Raw materials, La2O3, SrCO3 and MnO2, were used to obtain lanthanum strontium manganite (LSM) spherical particles with unstable structure by ball milling and spray drying. LSM spherical particles need to be degreased at low temperature to eliminate organic inside the particles. Both weight loss and heat change of curve of LSM spherical particles between 0-1300 ℃ were analyzed by TGA-DSC and determine the degreasing temperature range, in order to study the behavior change of unstable LSM spherical particles during degreasing process. Then degreasing temperature, heating rate and holding time were determined by experiments. The results show that degreasing temperature is 550 ℃, the heating rate is less than 5 ℃/min and the holding time is 4 h, the spherical appearance of LSM spherical particles is not damaged and the organic can be effectively removed.