Strange generation and subsequent extinction of crystal nuclei were
observed in the glassy state of salol (phenyl salicylate) during the course
of ageing at very low constant-temperatures. The presence/absence of
crystal nuclei within the glass were judged, by using a differential
scanning calorimeter (DSC), from whether the crystal growth and fusion
phenomena were observed in the following heating process or not. The
liquid sample was cooled rapidly at 200 K min−1
from 333 K above the fusion temperature down to a desired ageing temperature
(Ta)
below the glass transition temperature (Tg = 220 K), aged there for
different periods (ta),
and then heated up to 213 K at 200 K min−1. The
DSC measurement was carried out at 10 K min−1
from 213 to 333 K. The ageing periods were taken in a range
between 30 s and 316 min. At Ta = 213 K, crystal
nucleation was found to proceed for ageing longer than 100 min. No crystal nucleation was found at
Ta in between 123
and 193 K. At Ta
below 113 K, crystal nuclei were found immediately after the rapid cooling, then
extinguished, and again generated; some nuclei formed initially, survived for
longer ageing at 103 K. The generation and extinction phenomena of crystal
nuclei are discussed as a general event occurring in glasses located in an extremely
non-equilibrium state.
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