The carbon materials prepared from polyimide (PI) resin film were investigated by TG-DTG, X-ray powder diffraction (XRD), and X-ray photoelectron spectroscopy (XPS) analysis. TG-DTG study revealed that the weight loss of PI resin film during carbonization occurred in three stages, and the most serious changes occurred at 605.5 degrees C. XRD results indicated that a disorder structure occurred after the carbonization at 600 degrees C and graphite crystallite appeared gradually with increasing the temperature. And PI resin film still presented some characteristics of nongraphitizing carbon, after graphitizing at 2600 degrees C. XPS analysis identified that pyrrole type nitrogen was a main component of surface nitrogen atoms after carbonization. When the temperature reached 2600 degrees C, nitrogen atoms disappeared totally; the reason why oxygen atoms still existed in the material at so high temperature was our subject of interesting matter in the later study. (c) 2008 Wiley Periodicals, Inc.