IP Library Granted Patent US 12,006,220
Granted Patent B2
US 12,006,220 · App. 17/857,761 · Granted Jun 11, 2024

Large scale production of oxidized graphene

Inventors: Marie Bozalina (Montreal, CA); Philippe Perret (Longueuil, CA); Soroush Nazarpour (Saint-Laurent, CA)
Assignee: NanoXplore Inc.
C01B32/19C01B32/184C01B32/23C30B29/02C30B29/16C30B29/60C30B29/64C30B33/00C30B33/04C30B33/06H01G11/36H01M4/587B82Y30/00B82Y40/00C01B2204/04C01P2006/40Y10S977/734Y10S977/847Y10S977/948
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Quick Facts
Patent No.
US 12,006,220
App. No.
17/857,761
Granted
Jun 11, 2024
Kind
B2
Abstract

Embodiments described herein relate generally to the large scale production of functionalized graphene. In some embodiments, a method for producing functionalized graphene includes combining a crystalline graphite with a first electrolyte solution that includes at least one of a metal hydroxide salt, an oxidizer, and a surfactant. The crystalline graphite is then milled in the presence of the first electrolyte solution for a first time period to produce a thinned intermediate material. The thinned intermediate material is combined with a second electrolyte solution that includes a strong oxidizer and at least one of a metal hydroxide salt, a weak oxidizer, and a surfactant. The thinned intermediate material is then milled in the presence of the second electrolyte solution for a second time period to produce functionalized graphene.

Claims (42)

1. A method for producing functionalized graphene, comprising:

transferring graphite into a milling vessel, the graphite having a first thickness;

transferring a solvent into the milling vessel;

transferring a surfactant into the milling vessel;

transferring an oxidizing agent into the milling vessel; and

milling the graphite in the presence of the solvent, the surfactant, and the oxidizing agent to produce functionalized graphene, the functionalized graphene having a second thickness, the second thickness less than the first thickness.

2. The method of claim 1 , wherein the solvent includes at least one of water or ethanol.

3. The method of claim 1 , wherein the oxidizing agent includes a metal hydroxide salt.

4. The method of claim 3 , wherein the metal hydroxide salt includes potassium hydroxide.

5. The method of claim 1 , wherein the second thickness is less than about 200 nm.

6. The method of claim 1 , wherein the functionalized graphene is hydroxylated.

7. The method of claim 6 , further comprising:

converting a hydroxyl group of the functionalized graphene to a carbonyl group.

8. The method of claim 1 , wherein the functionalized graphene is carbonylated.

9. The method of claim 1 , wherein the second oxidizing agent includes a peroxide.

10. A method for producing functionalized graphene, comprising:

transferring graphite into a milling vessel, the graphite having a first aspect ratio;

transferring a first solvent into the milling vessel;

transferring an oxidizing agent into the milling vessel;

transferring a second solvent into the milling vessel; and

milling the graphite in the presence of the first solvent, the oxidizing agent, and the second solvent to produce functionalized graphene, the functionalized graphene having a second aspect ratio, the second aspect ratio larger than the first aspect ratio.

11. The method of claim 10 , wherein the first solvent includes a polar solvent and the second solvent includes a non-polar solvent.

12. The method of claim 11 , wherein the first solvent includes at least one of water or ethanol.

13. The method of claim 11 , wherein the second solvent includes at least one of toluene, N-ethyl-2-pyrrolidone, N,N-dimethylformamide, acetonitrile, chlorobenzene, or dimethyl sulfoxide.

14. The method of claim 10 , wherein the oxidizing agent is at least one of a peroxide, a chromate, a chlorate, or a perchlorate.

15. The method of claim 10 , wherein the functionalized graphene is hydroxylated.

16. The method of claim 15 , further comprising:

converting a hydroxyl group of the functionalized graphene to a carbonyl group.

17. The method of claim 10 , wherein the functionalized graphene is carbonylated.

18. A method for producing functionalized graphene, comprising:

transferring graphite into a milling vessel, the graphite having a first aspect ratio;

transferring a solvent into the milling vessel;

transferring a first surfactant into the milling vessel;

transferring an oxidizing agent into the milling vessel;

transferring a second surfactant into the milling vessel; and

milling the graphite in the presence of the solvent, the first surfactant, the oxidizing agent, and the second surfactant to produce functionalized graphene, the functionalized graphene having a second aspect ratio, the second aspect ratio larger than the first aspect ratio.

19. The method of claim 18 , wherein the first surfactant includes at least one of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, pyridinium, thionin acetate salt, or triton.

20. The method of claim 19 , wherein the second surfactant is different from the first surfactant and includes at least one of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, pyridinium, thionin acetate salt, or triton.

21. The method of claim 18 , wherein the functionalized graphene is hydroxylated.

22. The method of claim 21 , further comprising:

converting a hydroxyl group of the functionalized graphene to a carbonyl group.

23. The method of claim 18 , wherein the functionalized graphene is carbonylated.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 1, 2022
From: BOZALINA, MARIE; PERRET, PHILIPPE; NAZARPOUR, SOROUSH
To: GROUP NANOXPLORE INC.
Reel/Frame 061614/0648 →
CERTIFICATE OF AMALGAMATION Recorded Nov 1, 2022
From: GROUP NANOXPLORE INC.
To: NANOXPLORE INC.
Reel/Frame 061832/0278 →
Continuity (7)
Continuation 16692201 · Nov 22, 2019
Continuation 15854419 · Dec 26, 2017
Continuation 15413804 · Jan 24, 2017
Continuation 15163247 · May 24, 2016
Continuation PCTCA2015051292 · Dec 8, 2015
Provisional Application 62089583 · Dec 9, 2014
Related Publication 20230062310A1 · Mar 2, 2023
Cited By (2)
US 12,286,353 US 12,488,907