Carbon fibers were treated in a HF glow discharge in tetrafluoroethylene and octafluorocyclobutane in order to improve their adhesion to poly(tetrafluoroethylene) matrix. As the result of the plasma treatment, a thin (20-140 nm) fluoropolymer coating was deposited onto the fiber surface. The structure of this coating was studied by means of IR spectroscopy, XPS, AFM and SEM techniques. The coating material appeared to be similar to PTFE in its chemical composition but distinguished by branched, partially crosslinked, amorphous structure and included unsaturated chemical bonds. The coating thickness of 70 nm was sufficient to effectively screen the field of molecular forces of the initial substrate, thus, decreasing the surface energy of the fibers and improving their compatibility with the PTFE matrix. The adhesive strength in the PTFE-carbon fiber systems, measured by means of the microbond test, more than doubled upon the plasma treatment (the local interfacial shear strength increased from 10.7 to 29.7 MPa, apparent IFSS from 4.3 to 7.8 MPa), and the interfacial frictional stress increased by 70%. The new composite material consisting of 20% short coated carbon fibers in the PTFE matrix showed better mechanical, thermal and tribological characteristics as compared with the composite reinforced with untreated fibers. (C) Koninklijke Brill NV, Leiden, 2011