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

Journal Article · · Journal of Physical Chemistry. C
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  1. National Physical Lab. (United Kingdom)
  2. Instituto Nacional de Metrologia, Divisão de Metrologia de Materiais (Brazil)
  3. Tascon GmbH, Münster (Germany)
  4. ION-TOF GmbH, Münster (Germany)
  5. Univ. of Washington, Seattle, WA (United States)
  6. European Commission Joint Research Centre (Italy)
  7. Kratos Analytical Ltd., Manchester (United Kingdom)
  8. BAM Federal Institute for Materials Research and Testing (BAM 6.1), Berlin (Germany)
  9. Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
  10. Imperial College, London (United Kingdom)
  11. Korea Research Inst. of Standards and Science, Daejeon (Korea, Republic of)
  12. Inst. Politécnico Nacional, Zacatenco (México)
  13. Lehigh Univ., Bethlehem, PA (United States)
  14. Thermo Fisher Scientific (United Kingdom)
  15. Technical Univ. of Vienna (Austria)
  16. Univ. of Nottingham (United Kingdom). School of Chemistry
  17. Univ. of Twente, Enschede (Netherlands)
  18. Univ. of Manchester (United Kingdom)
  19. National Inst. of Metrology, Beijing (China)
  20. Xi’an-Jiaotong Liverpool Univ., Suzhou (China)

We report the results of a VAMAS (Versailles Project on Advanced Materials and Standards) inter-laboratory 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.

Research Organization:
Pacific Northwest National Laboratory (PNNL), Richland, WA (United States)
Sponsoring Organization:
USDOE
Grant/Contract Number:
AC05-76RL01830
OSTI ID:
1340750
Report Number(s):
PNNL-SA-121117; KP1704020
Journal Information:
Journal of Physical Chemistry. C, Vol. 120, Issue 42; ISSN 1932-7447
Publisher:
American Chemical SocietyCopyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 26 works
Citation information provided by
Web of Science

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Shell thickness determination for PTFE-PS core-shell nanoparticles using scanning transmission X-ray microscopy (STXM) journal May 2018
Importance of sample preparation on reliable surface characterisation of nano-objects: ISO standard 20579-4 journal July 2018
Intensity calibration for monochromated Al Kα XPS instruments using polyethylene journal March 2019
Provenance information as a tool for addressing engineered nanoparticle reproducibility challenges journal December 2016