Method of producing beta-sialon fluorescent material

Patent metadata

Field	Value
Publication number	US-11512248-B2
Application number	US-202017033576-A
Country	US
Kind code	B2
Filing date	Sep 25, 2020
Priority date	Sep 27, 2019
Publication date	Nov 29, 2022
Grant date	Nov 29, 2022

Abstract

Provided a method of producing a β-sialon fluorescent material having excellent emission intensity. The method includes providing a first composition containing aluminum, an oxygen atom, and a europium-containing silicon nitride, heat treating the first composition, contacting the heat-treated composition and a basic substance to obtain a second composition, and contacting the second composition resulting from contacting the heat-treated composition with the basic substance and an acidic liquid medium containing an acidic substance.

First claim

What is claimed is:

1. A method of producing a β-sialon fluorescent material, the method comprising:
providing a first composition containing aluminium, an oxygen atom, and a europium-containing silicon nitride;
heat treating the first composition;
contacting the heat-treated composition and a basic substance to obtain a second composition; and
acid-treating the second composition comprising contacting the second composition and an acidic liquid medium containing an acidic substance to obtain an acid-treated product,
wherein the acidic liquid medium contains water and hydrogen chloride as the acidic substance,
wherein the acidic liquid medium contains the acidic substance in an amount of from 0.1% by weight to 5% by weight,
wherein σ log of the β-sialon fluorescent material after the acid treating is a range of 0.279 to 0.299,
wherein the method further comprises, before heat treating the first composition, strongly pulverizing the first composition with a europium compound to obtain a pulverized product containing the europium compound and heat treating in a nitrogen atmosphere the pulverized product containing the europium compound, and
wherein the pulverized product has a specific surface area of 0.20 m 2 /g or more.

2. The method according to claim 1 , wherein the basic substance contains at least one selected from the group consisting of alkali metal hydroxides and ammonia.

3. The method according to claim 1 , wherein the contacting of the heat-treated composition and the basic substance is carried out at a temperature of from 50° C. to 650° C.

4. The method according to claim 1 , wherein the contacting of the heat-treated composition and the basic substance includes contacting at a first temperature, and contacting at a second temperature that is higher than the first temperature.

5. The method according to claim 1 , wherein the contacting of the heat-treated composition and the basic substance includes mixing the heat-treated composition and a solution containing the basic substance and a solvent, and at least partially removing the solvent.

6. The method according to claim 1 , wherein the basic substance to be contacted with the heat-treated composition is 0.5% by weight or more relative to the heat-treated composition.

7. The method according to claim 1 , wherein the heat treating of the first composition is carried out in presence of a europium compound.

8. The method according to claim 1 , wherein the heat treating of the first composition is carried out at a temperature of from 1300° C. to 1600° C.

9. The method according to claim 1 , wherein the heat treating of the first composition is carried out in a rare gas atmosphere.

10. The method according to claim 1 , wherein the providing of the first composition includes heat treating a mixture containing an aluminium compound, a europium compound, and silicon nitride.

11. The method according to claim 1 , wherein the providing of the first composition comprises heat treating a mixture containing raw materials for the first composition in a nitrogen atmosphere.

12. The method according to claim 1 , wherein the first composition is represented by a formula:
Si 6-z Al z O z N 8-z :Eu,
wherein z satisfies 0<z≤4.2.

13. The method according to claim 1 , wherein the β-sialon fluorescent material obtained by contacting the second composition with acidic liquid medium have a greater volume median diameter than the second composition.

14. The method according to claim 1 , wherein a ratio of the volume median diameter of the β-sialon fluorescent material after the acid treating to the volume median diameter of the second composition before the acid treating is 1.01 or more.

15. The method according to claim 1 , wherein the β-sialon fluorescent material obtained by contacting the second composition with acidic liquid medium have a smaller specific surface area than the second composition.

16. The method according to claim 1 , wherein a ratio of the specific surface area of the second composition before the acid treating to the specific surface area of the β-sialon fluorescent material after the acid treating is 1.01 or more.

17. The method according to claim 1 , wherein the β-sialon fluorescent material obtained by contacting the second composition with acidic liquid medium have a smaller σ log than the second composition.

18. The method according to claim 1 , wherein the β-sialon fluorescent material obtained by contacting the second composition with acidic liquid medium has improved luminance compared to the second composition.

19. The method according to claim 1 , wherein an amount of the acidic liquid medium used in the acid treating is from 100% by weight to 1000% by weight relative to the second composition.

20. The method according to claim 1 , the method further comprising washing the acid-treated product with a liquid medium.

21. The method according to claim 1 , wherein a mole ratio of the europium compound is 0.01% by mole or more and 5% by mole or less with respect to the first composition.

Assignees

• Nichia Corp

Inventors

• Aoyagi Kenichi
• Kaide Takashi
• Takahashi Yuya
• Hosokawa Shoji

Classifications

• C09K11/7734 Primary

  Aluminates · CPC title

• C09K11/0883 Primary

  Arsenides; Nitrides; Phosphides · CPC title

• C01B21/0826 Primary

  Silicon aluminium oxynitrides, i.e. sialons · CPC title

• C01F17/30

  Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 (C01F17/247 - C01F17/294 take precedence) · CPC title

• C09K11/77348

  Silicon Aluminium Nitrides or Silicon Aluminium Oxynitrides · CPC title