Microscratch testing method for systematic evaluation of the adhesion of atomic layer deposited thin films on silicon

The scratch test method is widely used for adhesion evaluation of thin films and coatings. Usual critical load criteria designed for scratch testing of coatings were not applicable to thin atomic layer deposition (ALD) films on silicon wafers. Thus, the bases for critical load evaluation were established and the critical loads suitable for ALD coating adhesion evaluation on silicon wafers were determined in this paper as L_CSi1, L_CSi2, L_CALD1, and L_CALD2, representing the failure points of the silicon substrate and the coating delamination points of the ALD coating. The adhesion performance of the ALD Al₂O₃, TiO₂, TiN, and TaCN+Ru coatings with a thickness range between 20 and 600 nm and deposition temperature between 30 and 410°C on silicon wafers was investigated. In addition, the impact of the annealing process after deposition on adhesion was evaluated for selected cases. The tests carried out using scratch and Scotch tape test showed that the coating deposition and annealing temperature, thickness of the coating, and surface pretreatments of the Si wafer had an impact on the adhesion performance of the ALD coatings on the silicon wafer. There was also an improved load carrying capacity due to Al₂O₃, the magnitude of which depended on the coating thickness and the deposition temperature. The tape tests were carried out for selected coatings as a comparison. The results show that the scratch test is a useful and applicable tool for adhesion evaluation of ALD coatings, even when carried out for thin (20 nm thick) coatings.