Fingerprints of homogeneous nucleation and crystal growth in polyamide 66 as studied by combined infrared spectroscopy and fast scanning chip calorimetry

Homogenous crystal nucleation and growth in polyamide 66 (PA66) are followed in situ by means of a combination of FTIR spectroscopy and fast scanning chip calorimetry (FSC). Therefore, a novel setup with a calorimetry chip equipped with an IR-transparent SiN membrane was developed, which enables to examine IR spectroscopic and FSC experiments on the identical specimen. Because of the small amount of sample material (~ 100 ng), it is possible to achieve heating and cooling rates up to 5000 Ks−1, and hence to quench the sample into a fully amorphous state without quenched-in homogeneous crystal nuclei. Annealing the film then allows to determine the onset of homogenous nucleation and crystal growth by means of FSC, whereas molecular interactions are unraveled by FTIR spectroscopy. It is demonstrated that different moieties of PA66 respond distinctly during crystallization; far-reaching interactions such as hydrogen bonding are established prior to onset of short-range steric hindrance.