Abstract: Resorcinol formaldehyde (RF) aerogel is prepared by using sol gel process and supercritical drying method, and carbonized resorcinol formaldehyde (CRF) aerogel with different microstructure is formed by pyrolyzing the RF aerogel at various temperature. Differential thermal analysis (DTA) and thermogravimetry analysis (TGA) are used to study the change of the ingredient of RF aerogel in order to find the best pyrolisis technique. The influence of the different pyrolisis temperature on the microstructure of CRF aerogel is studied by X ray differaction analysis. The results show that there are graphitic ribbons within the single particle of CRF aerogel, and the pyrolisis temperature and time has no significant influence on the microstructure of CRF aerogel.