Structure of Nano-sized CeO2 Materials: Combined Scattering and Spectroscopic Investigations

Marchbank, Huw R.; Clark, Adam H.; Hyde, Timothy I.; Playford, Helen Y.; Tucker, Matthew G.; Thompsett, David; Fisher, Janet M.; Chapman, Karena W.; Beyer, Kevin A.; Monte, Manuel; Longo, Alessandro; Sankar, Gopinathan

doi:10.1002/cphc.201600697

Title: Structure of Nano-sized CeO₂ Materials: Combined Scattering and Spectroscopic Investigations

Abstract

Here, the nature of nano-sized ceria, CeO₂, systems were investigated using neutron and X-ray diffraction and X-ray absorption spectroscopy. Whilst both diffraction andtotal pair distribution functions (PDFs) revealed that in all the samples the occupancy of both Ce⁴⁺ and O^2- are very close to the ideal stoichiometry, the analysis using reverse Monte Carlo technique revealedsignificant disorder around oxygen atoms in the nano sized ceria samples in comparison to the highly crystalline NIST standard.In addition, the analysis reveal that the main differences observed in the pair correlations from various X-ray and neutron diffraction techniques were attributed to the particle size of the CeO₂ prepared by the reported three methods. Furthermore, detailed analysis of the Ce L_3– and K-edge EXAFS data support this finding; in particular the decrease in higher shell coordination numbers with respect to the NIST standard, are attributed to differences in particle size.

Authors:

Marchbank, Huw R. ^[1]; Clark, Adam H. ^[1]; Hyde, Timothy I. ^[2]; Playford, Helen Y. ^[3]; Tucker, Matthew G. ^[4]; Thompsett, David ^[2]; Fisher, Janet M. ^[2]; Chapman, Karena W. ^[5]; Beyer, Kevin A. ^[5]; Monte, Manuel ^[6]; Longo, Alessandro ^[7]; Sankar, Gopinathan ^[1]

Univ. College London, London (United Kingdom)
Johnson Matthey Technology Centre, Reading (United Kingdom)
Rutherford Appleton Laboratory, Oxon (United Kingdom)
Rutherford Appleton Laboratory, Oxon (United Kingdom); Diamond Light Source, Oxon (United Kingdom); Spallation Neutron Source, Oak Ridge, TN (United States)
Argonne National Lab. (ANL), Argonne, IL (United States)
ESRF-The European Synchrotron, Grenoble, Cedex 9 (France)
ESRF-The European Synchrotron, Grenoble, Cedex 9 (France); Istituto per lo Studio dei Materiali Nanostrutturati, Palermo (Italy)

Publication Date:: Mon Aug 29 00:00:00 EDT 2016

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

Sponsoring Org.:: Argonne National Laboratory, Advanced Photon Source; Engineering and Physical Sciences Research Council (EPSRC); USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22), Scientific User Facilities Division

OSTI Identifier:: 1373885

Grant/Contract Number:: AC02-06CH11357

Resource Type:: Accepted Manuscript

Journal Name:: ChemPhysChem

Additional Journal Information:: Journal Volume: 17; Journal Issue: 21; Journal ID: ISSN 1439-4235

Publisher:: ChemPubSoc Europe

Country of Publication:: United States

Language:: English

Subject:: 36 MATERIALS SCIENCE; 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; ceria; EXAFS; pair distribution functions; Reverse Monte Carlo; Rietveld analysis

Citation Formats


                    Marchbank, Huw R., Clark, Adam H., Hyde, Timothy I., Playford, Helen Y., Tucker, Matthew G., Thompsett, David, Fisher, Janet M., Chapman, Karena W., Beyer, Kevin A., Monte, Manuel, Longo, Alessandro, and Sankar, Gopinathan. Structure of Nano-sized CeO2 Materials: Combined Scattering and Spectroscopic Investigations.  United States: N. p., 2016. 
Web.  doi:10.1002/cphc.201600697.

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                    Marchbank, Huw R., Clark, Adam H., Hyde, Timothy I., Playford, Helen Y., Tucker, Matthew G., Thompsett, David, Fisher, Janet M., Chapman, Karena W., Beyer, Kevin A., Monte, Manuel, Longo, Alessandro, & Sankar, Gopinathan. Structure of Nano-sized CeO2 Materials: Combined Scattering and Spectroscopic Investigations.  United States.  https://doi.org/10.1002/cphc.201600697

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                    Marchbank, Huw R., Clark, Adam H., Hyde, Timothy I., Playford, Helen Y., Tucker, Matthew G., Thompsett, David, Fisher, Janet M., Chapman, Karena W., Beyer, Kevin A., Monte, Manuel, Longo, Alessandro, and Sankar, Gopinathan. Mon .  
"Structure of Nano-sized CeO2 Materials: Combined Scattering and Spectroscopic Investigations".  United States.  https://doi.org/10.1002/cphc.201600697.  https://www.osti.gov/servlets/purl/1373885.

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@article{osti_1373885,

  title        = {Structure of Nano-sized CeO2 Materials: Combined Scattering and Spectroscopic Investigations},

  author       = {Marchbank, Huw R. and Clark, Adam H. and Hyde, Timothy I. and Playford, Helen Y. and Tucker, Matthew G. and Thompsett, David and Fisher, Janet M. and Chapman, Karena W. and Beyer, Kevin A. and Monte, Manuel and Longo, Alessandro and Sankar, Gopinathan},

  abstractNote = {Here, the nature of nano-sized ceria, CeO2, systems were investigated using neutron and X-ray diffraction and X-ray absorption spectroscopy. Whilst both diffraction andtotal pair distribution functions (PDFs) revealed that in all the samples the occupancy of both Ce4+ and O2- are very close to the ideal stoichiometry, the analysis using reverse Monte Carlo technique revealedsignificant disorder around oxygen atoms in the nano sized ceria samples in comparison to the highly crystalline NIST standard.In addition, the analysis reveal that the main differences observed in the pair correlations from various X-ray and neutron diffraction techniques were attributed to the particle size of the CeO2 prepared by the reported three methods. Furthermore, detailed analysis of the Ce L3– and K-edge EXAFS data support this finding; in particular the decrease in higher shell coordination numbers with respect to the NIST standard, are attributed to differences in particle size.},

  doi          = {10.1002/cphc.201600697},

  journal      = {ChemPhysChem},

  number       = 21,

  volume       = 17,

  place        = {United States},

  year         = {Mon Aug 29 00:00:00 EDT 2016},

  month        = {Mon Aug 29 00:00:00 EDT 2016}

}

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Title: Structure of Nano-sized CeO2 Materials: Combined Scattering and Spectroscopic Investigations

Abstract

Citation Formats

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

Automobile exhaust catalysts journal, November 2001

Mantid—Data analysis and visualization package for neutron scattering and μ SR experiments journal, November 2014

Methane partial oxidation on Pt/CeO2–ZrO2 in the absence of gaseous oxygen journal, February 2000

EXPGUI , a graphical user interface for GSAS journal, April 2001

Catalytic Abatement of Water Pollutants journal, February 1998

Structural defects in a nano-scale powder of CeO 2 studied by pulsed neutron diffraction journal, August 2000

EXAFS analysis of the L 3 edge of Ce in CeO 2 : effects of multi-electron excitations and final-state mixed valence journal, January 1999

Defect structures in doped CeO2 studied by using XAFS spectrometry journal, November 2000

Crystal-structure effects in the Ce L 3 -edge x-ray-absorption spectrum of CeO 2 : Multiple-scattering resonances and many-body final states journal, August 1994

Implementation of a combined SAXS/WAXS/QEXAFS set-up for time-resolved in situ experiments journal, October 2008

RMCProfile: reverse Monte Carlo for polycrystalline materials journal, July 2007

Neutron scattering lengths and cross sections journal, January 1992

Influence of double-electron transitions on the EXAFS L edges of rare-earth systems journal, May 1994

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Title: Structure of Nano-sized CeO₂ Materials: Combined Scattering and Spectroscopic Investigations

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

Automobile exhaust catalysts
journal, November 2001

Mantid—Data analysis and visualization package for neutron scattering and $μ$ SR experiments
journal, November 2014

Methane partial oxidation on Pt/CeO2–ZrO2 in the absence of gaseous oxygen
journal, February 2000

EXPGUI , a graphical user interface for GSAS
journal, April 2001

Catalytic Abatement of Water Pollutants
journal, February 1998

Structural defects in a nano-scale powder of CeO 2 studied by pulsed neutron diffraction
journal, August 2000

EXAFS analysis of the L ₃ edge of Ce in CeO ₂ : effects of multi-electron excitations and final-state mixed valence
journal, January 1999

Defect structures in doped CeO2 studied by using XAFS spectrometry
journal, November 2000

Crystal-structure effects in the Ce $L_{3}$ -edge x-ray-absorption spectrum of ${CeO}_{2}$ : Multiple-scattering resonances and many-body final states
journal, August 1994

Implementation of a combined SAXS/WAXS/QEXAFS set-up for time-resolved in situ experiments
journal, October 2008

RMCProfile: reverse Monte Carlo for polycrystalline materials
journal, July 2007

Neutron scattering lengths and cross sections
journal, January 1992

Influence of double-electron transitions on the EXAFS L edges of rare-earth systems
journal, May 1994

A profile refinement method for nuclear and magnetic structures
journal, June 1969

Polyhedral CeO ₂ Nanoparticles: Size-Dependent Geometrical and Electronic Structure
journal, March 2012

Catalytic converters: state of the art and perspectives
journal, July 1999

The Polaris powder diffractometer at ISIS
journal, June 1992

The time-resolved and extreme conditions XAS (TEXAS) facility at the European Synchrotron Radiation Facility: the general-purpose EXAFS bending-magnet beamline BM23
journal, October 2015

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

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journal, January 2003