The invention discloses micro/nano potassium yttrium tungstate near-spherical particles and a preparation method thereof. The preparation method comprises the following steps: regulating the pH value of a soluble tungstate solution to 7-8.5 and the pH value of Y<3+> of the yttrium ion solution to 5-6.5, mixing according to the tungstate ion:yttrium ion mol ratio of 2:1, regulating the pH value of the mixed solution to 5-7.5, uniformly stirring, adding acetylacetone accounting for 10-20 vol% of the mixed solution, and carrying out ultrasonic vibration to obtain a precursor solution; holding the precursor solution by hydrothermal sealing to obtain a white precipitate, wherein the hydrothermal temperature is 140-180 DEG C, and the holding time is 20-24 hours; and centrifuging the white precipitate, and carrying out heat treatment to obtain the micro/nano potassium yttrium tungstate near-spherical particles. The micro/nano potassium yttrium tungstate near-spherical particles are composed of KY(WO4)2 particles, the particle size is 0.100-1 mu m, and the particle shape is near-spherical. The invention enhances the luminescence efficiency of the powder, can be used as a luminescent material, and can be widely used in the fields of road signs, various energy-saving illuminators, biomedical labels, aviation display devices, various meters and computers, and the like.