IP Library Granted Patent US 9,340,430
Granted Patent B2
US 9,340,430 · App. 14/001,845 · Granted May 17, 2016

Crystalline graphene and method of making crystalline graphene

Inventors: Amartya Chakrabarti (Hoffman Estates, IL); Narayan S. Hosmane (DeKalb, IL)
Assignee: Board of Trustees of Northern Illinois University
C01B31/0492B82Y30/00B82Y40/00C01B31/04C01B31/0446C09D11/52
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Quick Facts
Patent No.
US 9,340,430
App. No.
14/001,845
Granted
May 17, 2016
Kind
B2
Abstract

A method of producing graphene comprises forming a composition comprising magnesium and carbon, and isolating graphene from the composition. The isolated graphene is crystalline.

Claims (74)

1. A method of producing isolated graphene, comprising isolating graphene from a composition comprising graphene and magnesium, wherein the isolated graphene contains less than 10% by weight of non-graphene material.

2. The method of claim 1 , further comprising forming the composition by a process comprising burning magnesium metal in an atmosphere comprising carbon dioxide.

3. The method of claim 1 , wherein the composition is formed in contact with solid carbon dioxide.

4. The method of claim 1 , further comprising forming the composition by a process comprising reducing carbon dioxide with magnesium metal.

5. The method of claim 4 , wherein forming the composition comprises producing molten metal comprising the magnesium.

6. The method of claim 1 , wherein the composition further comprises at least one additional element.

7. The method of claim 6 , wherein the at least one additional element comprises zinc.

8. The method of claim 1 , wherein the isolating comprises removing from the graphene at least one of magnesium oxide, magnesium metal and carbon.

9. The method of claim 8 , wherein the removing comprises washing with an aqueous solution of an acid, and filtering, to produce a filtrate comprising the graphene.

10. The method of claim 9 , wherein the filtrate comprises graphene having an average particle size of at most 300 nm.

11. The method of claim 1 , wherein the graphene is few-layer graphene.

12. The method of claim 1 , wherein an X-ray diffraction pattern under Cu Kα radiation of the isolated graphene has a (100) peak with a full-width at half-maximum intensity which is at most 150% of the full-width at half-maximum intensity of the (100) peak illustrated in FIG. 7 .

13. The method of claim 1 , wherein the isolated graphene has an average particle size of at most 500 nm.

14. The method of claim 1 , wherein the isolated graphene contains less than 5% by weight of non-graphene material.

15. The method of claim 1 , wherein the isolated graphene has an average particle size of at most 500 nm,

the isolated graphene contains less than 5% by weight of non-graphene material, and

an X-ray diffraction pattern under Cu Kα radiation of the isolated graphene has a (100) peak with a full-width at half-maximum intensity which is at most 150% of the full-width at half-maximum intensity of the (100) peak illustrated in FIG. 7 .

16. The method of claim 1 , wherein the isolated graphene is few layer graphene,

the isolated graphene has an average particle size of at most 300 nm,

the isolated graphene contains less than 5% by weight of non-graphene material, and

an X-ray diffraction pattern under Cu Kα radiation of the isolated graphene has a (100) peak with a full-width at half-maximum intensity which is at most 125% of the full-width at half-maximum intensity of the (100) peak illustrated in FIG. 7 .

17. The method of claim 1 , further comprising forming the composition by a process comprising reducing carbon dioxide with magnesium metal,

wherein the isolated graphene is few layer graphene,

the isolated graphene has an average particle size of at most 300 nm,

the isolated graphene contains less than 5% by weight of non-graphene material, and

an X-ray diffraction pattern under Cu Kα radiation of the isolated graphene has a (100) peak with a full-width at half-maximum intensity which is at most 125% of the full-width at half-maximum intensity of the (100) peak illustrated in FIG. 7 .

18. A method of forming a graphene ink, comprising:

preparing isolated graphene by the method of claim 1 , and

dispersing or suspending the isolated graphene into a liquid.

19. The method of claim 18 , wherein the liquid comprises water,

the isolated graphene has an average particle size of at most 500 nm,

the isolated graphene contains less than 5% by weight of non-graphene material, and

an X-ray diffraction pattern under Cu Kα radiation of the isolated graphene has a (100) peak with a full-width at half-maximum intensity which is at most 150% of the full-width at half-maximum intensity of the (100) peak illustrated in FIG. 7 .

20. The method of claim 18 , wherein the liquid comprises an organic liquid,

the isolated graphene has an average particle size of at most 500 nm,

the isolated graphene contains less than 5% by weight of non-graphene material, and

an X-ray diffraction pattern under Cu Kα radiation of the isolated graphene has a (100) peak with a full-width at half-maximum intensity which is at most 150% of the full-width at half-maximum intensity of the (100) peak illustrated in FIG. 7 .

21. The method of claim 18 , wherein the isolated graphene is few layer graphene,

the isolated graphene has an average particle size of at most 300 nm,

the isolated graphene contains less than 5% by weight of non-graphene material, and

an X-ray diffraction pattern under Cu Kα radiation of the isolated graphene has a (100) peak with a full-width at half-maximum intensity which is at most 125% of the full-width at half-maximum intensity of the (100) peak illustrated in FIG. 7 .

22. A method of preparing an electronic device, comprising:

preparing isolated graphene by the method of claim 1 , and

preparing the electronic device from the isolated graphene.

23. The method of claim 22 , wherein the isolated graphene has an average particle size of at most 500 nm,

the isolated graphene contains less than 5% by weight of non-graphene material, and

an X-ray diffraction pattern under Cu Kα radiation of the isolated graphene has a (100) peak with a full-width at half-maximum intensity which is at most 150% of the full-width at half-maximum intensity of the (100) peak illustrated in FIG. 7 .

24. The method of claim 22 , wherein the isolated graphene is few layer graphene,

the isolated graphene has an average particle size of at most 300 nm,

the isolated graphene contains less than 5% by weight of non-graphene material, and

an X-ray diffraction pattern under Cu Kα radiation of the isolated graphene has a (100) peak with a full-width at half-maximum intensity which is at most 125% of the full-width at half-maximum intensity of the (100) peak illustrated in FIG. 7 .

25. A method of preparing an electronic device, comprising:

forming isolated graphene by the method of claim 1 ,

dispersing or suspending the isolated graphene into a liquid, to form a graphene ink, and

preparing the electronic device from the graphene ink.

26. The method of claim 25 , wherein the preparing comprises printing the graphene ink on a substrate.

27. The method of claim 25 , wherein the liquid comprises water,

the isolated graphene has an average particle size of at most 500 nm,

the isolated graphene contains less than 5% by weight of non-graphene material, and

an X-ray diffraction pattern under Cu Kα radiation of the isolated graphene has a (100) peak with a full-width at half-maximum intensity which is at most 150% of the full-width at half-maximum intensity of the (100) peak illustrated in FIG. 7 .

28. The method of claim 25 , wherein the liquid comprises an organic liquid,

the isolated graphene has an average particle size of at most 500 nm,

the isolated graphene contains less than 5% by weight of non-graphene material, and

an X-ray diffraction pattern under Cu Kα radiation of the isolated graphene has a (100) peak with a full-width at half-maximum intensity which is at most 150% of the full-width at half-maximum intensity of the (100) peak illustrated in FIG. 7 .

29. The method of claim 25 , wherein the isolated graphene is few layer graphene,

the isolated graphene has an average particle size of at most 300 nm,

the isolated graphene contains less than 5% by weight of non-graphene material, and

an X-ray diffraction pattern under Cu Ku radiation of the isolated graphene has a (100) peak with a full-width at half-maximum intensity which is at most 125% of the full-width at half-maximum intensity of the (100) peak illustrated in FIG. 7 .

30. A method of producing isolated graphene, comprising:

reducing carbon dioxide with molten metal, the molten metal comprising magnesium, to form a composition comprising graphene and magnesium oxide,

isolating graphene from the composition, to form isolated crystalline graphene,

wherein the isolated crystalline graphene has an average particle size of at most 500 nm, and

the isolated crystalline graphene contains less than 5% by weight of non-graphene material.

31. A method of producing isolated graphene, comprising isolating graphene from a composition comprising graphene, magnesium and at least one additional element, wherein the at least one additional element comprises zinc.

Assignments (2)
CONFIRMATORY LICENSE Recorded Jan 2, 2015
From: NORTHERN ILLINOIS UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 034719/0438 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 14, 2014
From: CHAKRABARTI, AMARTYA; HOSMANE, NARAYAN S
To: BOARD OF TRUSTEES OF NORTHERN ILLINOIS UNIVERSITY
Reel/Frame 031966/0793 →
Continuity (2)
Provisional Application 61533045 · Sep 9, 2011
Related Publication 20140193575A1 · Jul 10, 2014