Method of manufacturing inorganic oxide particle, method of manufacturing inorganic oxide layer, and light-emitting device including inorganic oxide layer manufactured by the method

Patent metadata

Field	Value
Publication number	US-12552680-B2
Application number	US-202217849542-A
Country	US
Kind code	B2
Filing date	Jun 24, 2022
Priority date	Jun 28, 2021
Publication date	Feb 17, 2026
Grant date	Feb 17, 2026

Abstract

A method of manufacturing an inorganic oxide particle having an inorganic oxide core and a hydroxyl group bonded to a surface thereof includes: preparing a first composition including an inorganic oxide core precursor and a proton supply compound; and heating the first composition. Additional embodiments provide a method of manufacturing an inorganic oxide layer including an inorganic oxide particle manufactured by the method, and a light-emitting device including an inorganic oxide layer manufactured by the method.

First claim

What is claimed is:

1 . A method of manufacturing an inorganic oxide particle comprising an inorganic oxide core and a hydroxyl group bonded to a surface of the inorganic oxide core, the method comprising:
preparing a first composition, the first composition comprising an inorganic oxide core precursor and a proton supply compound; and heating the first composition, wherein the proton supply compound comprises a carboxylic acid-containing compound and/or a peroxide-containing compound, and wherein the hydroxyl group is bonded only to the surface of the inorganic oxide core.

2 . The method of claim 1 , wherein the inorganic oxide core precursor comprises an oxide represented by Formula 1:
M 1 x M 2 1-x O y ,and  Formula 1
wherein, in Formula 1, M 1 and M 2 are each independently Zn, Mg, Co, Mn, Y, Al, Ti, Zr, Sn, W, Ta, Ni, Mo, Cu, Ag, or a combination thereof, 0≤x≤1, and 0<y≤5.

3 . A method of manufacturing an inorganic oxide particle comprising an inorganic oxide core and a hydroxyl group bonded to a surface of the inorganic oxide core, the method comprising:
preparing a first composition, the first composition comprising an inorganic oxide core precursor and a proton supply compound; and heating the first composition, wherein the proton supply compound comprises a carboxylic acid-containing compound and/or a peroxide-containing compound, wherein the carboxylic acid-containing compound is represented by Formula 2, and the peroxide-containing compound is represented by Formula 3:

wherein, in Formulae 2 and 3,
R 1 and R 2 are each independently hydrogen, deuterium, —F, —Cl, —Br, —I, a hydroxyl group, a cyano group, a nitro group, a C 1 -C 60 alkyl group unsubstituted or substituted with at least one R 10a , a C 2 -C 60 alkenyl group unsubstituted or substituted with at least one R 10a , a C 2 -C 60 alkynyl group unsubstituted or substituted with at least one R 10a , a C 1 -C 60 alkoxy group unsubstituted or substituted with at least one R 10a , a C 3 -C 60 carbocyclic group unsubstituted or substituted with at least one R 10a , a C 1 -C 60 heterocyclic group unsubstituted or substituted with at least one R 10a , a C 6 -C 60 aryloxy group unsubstituted or substituted with at least one R 10a , a C 6 -C 60 arylthio group unsubstituted or substituted with at least one R 10a , a C 7 -C 60 arylalkyl group unsubstituted or substituted with at least one R 10a , a C 2 -C 60 heteroarylalkyl group unsubstituted or substituted with at least one R 10a , —Si(Q 1 )(Q 2 )(Q 3 ), —N(Q 1 )(Q 2 ), —B(Q 1 )(Q 2 ), —C(═O)(Q 1 ), —S(═O) 2 (Q 1 ), or —P(═O)(Q 1 )(Q 2 ), and
R 10a is:
deuterium, —F, —Cl, —Br, —I, a hydroxyl group, a cyano group, or a nitro group;
a C 1 -C 60 alkyl group, a C 2 -C 60 alkenyl group, a C 2 -C 60 alkynyl group, or a C 1 -C 60 alkoxy group, each unsubstituted or substituted with deuterium, —F, —Cl, —Br, —I, a hydroxyl group, a cyano group, a nitro group, a C 3 -C 60 carbocyclic group, a C 1 -C 60 heterocyclic group, a C 6 -C 60 aryloxy group, a C 6 -C 60 arylthio group, a C 7 -C 60 arylalkyl group, a C 2 -C 60 heteroarylalkyl group, —Si(Q 11 )(Q 12 )(Q 13 ), —N(Q 11 )(Q 12 ), —B(Q 11 )(Q 12 ), —C(═O)(Q 11 ), —S(═O) 2 (Q 11 ), —P(═O)(Q 11 )(Q 12 ), or any combination thereof;
a C 3 -C 60 carbocyclic group, a C 1 -C 60 heterocyclic group, a C 6 -C 60 aryloxy group, a C 6 -C 60 arylthio group, a C 7 -C 60 arylalkyl group, or a C 2 -C 60 heteroarylalkyl group, each unsubstituted or substituted with deuterium, —F, —Cl, —Br, —I, a hydroxyl group, a cyano group, a nitro group, a C 1 -C 60 alkyl group, a C 2 -C 60 alkenyl group, a C 2 -C 60 alkynyl group, a C 1 -C 60 alkoxy group, a C 3 -C 60 carbocyclic group, a C 1 -C 60 heterocyclic group, a C 6 -C 60 aryloxy group, a C 6 -C 60 arylthio group, a C 7 -C 60 arylalkyl group, a C 2 -C 60 heteroarylalkyl group, —Si(Q 21 )(Q 22 )(Q 23 ), —N(Q 21 )(Q 22 ), —B(Q 21 )(Q 22 ), —C(═O)(Q 21 ), —S(═O) 2 (Q 21 ), —P(═O)(Q 21 )(Q 22 ), or any combination thereof; or
—Si(Q 31 )(Q 32 )(Q 33 ), —N(Q 31 )(Q 32 ), —B(Q 31 )(Q 32 ), —C(═O)(Q 31 ), —S(═O) 2 (Q 31 ), or —P(═O)(Q 31 )(Q 32 ), and
wherein Q 1 to Q 3 , Q 11 to Q 13 , Q 21 to Q 23 , and Q 31 to Q 33 are each independently: hydrogen; deuterium; —F; —CI; —Br; —I; a hydroxyl group; a cyano group; a nitro group; a C 1 -C 60 alkyl group; a C 2 -C 60 alkenyl group; a C 2 -C 60 alkynyl group; a C 1 -C 60 alkoxy group; a C 3 -C 60 carbocyclic group or a C 1 -C 60 heterocyclic group, each unsubstituted or substituted with deuterium, —F, a cyano group, a C 1 -C 60 alkyl group, a C 1 -C 60 alkoxy group, a phenyl group, a biphenyl group, or any combination thereof; a C 7 -C 60 arylalkyl group; or a C 2 -C 60 heteroarylalkyl group.

4 . The method of claim 1 , wherein the first composition further comprises a first solvent, and
the first solvent comprises an alcohol-based solvent, an ether-based solvent, an aliphatic hydrocarbon-based solvent, an aromatic hydrocarbon-based solvent, or any combination thereof.

5 . The method of claim 1 , wherein an amount of the proton supply compound in the first composition is in a range of about 0.01 parts by weight to about 30 parts by weight based on 100 parts by weight of the inorganic oxide core precursor.

6 . The method of claim 1 , wherein the heating of the first composition is performed at a temperature of 30° C. or higher.

7 . A method of manufacturing an inorganic oxide layer comprising an inorganic oxide particle comprising an inorganic oxide core and a hydroxyl group bonded to a surface of the inorganic oxide core, the method comprising:
providing, on a substrate, a second composition comprising the inorganic oxide particle and a second solvent; and heating the second composition, wherein the hydroxyl group is bonded only to the surface of the inorganic oxide core.

8 . The method of claim 7 , wherein an average particle diameter (D50) of the inorganic oxide particle is in a range of about 1 nm to about 30 nm.

9 . The method of claim 7 , wherein the second solvent comprises an alcohol-based solvent, a chlorine-based solvent, an ether-based solvent, an ester-based solvent, a ketone-based solvent, an aliphatic hydrocarbon-based solvent, or any combination thereof.

10 . The method of claim 7 , wherein an amount of the inorganic oxide particle in the second composition is in a range of about 0.1parts by weight to about 20 parts by weight based on 100 parts by weight of the second solvent.

11 . The method of claim 7 , wherein the heating of the second composition is performed at a temperature of 70° C. or higher.

12 . A light-emitting device comprising:
a first electrode; a second electrode facing the first electrode; and an interlayer between the first electrode and the second electrode and comprising an emission layer and an inorganic oxide layer, wherein the inorganic oxide layer is manufactured according to the method of claim 7 .

13 . The light-emitting device of claim 12 , wherein a thickness of the inorganic oxide layer is in a range of about 5 nm to about 200 nm.

14 . The light-emitting device of claim 12 , wherein the interlayer further comprises:
a hole transport region located between the first electrode and the emission layer; and an electron transport region located between the emission layer and the second electrode, and wherein the electron transport region comprises the inorganic oxide layer.

Assignees

• Samsung Display Co Ltd

Inventors

• Doh Hyunmi
• Lee Changhee
• Kang Jingoo
• Kim Sehun
• Kim Yonghwi
• Kim Jonghoon
• Noh Seunguk
• Park Myoungjin
• Jung Yunku

Classifications

• H10K2102/351

  Thickness · CPC title

• H10K2102/331

  Nanoparticles used in non-emissive layers, e.g. in packaging layer · CPC title

• H10K71/00

  Manufacture or treatment specially adapted for the organic devices covered by this subclass · CPC title

• H10K50/171

  Electron injection layers · CPC title

• H10K50/115

  comprising active inorganic nanostructures, e.g. luminescent quantum dots · CPC title