Poly(ether ether ketone)/carbon fiber composites (PEEK/Cf) were chemical etched by Cr2O3/H2SO4 solution, electroless plated with copper and then electroplated with nickel. The effects of chemical etching time and temperature on the adhesive strength between PEEK/Cf and Cu/Ni layers were studied by thermal shock method. The electrical resistance of some samples was measured. X-ray photoelectron spectroscopy (XPS) was used to analyze the surface composition and functional groups. Scanning electron microscopy (SEM) was performed to observe the surface morphology of the composite, the chemical etched sample, the plated sample and the peeled metal layer. The results indicated that C=O bond increased after chemical etching. With the increasing of etching temperature and time, more and more cracks and partially exposed carbon fibers appeared at the surface of PEEK/Cf composites, and the adhesive strength increased consequently. When the composites were etched at 60 degrees C for 25 min and at 70-80 degrees C for more than 15 min, the Cu/Ni metallization layer could withstand four thermal shock cycles without bubbling, and the electrical resistivity of the metal layer of these samples increased with the increasing of etching temperature and time. (C) 2010 Elsevier B.V. All rights reserved.