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Figure 45 and Figure 46 show absorbance at wavenumber of 2360 cm-1, corresponding to unbound CO2. Inspection of Figure 45 shows that the absorbance volume consist of two individual peaks, the first peak occurring at approximately 1500 s (25 minutes) and the second at approximately 2100 s (35 minutes). By identifying the presence of CO2 slightly later than the mass loss observed by TGA, in conjunction with the knowledge that the sample was exposed to scCO2 exclusively, it is determined that the mass loss observed by TGA is directly attributable to CO2. Figure 46 is not resolved into two distinct peaks, possibly owing to the reduced mass of CO2 release, leading to the appearance of a single peak. This method of identification is used qualitatively and as such no attempt to quantify the volume of CO2 observed by FT-IR is made. Although it is acknowledged that doing so would not be impossible, doing so is extremely convoluted and does not necessarily provide any information unobtainable by TGA. By conducting this study it is possible to demonstrate that CO2 may be used to manipulate the glass transition temperature and induce crystallisation within the polymer matrix. Where the impact of scCO2 processing upon the melting process of PEEK was previously unclear, it may now be seen that the CO2 used to process the material escapes prior to reaching the melting temperature. It follows that the impact of scCO2 processing upon the PEEK melt process is largely indirect and is a consequence of the production of dissimilar crystallites, principally those formed during the spontaneous thermodynamic crystallisation process and those induced due to the use of scCO2. In-situ measurements of the crystallisation process by HPDSC have shown that increasing the CO2 pressure reduces the Tg and TC but does not reduce the bulk melting temperature. The results suggest that the 178PDF Image | Supercritical Fluids and Their Application to the Recycling of High-Performance Carbon Fibre Reinforced Composite Materials
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