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Versailles Project on Advanced Materials and Standards Interlaboratory Study on Measuring the Thickness and Chemistry of Nanoparticle Coatings Using XPS and LEIS

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National Physical Laboratory, Teddington, Middlesex TW11 0LW, U.K.
Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMETRO), Divisão de Metrologia de Materiais (Dimat) Avenida Nossa Senhora das Graças, 50 Duque de Caxias, RJ 25250-020, Brazil
§ Tascon GmbH, Mendelstr. 17, D-48149 Münster, Germany
ION-TOF GmbH, Heisenbergstr. 15, 48149 Münster, Germany
National ESCA and Surface Analysis Center for Biomedical Problems, Departments of Bioengineering and Chemical Engineering, University of Washington, Seattle, Washington 98195-1653, United States
# European Commission, Directorate General Joint Research Centre, Directorate F – Health, Consumers and Reference Materials, Consumer Products Safety Unit, Via E. Fermi 2749 TP125 I21027 Ispra (VA), Italy
Kratos Analytical Ltd., Wharfside, Trafford Wharf Road, Manchester M17 1GP, U.K.
BAM Federal Institute for Materials Research and Testing (BAM 6.1), Unter den Eichen 44-46, D-12203 Berlin, Germany
Pacific Northwest National Laboratory, EMSL, Richland, Washington 99352, United States
Department of Materials, Imperial College London, South Kensington Campus, London SW7 2AZ, U.K.
Korea Research Institute of Standards and Science, 267 Gajeong-ro, Daejeon 34113, Korea
Instituto Politécnico Nacional, Centro de Nanociencias y Micro y Nanotecnologías, UPALM, Zacatenco, México D.F. CP. 07738, México
Surface Analysis Facility, Lehigh University, 7 Asa Drive, Bethlehem, Pennsylvania 18015, United States
Thermo Fisher Scientific, Unit 24, The Birches Industrial Estate, Imberhorne Lane, East Grinstead, West Sussex, RH19 1UB, U.K.
Institut fuer Angewandte Physik, TU Vienna, Wiedner Hauptstr 8-10, A 1040 Vienna, Austria
Nanoscale and Microscale Research Centre, School of Chemistry, University of Nottingham, University Park, Nottingham NG7 2RD, U.K.
× Industrial Focus Group XUV Optics, MESA+ Institute for Nanotechnology, University of Twente, P.O. Box 217, 7500 AE Enschede, The Netherlands
ζ School of Materials and Photon Science Institute, University of Manchester, Manchester M13 9PL, U.K.
National Institute of Metrology, Beijing 100029, P. R. China
Department of Chemistry, Xi’an-Jiaotong Liverpool University, Suzhou, China
*E-mail: [email protected]. Tel.: +44 20 8943 6193.
Cite this: J. Phys. Chem. C 2016, 120, 42, 24070–24079
Publication Date (Web):September 13, 2016
https://doi.org/10.1021/acs.jpcc.6b06713
Copyright © 2016 American Chemical Society

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    Abstract

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    We report the results of a Versailles Project on Advanced Materials and Standards (VAMAS) interlaboratory study on the measurement of the shell thickness and chemistry of nanoparticle coatings. Peptide-coated gold particles were supplied to laboratories in two forms: a colloidal suspension in pure water and particles dried onto a silicon wafer. Participants prepared and analyzed these samples using either X-ray photoelectron spectroscopy (XPS) or low energy ion scattering (LEIS). Careful data analysis revealed some significant sources of discrepancy, particularly for XPS. Degradation during transportation, storage, or sample preparation resulted in a variability in thickness of 53%. The calculation method chosen by XPS participants contributed a variability of 67%. However, variability of 12% was achieved for the samples deposited using a single method and by choosing photoelectron peaks that were not adversely affected by instrumental transmission effects. The study identified a need for more consistency in instrumental transmission functions and relative sensitivity factors since this contributed a variability of 33%. The results from the LEIS participants were more consistent, with variability of less than 10% in thickness, and this is mostly due to a common method of data analysis. The calculation was performed using a model developed for uniform, flat films, and some participants employed a correction factor to account for the sample geometry, which appears warranted based upon a simulation of LEIS data from one of the participants and comparison to the XPS results.

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    The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.jpcc.6b06713.

    • Protocol for sample preparation circulated to study participants; calculation of nanoparticle shell thickness by XPS using the TNP equation; supplementary figures include an example XPS C 1s narrow scan and photographs of type B samples deposited by participants (PDF)

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