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15.1867 16.0567 4.0833 1.4067 Centerpoint Factorial Point 15 Pressure (MPa) 19.1667 5 30 Soak Time (min) 453.15 10 413.15 Temperature (K) 11.9633 Figure 39: Cube plot showing the percentage crystallisation observed by DSC for PEEK processed with scCO2. DOE conditions; T = 413 – 453 K, P = 5 – 15 MPa, tr = 10 – 30 min, centre-point T = 433 K, P = 10 MPa, tr = 20 min It is important to state that Figure 39 shows the percentage crystallisation observed by DSC, post scCO2 processing. The PEEK samples, being amorphous prior to processing, would typically show a %XC of 18 % at Tc when analysed by DSC as detailed in Chapter 4.1.1. FT-IR analysis of quenched PEEK150PF samples showed that the samples generated could potentially have a %XC of 2.3 % and therefore the maximum %XC that could be observed would be 20.3 %. This would indicate that the polymer was 100 % amorphous post processing and the crystallisation process takes place exclusively within the DSC. Conversely, the minimum %XC observable by DSC is 0 and relates to the maximum crystallisation possible taking place during the polymer processing. The crystallisation process is irreversible and therefore not observable during the DSC analysis. By using these 2.1033 18.5700 11.2300 165PDF Image | Supercritical Fluids and Their Application to the Recycling of High-Performance Carbon Fibre Reinforced Composite Materials
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