Method for producing a graphene film

Patent metadata

Field	Value
Publication number	US-12037248-B2
Application number	US-202318211682-A
Country	US
Kind code	B2
Filing date	Jun 20, 2023
Priority date	Dec 15, 2015
Publication date	Jul 16, 2024
Grant date	Jul 16, 2024

Abstract

Disclosed herein are methods for forming a graphene film on a substrate, the methods comprising depositing graphene on a surface of the substrate by a first vapor deposition step to form a discontinuous graphene crystal layer; depositing a graphene oxide layer on the discontinuous graphene crystal layer to form a composite layer; and depositing graphene on the composite layer by a second vapor deposition step, wherein the graphene oxide layer is substantially reduced to a graphene layer during the second vapor deposition step. Transparent coated substrates comprising such graphene films are also disclosed herein, wherein the graphene films have a resistance of less than about 10 KΩ/sq.

First claim

What is claimed is:

1. A method for forming a graphene film on a substrate, the method comprising:
(a) depositing graphene on a surface of the substrate by a first vapor deposition step to form a discontinuous graphene crystal layer;
(b) depositing a graphene oxide layer on the discontinuous graphene crystal layer to form a composite layer; and
(c) depositing graphene on the composite layer by a second vapor deposition step;
wherein the graphene oxide layer is substantially reduced to a graphene layer during the second vapor deposition step.

2. The method of claim 1 , wherein the first and/or second vapor deposition steps comprise plasma-enhanced chemical vapor deposition.

3. The method of claim 1 , wherein the first and/or second vapor deposition steps comprise contacting the substrate with a plasma comprising a carbon-source gas and optionally comprising hydrogen gas.

4. The method of claim 3 , wherein the carbon-source gas is chosen from CH 4 , C 2 H 2 , CF 4 , CHF 3 , C 2 F 6 , and combinations thereof.

5. The method of claim 3 , wherein the first and/or second vapor deposition steps comprise:
(a) placing the substrate in a reaction chamber;
(b) optionally introducing hydrogen gas into the reaction chamber;
(c) heating the reaction chamber to a deposition temperature
(d) applying a radio frequency (RF) current to the chamber;
(e) introducing the carbon-source gas into the reaction chamber; and
(f) holding at the deposition temperature for a growth time sufficient to deposit graphene on the substrate.

6. The method of claim 5 , wherein the hydrogen gas has a flow rate ranging from 0 to about 40 sccm and the carbon-source gas has a flow rate ranging from about 1 to about 20 sccm.

7. The method of any one of claim 5 , wherein the deposition temperature ranges from about 500° C. to about 1100° C.

8. The method of any one of claim 5 , wherein the reaction chamber is heated to the deposition temperature at a heating ramp rate ranging from about 1° C./min to about 50° C./min.

9. The method of any one of claim 5 , wherein the RF current has a power ranging from about 50 W to about 200 W.

10. The method of any one of claim 5 , wherein the growth time ranges from about 5 minutes to about 30 minutes.

11. The method of claim 5 , wherein:
depositing the graphene oxide layer comprises dip coating the substrate in a suspension of graphene oxide at a pull rate ranging from about 2 mm/min to about 50 mm/min;
the graphene oxide suspension has a concentration ranging from about 0.1 to 1.0 mg/mL; and
the graphene oxide comprises graphene oxide sheets having a thickness of one to three layers.

12. The method of claim 1 , wherein during the second vapor deposition step graphene is deposited on the composite layer to form at least one vertical sheet extending from the substrate surface in a substantially perpendicular direction relative to the substrate surface and at least one horizontal sheet extending in a substantially parallel direction relative to the substrate surface.

13. The method of claim 1 , wherein the substrate is chosen from glass, glass-ceramic, and crystalline substrates.

Assignees

• Corning Inc
• Shanghai Inst Ceramics Cas

Inventors

• Bi Hui
• Huang Fuqiang
• Liu Xinyuan
• Song Zhen
• Tang Yufeng
• Xiu Tongping

Classifications

• C23C16/50

  using electric discharges {(generation and control of plasma in discharge tubes for surface treatment H01J37/32, H01J37/34)} · CPC title

• C03C2218/153

  by plasma-enhanced cvd · CPC title

• C03C2218/111

  by dipping, immersion · CPC title

• C03C2217/70

  Properties of coatings · CPC title

• C03C2217/40

  Coatings comprising at least one inhomogeneous layer · CPC title