IP Library Granted Patent US 10,669,155
Granted Patent B2
US 10,669,155 · App. 15/862,039 · Granted Jun 2, 2020

Method for synthesizing graphene from encapsulated particles

Inventors: Zhiyong Cai (Madison, WI); Qiangu Yan (Starkville, MS); Jilei Zhang (Starkville, MS); Jinghao Li (Madison, WI); Bruno Sisto Marcoccia (Charlotte, NC); James David Freiberg (Baraboo, WI)
C01B32/184B01J13/02B01J13/06C01B32/194B01J23/70B82Y30/00B82Y40/00Y02P20/145Y10S977/734Y10S977/842
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Quick Facts
Patent No.
US 10,669,155
App. No.
15/862,039
Granted
Jun 2, 2020
Kind
B2
Abstract

A method of synthesizing a graphene-based material comprises exposing graphene-encapsulated metal nanoparticles, each nanoparticle comprising a graphene shell surrounding a metal core, to a cracking and welding gas composition under conditions sufficient to crack graphene shells and to reconstruct cracked graphene shells to form the graphene-based material.

Claims (24)

1. A method of synthesizing a graphene-based material, the method comprising exposing graphene-encapsulated metal nanoparticles, each nanoparticle comprising a graphene shell surrounding a metal core, to a cracking and welding gas composition under conditions sufficient to crack graphene shells and to reconstruct cracked graphene shells to form the graphene-based material.

2. The method of claim 1 , wherein the cracking and welding gas composition is selected to maximize the yield of the graphene-based material.

3. The method of claim 2 , wherein the yield is at least 90%.

4. The method of claim 1 , wherein the cracking and welding gas composition comprises one or more of methane, ethane, propane, natural gas.

5. The method of claim 4 , wherein the cracking and welding gas composition further comprises argon.

6. The method of claim 1 , wherein the exposure is carried out at a temperature of at least 1000° C. for at least 30 minutes.

7. The method of claim 1 , wherein prior to exposing the graphene-encapsulated metal nanoparticles to the cracking and welding gas composition, the graphene-encapsulated metal nanoparticles are exposed to argon at an elevated temperature for a period of time.

8. The method of claim 1 , wherein the graphene-based material comprises flat or curved graphene sheets.

9. The method of claim 1 , wherein the cracking and welding gas composition comprises one or more of methane, ethane, propane and natural gas, the graphene-based material comprises flat or curved graphene sheets, and the yield of the graphene-based material is at least 90%.

10. The method of claim 1 , further comprising exposing a carbon-metal based precursor to an inert gas composition at an elevated temperature for a period of time sufficient to convert the carbon to graphene, thereby forming the graphene-encapsulated metal nanoparticles.

11. The method of claim 10 , wherein the elevated temperature is in the range of from 700° C. to 1000° C.

12. The method of claim 10 , wherein the carbon of the carbon-metal based precursor is provided by a biomass feedstock.

13. The method of claim 12 , wherein the biomass feedstock comprises kraft lignin.

14. The method of claim 10 , further comprising forming the carbon-metal based precursor by mixing a first solution comprising a first solvent and a carbon source with a second solution comprising a second solvent and a metal source to form a carbon-metal mixture.

15. The method of claim 14 , wherein the carbon source comprises kraft lignin and the first solvent is tetrahydrofuran.

16. The method of claim 14 , wherein the metal salt is a metal nitrate.

17. The method of claim 14 , wherein the metal is iron and the metal source is present in the carbon-metal mixture at an amount in the range of from 5 to 15% by weight.

18. The method of claim 14 , further comprising exposing the carbon-metal mixture to another inert gas composition at another elevated temperature for another period of time sufficient to at least partially decompose the carbon source, followed by ground-milling.

19. A method of synthesizing a graphene-based material, the method comprising:

mixing a first solution comprising a first solvent and a carbon source with a second solution comprising a second solvent and a metal source to form a carbon-metal mixture;

exposing the carbon-metal mixture to an inert gas composition at an elevated temperature and for a period of time sufficient to at least partially decompose the carbon source, followed by ground-milling, thereby forming a carbon-metal precursor;

exposing the carbon-metal based precursor to another inert gas composition at another elevated temperature for another period of time sufficient to convert the carbon to graphene, thereby forming graphene-encapsulated metal nanoparticles, each nanoparticle comprising a graphene shell surrounding a metal core; and

exposing the graphene-encapsulated metal nanoparticles to a cracking and welding gas composition under conditions sufficient to crack graphene shells and to reconstruct cracked graphene shells to form the graphene-based material.

20. The method of claim 19 , wherein the carbon source comprises kraft lignin.

Assignments (4)
TERM LOAN PATENT SECURITY AGREEMENT Recorded Mar 1, 2023
From: DOMTAR PAPER COMPANY, LLC
To: COBANK, ACB, AS COLLATERAL AGENT
Reel/Frame 062902/0610 →
SECURITY AGREEMENT (ABL) Recorded Dec 1, 2021
From: DOMTAR PAPER COMPANY, LLC; EAM CORPORATION
To: BARCLAYS BANK PLC, AS COLLATERAL AGENT
Reel/Frame 058293/0927 →
SECURITY AGREEMENT (FIRST LIEN) Recorded Dec 1, 2021
From: DOMTAR PAPER COMPANY, LLC; EAM CORPORATION
To: BARCLAYS BANK PLC, AS COLLATERAL AGENT
Reel/Frame 058293/0941 →
SECURITY AGREEMENT (NOTES) Recorded Dec 1, 2021
From: DOMTAR PAPER COMPANY, LLC; EAM CORPORATION
To: THE BANK OF NEW YORK MELLON, AS COLLATERAL AGENT
Reel/Frame 058294/0043 →
Continuity (3)
Continuation In Part 15400281 · Jan 6, 2017
Provisional Application 62443207 · Jan 6, 2017
Related Publication 20180194630A1 · Jul 12, 2018