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observation of Figure 39. It is further observed that a single endothermic peak, corresponding to the melting of the polymer is observed. By contrast, when processed at 453 K for 10 minutes with a CO2 pressure of 15 MPa the spontaneous thermodynamic crystallisation process is observed by DSC, with the reduced integral (compare to amorphous material, Figure 32, Page 154) being a consequence of the induction of crystallisation by scCO2. It is apparent that the crystallites within the polymer were formed by two dissimilar processes and inspection of the endotherm associated with the melting of the polymer reveals two distinct melt transitions. Analysis of the DSC thermograms identified that where the polymer was processed for extended time periods, allowing the thermodynamic crystallisation process to prevail, a single melt peak was observed and that in the case of the example presented in Figure 40, the melting temperature was 616 K in agreement with the virgin material. Conversely, with respect to the double melting peak presented in Figure 40, the lower transition takes place at 609 K and the upper transition takes place at 619 K. Thus, empirical findings suggest that the processing of PEEK with scCO2 manipulates the glass transition temperature and induces crystallisation, which in turn may indirectly alter the melting process due to the formation of dissimilar crystallites. 4.1.3. High-Pressure Differential Scanning Calorimetry The measurements presented so far are concerned with identifying the effects of scCO2 on polymer matrix by analysing the material post processing. Identification of the effects of scCO2 on the melting process are restricted to considering the formation of crystallites at, or near to, the crystallisation temperature. In carrying out such an investigation, it is not known whether CO2 is present within the polymer upon reaching the melt temperature, and 168PDF Image | Supercritical Fluids and Their Application to the Recycling of High-Performance Carbon Fibre Reinforced Composite Materials
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