Aging and Solidification of Supercooled Glycerol

We experimentally investigate the solidification of supercooled glycerol during aging that has recently been observed by Zondervan et al. We find that a slow cooling at 5 K/h prior to the aging is required for solidification to take place. Furthermore, we show that the time of onset depends strongly on the aging temperature which we varied between 220 and 240 K. The nature of the solid phase remains unclear. The experiments show that upon heating the solid glycerol melts at the crystal melting point. However, rheology experiments in the plate−plate geometry revealed the growth of a soft, slushlike phase that is distinct from a crystal grown by seeding at the same aging temperature. The slushlike glycerol grows from a nucleation point at almost the same speed as a seeded crystal quenched to the same temperature, but its shear modulus is almost 2 orders of magnitude lower than the crystal phase, which we measure independently. While solidification was reproducible in the Couette geometry, it was not in the plate−plate geometry.