Polyphenylene sulfide sulfone (PPSS) was synthesized by one‐step method and utilized as a sizing agent for carbon fibers. The effects of various monomer ratios, reaction time, and reaction temperature were investigated on the molecular weight of PPSS. The thermal analysis revealed that the product PPSS exhibited a glass transition temperature exceeding 215.5°C, indicating exceptional thermal stability. After PPSS sizing treatment, the grooves on the surface of carbon fibers were filled, resulting in a substantial enhancement of the microinterface properties. The surface energy was increased by 8.2%, while the maximum weight loss temperature was 27.8% higher than that of the commercial carbon fiber. The tensile strength of the carbon fiber after heat treatment reached 2196 MPa, representing a 45.9% increase over that of the commercial carbon fiber.