Poly(ethylene-co-vinylacetate) (EVA) microspheres were prepared by thermally induced phase separation (TIPS) in toluene. The microsphere formation occurred by the nucleation and growth mechanism in metastable region. The effects of the concentration and component of the polymer and cooling rate on microsphere formation were investigated. The microsphere formation and growth were followed by the cloud point of the optical microscope measurement. The microsphere size distribution, which was obtained by particle size analyzer, became broader when the polymer concentration was higher, the content of vinyl acetate in EVA copolymer was higher, the cooling rate of EVA copolymer solution were lower. The content of disperse dye in EVA microsphere was obtained by TGA thermal analysis, the dye content of EVA15 and EVA18 were 3.5 and 2.0 wt% respectively.