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W/O emulsion was prepared with nano-TiO2 hydrosol as inner water phase,cyclohexane as oil phase and Span-80 as surfactant.The uniform and monodisperse nano-TiO2 hydrosol microcapsules were prepared in W/O/W multiple emulsion system with the stable W/O emulsion as capsule core and poly (vinyl alcohol) as wall material.TiO2 microspheres composed of anatase nano-particles can be obtained after the microcapsules were calcined at 500 ℃.