An in situ and ex situ study of the microstructural evolution of a novel lithium silicate glass-ceramic during crystallization firing.

OBJECTIVE: To elucidate the compositional and microstructural developments of a novel lithium silicate glass-ceramic during its crystallization cycle. METHODS: Blocks of a lithium silicate glass-ceramic (Obsidian®, Glidewell Laboratories) were cut into 1mm thick plates and polished to 1µm finish. Some of them were crystallized prior to polishing. Firstly, ex situ compositional and microstructural characterizations of both the pre- and post-crystallized samples were performed by wavelength dispersive X-ray fluorescence, field-emission scanning electron microscopy, and X-ray diffractometry. Secondly, the pre-crystallized samples were subjected to in situ compositional and microstructural characterizations under non-isothermal heating by simultaneous thermogravimetry/differential scanning calorimetry, X-ray thermo-diffractometry, and field-emission scanning electron thermo-microscopy. RESULTS: The microstructure of pre-crystallized Obsidian® consists of an abundant population of perlitic-like/dendritic lithium silicate (Li2SiO3) nanocrystals in a glass matrix. Upon heating, the residual glassy matrix does not crystallize into any form of SiO2; elemental oxides do not precipitate unless over-heated above 820°C; and the Li2SiO3 nanocrystals do not react with the glassy matrix to form typical lithium disilicate (Li2Si2O5) crystals. Nonetheless, the Li2SiO3 nanocrystals grow and spheroidize through the solution-reprecipitation process in the softened glass, and new lithium orthophosphate (Li3PO4) nanocrystals precipitate from the glass matrix. SIGNIFICANCE: The identification of compositional and microstructural developments of Obsidian® indicates that, by controlling the firing conditions, it is possible to tailor its microstructure, which in turn could affect its mechanical and optical properties, and ultimately its clinical performance.

Fractographic analysis of lithium silicate crown failures during sintering.

The two-step production process of glass-ceramic dental restorations involves a computer-aided design/computer-aided machining step followed by a crystallization firing for the final material properties to be achieved. Certain firing parameters are believed to trigger spontaneous fracture of crowns during the cooling process. In this study, cooling fractures have been reproducibly observed and investigated using fractography combined with material (glass transition temperature) and process (cooling rate) characterization. Stress distribution was visualized using birefringence measurements. Fractographic observations revealed fracture starting at the intaglio side of the crowns specifically at contact points with the support firing pins. Further analysis showed that a fast cooling rate was applied during the glass transition region. Thermal stresses were concentrated around the firing pin supports and released the fracture. To prevent such fractures, a slow cooling protocol below the glass transition temperature is our recommendation to dental technicians. Furthermore, the use of planar firing pad or paste supports is advised over the use of point contact supports.