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reactor was then simultaneously heated and pressurised to the conditions as stipulated by the designed experiment (Table 1). Once the desired conditions were attained, the pre- determined experiment time was allowed to elapse prior to cooling the reactor. The reactor was depressurised when the temperature reached 323 K. Analysis of the effects of scCO2 processing of PEEK was carried out using DSC, FT-IR and TGA as detailed in Chapter 3.4.2. Heating and cooling processes were generally on the order of 30 minutes. Supercritical Carbon Dioxide Induced Crystallisation It is necessary to define ‘supercritical CO2 induced crystallisation’ as opposed to spontaneous thermodynamic crystallisation. Supercritical CO2 (scCO2) induced crystallisation is defined as formation of crystalline regions within the PEEK matrix below the Tc, induced by the plasticisation effect attributed to scCO2. To quantitatively assess this process there are two approaches available, the first is to process the polymer with scCO2 and then carryout analysis by DSC (as discussed previously), the second method is to analyse an amorphous PEEK sample by means of High-Pressure DSC (HPDSC). HPDSC allows for the in- situ measurement of the crystallisation process and will highlight the effects of scCO2. Post- processing DSC analysis in the absence of CO2 provides detailed information about the effects of scCO2 processing and separates the manipulation of the crystallisation temperature from the CO2 induced crystallisation. A combination of both methods allows for a holistic approach and was used in this research. 86PDF Image | Supercritical Fluids and Their Application to the Recycling of High-Performance Carbon Fibre Reinforced Composite Materials
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