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two boundary conditions it is then possible to use the data obtained from DSC analysis, presented in Figure 39, to determine the impact of scCO2 on the crystallisation of PEEK. It is observed that when the processing temperature is 413 K a high CO2 pressure is required to induce crystallisation within the polymer, a %XC 15.2 % is observed when the pressure is 15 MPa in comparison to 18.6 % when the CO2 pressure is 5 MPa. At the centre-point, T = 433 K, P = 10 MPa and tr = 20 min, a %XC of 12 % is observed indicating the induction of approximately 6 %XC as a result of scCO2 processing. The expectation would be that by increasing the processing temperature beyond Tc the polymer would undergo crystallisation, as is the case in the absence of CO2. However, this differs from the empirical observations and it is apparent that whilst scCO2 can induce crystallisation, the induced crystallisation process takes place at a reduced rate compared to the spontaneous thermodynamic crystallisation process. Whilst not immediately intuitive, this is consistent with the scCO2 plasticisation effect. With the CO2 effusing between the polymer chains, increasing the free volume and facilitating the movement of the molecular chains, in order for crystallisation to take place there is a requirement to displace the CO2 and allow the polymer chains to compact, forming crystals. This is likely to be a time dependent process and therefore the %XC will be proportional to the soak time. Increasing the CO2 pressure under such conditions exerts greater pressure on the bulk material, and may be responsible for forcing the molecular chains together more rapidly to form crystallites. The displacement of CO2 must still take place and therefore %XC is still directly proportional to time. This effect is demonstrated in Figure 39 where it can be seen that the %XC observed by DSC reduces from 11.2 % to 2.1 % when the soak time is increase from 10 to 30 minutes. 166PDF Image | Supercritical Fluids and Their Application to the Recycling of High-Performance Carbon Fibre Reinforced Composite Materials
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