Thermal decomposition of C60 was studied by x-ray diffraction and time-of-flight mass spectroscopy, which was carried out in a high-purity argon gas for 3h at the temperature ranging from 500 to 1000°C. The diffraction peaks corresponding to C60 of cubic system were detected in the samples heated below 500°C. With the increase of temperature, these peaks of C60 were broadened, and the diffraction peaks corresponding to chaoite of hexagonal system were detected. From time-of-flight spectroscopy, it was found that two molecules of C22 and C48 were produced by heating C60 at 600°C, though not resolved C60 remained. The decomposition of C60 advanced with the increase of temperature. At 1000°C, it was found that C60 was decomposed into five molecules, such as C9, C22, C25, C35 and C48.