A comparative transmission electron microscopy, energy dispersive x-ray spectroscopy and spatially resolved micropillar compression study of the yttria partially stabilised zirconia – Porcelain interface in dental prosthesis

Lunt, Alexander J.G.; Mohanty, Gaurav; Ying, Siqi; Dluhoš, Jiří; Sui, Tan; Neo, Tee K.; Michler, Johann; Korsunsky, Alexander M.

Thin Solid Films 596 (2015)

Recent studies into the origins of failure of yttria partially stabilised zirconia-porcelain veneered prosthesis have revealed the importance of micro-to-nano scale characterisation of this interface zone. Current understanding suggests that the heat treatment, residual stresses and varying microstructure at this location may contribute to near-interface porcelain chipping. In this study the chemical, microstructural and mechanical property variation across the interfacial zone has been characterised at two differing length scales and using three independent techniques; energy dispersive X-ray spectroscopy, transmission electron microscopy and micropillar compression. Energy dispersive X-ray spectroscopy mapping of the near-interface region revealed, for the first time, that the diffusional lengths of twelve principal elements are limited to within 2-6 μm of the interface. This study also revealed that 0.2-2 μm diameter zirconia grains had become detached from the bulk and were embedded in the near-interface porcelain. Transmission electron microscopy analysis demonstrated the presence of nanoscale spherical features, indicative of tensile creep induced voiding, within the first 0.4-1.5 μm from the interface. Within zirconia, variations in grain size and atomistic structure were also observed within the 3 μm closest to the interface. Micropillar compression was performed over a 100 μm range on either side of the interface at the spatial resolution of 5 μm. This revealed an increase in zirconia and porcelain loading modulus at close proximities (< 5 μm) to the interface and a decrease in zirconia modulus at distances between 6 and 41 μm from this location. The combination of the three experimental techniques has revealed intricate details of the microstructural, chemical and consequently mechanical heterogeneities in the YPSZ-porcelain interface, and demonstrated that the length scales typically associated with this behaviour are approximately ± 5 μm.