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Figure 39: Cube plot showing the percentage crystallisation observed by DSC for PEEK processedwithscCO2.DOEconditions;T=413–453K,P=5–15MPa,tr =10–30min, centre-point T = 433 K, P = 10 MPa, tr = 20 min ....................................................................165 Figure 40: DSC thermograms for PEEK 150PF samples processed from amorphous state using scCO2, T = 453 K. DSC Method 1 ............................................................................................167 Figure 41: HPDSC thermogram for amorphous PEEK in-situ measurement, PiCO2 = 3.0 MPa, HPDSC method 5....................................................................................................................170 Figure 42: HPDSC thermogram for amorphous PEEK in-situ measurement, PiCO2 = 3.5 MPa, HPDSC method 1....................................................................................................................171 Figure 43: Mass loss observed by TGA as a function of Lag Time for PEEK processed with scCO2, P = 20.0 MPa, T = 413 K, t = 30 min ............................................................................173 Figure 44: TGA thermogram for PEEK450PF processed in scCO2 showing the furnace temperature and 1st order differential of mass loss (DTG), P = 20.0 MPa, T = 413 K, t = 30 min. TGA Method 1................................................................................................................175 Figure 45: 3D FT-IR spectrum for analysis of TGA exhaust gasses from PEEK450PF processed in scCO2, lag time = 60 min, (Processing conditions; P = 20.0 MPa, T = 413 K, t = 30 min)...177 Figure 46: 3D FT-IR spectrum for analysis of TGA exhaust gasses from PEEK450PF processed in scCO2, lag time = 180 min, (Processing conditions; P = 20.0 MPa, T = 413 K, t = 30 min).177 Figure 47: Phenol concentration [PhOH] with respect to ethanol concentration [EtOH], 623 K, 30 min, 10 mg ml-1 Cs2CO3, P = 15.8 – 25.5 MPa. Determined by HPLC............................180 Figure 48: Optical Microscopy image of PEEK, Victrex 150CA30, post processing in scH2O, 648 K, 25 min, 30 MPa, showing the macro-porous structure..............................................181 Figure 49: SEM Micrographs of post processed PEEK 150CA30, 30 min, 623 K, 10 mg ml-1 Cs2CO3, a) [EtOH] = 20 %v, 16.7 MPa, b) [EtOH] = 100 %, 23.9 MPa.....................................181 16PDF Image | Supercritical Fluids and Their Application to the Recycling of High-Performance Carbon Fibre Reinforced Composite Materials
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