Good dispersion and interfacial compatibility are the key issues to realize the full potential of the physical–mechanical properties of nanocarbon-materials reinforced composites. Styrene–maleic-anhydride-copolymer (SMA)-treated graphene oxide (GO), carboxylated multiwalled carbon nanotubes (MWNTs-COOH), and solid-state shear milling (S3M) were applied to further improve the physical–mechanical properties of the nanocomposite fibers. The results show that a mixture of GO/MWNTs-COOH exhibits good dispersion and interfacial compatibility in polyamide-66 (PA66) matrix. Consequently, the physical–mechanical properties of the fibers, which were spun from the nanocomposite of GO/MWNTs-COOH treated using SMA and S3M methods, show a significant enhancement compared to the untreated fibers as well as better crystallization and thermal properties. In particular, the tensile strength of the PA66/GO/MWNTs-COOH nanocomposite fibers with a loading of 0.3 wt % GO/MWNTs-COOH reaches a maximum (979 MPa), which is the highest among all of the reported literature values. Moreover, the fibers were fabricated by a facile process with efficiency, holding great potential for industrial applications.
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