Phase Chang Material Microcapsules were prepared by a simple coacervation method, and were observed the surface of manufacturing process on microcapsules by optical microscope. The experimental result shows that the wall/core ratio 26.1% was obtained after 4hr coacervation better than others. The various dispersants could be affected the wall/core ratio of microcapsule. It was able to determined that microcapsules made from polystyrene and Na2SO4•10H2O each wall and core by FTIR. Diameter of microcapsules were tested by MasterSizer(MAL30007S MALVERN UK) and found diameter of microcapsules had larger relation with stirring speed. Thermal properties of Phase Change Material was examined by DSC and still had great thermal effective though this produce process.