In this study the recovery method of fluorine in waste and characteristics of NaF powder prepared with the reaction of NaOH and NH4F in waste which was generated from nuclear fuel powder production process were investigated. The NaOH was selected to reasonable and suitable material for recovery of the fluorine in waste because it can be used in the pre0-treatment step for removal of a trace uranium in wastes. As experimental results the concentration of the fluorine in waste was about 100 g/F/L and the recovery efficiency of fluorine was showed to 86% at 1.2mole ratio of Na/F respectively. And shape of the NaF particles was appeared to mixed up with cubic and tetragonal structures. Also this fine NaF particles stongly agglomerated could be grown up from about 5 ${mu}{ extrm}{m}$ to 20-30${mu}{ extrm}{m}$ by control of the NaOH feed rate. Otherwise F concentration of the final filtrate could be reduced to lower than 2 ppm if treating with the lime and adding the HNO3