Method of manufacturing fluoride phosphor, white light emitting apparatus, display apparatus, and lighting device

Patent metadata

Field	Value
Publication number	US-10000695-B2
Application number	US-201514981887-A
Country	US
Kind code	B2
Filing date	Dec 28, 2015
Priority date	Dec 26, 2014
Publication date	Jun 19, 2018
Grant date	Jun 19, 2018

Abstract

A method of manufacturing a fluoride phosphor, the method comprising: preparing a hydrofluoric (HF) solution in which a first source material and a fluoride containing Mn 4+ are dissolved; and forming fluoride particles by introducing a second source material to the HF solution in each of a plurality of instances.

First claim

What is claimed is:

1. A method of manufacturing a fluoride phosphor, the method comprising,
preparing a hydrofluoric (HF) solution dissolving a first source material containing M, where M is at least one selected from the group consisting of silicon (Si), titanium (Ti), zirconium (Zr), hafnium (Hf), germanium (Ge) and tin (Sn), and a fluoride containing Mn 4+ ; and
forming fluoride particles by introducing a second source material containing A, where A is at least one selected from the group consisting of lithium (Li) sodium (Na) potassium (K), rubidium (Rb), and cesium (Cs), to the HF solution in each of a plurality of instances,
where the fluoride particles have a chemical formula of A x MF y :Mn 4+ ;
a compositional ratio (x) of A satisfies 2≤x≤3; and
a compositional ratio (y) of F satisfies 4≤x≤7, and
wherein the introducing of the second source material to the HF solution is repeated until a quartile deviation (Q.D.) of a size distribution of the fluoride particles is equal or less than 0.2.

2. The method of claim 1 ,
wherein the Mn 4+ -containing fluoride includes a manganese fluoride having an A x MnF y composition.

3. The method of claim 1 ,
wherein the first source material containing M includes at least one selected from the group consisting of H x MF y , A x MF y , and MO 2 .

4. The method of claim 1 ,
wherein the second source material containing A includes AHF 2 .

5. The method of claim 1 ,
wherein a number of the instances of introducing the second source material is greater than or equal to four,
wherein fluoride seeds form in a first instance of the instances,
wherein the fluoride seeds grow to the fluoride particles in remaining instances of the instances.

6. The method of claim 1 ,
wherein the forming of the fluoride particles includes:
forming fluoride seeds by a primary introduction of the second source material; and
growing the fluoride seeds to form the fluoride particles by at least one secondary introduction of the second source material.

7. The method of claim 6 ,
wherein an amount of the second source material introduced in the primary introduction ranges from 5 to 30 wt % of a total amount of the second source material.

8. The method of claim 6 ,
wherein an interval between the primary introduction and the at least one secondary introduction ranges from 5 to 30 minutes.

9. The method of claim 6 , wherein the at least one secondary introduction of the second source material comprises a plurality of secondary introductions of the second source material.

10. The method of claim 9 , wherein a number of the secondary introductions of the second source material is greater than or equal to three.

11. The method of claim 1 , wherein introducing the second source material to the HF solution is repeated until a mass median diameter (d50) of the fluoride particles ranges from about 5 to about 25 μm.

12. The method of claim 1 , further comprising:
cleaning the fluoride particles; and
removing fine powder from surfaces of the fluoride particles by introducing the cleaned fluoride particles to an organic solvent and performing a sonification process thereon.

13. The method of claim 1 , wherein the preparing of the HF solution includes:
introducing the first source material to the HF solution; and
introducing the fluoride containing Mn 4+ to the HF solution to which the first source material has been introduced.

14. The method of claim 1 , further comprising:
if one of the first and second source materials is in excess after the forming of the fluoride particles, additionally introducing the other of the first and second source materials to the HF solution with the one of the first and second source material in excess to coat the fluoride particles with an Mn-free fluoride.

15. The method of claim 1 , further comprising:
after forming the fluoride particles, cleaning the fluoride particles; and
introducing the cleaned fluoride particles and an organic material to a solvent to coat surfaces of the fluoride particles with the organic material.

16. A method of manufacturing a fluoride phosphor, the method comprising:
introducing a first source material containing M to a hydrofluoric (HF) solution;
introducing a fluoride containing Mn 4+ to the HF solution;
dividedly introducing a second source material containing A to the HF solution a plurality of times to form fluoride particles satisfying A x MF y :Mn 4+ ; and
if one of the first and second source materials is in excess after the fluoride particles are formed, additionally introducing the other of the first and second source materials to the HF solution in which the fluoride particles have been formed, to coat the fluoride particles with an Mn-free fluoride,
wherein M is at least one selected from the group consisting of silicon (Si), titanium (Ti), zirconium (Zr), hafnium (Hf), germanium (Ge), and tin (Sn), A is at least one selected from the group consisting of lithium (Li), sodium (Na), potassium (K), rubidium (Rb), and cesium (Cs), a compositional ratio (x) of A satisfies 2≤x≤3, and a compositional ratio (y) of F satisfies 4≤y≤7.

17. The method of claim 16 , the second source material is introduced in a saturation solution state or in a powder state.

18. A method of manufacturing a fluoride phosphor, the method comprising:
preparing a hydrofluoric (HF) solution dissolving a first source material containing M and a fluoride containing Mn4+; and
forming fluoride particles by introducing a second source material containing A to the HF solution in each of a plurality of instances,
wherein the fluoride particles have a chemical formula of AxMFy:Mn4+:
a compositional ratio (x) of A satisfies 2≤x≤3; and
a compositional ratio (y) of F satisfies 4≤y≤7,

wherein the forming of the fluoride particles includes:
forming fluoride seeds by a primary introduction of the second source material; and
growing the fluoride seeds to form the fluoride particles by at least one secondary introduction of the second source material, and

wherein an amount of the second source material introduced in the primary introduction ranges from 5 to 30 wt % of a total amount of the second source material.

Assignees

• Min Chan Suk
• Kim Tae Hoon
• Park Jong Won
• You Ji Ho
• Oh Jeong Rok
• Yoon Chul Soo
• Lee In Hyung
• Lee Chi Woo
• Samsung Electronics Co Ltd

Inventors

• Min Chan Suk
• Kim Tae Hoon
• Park Jong Won
• You Ji Ho
• Oh Jeong Rok
• Yoon Chul Soo
• Lee In Hyung
• Lee Chi Woo

Classifications

• H10W90/753

  between laterally-adjacent chips · CPC title

• H10W74/00

  Encapsulations, e.g. protective coatings · CPC title

• H10W72/884

  Die-attach connectors and bond wires · CPC title

• H01L33/00

  Electricity · mapped topic

• C09K11/025

  non-luminescent particle coatings or suspension media · CPC title