Advanced oxidation process for the exfoliation of two dimensional matertals

Patent metadata

Field	Value
Publication number	US-11225415-B2
Application number	US-201816054868-A
Country	US
Kind code	B2
Filing date	Aug 3, 2018
Priority date	Aug 4, 2017
Publication date	Jan 18, 2022
Grant date	Jan 18, 2022

Abstract

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

First claim

What is claimed is:

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.

Assignees

• Uchicago Argonne Llc

Inventors

• Markou Demetrios
• Sumant Anirudha V

Classifications

• B01J8/085 Primary

  Feeding reactive fluids (for solid material, see B01J8/0015) · CPC title

• B82Y30/00

  Nanotechnology for materials or surface science, e.g. nanocomposites · CPC title

• C01B32/19

  by exfoliation · CPC title

• C01B2204/02

  Single layer graphene · CPC title

• B01J8/16

  with particles being subjected to vibrations or pulsations (B01J8/40 takes precedence) · CPC title