IP Library Granted Patent US 11,225,415
Granted Patent B2
US 11,225,415 · App. 16/054,868 · Granted Jan 18, 2022

Advanced oxidation process for the exfoliation of two dimensional matertals

Inventors: Demetrios Markou (Lemont, IL); Anirudha V. Sumant (Plainfield, IL)
Assignee: UChicago Argonne, LLC
C01B32/192B01J8/085B01J8/087B01J8/10B01J8/16B01J19/008B01J19/02B01J19/10B01J19/123B01J19/18C01B32/19C01G39/06B01J2208/00176B01J2208/00212B01J2208/00867B01J2219/00094B01J2219/00189B01J2219/0209B01J2219/0254B01J2219/0286B01J2219/089B01J2219/0871B01J2219/1203B82Y30/00B82Y40/00C01B2204/02C01B2204/04C01P2002/82C01P2002/84C01P2004/20
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Quick Facts
Patent No.
US 11,225,415
App. No.
16/054,868
Granted
Jan 18, 2022
Kind
B2
Abstract

A system for extracting two dimensional materials from a bulk material by functionalization of the bulk material in a reactor.

Claims (27)

1. A method of exfoliating two-dimensional materials comprising:

adding a bulk material to a polar solvent in a reactor vessel;

dissolving ozone in the polar solvent that is chilled to between between 5° C. and 15° C.;

exposing the polar solvent to shear forces imparted by a shear emulsifier; and

exfoliating two-dimensional material from the bulk material.

2. The method of claim 1 , wherein the bulk material is selected from the group consisting of graphite, Molybdenum disulfide (MoS 2 ), Molybdenum diselenide (MoSe 2 ), hexagonal boron nitride (h-BN), Tungsten disulfide(WS 2 ), and Tungsten diselenide (WSe 2 ).

3. The method of claim 1 , wherein the two-dimensional material is graphene.

4. The method of claim 1 , wherein the two-dimensional material formed is from bulk is Molybdenum disulfide (MoS 2 ), Molybdenum diselenide (MoSe 2 ), hexagonal boron nitride (h-BN), Tungsten disulfide(WS 2 ), and Tungsten diselenide (WSe 2 ).

5. The method of claim 1 , wherein the two-dimensional material is single layer.

6. The method of claim 1 , wherein the two-dimensional material is few layer.

7. The method of claim 1 , wherein the two-dimensional material is multi layer.

8. The method of claim 1 , further comprising agitating the polar solvent.

9. The method of claim 8 , wherein the polar solvent has a temperature above 25° C.

10. The method of claim 1 , wherein no chemical preprocessing of the bulk material is necessary.

11. The method of claim 10 , further comprising exposing the solvent to ultraviolet (UV) radiation to enhance radical formation in the working H 2 O 2 or H 2 O or H 2 O/H 2 O 2 solvent.

12. The method of claim 1 , wherein the working solvent can be H 2 O 2 , H 2 O, an inert PFC, or a mixture of these in any combination.

13. A method of exfoliating two-dimensional materials comprising:

adding a bulk material to a polar solvent in a reactor vessel, the polar solvent selected from the group consisting of H 2 O 2 , H 2 O, or a combination thereof;

dissolving ozone in the polar solvent;

exposing the polar solvent to ultraviolet (UV) radiation to enhance radical formation in the polar solvent; and

exfoliating two-dimensional material from the bulk material by advanced oxidation process.

14. The method of claim 13 , wherein the bulk material is selected from the group consisting of graphite, Molybdenum disulfide (MoS 2 ), Molybdenum diselenide (MoSe 2 ), hexagonal boron nitride (h-BN), Tungsten disulfide(WS 2 ), and Tungsten diselenide (WSe 2 ).

15. The method of claim 13 , wherein the two-dimensional material is graphene.

16. The method of claim 13 , wherein the two-dimensional material formed is from bulk is Molybdenum disulfide (MoS 2 ), Molybdenum diselenide (MoSe 2 ), hexagonal boron nitride (h-BN), Tungsten disulfide(WS 2 ), and Tungsten diselenide (WSe 2 ).

17. The method of claim 13 , wherein the polar solvent is chilled from around room temperature to between 5° C. and 15° C.

18. The method of claim 13 , further comprising, after dissolving ozone in the polar solvent, agitating the polar solvent by ultrasound in combination with shear forces imparted by a shear emulsifier, facilitating the exfoliating.

19. The method of claim 18 , wherein the polar solvent has a temperature above 25° C.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 23, 2019
From: SUMANT, ANIRUDHA V.
To: UCHICAGO ARGONNE, LLC
Reel/Frame 049831/0080 →
CONFIRMATORY LICENSE Recorded Apr 3, 2019
From: UCHICAGO ARGONNE, LLC
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 048789/0362 →
Continuity (2)
Provisional Application 62541498 · Aug 4, 2017
Related Publication 20190039905A1 · Feb 7, 2019