In glass‐ceramics (GCs), on cooling from the crystallization temperature, internal residual stresses are generated due to the difference between the thermal expansion coefficient (TEC) of the crystal phase(s) and the residual glass. These stresses could degrade or promote their mechanical properties. In this work, we varied the magnitude of the residual stresses in lithium silicate GCs by designing their microstructures. The level of internal stresses was measured using (Synchrotron) X‐ray diffraction. The effects of anisotropy of thermal expansion, crystal shape, and intensity of the residual stresses were analyzed and compared using theoretical models. We extended the Hsueh‐Becher model to include the thermal expansion anisotropy of the orthorhombic lithium disilicate (LS2) crystals. We found that the average residual stresses within the LS2 crystals are compressive or null (−100 to ~0) and highly anisotropic. Most importantly, within the limits of this study, we found no evidence for the influence of (compressive or null) residual stresses on the fracture toughness of the studied GCs. Within the crystal size range from 1 to 5 μm, a highly crystallized volume fraction coupled to relatively large crystals (5 μm) of high elastic modulus improved the glass‐ceramic fracture toughness. This result can guide the microstructural design of novel tough GCs.

An interesting technique was proposed by Ray et al. over a decade ago to determine the number density of nucleation sites, Nq, or the nucleation rate, I(T), in glasses that exhibit internal nucleation. Their approach is based on the measurement of the areas under the differential scanning calorimetry (DSC) crystallization peaks of partially crystallized glass samples. In this study, we review their method and test a modified equation recently proposed by some of us, which also takes into account the crystal morphology and impingement. We compare Nq obtained with both methods for a Li2O·2SiO2 glass. Small glass monoliths were treated at 620°C for different time periods for crystal growth, without any nucleation treatment, and subsequently analyzed by DSC up to 800°C. We thus estimated Nq from the area under the DSC crystallization peaks. The corrected approach resulted in Nq values which were not affected by the pair of growth times chosen, as expected, but the obtained values were two‐ to fivefold lower than those calculated with the Ray model. Taking into account previously reported nucleation rates and the corresponding induction periods as a function of temperature (for specimens of the same glass batch), we estimated the number of nuclei formed during the DSC heating/cooling steps, and also measured them by optical microscopy (OM). Finally, we compared the obtained values from OM with the Nq values determined by the DSC method. The Nq resulting from the original and new equations were approximately two orders of magnitude larger than those experimentally determined for the same glass using optical microscopy. This difference is attributed to the formation of new nuclei during the heating and cooling paths of the DSC runs and to surface crystallization, which are not taken into account in the DSC expressions.

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