Indentation tests have been performed on silicon wafer substrates with surface layers of ZrO₂. The surface layers have been deposited with a newly developed atomic layer deposition (ALD) process using a Savannah 100 ALD reactor. Substrates with 50 nm nominal thickness layers have been tested using nano-indentation. Indentations were made using a Hysitron nano-indenter at 50 nm and100 nm depth. Subsequent indentations have been studied in cross-section using transmission electron microscopy with specimens prepared using the FIB lift-out technique and ion milling. The layer structure and the layer-substrate interface have been studied. Cross-sections show adhesion of the surface layers to the substrate even through the indentation profile. Underneath the indentations plastic deformation is observed to have occurred by dislocation generation, the formation of amorphous silicon a-Si, and by phase transformation from diamond silicon Si-I to the more dense Si-III phase. The contact surface is studied in detail to examine the contact-induced deformation in the ZrO₂ surface layer. Hardness and elastic modulus are determined from the indentation load-unload curves for the substrate and for the layer and these are compared with values in the literature.

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