In-situ SEM cyclic nanoindentation of pre-sintered and sintered zirconia materials.

Efficient diamond machining of zirconia requires a comprehensive understanding of repetitive diamond indentation mechanics. This paper reports on in-situ cyclic nanoindentations of pre-sintered and sintered zirconia materials performed inside a scanning electron microscope (SEM). In-situ SEM imaging of cyclic indentation processes and high-magnification SEM mapping of indentation imprints were conducted. The elastic and plastic behaviors of pre-sintered and sintered zirconia materials were investigated as a function of the cyclic nanoindentation number using the Sakai and Sakai-Nowak models. For pre-sintered zirconia, cyclic nanoindentation induced quasi-plastic deformation, causing localized agglomeration of zirconia crystals with microcracks and large cracking along the indentation edge. Severely compressed, fragmented, and pulverized zirconia crystals and smeared surfaces were also observed. For sintered zirconia, shear bands dominated quasi-plastic deformation with the formation of edge pile-ups and localized microfractures occurred at indentation apex and diagonals. All elastic and plastic behaviors for pre-sintered and sintered zirconia materials revealed significantly microstructure-dependent. Pre-sintered zirconia yielded significantly lower contact hardness, Young's moduli, resistance to plasticity, elastic deformation components, and resistance to machining-induced cracking, and higher elastic and plastic displacements than sintered state. Meanwhile, all the behaviors for the two materials were independent from the cyclic nanoindentation number. A model was proposed for cyclic nanoindentation mechanics, revealing their cyclic indentation-induced microstructural changes in the two zirconia materials. This study advances the fundamental understanding of nanoindentation mechanics of zirconia materials.