Thickness determination of metal multilayers by ED-XRF multivariate analysis using Monte Carlo simulated standards

We present the thickness measurement of multilayer samples by X-ray fluorescence (XRF) using calibration curves obtained from simulated spectra through Monte Carlo (MC) algorithm. The XRF is a widespread technique for the analysis of single and multilayer films but the accuracy of quantitative analysis must be increased. Moreover, the use certified standards is not easy to implement due to the high variability of combination and/or concentration in layered samples. The results of this work were compared with fundamental parameter (FP) method and focussed ion beam scanning electron microscopy (FIB-SEM) analysis. The results show good quantitative values even without the use of any standard with known thickness. In addition to having built the calibration curves with a simple univariate approach, also multivariate data analysis was performed to consider multiple variables simultaneously. From the comparison of the obtained results, it can be inferred that the univariate analysis worked well in the case of single layer samples and in the determination of the upper layer in multilayer samples but only multivariate analysis, taking into account the matrix effect of each layer, provided maximum accuracy on each layer of multilayer samples.