IP Library Granted Patent US 10,322,935
Granted Patent B2
US 10,322,935 · App. 15/270,855 · Granted Jun 18, 2019

Large scale production of thinned graphite, graphene, and graphite-graphene composites

Inventors: Marie Bozalina (Montreal, CA); Philippe Perret (Longueuil, CA); Soroush Nazarpour (Montreal, CA)
Assignee: NanoXplore Inc.
C01B31/0446B02C17/20B02C17/22C01B32/184C01B32/20C01B32/225C09D1/00C09D5/084C09D5/24C09K5/14C10M103/02C30B29/02C30B29/64C30B33/00H01B1/04B82Y40/00C01B2204/04C10M2201/0413
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Quick Facts
Patent No.
US 10,322,935
App. No.
15/270,855
Granted
Jun 18, 2019
Kind
B2
Abstract

Embodiments described herein relate generally to large scale synthesis of thinned graphite and in particular, few layers of graphene sheets and graphene-graphite composites. In some embodiments, a method for producing thinned crystalline graphite from precursor crystalline graphite using wet ball milling processes is disclosed herein. The method includes transferring crystalline graphite into a ball milling vessel that includes a grinding media. A first and a second solvent are transferred into the ball milling vessel and the ball milling vessel is rotated to cause the shearing of layers of the crystalline graphite to produce thinned crystalline graphite.

Claims (35)

1. A method, comprising:

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

transferring a solvent into the milling vessel;

transferring a metal hydroxide salt to the milling vessel;

rotating the milling vessel to cause shearing of layers of the crystalline graphite to produce thinned crystalline graphite.

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

3. The method of claim 2 , wherein the polar solvent includes at least one of water, ethanol, methanol, and 1-propanol.

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

5. The method of claim 1 , wherein the metal hydroxide salt includes a hydroxide of at least one of Li, Na, K, Cs, Be, Mg, Ca, Sr, Ba, B, Al, Ga, In, Rb, and Ti.

6. The method of claim 1 , further comprising:

transferring an oxidizer to the milling vessel.

7. The method of claim 6 , wherein the oxidizer is hydrogen peroxide.

8. The method of claim 1 , further comprising:

transferring a surfactant to the milling vessel.

9. The method of claim 8 , wherein the surfactant includes at least one of sodium dodecyl sulfate, pyridinium, thionin acetate salt, and triton.

10. The method of claim 1 , wherein the milling vessel is rotated for a time period in a range of about 2 hours to about 12 hours.

11. A method, comprising:

combining a crystalline graphite with a solution in a milling vessel, the solution including a solvent and at least one of a metal hydroxide salt, an oxidizer, and a surfactant; and

milling the crystalline graphite in the presence of the solution for a time period to produce a thinned crystalline graphite.

12. The method of claim 11 , wherein the solution includes the metal hydroxide salt, the oxidizer, and the surfactant.

13. The method of claim 12 , wherein the metal hydroxide salt is about 2% to about 50% of the solution by volume.

14. The method of claim 12 , wherein the oxidizer is less than about 3% of the solution by volume.

15. The method of claim 12 , wherein a concentration of the surfactant in the solution is about 10 μMolar to about 100 μMolar.

16. The method of claim 11 , wherein the time period is in a range of about 2 hours to about 12 hours.

17. The method of claim 11 , further comprising:

washing the thinned crystalline graphite with water.

18. The method of claim 17 , further comprising:

washing the thinned crystalline graphite with hydrochloric acid.

19. A method, comprising:

combining a crystalline graphite with a solution in a milling vessel, the solution including a solvent, a metal hydroxide salt, an oxidizer, and a surfactant;

milling the crystalline graphite in the presence of the solution for a time period in a range of about 2 hours to about 12 hours to produce a thinned crystalline graphite; and

washing the thinned crystalline graphite with at least one of water and hydrochloric acid.

20. The method of claim 19 , wherein the metal hydroxide salt includes at least one of an alkali metal, an alkaline earth metal, and a boron group element.

21. The method of claim 19 , wherein the oxidizer is hydrogen peroxide.

22. The method of claim 19 , wherein the surfactant includes at least one of sodium dodecyl sulfate, pyridinium, thionin acetate salt, and triton.

Assignments (2)
CHANGE OF NAME Recorded Apr 24, 2018
From: GROUP NANOXPLORE INC.
To: NANOXPLORE INC.
Reel/Frame 046003/0331 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 25, 2017
From: BOZALINA, MARIE; PERRET, PHILIPPE; NAZARP0UR, SOROUSH
To: GROUP NANOXPLORE INC.
Reel/Frame 043092/0013 →
Continuity (5)
Continuation 14978566 · Dec 22, 2015
Continuation PCTCA2015050525 · Jun 8, 2015
Provisional Application 62035963 · Aug 11, 2014
Provisional Application 62008729 · Jun 6, 2014
Related Publication 20170096343A1 · Apr 6, 2017
Cited By (3)
US 12,286,353 US 12,428,303 US 12,488,907