Wet-composition-induced amorphous adhesion toward a high interfacial shear strength between carbon fiber and polyetherketoneketone
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摘要: 炭纤维与聚醚酮酮之间的界面粘接是影响其复合材料力学性能的关键因素，因此如何高效地将聚醚酮酮浸透到炭纤维束中尤为关键。本工作基于聚醚酮酮的高溶解性，采用湿法加工策略将其引入到炭纤维表面。聚醚酮酮优异的润湿性保证了其在炭纤维表面的完全覆盖和紧密结合，使微液滴法评估界面剪切强度成为可能。通过溶液浸渍，聚醚酮酮可以完全均匀地填充炭纤维束内部，从而获得较高的层间剪切强度。研究表明炭纤维与聚醚酮酮的最大界面剪切强度和层间剪切强度分别达到107.8和99.3 MPa。这种优异的力学性能归因于理想复合所带来的限域效应，使得聚醚酮酮在炭纤维间形成了非晶态结构，从而显著提高了粘附作用。Abstract: Interfacial adhesion between carbon fiber (CF) and polyetherketoneketone (PEKK) is a key factor that affects the mechanical performances of their composites. Therefore, it is of great importance to impregnate PEKK into CF bundles as efficiently as possible. Here we report that owing to the high dissolubility, PEKK can be introduced onto CF surfaces via a wet strategy. The excellent wettability of PEKK guarantees a full covering and tight binding on CFs, making it possible to evaluate the interfacial shear strength (IFSS) with the microdroplet method. Furthermore, the interior of CF bundles can be completely and uniformly filled with PEKK by the solution impregnation, leading to a high interlaminar shear strength (ILSS). The maximum IFSS and ILSS can reach 107.8 and 99.3 MPa, respectively. Such superior shear properties are ascribed to the formation of amorphous PEKK confined in the limited spacing between CFs.
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Key words:
- Polyetherketoneketone /
- Carbon fiber /
- Wettability /
- Amorphous adhesion /
- Interfacial strength
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Figure 1. Strategies to evaluate the interfacial properties between CF and PEKK. (a-c) The set-up for the microdroplet test, a snapshot showing a test where multi microdroplets are formed along a CF, and an SEM image showing the slippage of a droplet after the test. (d–f) The set-up for a short beam shear test based on the three-point bending, and two photos for a CF/PEKK sample before and after the test
Figure 2. Effect of wettability on the microdroplet formation and impregnation into CF bundles. (A) PEKK was well dissolved in 4CP-DCE, but not dissolved in water. (B) The unsized CFs had a smooth fiber surface. (C) It is difficult to prepare a microdroplet by using PEKK melt. (D,E) The PEKK droplet was more elliptical than the epoxy (AG80) one. The contact angle was 21.8° and 35.1°, respectively. (F) The morphology of melt-impregnated CF/PEKK composites along the fiber direction. There were evident voids and bare CF surfaces. (G,H) The solution impregnation resulted in a much more uniform composition
Figure 3. Effect of solvent treatment on chemical properties of CF. (a) The whole XPS spectra were non-distinguishable for the untreated and solvent-soaked CFs. (b) The enlarged C1s peaks, where the fitted four peaks include the strongest sp2 component (1) and three small ones for sp3 (2), C＝O (3), and ―COOH (4), respectively
Figure 4. Microdroplet tests of CF/PEKK interfaces. (a) Typical load–displacement curves for CF/PEKK specimens treated at 340 °C. (b) IFSS value as a function of treatment temperature. Two types of CF/epoxy interfaces were evaluated for comparison. The reported results for CF/PEEK[12], CF/PPEK[28], and CF/PPS[29] are also plotted. (c) SEM images of a tested CF/PEKK specimen (340 °C). There was residual PEKK on fiber surface, indicating that the failure was at the weak part in microdroplet rather than at the contact. (d) The 240-°C treatment induced a weak interface, leading to an overall exposure of fiber surface after the test. (e,f) The debonding of CF/epoxy depends on the content of epoxy groups, leading to a partially covered (e) and a bare fiber surface (f), respectively
Figure 5. Shear properties of CF/PEKK composites. (a,b) Typical load–deflection and stress–strain curves for the ILSS and flexural tests, for the CF/PEKK-360 composites. (c,d) The ILSS and flexural strength and modulus of CF/PEKK composites molded at different temperatures, as compared to those of the CF/AG80. (e) Fracture morphologies of CF/PEKK specimens after the flexural test
Figure 6. Fracture microstructures of the (a) CF/PEKK-360 and (b) CF/AG80 composites. From left to right are the side views, cross-sectional views, and the exposed CFs
Figure 7. Reduced PEKK crystallinity by the confinement of CFs. (a,b) DSC thermograms and XRD diffractograms of CF/PEKK composites (a–d refer to the hot compression at 320, 340, 360 and 380 °C), as compared to a composite composed by short-cut CFs and PEKK (e, hot compressed at 360 °C) and pure PEKK (f and g refer to the treatment at 360 °C with and without preheating). (c,d) The fracture morphologies of a short-cut CF/PEKK composite and the CF/PEKK-360 composite, showing the spherulitic structures in the former and amorphousity in the latter
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