IP Library Granted Patent US 9,890,046
Granted Patent B2
US 9,890,046 · App. 15/413,804 · Granted Feb 13, 2018

Large scale production of oxidized graphene

Inventors: Marie Bozalina (Montreal, CA); Philippe Perret (Longueuil, CA); Soroush Nazarpour (Montreal, CA)
Assignee: Group NanoXplore Inc.
C01B31/043C30B29/16C30B29/64C30B33/00H01G11/36H01M4/587B82Y30/00B82Y40/00Y10S977/734Y10S977/847Y10S977/948
View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 9,890,046
App. No.
15/413,804
Granted
Feb 13, 2018
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 (49)

1. A method for producing functionalized graphene, comprising:

transferring a crystalline graphite into a milling vessel, the milling vessel including a media;

transferring an electrolyte solution into the milling vessel, the electrolyte solution including at least one of a metal hydroxide salt, a weak oxidizer, and a surfactant;

rotating the milling vessel for a first time period to cause shearing of layers of the crystalline graphite to produce a thinned intermediate material;

transferring a strong oxidizer into the milling vessel;

rotating the milling vessel for a second time period to generate an electrostatic charge and to produce functionalized graphene.

2. The method of claim 1 , wherein the electrolyte solution includes polar solvent.

3. The method of claim 1 , wherein the metal hydroxide salt in the electrolyte solution includes at least one of an alkali metal, an alkaline earth metal, and a boron group element.

4. The method of claim 1 , wherein the weak oxidizer in the electrolyte solution includes at least one of hydrogen peroxide, chromate, chlorate, and perchlorate.

5. The method of claim 1 , wherein the surfactant in the electrolyte solution includes at least one of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, pyridinium, thionin acetate salt, and triton.

6. The method of claim 1 , wherein the strong oxidizer includes at least one of potassium permanganate, iron chloride, persulfate, and fluorine.

7. The method of claim 1 , wherein the first time period is about 2 hours to about 4 hours.

8. The method of claim 1 , wherein the second time period is about 4 hours to about 10 hours.

9. A method for producing functionalized graphene, comprising:

transferring a crystalline graphite into a first milling vessel, the first milling vessel including a first media;

transferring a first electrolyte solution into the first ball milling vessel, the first electrolyte solution including at least one of a metal hydroxide salt, a weak oxidizer, and a surfactant;

rotating the first milling vessel to produce an intermediate material;

transferring the intermediate material to a second milling vessel; the second milling vessel including a second media;

transferring a second electrolyte solution into the second ball milling vessel, the second electrolyte solution including a strong oxidizer and at least one of a metal hydroxide salt, a weak oxidizer, and a surfactant;

rotating the second milling vessel to generate an electrostatic charge and to produce functionalized graphene.

10. The method of claim 9 , wherein the first milling vessel is a ball mill.

11. The method of claim 9 , wherein the first milling vessel is an attritor mill.

12. The method of claim 9 , wherein the first milling vessel and the first media are configured to conduct electrostatic charge.

13. The method of claim 9 , wherein the second milling vessel and the second media are configured to conduct electrostatic charge.

14. A method for producing functionalized graphene, comprising:

transferring a crystalline graphite into a first milling vessel, the first milling vessel including a first media;

transferring a first solvent into the first milling vessel;

transferring a first metal hydroxide salt into the first milling vessel, the first metal hydroxide salt formulated to release a first hydroxyl ion upon ionization by a first electrostatic charge;

transferring at least one of a first weak oxidizer and a first surfactant into the first milling vessel;

rotating the first milling vessel to cause shearing of layers of the crystalline graphite to produce an intermediate material;

transferring the intermediate material to a second milling vessel, the second milling vessel including a second media;

transferring a second solvent into the second milling vessel;

transferring a second metal hydroxide salt into the second milling vessel;

transferring at least one of a second weak oxidizer and a second surfactant into the second milling vessel;

transferring a strong oxidizer into the second balling milling vessel;

rotating the second milling vessel to generate an electrostatic charge and to produce functionalized graphene.

15. The method of claim 14 , wherein the first solvent includes a polar solvent.

16. The method of claim 15 , wherein the polar solvent includes one or more of water, ethanol, methanol and 1-propanol.

17. The method of claim 14 , wherein the first metal hydroxide salt includes at least one of an alkali metal, an alkaline earth metal, and a boron group element.

18. The method of claim 14 , wherein the second metal hydroxide salt includes at least one of an alkali metal, an alkaline earth metal, and a boron group element.

19. The method of claim 14 , wherein the first weak oxidizer includes at least one of hydrogen peroxide, chromate, chlorate, and perchlorate.

20. The method of claim 19 , wherein the non-polar solvent includes at least one of toluene, N-Methyl-2-pyrrolidone, heptane, N,N-Dimethylformamide, acetonitrile, chlorobenzene, and dimethyl sulfoxide.

21. The method of claim 14 , wherein the second weak oxidizer includes at least one of hydrogen peroxide, chromate, chlorate, and perchlorate.

22. The method of claim 14 , wherein the first surfactant and/or the second surfactant includes at least one of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, pyridinium, thionin acetate salt, and triton.

23. The method of claim 14 , wherein the second solvent includes a non-polar solvent.

24. The method of claim 14 , wherein:

the first solvent includes a polar solvent,

the second solvent includes a non-polar solvent, and

a volume ratio of the polar solvent to the non-polar solvent is in a range from about 10:1 to about 1,000:1.

Assignments (2)
CERTIFICATE OF AMALGAMATION Recorded Dec 14, 2017
From: GROUP NANOXPLORE INC.
To: NANOXPLORE INC.
Reel/Frame 044872/0303 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 25, 2017
From: BOZALINA, MARIE; PERRET, PHILIPPE; NAZARPOUR, SOROUSH
To: GROUP NANOXPLORE INC.
Reel/Frame 043092/0038 →
Continuity (4)
Continuation 15163247 · May 24, 2016
Continuation PCTCA2015051292 · Dec 8, 2015
Provisional Application 62089583 · Dec 9, 2014
Related Publication 20170225953A1 · Aug 10, 2017