Abstract: The phenolic aldehyde were synthesized and then were carbonized to make carbon materials of the resin. The elements and structure of carbon materials of the resin were analyzed. The results found that the carbon materials of the resin treated at 620℃ have weekly appeared (100) crystal plane diffraction peak, it means that some graphite crystallite have produced. But the graphitization degree of the carbon materials of the resin treated at 1000℃ is still lower, and it is belong to the range of amorphous carbon. All the elementary mass fraction of the carbon materials of the resin are regularly changed with the treatment temperature increase, thereinto carbon content is accretion, hydrogen and oxygen contents are decline. The disengage speed of hydrogen is higher than that of oxygen in the same carbonization condition. Both temperature and ambience are all the factor of effect on the specific surface of the carbon materials, and the effect of ambience is more intensity.