Processes for preparing color stable red-emitting phosphor particles having small particle size
US-11952521-B2 · Apr 9, 2024 · US
US12528985B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-12528985-B2 |
| Application number | US-202418611080-A |
| Country | US |
| Kind code | B2 |
| Filing date | Mar 20, 2024 |
| Priority date | Dec 13, 2016 |
| Publication date | Jan 20, 2026 |
| Grant date | Jan 20, 2026 |
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A process for preparing a Mn +4 doped phosphor of formula I A x [MF y ]:Mn +4 I includes combining a first solution comprising a source of A and a second solution comprising H 2 MF 6 in the presence of a source of Mn, to form the Mn +4 doped phosphor; wherein A is Li, Na, K, Rb, Cs, or a combination thereof; M is Si, Ge, Sn, Ti, Zr, Al, Ga, In, Sc, Y, La, Nb, Ta, Bi, Gd, or a combination thereof; x is the absolute value of the charge of the [MF y ] ion; y is 5, 6 or 7; and wherein a value of a Hammett acidity function of the first solution is at least −0.9. Particles produced by the process may have a particle size distribution with a D 50 particle size of less than 10 μm.
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The invention claimed is: 1 . A Mn +4 doped phosphor of formula I A x [ MF y ] : Mn + 4 I the phosphor comprising a monodisperse population of particles having a particle size distribution comprising a D50 particle size of less than about 10 μm; wherein A is Li, Na, K, Rb, Cs, or a combination thereof; M is Si, Ge, Sn, Ti, Zr, Al, Ga, In, Sc, Y, La, Nb, Ta, Bi, Gd, or a combination thereof; x is an absolute value of a charge of the [MF y ] ion; y is 5, 6 or 7; and wherein the phosphor has a quantum efficiency of greater than 85% under blue excitation. 2 . The Mn +4 doped phosphor according to claim 1 , wherein the phosphor has an aspect ratio of a plurality of particles of the monodisperse population of less than or equal to 3/1. 3 . The Mn +4 doped phosphor according to claim 1 , wherein the phosphor has an amount of manganese from about 1.2 mol % to about 21 mol %. 4 . The Mn +4 doped phosphor according to claim 1 , wherein a span of the particle size distribution is less than 1.1. 5 . The Mn +4 doped phosphor according to claim 1 , wherein the phosphor is coated with a manganese-free shell. 6 . The Mn +4 doped phosphor according to claim 5 , wherein the manganese-free shell comprises a metal fluoride. 7 . The Mn +4 doped phosphor according to claim 5 , wherein the manganese-free shell is disposed on the phosphor. 8 . The Mn +4 doped phosphor according to claim 6 , wherein the metal fluoride is KMgF 3 . 9 . The Mn +4 doped phosphor according to claim 1 , wherein M is Si and A is Na or K. 10 . The Mn +4 doped phosphor according to claim 1 , wherein the phosphor comprises a D50 particle size from 5 μm to 8 μm. 11 . A Mn +4 doped phosphor of formula I A x [ MF y ] : Mn + 4 I the phosphor comprising a monodisperse population of particles having a particle size distribution comprising a D50 particle size of less than about 10 μm, wherein the phosphor is coated with a manganese-free shell, wherein A is Li, Na, K, Rb, Cs, or a combination thereof; M is Si, Ge, Sn, Ti, Zr, Al, Ga, In, Sc, Y, La, Nb, Ta, Bi, Gd, or a combination thereof; x is an absolute value of a charge of the [MF y ] ion; y is 5, 6 or 7. 12 . The Mn +4 doped phosphor according to claim 11 , wherein the manganese-free shell comprises a metal fluoride. 13 . The Mn +4 doped phosphor according to claim 12 , wherein the metal fluoride is KMgF 3 . 14 . The Mn +4 doped phosphor according to claim 11 , wherein the phosphor has an aspect ratio of a plurality of particles of the monodisperse population of less than or equal to 3/1. 15 . The Mn +4 doped phosphor according to claim 11 , wherein the phosphor has an amount of manganese from about 1.2 mol % to about 21 mol %. 16 . The Mn +4 doped phosphor according to claim 11 , wherein a span of the particle size distribution is less than 1.1. 17 . The Mn +4 doped phosphor according to claim 11 , wherein the manganese-free shell is disposed on the phosphor. 18 . The Mn +4 doped phosphor according to claim 11 , wherein M is Si and A is Na or K. 19 . The Mn +4 doped phosphor according to claim 11 , wherein the phosphor has a quantum efficiency of greater than 85% under blue excitation. 20 . The Mn +4 doped phosphor according to claim 11 , wherein the phosphor comprises a D50 particle size from 5 μm to 8 μm. 21 . A phosphor composition comprising the Mn +4 doped phosphor according to claim 1 and further comprising one or more materials selected from the group consisting of other phosphors, quantum dot materials, scattering particles, electroluminescent polymers and dyes. 22 . The phosphor composition according to claim 21 , wherein the Mn +4 doped phosphor has an aspect ratio of a plurality of particles of the monodisperse population of less than or equal to 3/1. 23 . The phosphor composition according to claim 21 , wherein the M n+4 doped phosphor has an amount of manganese from about 1.2 mol % to about 21 mol %. 24 . The phosphor composition according to claim 21 , wherein a span of the particle size distribution is less than 1.1. 25 . The phosphor composition according to claim 21 , wherein the Mn +4 doped phosphor is coated with a manganese-free shell. 26 . The phosphor composition according to claim 25 , wherein the manganese-free shell comprises a metal fluoride. 27 . The phosphor composition according to claim 25 , wherein the manganese-free shell is disposed on the Mn +4 doped phosphor. 28 . The phosphor composition according to claim 26 , wherein the metal fluoride is KMgF 3 . 29 . The phosphor composition according to claim 21 , wherein M is Si and A is Na or K. 30 . The phosphor composition according to claim 21 , wherein the Mn +4 doped phosphor has a quantum efficiency of greater than 85% under blue excitation. 31 . The phosphor composition according to claim 21 , wherein the other phosphors comprise β-SiAlON or a yellow phosphor. 32 . The phosphor composition according to claim 21 , wherein the one or more materials comprises quantum dots. 33 . A silicone slurry composition comprising an Mn +4 doped phosphor of formula I suspended in the slurry, A x [ MF y ] : Mn + 4
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