy for Nanotechnology journal, September 2003

Generalized Gradient Approximation Made Simple journal, October 1996

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Glossary of terms used in photocatalysis and radiation catalysis (IUPAC Recommendations 2011) journal, March 2011

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Conversion of CO 2 from Air into Methanol Using a Polyamine and a Homogeneous Ruthenium Catalyst journal, January 2016

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Nanowire–Bacteria Hybrids for Unassisted Solar Carbon Dioxide Fixation to Value-Added Chemicals journal, April 2015

Theory-driven design of high-valence metal sites for water oxidation confirmed using in situ soft X-ray absorption journal, November 2017

From ultrasoft pseudopotentials to the projector augmented-wave method journal, January 1999

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Carbon Dioxide Conversion to Methanol over Size-Selected Cu 4 Clusters at Low Pressures journal, July 2015

Surface Modification of Small Particle TiO 2 Colloids with Cysteine for Enhanced Photochemical Reduction: An EPR Study † journal, January 1996

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Tailoring Copper Nanocrystals towards C 2 Products in Electrochemical CO 2 Reduction journal, April 2016

Recent advances in hybrid photocatalysts for solar fuel production journal, January 2012

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Photocatalysis for Hydrogen Production and CO 2 Reduction: The Case of Copper‐Catalysts journal, September 2018

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Asymmetric copper-catalyzed C-N cross-couplings induced by visible light journal, February 2016

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First turnover analysis of water-oxidation catalyzed by Co-oxide nanoparticles journal, January 2015

Artificial Z-Scheme Constructed with a Supramolecular Metal Complex and Semiconductor for the Photocatalytic Reduction of CO 2 journal, March 2013

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Computational studies of electrochemical CO 2 reduction on subnanometer transition metal clusters journal, January 2014

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Title: Facet-dependent active sites of a single Cu₂O particle photocatalyst for CO₂ reduction to methanol

The importance of surface morphology in controlling the selectivity of polycrystalline copper for CO2 electroreduction
journal, January 2012

CO₂ Reduction at Low Overpotential on Cu Electrodes Resulting from the Reduction of Thick Cu₂O Films
journal, April 2012

Highly active oxide photocathode for photoelectrochemical water reduction
journal, May 2011

New Developments in Transmission Electron Microscopy for Nanotechnology
journal, September 2003

Generalized Gradient Approximation Made Simple
journal, October 1996

Cu ₂ O/Reduced Graphene Oxide Composites for the Photocatalytic Conversion of CO ₂
journal, February 2014

Glossary of terms used in photocatalysis and radiation catalysis (IUPAC Recommendations 2011)
journal, March 2011

Challenges and Prospects in Solar Water Splitting and CO ₂ Reduction with Inorganic and Hybrid Nanostructures
journal, March 2018

Nanostructured transition metal dichalcogenide electrocatalysts for CO ₂ reduction in ionic liquid
journal, July 2016

Conversion of CO ₂ from Air into Methanol Using a Polyamine and a Homogeneous Ruthenium Catalyst
journal, January 2016

Projector augmented-wave method
journal, December 1994

Electroreduction of carbon monoxide to liquid fuel on oxide-derived nanocrystalline copper
journal, April 2014

Conduction-electron g factors in the noble metals
journal, May 1989

Nanowire–Bacteria Hybrids for Unassisted Solar Carbon Dioxide Fixation to Value-Added Chemicals
journal, April 2015

Theory-driven design of high-valence metal sites for water oxidation confirmed using in situ soft X-ray absorption
journal, November 2017

From ultrasoft pseudopotentials to the projector augmented-wave method
journal, January 1999

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

Electron beam damage in oxides: a review
journal, December 2015

Morphology-Dependent Interactions of ZnO with Cu Nanoparticles at the Materials’ Interface in Selective Hydrogenation of CO2 to CH3OH
journal, January 2011

A hard X-ray nanoprobe beamline for nanoscale microscopy
journal, September 2012

Visualizing Gas Molecules Interacting with Supported Nanoparticulate Catalysts at Reaction Conditions
journal, January 2012

Differential stress induced by thiol adsorption on facetted nanocrystals
journal, September 2011

Controlled synthesis of concave Cu ₂ O microcrystals enclosed by {hhl} high-index facets and enhanced catalytic activity
journal, January 2013

Chemical actinometry (IUPAC Technical Report)
journal, January 2004

Copper in Photocatalysis
journal, July 2014

Electrodeposition of Cu[sub 2]O: An Excellent Method for Obtaining Films of Controlled Morphology and Good Performance in Li-Ion Batteries
journal, January 2005

A density functional theory study of the adsorption behaviour of CO ₂ on Cu ₂ O surfaces
journal, July 2016

Partially oxidized atomic cobalt layers for carbon dioxide electroreduction to liquid fuel
journal, January 2016

A Simple Two-Step Electrodeposition of Cu ₂ O/ZnO Nanopillar Solar Cells
journal, March 2010

Artificial Photosynthesis on TiO ₂ -Passivated InP Nanopillars
journal, August 2015

Metal-free efficient photocatalyst for stable visible water splitting via a two-electron pathway
journal, February 2015

Activating lattice oxygen redox reactions in metal oxides to catalyse oxygen evolution
journal, January 2017

High Selectivity for Ethylene from Carbon Dioxide Reduction over Copper Nanocube Electrocatalysts
journal, February 2015

Thermodynamic and achievable efficiencies for solar-driven electrochemical reduction of carbon dioxide to transportation fuels
journal, October 2015

Electrocatalytic CO2 Conversion to Oxalate by a Copper Complex
journal, January 2010

Controllable proton and CO2 photoreduction over Cu2O with various morphologies
journal, September 2013

Efficiency of ab-initio total energy calculations for metals and semiconductors using a plane-wave basis set
journal, July 1996

First-Principles Predictions of the Structure, Stability, and Photocatalytic Potential of Cu ₂ O Surfaces
journal, September 2013

Carbon Dioxide Fixation into Chemicals (Methyl Formate) at High Yields by Surface Coupling over a Pd/Cu/ZnO Nanocatalyst
journal, May 2007

Highly active copper-ceria and copper-ceria-titania catalysts for methanol synthesis from CO2
journal, July 2014

A generalized method for high throughput in-situ experiment data analysis: An example of battery materials exploration
journal, April 2015

Pd@TiO ₂ /carbon nanohorn electrocatalysts: reversible CO ₂ hydrogenation to formic acid
journal, January 2018

Visualizing Redox Dynamics of a Single Ag/AgCl Heterogeneous Nanocatalyst at Atomic Resolution
journal, February 2016

High-Selectivity Electrochemical Conversion of CO ₂ to Ethanol using a Copper Nanoparticle/N-Doped Graphene Electrode
journal, September 2016

Carbon Dioxide Conversion to Methanol over Size-Selected Cu ₄ Clusters at Low Pressures
journal, July 2015

Surface Modification of Small Particle TiO ₂ Colloids with Cysteine for Enhanced Photochemical Reduction: An EPR Study ^†
journal, January 1996

Co-ordination of copper(II) ions doped in pentacyanonitrosylferrate(2–) and tetrathiocyanatometallate(II) salts: an electron spin resonance study
journal, January 1975

Tailoring Copper Nanocrystals towards C ₂ Products in Electrochemical CO ₂ Reduction
journal, April 2016

Recent advances in hybrid photocatalysts for solar fuel production
journal, January 2012

Photoelectrochemical reduction of aqueous carbon dioxide on p-type gallium phosphide in liquid junction solar cells
journal, September 1978

Photocatalytic CO2 reduction with high turnover frequency and selectivity of formic acid formation using Ru(II) multinuclear complexes
journal, August 2012

Photocatalysis for Hydrogen Production and CO ₂ Reduction: The Case of Copper‐Catalysts
journal, September 2018

Artificial photosynthesis for solar fuels
journal, January 2012

Asymmetric copper-catalyzed C-N cross-couplings induced by visible light
journal, February 2016

Shape effects of cuprous oxide particles on stability in water and photocatalytic water splitting
journal, January 2015

Determination of the quantum yield of the ferrioxalate actinometer with electrically calibrated radiometers
journal, September 1981

First turnover analysis of water-oxidation catalyzed by Co-oxide nanoparticles
journal, January 2015

Artificial Z-Scheme Constructed with a Supramolecular Metal Complex and Semiconductor for the Photocatalytic Reduction of CO ₂
journal, March 2013

Water splitting–biosynthetic system with CO ₂ reduction efficiencies exceeding photosynthesis
journal, June 2016

Aqueous CO ₂ Reduction at Very Low Overpotential on Oxide-Derived Au Nanoparticles
journal, November 2012

High-Flux Solar-Driven Thermochemical Dissociation of CO2 and H2O Using Nonstoichiometric Ceria
journal, December 2010

Computational studies of electrochemical CO ₂ reduction on subnanometer transition metal clusters
journal, January 2014

Two-dimensional detector software: From real detector to idealised image or two-theta scan
journal, January 1996

High Selectivity for Ethylene from Carbon Dioxide Reduction over Copper Nanocube Electrocatalysts
journal, February 2015

Methanol-based acetoin production by genetically engineered Bacillus methanolicus
journal, January 2020