# US 12,217,958 B2 · Method of pre-treating substrate and method of directly forming graphene using the same

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- Number: US 12,217,958 B2
- Document ID: US12217958B2
- Status: Granted
- Kind: B2
- Application number: 16/807,702
- Filed: 2020-03-03
- Published: 2020-09-10
- Granted: 2025-02-04
- Earliest claimed: 2019-03-04
- Assignees: Samsung Electronics Co., Ltd.
- Applicants: Samsung Electronics Co., Ltd.
- Inventors: Keunwook Shin; Janghee Lee; Seunggeol Nam; Hyeonjin Shin; Hyunseok Lim; Alum Jung; Kyung-Eun Byun; Jeonil Lee; Yeonchoo Cho
- Web page: https://patentgrep.com/patent/US12217958B2

## CPC

- H10P 14/3406: {Carbon, e.g. diamond-like carbon}
- C23C 16/02: Pretreatment of the material to be coated (C23C16/04 takes precedence)
- C23C 16/26: Deposition of carbon only
- H10P 14/2901: {Materials}
- H10P 14/3438: {Doping during depositing}
- H10P 14/36: {characterised by treatments done before the formation of the materials}
- H10P 14/24: using chemical vapour deposition [CVD]
- H10P 14/3206: {Carbon, e.g. diamond-like carbon}
- H10P 14/3256: {Microstructure}
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
- C23C: COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04)

## Abstract

A method of pre-treating a substrate on which graphene will be directly formed may include pre-treating the substrate using a pre-treatment gas including at least a carbon source and hydrogen.

## Claims

### Claim 1

A method of pre-treating a substrate on which graphene is to be directly formed, the method comprising:
pre-treating the substrate using a pre-treatment gas including at least a carbon source and hydrogen,
wherein, in an initial period of the pre-treating the substrate, the carbon source and the hydrogen are simultaneously supplied to a chamber in which the substrate is disposed,
wherein the pre-treating the substrate is performed in the chamber, and
wherein a graphene seed is present on the substrate immediately after the pre-treating the substrate as a result of the pre-treating and a graphene layer is not present on the substrate immediately after the pre-treating the substrate.

### Claim 2 (depends on 1)

The method of claim 1, wherein the pre-treatment gas further includes N2, a noble gas, or both N2 and a noble gas.

### Claim 3 (depends on 2)

The method of claim 2, wherein the pre-treating the substrate includes discontinuously supplying the at least one of the carbon source and the hydrogen of the pre-treatment gas to the substrate.

### Claim 4 (depends on 2)

The method of claim 2, the pre-treating the substrate includes supplying the carbon source and the hydrogen individually to the chamber where the substrate is placed, and the carbon source and the hydrogen are mixed in the chamber during the pre-treating the substrate.

### Claim 5 (depends on 1)

The method of claim 1, wherein
the carbon source is represented by the formula CxHy,
x is in a range from 2 to 12, and
y is in a range from 2 to 26.

### Claim 6 (depends on 1)

The method of claim 1, wherein the pre-treating the substrate includes continuously supplying the carbon source and the hydrogen in the pre-treatment gas during the pre-treating the substrate.

### Claim 7 (depends on 6)

The method of claim 6, wherein a supply rate of the carbon source to the substrate and a supply rate of the hydrogen to the substrate are maintained constant during the pre-treating the substrate.

### Claim 8 (depends on 6)

The method of claim 6, wherein a supply rate of the carbon source to the substrate, a supply rate of the hydrogen to the substrate, or both the supply rate of the carbon source and the supply rate of the hydrogen to the substrate is changed during the pre-treating the substrate.

### Claim 9 (depends on 8)

The method of claim 8, wherein the supply rate of the carbon source to the substrate is changed according to time during the pre-treating the substrate.

### Claim 10 (depends on 8)

The method of claim 8, wherein the supply rate of the hydrogen to the substrate is changed according to time during the pre-treating the substrate.

### Claim 11 (depends on 8)

The method of claim 8, wherein both the supply rate of the carbon source to the substrate and the supply rate of the hydrogen to the substrate are changed according to time during the pre-treating the substrate.

### Claim 12 (depends on 1)

The method of claim 1, wherein the pre-treating the substrate includes discontinuously supplying the carbon source in the pre-treatment gas to the substrate, discontinuously supplying the hydrogen in the pre-treatment gas to the substrate, or discontinuously suppling both the carbon source and the hydrogen gas in the pre-treatment gas to the substrate.

### Claim 13 (depends on 12)

The method of claim 12, wherein the carbon source is continuously supplied to the substrate and the hydrogen is discontinuously supplied to the substrate during the pre-treating the substrate.

### Claim 14 (depends on 12)

The method of claim 12, wherein the carbon source is discontinuously supplied to the substrate and the hydrogen is continuously supplied to the substrate during the pre-treating the substrate.

### Claim 15 (depends on 12)

The method of claim 12, wherein both of the carbon source and the hydrogen are discontinuously supplied to the substrate during the pre-treating the substrate.

### Claim 16 (depends on 1)

The method of claim 1, wherein
the pre-treating the substrate includes preparing a mixed pre-treatment gas, based on mixing the carbon source and the hydrogen outside of a chamber, and supplying the mixed pre-treatment gas to the chamber while the substrate is placed in the chamber.

### Claim 17 (depends on 16)

The method of claim 16, wherein a supply rate of the mixed pre-treatment gas changes over time during the supplying the mixed pre-treatment gas to the chamber while substrate is placed in the chamber.

### Claim 18 (depends on 1)

The method of claim 1, wherein
the pre-treating the substrate includes supplying the carbon source and the hydrogen individually supplied to the chamber where the substrate is placed, and
the carbon source and the hydrogen are mixed in the chamber during the pre-treating the substrate.

### Claim 19 (depends on 1)

The method of claim 1, further comprising:
forming the carbon source using a liquid source or a solid source before the pre-treating the substrate.

### Claim 20 (depends on 1)

The method of claim 1, wherein the pre-treating the substrate includes:
forming a plasma from the pre-treatment gas; and
exposing the substrate to the plasma.

### Claim 21 (depends on 1)

The method of claim 1, wherein the substrate is a non-metal substrate.

### Claim 22 (depends on 21)

The method of claim 21, wherein the non-metal substrate includes a semiconductor substrate or a dielectric substrate.

### Claim 23 (depends on 1)

A method of forming graphene, the method comprising:
preparing a pre-treated substrate by performing the method of claim 1 to pretreat the substrate; and
directly growing graphene on the pre-treated substrate.

### Claim 24 (depends on 23)

The method of claim 23, wherein the directly growing the graphene includes using a source of carbon that is formed using a liquid source or a solid source.

### Claim 25 (depends on 24)

The method of claim 24, wherein
the liquid source includes an aromatic hydrocarbon benzene having at least one of a benzene ring, a toluene, a xylene, or anisole, or a derivative of these materials.

### Claim 26 (depends on 24)

The method of claim 24, wherein the liquid source includes an aliphatic hydrocarbon hexane having a C—C single bond, an octane, or an ethanol.

### Claim 27 (depends on 23)

The method of claim 23, wherein the directly growing graphene includes a doping process.

### Claim 28 (depends on 27)

The method of claim 27, wherein
the doping process uses a doping gas, and
the doping gas includes NH3, NO2, BH3, B2H6, or a combination thereof.

### Claim 29 (depends on 1)

The method of claim 1, wherein
during the pre-treating the substrate, the carbon source is supplied to the chamber via a first gas line and the hydrogen is supplied to the chamber via a second gas line,
the first gas line and the second gas line are separate from each other and do not merge before connecting to the chamber, and
in the initial period of the pre-treating the substrate, a gas flow rate of the carbon source is greater than a gas flow rate of the hydrogen.

### Claim 30 (depends on 1)

The method of claim 1, wherein
the carbon source is supplied to the chamber via a first gas line and the hydrogen is supplied to the chamber via a second gas line different from the first gas line,
the first gas line is directly connected to the chamber, and
the second gas line is directly connected to the chamber.

### Claim 31 (depends on 2)

The method of claim 2, wherein the pre-treating the substrate includes preparing a mixed pre-treatment gas, based on mixing the carbon source and the hydrogen outside a chamber, and supplying the mixed pre-treatment gas to the chamber while the substrate is placed in the chamber.