The crystallization of polypropylene (PP) particles in PP/decalin solution was conducted using the thermally induced phase separation(TIPS). During the control of particles sizes followed by the cooling of PP/decalin solution, particles were formed controllably, the concentrated PP resulted in an increase in the average diameter of PP particles. The effects of surfactants changes on particles sizes were investigated by using a field emission scanning electron microscope (FE-SEM). The PP crystals showed spherical shapes with a diameter 5∼18 μm. Additionally, as an effect of concentration of PP, the size distribution of the PP particles became broad with higher concentration of PP in the solution.