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.