New Insights into the Bulk and Surface Defect Structures of Ceria Nanocrystals from Neutron Scattering Study

Luo, Si; Li, Meijun; Fung, Victor; Sumpter, Bobby; Liu, Jue; Wu, Zili; Page, Katharine

doi:10.1021/acs.chemmater.1c00156

Title: New Insights into the Bulk and Surface Defect Structures of Ceria Nanocrystals from Neutron Scattering Study

Abstract

Neutron diffraction and pair distribution function studies coupled with Raman spectroscopy have successfully unraveled the detailed oxygen defect structures of ceria nanocubes and nanorods. Two types of defect sites are revealed for the ceria nanocrystals: surface and bulk defects. It is proposed that the surface oxygen defects in both types of CeO₂ nanocrystals are predominantly the partially reduced Ce₃O_5+x, with the bulk defect structures dominated by interstitial Frenkel-type oxygen vacancies. Ceria nanorods possess much higher concentration of surface oxygen defects relative to the nanocubes, albeit with only slightly higher concentration of bulk Frenkel-type oxygen vacancies. Upon annealing the nanorod sample at 600 °C under vacuum (~10^–4 to 10^–5 mbar), a partially reduced ceria phase with long-range oxygen vacancy ordering (Ce₃O_5+x) has been observed experimentally for the first time. This intriguing observation that surface defect phases can take on ordered defect sublattices under certain conditions is of great value in understanding the temperature-dependent catalytic performance of ceria nanocrystals. Furthermore, a drastic decrease of the surface vacancies in the ceria nanocrystals is observed upon exposure to SO₂, especially for the nanorods, a likely origin for the sulfur poisoning effect on ceria-based materials. This study suggests that tailoring surface morphology is a promisingmore »« less

Authors:

^[1];

^[2];

^[3];

^[4];

^[1];

^[5]

Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Sciences (CNMS); Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Sciences (CNMS)
Univ. of Tennessee, Knoxville, TN (United States); Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Univ. of Tennessee, Knoxville, TN (United States)

Publication Date:: Thu May 27 00:00:00 EDT 2021

Research Org.:: Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

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

OSTI Identifier:: 1797634

Grant/Contract Number:: AC05-00OR22725

Resource Type:: Accepted Manuscript

Journal Name:: Chemistry of Materials

Additional Journal Information:: Journal Volume: 33; Journal Issue: 11; Journal ID: ISSN 0897-4756

Publisher:: American Chemical Society (ACS)

Country of Publication:: United States

Language:: English

Subject:: 36 MATERIALS SCIENCE; oxides; nanocubes; oxygen; defects; nanorods

Citation Formats


                    Luo, Si, Li, Meijun, Fung, Victor, Sumpter, Bobby, Liu, Jue, Wu, Zili, and Page, Katharine. New Insights into the Bulk and Surface Defect Structures of Ceria Nanocrystals from Neutron Scattering Study.  United States: N. p., 2021. 
Web.  doi:10.1021/acs.chemmater.1c00156.

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                    Luo, Si, Li, Meijun, Fung, Victor, Sumpter, Bobby, Liu, Jue, Wu, Zili, & Page, Katharine. New Insights into the Bulk and Surface Defect Structures of Ceria Nanocrystals from Neutron Scattering Study.  United States.  https://doi.org/10.1021/acs.chemmater.1c00156

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                    Luo, Si, Li, Meijun, Fung, Victor, Sumpter, Bobby, Liu, Jue, Wu, Zili, and Page, Katharine. Thu .  
"New Insights into the Bulk and Surface Defect Structures of Ceria Nanocrystals from Neutron Scattering Study".  United States.  https://doi.org/10.1021/acs.chemmater.1c00156.  https://www.osti.gov/servlets/purl/1797634.

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@article{osti_1797634,

  title        = {New Insights into the Bulk and Surface Defect Structures of Ceria Nanocrystals from Neutron Scattering Study},

  author       = {Luo, Si and Li, Meijun and Fung, Victor and Sumpter, Bobby and Liu, Jue and Wu, Zili and Page, Katharine},

  abstractNote = {Neutron diffraction and pair distribution function studies coupled with Raman spectroscopy have successfully unraveled the detailed oxygen defect structures of ceria nanocubes and nanorods. Two types of defect sites are revealed for the ceria nanocrystals: surface and bulk defects. It is proposed that the surface oxygen defects in both types of CeO2 nanocrystals are predominantly the partially reduced Ce3O5+x, with the bulk defect structures dominated by interstitial Frenkel-type oxygen vacancies. Ceria nanorods possess much higher concentration of surface oxygen defects relative to the nanocubes, albeit with only slightly higher concentration of bulk Frenkel-type oxygen vacancies. Upon annealing the nanorod sample at 600 °C under vacuum (~10–4 to 10–5 mbar), a partially reduced ceria phase with long-range oxygen vacancy ordering (Ce3O5+x) has been observed experimentally for the first time. This intriguing observation that surface defect phases can take on ordered defect sublattices under certain conditions is of great value in understanding the temperature-dependent catalytic performance of ceria nanocrystals. Furthermore, a drastic decrease of the surface vacancies in the ceria nanocrystals is observed upon exposure to SO2, especially for the nanorods, a likely origin for the sulfur poisoning effect on ceria-based materials. This study suggests that tailoring surface morphology is a promising strategy to control defect properties of ceria nanomaterials. It also provides fundamental insights to stabilize surface oxygen defects in CeO2 nanocrystals to achieve high redox performance under corrosive environments such as under SO2/SOx exposure.},

  doi          = {10.1021/acs.chemmater.1c00156},

  journal      = {Chemistry of Materials},

  number       = 11,

  volume       = 33,

  place        = {United States},

  year         = {Thu May 27 00:00:00 EDT 2021},

  month        = {Thu May 27 00:00:00 EDT 2021}

}

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Title: New Insights into the Bulk and Surface Defect Structures of Ceria Nanocrystals from Neutron Scattering Study

Abstract

Citation Formats

Extra-Low-Temperature Oxygen Storage Capacity of CeO 2 Nanocrystals with Cubic Facets journal, February 2011

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Raman Spectroscopy of nanomaterials: How spectra relate to disorder, particle size and mechanical properties
journal, March 2007

Promotional effect of potassium on soot oxidation activity and SO2-poisoning resistance of Cu/CeO2 catalyst
journal, May 2008

Lattice Oxygen Activity in Pr- and La-Doped CeO ₂ for Low-Temperature Soot Oxidation
journal, December 2013

Evaluation of regeneration of spent three-way catalysts for catalytic oxidation of aromatic hydrocarbons
journal, April 2011

Fundamental Understanding of the Interaction of Acid Gases with CeO ₂ : From Surface Science to Practical Catalysis
journal, March 2016

Defect-Site Promoted Surface Reorganization in Nanocrystalline Ceria for the Low-Temperature Activation of Ethylbenzene
journal, March 2007

Shape-Selective Synthesis and Oxygen Storage Behavior of Ceria Nanopolyhedra, Nanorods, and Nanocubes
journal, December 2005

Renewable Hydrogen from Ethanol by Autothermal Reforming
journal, February 2004

Structural Characterization of CeO ₂ −MO ₂ (M = Si ⁴⁺ , Ti ⁴⁺ , and Zr ⁴⁺ ) Mixed Oxides by Raman Spectroscopy, X-ray Photoelectron Spectroscopy, and Other Techniques
journal, October 2003

Surface-structure sensitivity of CO oxidation over polycrystalline ceria powders
journal, August 2005

Stabilized Gold Nanoparticles on Ceria Nanorods by Strong Interfacial Anchoring
journal, December 2012

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

Surface Stabilizes Ceria in Unexpected Stoichiometry
journal, March 2017

Defective structure, oxygen mobility, oxygen storage capacity, and redox properties of RE-based (RE = Ce, Pr) solid solutions
journal, July 2004

Template-Free Hydrothermal Synthesis of CeO ₂ Nano-octahedrons and Nanorods: Investigation of the Morphology Evolution
journal, May 2008

Identifying Defects in Ceria-Based Nanocrystals by UV Resonance Raman Spectroscopy
journal, October 2009

SO ₂ Poisoning Structures and the Effects on Pure and Mn Doped CeO ₂ : A First Principles Investigation
journal, October 2012

Lattice Defects and Oxygen Storage Capacity of Nanocrystalline Ceria and Ceria-Zirconia
journal, November 2000

Oxygen Defects and Surface Chemistry of Ceria: Quantum Chemical Studies Compared to Experiment
journal, December 2012

The Structures of C–Ce2O3+δ, Ce7O12, and Ce11O20
journal, November 1999

Electron Localization Determines Defect Formation on Ceria Substrates
journal, July 2005

Improved activity and significant SO2 tolerance of samarium modified CeO2-TiO2 catalyst for NO selective catalytic reduction with NH3
journal, May 2019

Ceria Catalysts at Nanoscale: How Do Crystal Shapes Shape Catalysis?
journal, June 2017

Surface-dependent oxidation of H 2 on CeO 2 surfaces
journal, January 2013

Effects of platinum and palladium impregnation on the performance and durability of automobile exhaust oxidizing catalysts
journal, February 1978

Fundamentals and Catalytic Applications of CeO ₂ -Based Materials
journal, April 2016

Probing Defect Sites on CeO ₂ Nanocrystals with Well-Defined Surface Planes by Raman Spectroscopy and O ₂ Adsorption ^†
journal, November 2010

Oxygen Vacancy Clusters Promoting Reducibility and Activity of Ceria Nanorods
journal, March 2009

A review on oxygen storage capacity of CeO2-based materials: Influence factors, measurement techniques, and applications in reactions related to catalytic automotive emissions control
journal, May 2019

Dopant-Induced Modification of Active Site Structure and Surface Bonding Mode for High-Performance Nanocatalysts: CO Oxidation on Capping-free (110)-oriented CeO ₂ :Ln (Ln = La–Lu) Nanowires
journal, September 2013