IP Library › Granted Patent US 10,304,937
Granted Patent B2
US 10,304,937 · App. 14/773,011 · Granted May 28, 2019

Scalable process for producing exfoliated defect-free, non-oxidised 2-dimensional materials in large quantities

Inventors: Jonathan Coleman (Dublin, IE); Keith Paton (Co. Dublin, IE)
Assignee: The Provost, Fellows, Foundation Scholars, and the Other Members of Board, of the College of the Holy and Undivided Trinity of Queen Elizabeth Near Dublin
H01L29/45C01B19/007C01B19/04C01B21/064C01B21/0648C01B21/083C01B32/19C01G39/00C01G39/06C01G41/00C09C1/46C09C3/04H01G4/008H01G9/042H01G9/2045H01G11/36H01L31/022425H01L33/40H01L51/441H01M4/583C01P2002/82C01P2004/04C01P2004/24Y02P20/582
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Quick Facts
Patent No.
US 10,304,937
App. No.
14/773,011
Granted
May 28, 2019
Kind
B2
Abstract

A process for exfoliating untreated 3-dimensional material to produce a 2-dimensional material, said process comprising the steps of mixing the untreated 3-dimensional material in a liquid to provide a mixture; applying shear force to said mixture to exfoliate the 3-dimensional material and produce dispersed exfoliated 2-dimensional material in solution; and removing the shear force applied to said mixture, such that the dispersed exfoliated 2-dimensional material remains free and unaggregated in solution.

Claims (21)

1. A process for exfoliating an untreated 3-dimensional layered material to produce a 2-dimensional material, said process comprising the steps of:

mixing the untreated 3-dimensional layered material in a liquid to provide a mixture;

applying a shear force to said mixture to exfoliate the 3-dimensional layered material and produce a dispersed and exfoliated 2-dimensional material in solution; and

removing the shear force applied to said mixture, such that the dispersed exfoliated 2-dimensional material remains free and unaggregated in solution,

wherein the shear force generates a shear rate greater than 1000 s −1 , and

wherein the liquid does not contain a thickening or gelating agent.

2. The process according to claim 1 , wherein flakes of 2-dimensional material and unexfoliated 3-dimensional layered material are removed from the solution by low-speed centrifugation, gravity settling, filtration or flow separation.

3. The process according to claim 1 , wherein the 2-dimensional material is substantially non-oxidised.

4. The process according to claim 1 , further comprising the step of allowing the formation of a thin film layer from said mixture.

5. The process according to claim 1 , further comprising the step of allowing the formation of a thin film layer from said mixture and wherein the step of forming the thin film layer is formed by vacuum filtration or accelerated evaporation.

6. The process according to claim 1 , wherein the 3-dimensional layered material is selected from the group consisting of a 3-dimensional layered compound, a 3-dimensional layered element, a transition metal dichalcogenide having the formula MX n , wherein 1≤n≤3, a transition metal oxide, boron nitride (BN), Bi 2 Te 3 , Sb 2 Te 3 , TiNCl, and an inorganic layered compound.

7. The process according to claim 1 , wherein the 3-dimensional layered material is graphite.

8. The process according to claim 1 , wherein the liquid may be a solvent, a water-surfactant solution or a solution of a polymer in a solvent wherein the solvent has a surface tension range of between 32-48 mJ/m 2 .

9. The process according to claim 1 , wherein the exfoliated 2-dimensional material is concentrated and washed using cross-flow or tangential filtration.

10. The process according claim 1 , further comprising the step of inserting the exfoliated 2-dimensional material into a matrix to form a composite.

11. The process according to claim 1 , further comprising the step of inserting the exfoliated 2-dimensional material into a matrix to form a composite and wherein the matrix is a polymer or copolymer selected from the group consisting of a thermoplastic, a thermoset, an elastomer and a biopolymer.

12. A device comprising a mixture of exfoliated 2-dimensional material produced according to the process comprising the steps of mixing an untreated 3-dimensional layered material in a liquid to provide a mixture; applying shear force to said mixture to exfoliate the 3-dimensional layered material and produce a dispersed and exfoliated 2-dimensional material in solution; and removing the shear force applied to said mixture, such that the dispersed exfoliated 2-dimensional material remains free and unaggregated in solution and any other nano-material, wherein the shear force generates a shear rate greater than 1000 s −1 , and wherein the liquid does not contain a thickening or gelating agent.

13. The device according to claim 12 , wherein the exfoliated material is graphene.

14. The device according to claim 12 , wherein the nano-material is selected from the group comprising graphene, inorganic layered compounds, a one-dimensional nano-material or nanoparticles.

15. The device according to claim 12 , wherein the device is selected from the group comprising electrodes, transparent electrodes, capacitors, transistors, solar cells, light emitting diodes, batteries, battery electrodes, capacitors, super-capacitors, sensors, nano-transistors, nano-capacitors, nano-light emitting diodes, and nano-solar cells.

16. A dye-sensitised solar cell electrode comprising exfoliated graphene produced by the process comprising the steps of mixing an untreated 3-dimensional layered material in a liquid to provide a mixture; applying shear force to said mixture to exfoliate the 3-dimensional layered material and produce a dispersed and exfoliated 2-dimensional material in solution; and removing the shear force applied to said mixture, such that the dispersed exfoliated 2-dimensional material remains free and unaggregated in solution, wherein the shear force generates a shear rate greater than 1000 s −1 , and wherein the liquid does not contain a thickening or gelating agent.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 12, 2018
From: THOMAS SWAN & CO. LIMITED
To: THE PROVOST, FELLOWS, FOUNDATION SCHOLARS, AND THE OTHER MEMBERS OF BOARD, OF THE COLLEGE OF THE HOLY AND UNDIVIDED TRINITY OF QUEEN ELIZABETH NEAR DUBLIN
Reel/Frame 046056/0137 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 12, 2018
From: COLEMAN, JONATHAN
To: THE PROVOST, FELLOWS, FOUNDATION SCHOLARS, AND THE OTHER MEMBERS OF BOARD, OF THE COLLEGE OF THE HOLY AND UNDIVIDED TRINITY OF QUEEN ELIZABETH NEAR DUBLIN
Reel/Frame 046056/0164 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 12, 2018
From: PATON, KEITH
To: THOMAS SWAN & CO. LIMITED
Reel/Frame 046348/0187 →
Priority Claims (1)
GB 1304770.9 · Mar 15, 2013 · national
Continuity (2)
Provisional Application 61786068 · Mar 14, 2013
Related Publication 20160009561A1 · Jan 14, 2016