Abstract: The temperature and atmosphere of heat treatment showed important effects on the carbon and hydrogen contents in final carbonized poly(p-phenylene) resin. The carbon contents of samples treated in an inert atmosphere were lower than those of samples treated in reductive atmosphere at the same temperatures; but hydrogen contents of samples were just the opposite to it. And the samples treated at 1 000℃ still contained hydrogen. The specific surface areas of samples treated at 1 000℃ in an inert atmosphere dropped to 15 6% as compared with those for the sample treated at 1 000℃ in reductive atmosphere. The specific surface areas of carbonized product decreased with increase in carbonization temperature. The IR and X-ray diffraction spectral analysis showed that the samples treated at 700℃ began to form fused benzene ring structure, but the carbons still belong to amorphous carbon. At 1 000℃ there appeared some graphite characteristic diffraction peaks in XRD spectra and higher graphitization level.