The fiber-matrix adhesion mechanism in high modulus pitch-based carbon fiber-epoxy matrix composites has been studied. The surface morphology and chemistry of the carbon fibers were examined by microscopic (SEM, STM), thermodynamic and spectroscopic (XPS, Raman) techniques. The interlaminar shear strength and transverse tensile strength of the composites made from surface-treated and untreated fibers were also obtained. In the microscopic analysis, there was no difference in the surface roughness between the surface-treated and untreated fibers. In the thermodynamic and spectroscopic analyses, surface treatment of the carbon fibers increased the amount of surface oxygen. The results indicated that the major role of the surface treatment on the carbon fiber-epoxy resin adhesion is not the mechanical interlocking effect by the surface roughness. The formation of surface oxygen-containing functional groups is assumed to account for the increase in fiber-matrix interfacial adhesion.