Recently developed polyketone fiber has various applications in the mechanical rubber goods as reinforcement because of its good mechanical properties. However, its surface is not suitable for good adhesion with the rubber matrix. Thus, a surface modification is essential to obtain the good interfacial adhesion. Plasma treatment, in this study, has been conducted to modify the surface of the polyketone fiber. The morphological changes of the fibers by oxygen plasma treatment were observed by using SEM and AFM. The chemical composition changes of PK fiber surface treated with oxygen plasma were investigated using an XPS (X-ray photoelectron spectroscopy). Finally, the effect of these changes on the interfacial adhesion between fiber and rubber was analyzed by using a microdroplet debonding test. By the plasma treatment, oxygen moieties on the fiber surface increased with processing time and power. The surface RMS roughness increases until the proper processing condition, but a long plasma processing time resulted in a rather reduced roughness because of surface degradation. When the treatment time and power were 60 s and 80 W, respectively, the highest interfacial shear strength (IFSS) was obtained between the PK fiber and natural rubber. However, as the treatment time and power were higher than 60 s and 80 W, respectively, the IFSS decreased because of degradation of the PK fiber surface by severe plasma treatment.