The surface of PAN-based carbon fiber was directly modified with fluorine-oxygen mixtures at room temperature. The surface characteristics of the modified fiber were determined by using X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and dynamic contact angle analyzer. The surface free energy was also calculated with the Owens-Wendt geometric mean method using water and methylene iodide contact angle. The surface of carbon fiber was changed into hydrophilicity by the formation of semicovalent C-F bond and C-O bond depending
on reaction conditions and the surface free energy of oxyfluorinated fiber was significantly increased.