The heated process of raw materials for electron trapping materials (ETM) is investigated by thermo-analysis method. The temperature ranges of raw materials experienced some physical and chemical change processes, such as dehydration, organic solvent removal, crystal sulphur burning, oxidation of alkaline earth sulfides and solid phase reaction (rare earth doped) and so on, are obtained. The experimental results also show that the presence of trace oxygen in shielded gas is very harmful to prepare the ETM.The raw material thermo-analysis results provide very important experimental reference for optimizing the ETM preparation techniques.