Study of microstructure of oriented PET fibres exposed to supercritical carbon dioxide

Samples of partially oriented yarn (POY) PET fibers were uniaxially drawn at temperatures below, near, and above the glass transition temperature at a constant draw ratio before exposure to supercritical carbon dioxide (scCO₂) in the presence of tension at a temperature of 80 °C and a pressure of 220 bar. The effects of drawing temperature and scCO₂ exposure on structural changes and on mesomorphic transitions, in particular, were investigated using differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), and birefringence and density measurements. A good correlation was obtained among the results obtained from various techniques. Results indicated that the development of a transient mesophase structure depended strongly on process temperature. By drawing PET fibers in the samples at temperatures below the glass transition (cold-drawing), a mesophase structure developed in which the highly extended chains played a key role in structural changes incurred. Meanwhile, exposure to scCO₂ led to the plasticization of the samples accompanied by their reduced glass transition and cold crystallization temperatures. This process also gave rise to the appearance of a second melting peak at about 135 °C that is related to the melting of imperfect and thin crystals, thereby inducing structural changes in the treated fibers. In the case of samples subjected to cold drawing and to scCO₂ exposure, the transformation of the mesophase structure into the crystalline phase was found to be strongly affected by scCO₂ exposure, while this same effect was negligible in the case of hot drawn samples.