Fe3+　and　Eu3+　co-doped　TiO2　(Fe3+-Eu3+/TiO2)　hollow　microspheres　were　prepared　by　the　sol-gel　method　and　characterized　by　techniques　such　as　XRD,　TEM,　BET　and　XPS　etc.　Photocatalytic　degradation　of　methylene　blue　(MB)　was　used　as　a　probe　reaction　to　evaluate　their　photocatalytic　activity.　The　results　show　that　the　surface　of　SiO2　microspheres　evenly　coated　with　a　layer　of　TiO2　and　the　treatment　ultrasound　is　beneficial　to　improve　the　dispersion　of　the　SiO2@TiO2　composite　microspheres.　Part　of　the　Fe3+-Eu3+/TiO2　hollow　microspheres　were　collapse,　which　were　obtained　through　grinding　before　alcining　the　SiO2@TiO2　composite　microspheres.　While　the　better　structural　integrity　of　Fe3+-Eu3+/TiO2　hollow　microspheres　were　prepared　by　grinding　after　calcining　or　without　grinding.　XRD　and　BET　analysis　indicate　that　Fe3+-Eu3+/TiO2　hollow　microspheres　exist　in　the　form　of　anatase　and　have　good　mesoporous　structure.　The　co-doping　of　Fe3+　and　Eu3+　shows　a　synergistic　effect　in　TiO2　hollow　microspheres,　which　can　decrease　the　particle　size　of　Fe3+-Eu3+/TiO2　hollow　microspheres　and　and　increase　the　specific　surface　area.　When　the　doping　content　of　Fe3+　and　Eu3+　is　1.0%　and　0.5%　respectively,　Fe3+-Eu3+/TiO2　hollow　microspheres　exhibit　the　best　photocatalytic　activity.　©　2016,　BUAA　Culture　Media　Group　Ltd.　All　right　reserved.