# US 12,765,158 B2 · Process for the halogen treatment of metal oxide layers

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- Number: US 12,765,158 B2
- Document ID: US12765158B2
- Status: Granted
- Kind: B2
- Application number: 17/707,465
- Filed: 2022-03-29
- Published: 2023-10-05
- Granted: 2026-10-13
- Earliest claimed: 2022-03-29
- Assignees: Huawei Technologies Canada Co., Ltd.; Dong Seob Chung; Hany Maher Aziz
- Applicants: Huawei Technologies Canada Co., Ltd.; Dong Seob Chung; Hany Maher Aziz
- Inventors: Dong Seob Chung; Hany Maher Aziz
- Web page: https://patentgrep.com/patent/US12765158B2

## CPC

- H10K 50/115: comprising active inorganic nanostructures, e.g. luminescent quantum dots
- H10K 71/00: Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K 71/30: Doping active layers, e.g. electron transporting layers
- H10K: ORGANIC ELECTRIC SOLID-STATE DEVICES

## Abstract

This invention is related to a new treatment process employed during preparation of the ZnO ETL in a QDLED. The treatment involves exposing the ZnO layer to fluorine (F). In embodiments of this invention, the exposure of the ZnO layer to the F is performed using a fluorine plasma environment (e.g., using CF4, CHF3, C4F8 or SF6). Alternatively, the F exposure may be done by exposing the ZnO ETL to a suitable fluorine-containing substance such as fluorine gas or fluorinated solvents. The F plasma treatment of the ZnO improves both QDLED device EQE and EL stability.

## Claims

### Claim 1

A process for preparing a halogen-doped metal oxide material comprising the step of exposing a metal oxide layer to a halogen source, wherein the halogen source is selected from a halogen-containing plasma, a halogenated solvent and a halogen gas, and wherein the metal oxide layer is an electron transport layer (ETL) deposited during manufacture of a light emitting device (LED).

### Claim 2 (depends on 1)

The process of claim 1, wherein the halogen is selected from fluorine (F), bromine (Br), iodine (I), chlorine (CI), or a combination thereof.

### Claim 3 (depends on 2)

The process of claim 2, wherein the halogen is F.

### Claim 4 (depends on 1)

The process of claim 1, wherein the halogen source is a fluorine-containing plasma.

### Claim 5 (depends on 4)

The process of claim 4, wherein the fluorine-containing plasma is generated using CF4, CHF3, C4F8 or SF6.

### Claim 6 (depends on 1)

The process of claim 1, wherein the metal oxide layer comprises a metal oxide selected from ZnO, TiOx, SnOx, MgO, indium tin oxide (ITO), or a combination thereof.

### Claim 7 (depends on 6)

The process of claim 6, wherein the metal oxide is ZnO.

### Claim 8 (depends on 7)

The process of claim 7, wherein the metal oxide is nanoparticle ZnO.

### Claim 9 (depends on 1)

The process of claim 1, wherein the LED is a quantum-dot light emitting device (QDLED).

### Claim 10 (depends on 1)

The process of claim 1, wherein the step of exposing the metal oxide layer to a halogen-containing plasma is carried out as a low kinetic energy plasma treatment step, wherein the low kinetic plasma treatment step is carried out using a mid-chamber plasma configuration, a downstream plasma treatment, or an ICP (inductively-coupled plasma) reactor.

### Claim 11

A method comprising converting a metal oxide layer to a halogen-doped metal oxide through exposure to a halogen source, wherein the halogen source is selected from a halogen-containing plasma, a halogenated solvent and a halogen gas, and wherein the halogen-doped metal oxide forms an electron transport layer (ETL) of a light emitting device (LED).

### Claim 12 (depends on 11)

The method of claim 11, wherein the halogen source is a halogen-containing plasma.

### Claim 13 (depends on 12)

The method of claim 12, wherein the halogen is F.

### Claim 14 (depends on 13)

The method of claim 13, wherein the metal oxide is ZnO.

### Claim 15 (depends on 14)

The method of claim 14, wherein the LED is a quantum-dot light emitting device (QDLED).