On the Determination of the Concentration of Crystal Nuclei in Glasses by DSC

Author(s)

Cabral, Aluisio A. ^[1] ; Ferreira, Eduardo B. ^[2] ; Villas-Boas, Mariana O. C. ^[3] ; Zanotto, Edgar D. ^[3]

Affiliation

^[1] Inst Fed Maranhao IFMA, Dept Fis, BR-65030001 Sao Luis, MA - Brazil

^[2] Univ Sao Paulo, Dept Engn Mat, Escola Engn Sao Carlos, BR-13566590 Sao Carlos, SP - Brazil

^[3] Univ Fed Sao Carlos, UFSCar, DEMa, Vitreous Mat Lab, LaMaV, Dept Mat Engn, BR-13565905 Sao Carlos, SP - Brazil

• Document type: Journal article
• Source: Journal of the American Ceramic Society; v. 96, n. 9, p. 2817-2823, SEP 2013.
• Web of Science Citations: 4

Abstract

An interesting technique was proposed by Ray etal. 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<bold>2</bold>SiO2 glass. Small glass monoliths were treated at 620 degrees C for different time periods for crystal growth, without any nucleation treatment, and subsequently analyzed by DSC up to 800 degrees 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. (AU)

• FAPESP's process: 07/08179-9 - Kinetic processes in glasses and glass ceramics
• Grantee: Edgar Dutra Zanotto
• Support Opportunities: Research Projects - Thematic Grants