This Study applies to Stöber method for synthesis an characterization of even-sized SiO2 micrometer sphere; and then applies to sol-gel method for encapsulation for one layer of ZnO at SiO2 spherical surface after regarded it as core so that synthesis SiO2/ZnO core-shell spheres successfully. And observe morphology by FE-SEM and crossection by TEM. The TEM specimen were cut by two-beam FIB. Besides, EDS, XRD and UV-Visible spectroscopy were using for the analysis of composition, crystallization structure, and absorption spectrum, respectively. Experimental results showed that, SiO2 spherical surface became smooth after deposition for zinc oxide. The specimen made by FIB more obviously was observed for core-shell distribution by TEM. EDS analysis made us clearly see shell signal with ZnO content, but core signal only is SiO2 content. XRD analysis indicated its core-shell sphere signal possessing ZnO content, but UV-Visible absorption spectrometer displayed ZnO has been absorbed in range of UV light, in contrast, it is not absorbed in range of visible light.