Iron-doped　titanium　dioxide　hollow　microspheres　were　prepared　hydrothermally　using　titanium　tetrafluoride　and　ferric　nitrate　nonahydrate　in　aqueous　solution　as　starting　materials,　and　were　characterized　by　scanning　electron　microscopy　(SEM),　transmission　electron　microscopy　(TEM),　X-ray　diffraction　(XRD),　surface　area　(BET)　and　X-ray　photoelectron　spectroscopy　(XPS).　Photocatalytic　activity　of　the　microspheres　was　evaluated　on　photocatalytic　degradation　of　aqueous　methylene　blue　(MB).　TiO2　in　hollow　microspheres　created　at　160　were　anatase　crystal　and　doping　a　relatively　small　amount　of　iron　did　not　alter　morphology　and　crystal　structure　of　TiO2.　Iron　doping　could　significantly　improve　the　photocatalytic　activity　of　TiO2　hollow　microspheres.　The　TiO2　hollow　microspheres　obtained　at　a　condition　of　160　for　12　h　had　optimal　dimensional　uniformity　and　photocatalytic　activity,　which　the　best　photocatalytic　effect　were　observed　on　hollow　microspheres　with　a　1.5%　ratio　of　iron　over　titanium　because　of　the　smallest　size　and　the　highest　surface　area.　©　All　Right　Reserved.