High-performance polyimide fibers possess man), excellent properties, e.g., outstanding thermal stability and mechanical properties and excellent radiation resistant and electrical properties. However, the preparation of fibers with good mechanical properties is very difficult. In this report, a biphenvl polyimide from 3,3',4,4'-biphenyltetracarboxylic dianhydride and 4,4'-oxydianiline is synthesized in p-chlorophenol by one-step polymerization. The solution is spun into a coagulation bath of water and alcohol via dry-jet wet-spinning technology. Then, the fibers are drawn in two heating tubes. Thermal gravimetric analysis, thermal mechanical analysis, and dynamic mechanical analysis (DMA) are performed to study the properties of the fibers. The results show that the fibers have a good thermal stability at a temperature of more than 400degreesC. The linear coefficient of thermal expansion is negative in the solid state and the glass transition temperature is about 265degreesC. DMA spectra indicate that the tandelta of the fibers has three transition peaks, namely, alpha, beta, and gamma transition. The alpha and gamma transition temperature, corresponding to the end-group motion and glass transition, respectively, extensively depends on the applied frequency, while the beta transition does not. The activation energy of a and gamma transition is calculated using the Arrhenius equation and is 38.7 and 853 kJ/mol, respectively. (C) 2004 Wiley Periodicals, Inc.