IP Library Granted Patent US 10,882,276
Granted Patent B2
US 10,882,276 · App. 15/716,706 · Granted Jan 5, 2021

Continuous production of exfoliated 2D layered materials by compressive flow

Inventors: Richard B. Kaner (Pacific Palisades, CA); Emily Phuong Nam Nguyen (Abbotsford, AU); Syed Reza Rizvi (Oshawa, CA)
Assignee: The Regents of the University of California
B32B9/041B05B1/02B05B1/044B32B33/00C01B21/0648C01B32/19C01G39/06C01B21/06C01B32/225C01P2002/72C01P2002/82C01P2002/84C01P2004/04C01P2004/24H01J37/26
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Quick Facts
Patent No.
US 10,882,276
App. No.
15/716,706
Granted
Jan 5, 2021
Kind
B2
Abstract

Described herein are methods for continuous production of an exfoliated two-dimensional (2D) material comprising passing a 2D material mixture through a convergent-divergent nozzle, the 2D material mixture comprising a 2D layered material and a compressible fluid. The method of the present disclosure employs physical compression and expansion of a flow of high-pressure gases, leaving the 2D layered material largely defect free to produce an exfoliated 2D layered in a simple, continuous, and environmentally friendly manner.

Claims (31)

1. A method for continuous production of an exfoliated two-dimensional (2D) material comprising

a) providing a 2D layered material;

b) providing a compressible fluid;

c) mixing the 2D layered material with the compressible fluid thereby forming a 2D material mixture; and

d) passing the 2D material mixture through a convergent-divergent nozzle to exfoliate the 2D layered material before the compressible fluid intercalates the 2D layered material.

2. The method of claim 1 wherein the 2D layered material comprises graphite, graphene, boron nitride (BN), single-layer BN, molybdenum disulfide (MoS 2 ), single-layer MoS 2 , or any combination thereof.

3. The method of claim 1 wherein the compressible fluid comprises air, nitrogen, carbon dioxide, helium, or any combination thereof.

4. The method of claim 1 wherein a concentration of the 2D layered material in the 2D material mixture is about 0.01 milligrams per milliliter (mg/mL) to about 0.4 mg/mL.

5. The method of claim 1 wherein the convergent-divergent nozzle comprises a de Laval nozzle, a valve, an orifice, a thin tube, or any combination thereof.

6. The method of claim 5 wherein a valve comprises a needle valve, a butterfly valve, a globe valve, a pinch valve, an adjustable flow valve, a one-way flow valve, or any combination thereof.

7. The method of claim 1 , wherein passing the 2D material mixture through the convergent-divergent nozzle comprises applying a pressure to the 2D material mixture of about 200 pounds per square inch (psi) to about 4000 psi.

8. The method of claim 1 wherein the 2D material mixture enters the convergent-divergent nozzle at a velocity less than the speed of sound in the compressible fluid.

9. The method of claim 1 wherein the 2D material mixture exits the convergent-divergent nozzle at a velocity greater than the speed of sound in the compressible fluid.

10. The method of claim 1 , wherein the convergent-divergent nozzle has a throat dimension of about 0.005 millimeters (mm) to about 0.5 mm.

11. The method of claim 1 wherein the convergent-divergent nozzle has an inlet or an outlet dimension of about 3 mm to about 10 mm.

12. The method of claim 1 wherein the convergent-divergent nozzle has a length of about 15 centimeters (cm) to about 60 cm.

13. The method of claim 1 wherein the convergent-divergent nozzle has at least one of a throat-to-inlet dimension ratio and a throat-to-outlet dimension ratio of about 15 to about 60.

14. The method of claim 1 wherein a percent of the 2D layered material that produces the exfoliated 2D material is about 50% to about 100%.

15. The method of claim 1 wherein the exfoliated 2D material comprises a plurality of flakes with an aspect ratio of about 10 to about 300.

16. The method of claim 1 wherein the exfoliated 2D material comprises a plurality of flakes with an average thickness of about 0.35 nanometers (nm) to about 10 nm.

17. The method of claim 1 wherein the exfoliated 2D material comprises a plurality of flakes with an average length of about 50 nm to about 1,600 nm.

18. The method of claim 1 wherein the exfoliated 2D material comprises a plurality of flakes comprising at most about 20 layers.

19. The method of claim 1 wherein the 2D material mixture further comprises a solvent.

20. The method of claim 1 further comprising centrifuging the exfoliated 2D material.

21. The method of claim 20 wherein the centrifuging is performed at a rate of about 700 revolutions per minute (rpm) to about 4,000 rpm.

22. The method of claim 20 wherein the centrifuging is performed for a period of time of about 2 minutes to about 180 minutes.

23. A method for continuous production of exfoliated two-dimensional (2D) material comprising:

a) providing a 2D layered material;

b) providing a continuous flow of compressible fluid;

c) feeding the 2D layered material into the continuous flow of compressible fluid thereby forming a continuous flow of a mixture of the 2D layered material and compressible fluid; and

d) passing the continuous flow of the mixture of the 2D layered material and compressible fluid through a convergent-divergent nozzle to exfoliate the 2D layered material before the compressible fluid intercalates the 2D layered material.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 3, 2017
From: KANER, RICHARD B.; NGUYEN, EMILY PHUONG NAM; RIZVI, SYED REZA
To: THE REGENTS OF THE UNIVERSITY OF CALIFORNIA
Reel/Frame 044025/0109 →
Continuity (2)
Provisional Application 62402591 · Sep 30, 2016
Related Publication 20180093454A1 · Apr 5, 2018