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- EPMA (2) (entfernen)
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) and are traceable to the SI. 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. The mole fractions were also measured by non-destructive X-Ray Fluorescence (XRF) Analysis and Electron Probe Micro Analysis (EPMA) with Energy Dispersive X-ray Spectrometry (EDX).
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. These values are much smaller than that of Fe in a Fe-Ni alloy film in CCQM K-67 (0.0330 mol/mol). This means that the quantification of multi-element alloy films is possible by depth profiling analysis using the TNC method.
A diffusion couple between directionally solidified nickel and the single crystal Ni-base superalloy CMSX-10 was produced by hot pressing in vacuum. The diffusion couples were heat treated at temperatures between 1050 and 1250 °C. The exposed samples were characterized by SEM/EBSD/EPMA. The interdiffusion results in dissolution of the c¢-Ni3 Al in the superalloy and in growth of nickel grains towards CMSX-10. Rapid diffusion of aluminum from the superalloy into pure nickel leads to a significant formation of pores in the superalloy. The interdiffusion processes were modelled using the finite-element simulation software DICTRA with the databases TCNi5 and MobNi2, tailored specially for Ni-base superalloys. The effect of alloying elements on the interdiffusion profiles is discussed in terms of alloy thermodynamics. The calculated element concentration profiles are in good agreement with the EPMA measurements.
The interdiffusion modeling correctly predicts the shapes of the concentration profiles, e.g. kinks on the Al and Ti profiles in the vicinity of the original interface in the joint. The calculation predicts with reasonable accuracy the extent and the location of the Kirkendall porosity.