Final report of CCQM-K129 Measurement of Mole Fractions of Cu, In, Ga and Se in Cu(In,Ga)Se₂ Films

Abstract

CCQM key comparison K-129 for the quantitative analysis of Cu(In,Ga)Se2 (CIGS) films has been performed by the Surface Analysis Working Group (SAWG) of the Consultative Committee for Amount of Substance (CCQM). The objective of this key comparison is to compare the equivalency of the National Metrology Institutes (NMIs) and Designated Institutes (DIs) for the measurement of mole fractions of Cu, In, Ga and Se in a thin CIGS film. The measurand of this key comparison is the average mole fractions of Cu, In, Ga and Se of a test CIGS alloy film in the unit of mole fraction (mol/mol). Mole fraction with the metrological unit of % mol/mol can be practically converted to atomic fraction with the unit of at %. In this key comparison, a CIGS film with certified mole fractions was supplied as a reference specimen to determine the relative sensitivity factors (RSFs) of Cu, In, Ga and Se. The mole fractions of the reference specimen were certified by isotope dilution - inductively coupled plasma/mass spectrometry (ID-ICP/MS). A total number counting (TNC) method was recommended as a method to determine the signal intensities of the constituent elements acquired in the depth profiles by Secondary Ion Mass Spectrometry (SIMS), X-ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES). Seven NMIs and one DI participated in this key comparison. The mole fractions of the CIGS films were measured by depth profiling based-SIMS, AES and XPS. In this key comparison, the average degrees of equivalence uncertainties for Cu, In, Ga and Se are 0.0093 mol/mol, 0.0123 mol/mol, 0.0047 mol/mol and 0.0228 mol/mol, respectively. Main text To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).

Accurate experimental determination of gallium K- and L3-shell XRF fundamental parameters

“…Gallium is an important element for electronics (GaAs and related ternary and quaternary III-V materials), and Cu(In,Ga)Se 2 (CIGS) and related materials have become of particular interest recently for solar (PV) applications [6,7]. But here too, the quality of available literature data is rather poor: for the L3-shell fluorescence yield the different sources deviate by almost 100% and nominal uncertainties are in the order of 25% [8].…”

Traceable quantitative analysis of Ag x Cu1−x alloy films by ID ICP-MS, RBS and MEIS

“…The CMCs are claimed by the NMIs participating in the KC from the combination of the uncertainty of the KC reference value and the reported individual uncertainty. Two KCs have been performed by CCQM SAWG for the quantitative analyses of Fe-Ni alloy films and Cu(In,Ga)Se 2 films in CCQM K67 and K129, respectively [1,2].…”