US 11,939,503 B2
Method for preparing manganese-doped red phosphor, product, device, and backlight module
Lei Chen, Anhui (CN); Peng Cheng, Anhui (CN); Jie Chen, Anhui (CN); Yunfei Tian, Anhui (CN); Jialong Wang, Anhui (CN); Liangrui He, Anhui (CN); Qiuhong Zhang, Anhui (CN); and Haiyong Ni, Anhui (CN)
Assigned to Hefei University of Technology, Hefei (CN); and Intelligent Manufacturing Institute of HFUT, Hefei (CN)
Appl. No. 17/272,349
Filed by INTELLIGENT MANUFACTURING INSTITUTE OF HEFEI UNIVERSITY OF TECHNOLOGY, Anhui (CN)
PCT Filed Oct. 26, 2018, PCT No. PCT/CN2018/112158
§ 371(c)(1), (2) Date Apr. 28, 2021,
PCT Pub. No. WO2020/042319, PCT Pub. Date Mar. 5, 2020.
Claims priority of application No. 201811006339.7 (CN), filed on Aug. 30, 2018.
Prior Publication US 2021/0324265 A1, Oct. 21, 2021
Int. Cl. C09K 11/67 (2006.01); C09K 11/61 (2006.01); C09K 11/66 (2006.01); H01L 33/50 (2010.01)
CPC C09K 11/675 (2013.01) [C09K 11/617 (2013.01); C09K 11/665 (2013.01); H01L 33/502 (2013.01); H01L 2933/0041 (2013.01)] 5 Claims
OG exemplary drawing
 
1. A preparation method for manganese-doped red phosphor, wherein the method comprises:
1) mixing A2BF6 polycrystalline particles with grinding balls, wherein a mass ratio of the A2BF6 polycrystalline particles to the grinding balls is 1:1 to 1:2.5, and then ball-milling for 30 minutes to 120 minutes, wherein A is a monovalent cation, at least one selected from the group consisting of a potassium ion, a hydrogen ion, a lithium ion, a sodium ion and a cesium ion, and B is a tetravalent cation, at least one selected from the group consisting of a titanium ion a silicon ion, a germanium ion, a tin ion, and a zirconium ion;
2) secondary crystallization treatment: mixing A2BF6 powder obtained after ball-milling with a hydrofluoric acid, a mass concentration of the hydrofluoric acid is 30% to 59%, wherein a mass ratio of the A2BF6 powder obtained after ball-milling to the hydrofluoric acid is 1:1 to 2.5:1, and then at a revolving speed of 1 RPM to 1200 RPMs, stirring for 12 hours to 72 hours;
3) filtering out solid particles in A2BF6 and hydrofluoric acid solution after the secondary crystallization treatment, to obtain secondary crystallization A2BF6 particles;
4) according to a molar ratio of A2BF6 and A2MnF6 which is 93:7 to 90:10, weighing the secondary crystallization A2BF6 particles and A2MnF6, and then firstly dissolving A2MnF6 in a hydrofluoric acid, a mass concentration of the hydrofluoric acid is 30% to 59%, and then adding the secondary crystallization A2BF6 particles to a solution comprising the A2MnF6 and the hydrofluoric acid, and continuously stirring for 10 minutes to 360 minutes for ion exchange, wherein a ratio of a total mass of A2BF6 and A2MnF6 to a mass of the hydrofluoric acid is 1:1 to 4:1; and
5) filtering out solid particles in solution after the ion exchange, to obtain a filter cake, and then drying the filter cake to obtain the manganese-doped red phosphor.