Carbon Fibers Reinforced Polymer composites (CFRP) are high added value materials used in many manufactured products. Especially in aeronautics, thermosetting resins tend to be replaced by heat-resistant thermoplastic polymers. The aim of the work is to evaluate suitable operating conditions of thermoconversion for the recovery of carbon fibers from Poly Ether Ether Ketone (PEEK)/carbon fibers composites. Micro and pilot scale tests have been performed in nitrogen, wet nitrogen, air, and wet air. Thermogravimetric analysis of PEEK/carbon fiber composites showed a moderate decomposition onset temperature of the composite at 515 °C and 510 °C in dry nitrogen and dry air respectively. The oxidative atmosphere did not significantly impact this temperature since the first mass loss was not atmosphere dependent. However, after the first PEEK degradation reaction, the nature of the atmosphere appeared as a great issue. Total mass loss was significantly improved with temperature (full oxidation of polymer and carbon fibers up to 800 °C) and with reaction time using air. Indeed, at pilot scale, the matrix was fully degraded in air atmosphere at 550 °C for 1 h while only 42% and 46% was reached in nitrogen and steam/nitrogen respectively. Comparison of thermogravimetric data between wet and dry atmospheres revealed that steam plays a thermal retardant role leading to some differences on the matrix degradation and on the surface morphology of the carbon fiber at pilot scale. Air treatments at pilot scale induced a reduction of fiber diameters (< − 3.7%) but the tensile strengths of recovered carbon fibers were preserved with an average retention of mechanical properties of 81%-85%. It has been concluded that recycling of PEEK/carbon composite required an oxidant to split up carbon fibers from the PEEK matrix.
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