A new high-temperature resistance polyimide foam was synthesized from 2,3,3',4'-biphenyltetracarboxylic dianhydride (alpha-BPDA) and p-phenylenediamine (p-PDA). The structures and foaming process of polyimide precursor powders were characterized by wide-angle X-ray diffractometer (WXRD) and the self-made visualization device, respectively. The imidization degree, thermal mechanical properties and thermal stability of the polyimide foams with different post-treatment temperatures were also measured by fourier transform infrared spectrometer spectrum (FTIR), dynamic thermal mechanical anaylsis (DMTA), and thermogravimetric analysis (TGA). Results showed that the inflation onset temperatures of polyimide precursor powders ranged from 122 to 135 degrees C with varying the heating rate. And the increase in the imidization degree, glass transition temperatures (T-g) and temperatures for 5 wt% mass loss of high-temperature resistance polyimide foams can be achieved with increasing post-treatment temperature. It was quite surprising to find that T-g of high-temperature resistance polyimide foam posttreated at 420 C was up to above 450 degrees C, and the char yield at 800 degrees C was more than 60%. POLYM. ENG. SCI., 50:1261-1267, 2010. 2010 Society of Plastics Engineers