The aim of this study is to create composites based on the high-temperature polymer reinforced with the carbon fibers and to study interfacial interaction between carbon fibers and polymer matrix. We propose a new method to obtain polysulfone based composite materials reinforced with high-modulus carbon fibers. The influences of thermal oxidation of carbon fibers on mechanical and thermal properties of the composites were studied. It was found that the obtained composite materials have sufficiently high mechanical properties, tensile strength up to 1047 MPa and Young’s modulus up to 70.9 GPa were found. Considerable interest to the polymer composites is associated with their high performance and good mechanical and thermal properties, which enable a broad range of aerospace, automotive and medical applications. Additionally, the manufacturing process of such composites can easily be optimized and automatized, furthermore, it is not time-consuming process in relation with thermosetting polymer based composites.