Graphene synthesis

Patent metadata

Field	Value
Publication number	US-11885012-B2
Application number	US-202117342235-A
Country	US
Kind code	B2
Filing date	Jun 8, 2021
Priority date	Aug 14, 2015
Publication date	Jan 30, 2024
Grant date	Jan 30, 2024

Abstract

The invention relates to methods for the production of high quality graphene. In particular, the invention relates to single-step thermal methods which can be carried out in an ambient-air or vacuum environment using renewable biomass as a carbon source. Specifically, the invention comprises heating a metal substrate and carbon source in a sealed ambient environment to a temperature which produces carbon vapour from the carbon source such that the vapour comes into contact with the metal substrate, maintaining the temperature for a time sufficient to form a graphene lattice and then cooling the substrate at a controlled rate to form a deposited graphene.

First claim

The invention claimed is:

1. A method of preparing a deposited graphene in the form of a continuous film comprising the steps of:
sealing a metal substrate and a carbon source in an ambient environment at ambient temperature to create a sealed ambient environment comprising a sealed ambient atmosphere;
heating the sealed ambient environment to a temperature which produces carbon vapour from the carbon source such that the carbon vapour comes into contact with a surface of the metal substrate;
maintaining the temperature at 875° C. or above for a time sufficient to form a graphene lattice and then cooling the metal substrate at a controlled rate to form a deposited graphene continuous film on the surface of the metal substrate that contacts the carbon vapour;
wherein the carbon source is a liquid or solid biomass, is derived from a biomass, or is a purified biomass;
wherein the entire carbon source is not in contact with the metal substrate;
wherein the method is free from the use of compressed or feedstock gases;
wherein the sealed ambient atmosphere consists of air at atmospheric pressure or a vacuum; and
wherein the metal is a transition metal substrate.

2. The method according to claim 1 wherein the metal substrate is nickel or copper.

3. The method according to claim 2 wherein the metal substrate is polycrystalline nickel.

4. The method according to claim 1 wherein the carbon source is a liquid.

5. The method according to claim 1 wherein the carbon source is soybean oil.

6. The method according to claim 1 wherein a ratio of carbon source to surface area of the metal substrate is 0.01-0.03 mL/cm 2 .

7. The method according to claim 1 wherein the sealed ambient environment is contained in an inert container.

8. The method according to claim 7 wherein the metal substrate and carbon source are both located in the inert container.

9. The method according to claim 1 wherein the sealed ambient environment is a quartz, glass or other dielectric heat resistant container.

10. The method according to claim 1 , wherein the temperature sufficient to form the graphene lattice is maintained for 3-15 minutes.

11. The method according to claim 10 wherein the temperature sufficient to form a graphene lattice is maintained at 900° C.

12. The method according to claim 1 wherein the deposited graphene is in the form of 1-40 layers.

13. The method according to claim 1 wherein the substrate is cooled at a controlled rate to control the thickness of the deposited graphene.

14. The method according to claim 1 wherein the substrate is cooled to ambient temperature at a rate of 10-100° C./minute.

15. The method according to claim 1 further comprising the step of decoupling graphene from the substrate.

16. A method of preparing a deposited graphene in the form of a continuous film comprising the steps of:
sealing a metal substrate and a carbon source in an ambient environment at ambient temperature to create a sealed ambient environment comprising a sealed ambient atmosphere;
heating the sealed ambient environment to a temperature which produces carbon vapour from the carbon source such that the carbon vapour comes into contact with a surface of the metal substrate;
maintaining the temperature at 875° C. or above for a time sufficient to form a graphene lattice and then cooling the metal substrate at a controlled rate to form a deposited graphene continuous film on the surface of the metal substrate that contacts the carbon vapour;
wherein the carbon source is a liquid or solid biomass, is derived from a biomass, or is a purified biomass;
wherein the entire carbon source is not in contact with the metal substrate;
wherein the method is free from the use of compressed or feedstock gases;
wherein the sealed ambient atmosphere consists of air at atmospheric pressure or a vacuum;
wherein the metal is a transition metal substrate; and
wherein the substrate is cooled at a controlled rate to control the thickness of the deposited graphene.

Assignees

• Commw Scient Ind Res Org
• Commonwealth Scient And Industrial Research Organization

Inventors

• Seo Dong Han
• Pineda Shafique
• Han Zhao Jun
• Ostrikov Kostyantyn

Classifications

• C23C16/26 Primary

  Deposition of carbon only · CPC title

• C01B32/186

  by chemical vapour deposition [CVD] · CPC title

• C23C16/4485

  by evaporation without using carrier gas in contact with the source material (C23C16/4486 takes precedence) · CPC title

• C23C16/463

  Cooling of the substrate · CPC title

• G01N27/308

  at least partially made of carbon · CPC title