화학공학소재연구정보센터
Journal of Crystal Growth, Vol.400, 34-42, 2014
Attainment of unstable beta nucleation of glycine through novel swift cooling crystallization process
The sudden cooling of mother liquor from high temperature to a temperature below the ambient through the recently introduced swift cooling crystallization process yielded the beta nucleation of glycine even in the absence of anti-solvents and additives. Experiments were continued at different supersaturation and stirring levels. The nucleation matrix resulted out of these 135 experiments revealed that, even at lower supersaturation and lower stirring rates, the unstable beta nucleation could be achieved. This attained result contrasts the existing reports in which beta nucleation is achieved only at higher supersaturation levels. The intermediate supersaturation and stirring levels facilitate both the beta and alpha nucleation through solution mediated phase transformation while the higher supersaturation and stirring levels facilitate only the alpha nucleation of glycine in the system. The swift cooling method adopted declines the energy barrier that inherently exists for beta and enables its nucleation in the system. Analytically the nucleation parameters of beta and alpha polymorphs were estimated based on Classical Nucleation Theory. Form of crystallization of the nucleated polymorphs of glycine was confirmed by powder x-ray diffraction analysis. (C) 2014 Elsevier B.V. All rights reserved.