Metal halide colloidal nanoparticles and method for producing the same

Patent metadata

Field	Value
Publication number	US-12139653-B2
Application number	US-202217574717-A
Country	US
Kind code	B2
Filing date	Jan 13, 2022
Priority date	Jan 13, 2021
Publication date	Nov 12, 2024
Grant date	Nov 12, 2024

Abstract

The present invention relates to metal halide colloidal nanoparticles represented by a following Chemical Formula 1 and a method for producing the same:A3MX6  [Chemical Formula 1]wherein in the Chemical Formula 1, A is an alkali metal element, M is a rare-earth metal element, and X is a halogen element.

First claim

What is claimed is:

1. Metal halide colloidal nanoparticles represented by the following Chemical Formula 1:
A 3 MX 6   [Chemical Formula 1]

wherein in the Chemical Formula 1, A is an alkali metal element, M is a rare-earth metal element, and X is a halogen element,
wherein the metal halide colloidal nanoparticles absorb an excitation wavelength in a range of 250 to 320 nm and thus emit light in a light-emission spectrum of 500 to 570 nm or 580 to 630 nm, and
wherein the metal halide colloidal nanoparticles absorb an excitation wavelength in a range of 320 to 450 nm and thus emit light in a light-emission spectrum of 380 to 480 nm.

2. The metal halide colloidal nanoparticles of claim 1 , wherein A is Cs, Rb, K, Na, Li, or a combination thereof,
M is gadolinium (Gd), yttrium (Y), ytterbium (Yb), erbium (Er), europium (Eu), cerium (Ce), terbium (Tb), or a combination thereof, and
X is F, Cl, Br, I, or a combination thereof.

3. The metal halide colloidal nanoparticles of claim 1 , wherein an average particle diameter of each of the metal halide colloidal nanoparticles is in a range of 1 to 100 nm.

4. The metal halide colloidal nanoparticles of claim 1 , wherein a surface of the metal halide colloidal nanoparticle is coated with an organic ligand.

5. The metal halide colloidal nanoparticles of claim 4 , wherein the organic ligand includes at least one selected from a group consisting of a compound derived from R 1 COOH, a compound derived from R 2 NH 2 , a compound derived from R 2 R 3 NH, a compound derived from R 2 R 3 R 4 N, and a compound derived from a first non-polar solvent,
wherein R 1 , R 2 , R 3 and R 4 are the same as or different from each other, and each of R 1 , R 2 , R 3 and R 4 independently represents a saturated or unsaturated alkyl group having 2 to 28 carbon atoms.

6. The metal halide colloidal nanoparticles of claim 5 , which are coated with an organic ligand including a compound derived from R 1 COOH, wherein R 1 COOH comprises one acid selected from a group consisting of oleic acid, stearic acid, myristic acid, lauric acid, palmitic acid, elaidic acid, eicosanoic acid, heneicosanoic acid, tricosanoic acid, docosanoic acid, tetracosanoic acid, hexacosanoic acid, heptacosanoic acid, octacosanoic acid, and cis-13-docosenoic acid.

7. The metal halide colloidal nanoparticles of claim 5 , which are coated with an organic ligand including a compound derived from R 2 NH 2 , or a compound derived from R 2 R 3 NH, or a compound derived from R 2 R 3 R 4 N, wherein R 2 NH 2 comprises one amine selected from a group consisting of octylamine, nonylamine, heptylamine, hexylamine, pentylamine, hexadecanamine, octadecylamine, dodecylamine, and oleylamine,
wherein R 2 R 3 NH comprises one amine selected from a group consisting of dimethylamine, diethylamine, dipropylamine, and dioctylamine, wherein R 2 R 3 R 4 N comprises trioctylamine.

8. The metal halide colloidal nanoparticles of claim 5 , wherein the first non-polar solvent comprises at least one solvent selected from a group consisting of heptadecane, nonadecane, octadecene, heptadecane, dodecane, or octadecane.

9. A method for producing metal halide colloidal nanoparticles, the method comprising:
(a) preparing a mixed solution including R 1 COOH, R 2 NH 2 , R 2 R 3 NH, or R 2 R 3 R 4 N, and a first non-polar solvent,
wherein R 1 , R 2 , R 3 and R 4 are the same as or different from each other, and each of R 1 , R 2 , R 3 and R 4 independently represents a saturated or unsaturated alkyl group having 2 to 28 carbon atoms;
(b) adding an alkali metal precursor and a rare-earth metal precursor to the mixed solution and stirring the mixed solution to produce a stirred solution; and
(c) reacting the stirred solution to produce metal halide colloidal nanoparticles represented by a following Chemical Formula 1,
A 3 MX 6   [Chemical Formula 1]

wherein in the Chemical Formula 1, A is an alkali metal element, M is a rare-earth metal element, and X is a halogen element.

10. The method of claim 9 , wherein A is Cs, Rb, K, Na, Li, or a combination thereof,
M is gadolinium (Gd), yttrium (Y), ytterbium (Yb), erbium (Er), europium (Eu), cerium (Ce), terbium (Tb), or a combination thereof, and
X is F, Cl, Br, I, or a combination thereof.

11. The method of claim 9 , wherein R 1 COOH comprises one acid selected from a group consisting of oleic acid, stearic acid, myristic acid, lauric acid, palmitic acid, elaidic acid, eicosanoic acid, heneicosanoic acid, tricosanoic acid, docosanoic acid, tetracosanoic acid, hexacosanoic acid, heptacosanoic acid, octacosanoic acid, and cis-13-docosenoic acid.

12. The method of claim 9 , wherein R 2 NH 2 comprises one amine selected from a group consisting of octylamine, nonylamine, heptylamine, hexylamine, pentylamine, hexadecanamine, octadecylamine, dodecylamine, and oleylamine,
wherein R 2 R 3 NH comprises one amine selected from a group consisting of dimethylamine, diethylamine, dipropylamine, and dioctylamine,
wherein R 2 R 3 R 4 N comprises trioctylamine.

13. The method of claim 9 , wherein in the (a), R 1 COOH: R 2 NH 2 , or R 1 COOH: R 2 R 3 NH, or R 1 COOH: R 2 R 3 RAN are mixed with each other in a molar ratio of 1:0.5 to 2, and
R 1 COOH: the first non-polar solvent is mixed with each other in a molar ratio of 1:10 to 40.

14. The method of claim 9 , wherein the (b) comprises producing the stirred solution by stirring the mixed solution in a vacuum state at 100 to 150° C. for 1 to 10 hours.

15. The method of claim 9 , wherein the (c) comprises producing metal halide colloidal nanoparticles by reacting the stirred solution at 200 to 285° C. for 15 to 120 minutes under presence of an inert gas.

16. A light emitting device including the metal halide colloidal nanoparticles of claim 1 .

Assignees

• Chung Ang Univ Academic Cooperation Foundation
• Univ Chung Ang Ind Acad Coop Found

Inventors

• Paik Tae Jong
• Lee Min Ji

Classifications

• C09K11/7748

  with alkali or alkaline earth metals · CPC title

• B82Y20/00

  Nanooptics, e.g. quantum optics or photonic crystals · CPC title

• C01P2004/64

  Nanometer sized, i.e. from 1-100 nanometer · CPC title

• C09K11/025 Primary

  non-luminescent particle coatings or suspension media · CPC title

• B82Y40/00

  Manufacture or treatment of nanostructures · CPC title