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Nucleation efficacy and flexural strength of novel leucite glass-ceramics

: Cattell, M.J.; Patzig, C.; Bissasu, S.; Tsoutsos, A.; Karpukhina, N.


Dental materials 36 (2020), No.5, pp.592-602
ISSN: 0109-5641
ISSN: 1879-0097
Journal Article
Fraunhofer IMWS ()

Objectives. To optimize the nucleation mechanism in leucite glass-ceramics to allow more efficacious glass-ceramic manufacture and improvements in microstructure and mechanical reliability. Materials and methods. An alumino-silicate glass was designed and synthesized using melt quench methods. The glass was crushed and milled using various milling times (48–93 h) and spray drying. Nucleation and growth heat treatment schedules were applied to synthesize glass-ceramics. Glass/glass-ceramic powders and frit specimens were characterized using differential scanning calorimetry (DSC), transmission electron microscopy (TEM), energy-dispersive X-ray spectrometry (EDX), magic angle spinning nuclear magnetic resonance spectroscopy (MAS-NMR) and X-ray diffraction analyses (XRD). Glass-ceramic specimens were tested using the biaxial flexural strength test (BFS). Results. Application of defined nucleation heat treatments resulted in the synthesis of Na/Ca titanates. NMR indicated changes to the 23Na glass spectra in the nucleated glass and TEM/EDX the presence of Na/Ca/Ti domains (<200 nm) within the leucite crystals and associated with the nucleation of the leucite phase. XRD confirmed the presence of a bulk leucite phase in the glass-ceramics. SEM/TEM confirmed the crystallization of the leucite phase (65.5–69.3%) in a thermally matched glass, in conjunction with the nano Na/Ca titanate phase. The leucite glass-ceramics resulted in a high BFS (255–268 MPa), with reduction in powder milling time prior to heat treatments having no significant effect on flexural strength and reliability (p > 0.05). Significance. Na/Ca titanates were synthesized in leucite glass-ceramics for the first time and associated with its nucleation and efficacious growth. This nucleation optimization provides opportunities for more efficient manufacturing and microstructural/mechanical reliability improvements. Improved synthesis of high strength/reliable leucite glass-ceramics is useful for construction of esthetic minimally invasive restorations.