Journal Article
CCQM pilot study CCQM-P140: quantitative surface analysis of multi-element alloy films
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Authors
Kyung Joong KIM, Jong Shik JANG, An Soon KIM, Jung Ki SUH, Yong-Duck CHUNG, Vasile-Dan Hodoroaba, Thomas Wirth, Wolfgang Unger, Hee Jae Kang, Oleg Popov, Inna Popov, Ilya Kuselman, Yeon Hee Lee, David E Sykes, Meiling Wang, Hai Wang, Toshiya Ogiwara, Mitsuaki Nishio, Shigeo Tanuma, David Simons, Christopher Szakal, William Osborn, Shinya Terauchi, Mika Ito, Akira Kurokawa, Toshiyuki Fujimoto, Werner Jordaan, Chil Seong Jeong, Rasmus Havelund, Steve Spencer, Alex Shard, Cornelia Streeck, Burkhard Beckhoff, Axel Eicke, Ralf Terborg
A pilot study for a quantitative surface analysis of multi-element alloy films has been performed by the Surface Analysis Working Group (SAWG) of the Consultative Committee for Amount of Substance (CCQM). The aim of this pilot study is to evaluate a protocol for a key comparison to demonstrate the equivalence of measures by National Metrology Institutes (NMIs) and Designated Institutes (DI) for the mole fractions of multi-element alloy films.A Cu(In,Ga)Se 2 (CIGS) film with non-uniform depth distribution was chosen as a representative multi-element alloy film. The mole fractions of the reference and the test CIGS films were certified by isotope dilution -inductively coupled plasma/mass spectrometry. A total number counting (TNC) method was used as a method to determine the signal intensities of the constituent elements acquired in SIMS, XPS and AES depth profiling. TNC method is comparable with the certification process because the certified mole fractions are the average values of the films.The mole fractions of the CIGS films were measured by Secondary Ion Mass Spectrometry (SIMS), Auger Electron Spectroscopy (AES), X-ray Photoelectron Spectroscopy (XPS), X-Ray Fluorescence (XRF) Analysis and Electron Probe Micro Analysis (EPMA) with Energy Dispersive X-ray Spectrometry (EDX). Fifteen laboratories from eight NMIs, one DI, and six non-NMIs participated in this pilot study.The average mole fractions of the reported data showed relative standard deviations from 5.5 % to 6.8 % and average relative expanded uncertainties in the range from 4.52 % to 4.86 % for the four test CIGS specimens. These values are smaller than those in the key comparison K-67 for the measurement of mole fractions of Fe-Ni alloy films. As one result it can be stated that SIMS, XPS and AES protocols relying on the quantification of CIGS films using the TNC method are mature to be used in a CCQM key comparison.
KSP Keywords
AES depth profiling, Alloy films, Amount of substance, Auger Electron Spectroscopy, CIGS film, Certification process, Depth distribution, Depth profiling(DP), Electron Probe Micro Analysis, Electron spectroscopy(82.80.Pv), Energy dispersive X-ray(EDX)
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