This paper reports the preparation of nano-TiO2 (about 10 nm) powder by the method of precipitation. In detail, some breparation conditions were investigated in order to find out how to control the grain size and reduce the agglomeration of powders. Also, the reflex spectra of nano-scale powders with different grain size were studied. It tvas found that the wave length and width of reflex spectra are connected with the grain size of nano-TiO2 powders This paper reports the preparation of nano-TiO2 (about 10 nm) powder by the method of precipitation. In detail, some breparation conditions were investigated in order to find out how to control the grain size and reduce the agglomeration of powders. Also, the reflex spectra of nano-scale powders with different grain size were studied. It tvas found that the wave length and width of reflex spectra are connected with the grain size of nano-TiO2 powders