This article describes the preparation of monodispersed microspheres of glycidyl methacrylate, 2-hydroxyethyl methacrylate, and triethylene glycol dimethacrylate by radical polymerization. The initial stage of the polymerization reaction began in the liquid phase. As the polymerization proceeded, a nuclear polymer chain of microspheres was generated from soluble oligomeric radicals and then solidified from the liquid phase. The radius of the microspheres was controlled by polymerization parameters, such as monomer concentration, polymerization time, and the kind of polymerization solvent. A small number of thin platelike substances may be produced by the anisotropy of the two-dimensional monomer added to the oligomeric radicals. The monodispersed microspheres were achieved through the use of the following : (1) a fluorinated tube in which the polymerization reaction proceeded; (2) a monomer concentration of about 1 mol/L; (3) a higher concentration of crosslinking reagent than used commercially; (4) the prevention of the occurrence of polymer microsphere aggregation; (5) pouring the solution mixtures into a large amount of cooled acetone after the polymerization reaction; and (6) the use of a low-temperature purification process and centrifugation at low temperature. This article describes the mechanism of microsphere formation and growth by solution polymerization.