A series of multi-walled carbon nanotubes (MWNTs)/poly(ether ether ketone)(PEEK) nanocomposite fibers were fabricated by mixing, melt extruding PEEK with different loadings and species of MWNTs, and melt-spun the blended chips. Nanocomposite fibers were heat-stretched and heat-treated. The morphology and dispersibility of MWNTs in nanocomposite fibers were observed using a field emission environmental scanning electron microscope (FESEM) and a transmission electron microscope (TEM). The thermal and crystallization behavior of nanocomposite fibers were characterized using differential scanning calorimetry (DSC) and an X-ray diffractometer (XRD). Mechanical properties were tested using a tensile strength tester. MWNTs tend to aggregate when the loading exceeds 0.8 wt%. Functional groups on MWNTs improve the hydrophobicity and the dispersibility of MWNTs in PEEK matrix. The enhancement of mechanical properties depends on the loading and species of functional groups. The most effectively reinforced effect is in the sequence, carboxylic MWNTs (MWNT-COOH) > hydroxyl MWNTs (MWNT-OH) > MWNTs, which can be explained by the strong hydrogen bonding and the affinity between MWNT-COOH and PEEK, MWNT-OH and PEEK, and possible formation of a chemical bond between MWNT-COOH and PEEK. A nanocomposite fiber with excellent mechanical property was fabricated using 0.8 wt% MWNT-COOH as filler. The Young's modulus is 1.7 GPa; and the stress is 648 MPa. (C) 2012 Elsevier B.V. All rights reserved.