Quantitative Analysis of X-ray Fluorescence Absorption and Emission for Thickness Determination of ALD-Grown Metal and Oxide Nanoscaled Films

This study describes the use of X-ray fluorescence spectroscopy (XRF) to determine the thickness of nanoscaled thin films of insulating oxides such as Al₂O₃, HfO₂, and ZrO₂, semiconducting oxides such as TiO₂, ZnO, and metals like Pt, on silicon substrates synthesized by atomic layer deposition (ALD) technology. XRF thickness measurements were compared with the predicted layer thickness based on calculations from known ALD growth rates for each metal or metal oxide films. The ALD growth rates have been calibrated with TEM cross-sectional measurements of the resulting film thickness. The results showed good agreement between the two methods, indicating the XRF technique was successful. Quantitative XRF spectroscopy employing XRF absorption and emission line analysis has been demonstrated to be a powerful non-destructive tool for thickness determination of deposited high-k transition metal oxides and other technologically important nano-scaled thin films like Pt and other metal contacts and reveals new untapped application potential for XRF.