Final report on Key Comparison K67 and parallel Pilot Study P108: Measurement of composition of a thin Fe-Ni alloy film

CCQM K67 key comparison and P108 pilot study on quantitative analysis of alloy films has been completed in the Surface Analysis Working Group (SAWG) of the Consultative Committee for Amount of Substance (CCQM). The aim of this key comparison and pilot study is to compare the equivalence in the measurement capability of National Metrology Institutes (NMIs) and Designated Institutes (DIs) for the composition of thin alloy films expressed in atomic percent. In this study, a Fe-Ni alloy film with a certified composition was available to be used as a reference specimen to determine the relative sensitivity factors (RSFs) of Fe and Ni to improve the equivalence in the measurement of composition if required. The composition of the reference specimen was certified by inductively coupled plasma mass spectrometry (ICP-MS) with isotope dilution method. The in-depth and lateral homogeneities of composition were confirmed by secondary ion mass spectrometry (SIMS) using C-60 primary ions. Five laboratories participated in the key comparison as shown above. Four of the laboratories used x-ray photoelectron spectroscopy (XPS) and one laboratory used Auger electron spectroscopy (AES). One laboratory participated in the parallel P108 pilot study using electron probe micro analysis (EPMA) and XPS.