IP Library Granted Patent US 7,658,901
Granted Patent B2
US 7,658,901 · App. 11/249,404 · Granted Feb 9, 2010

Thermally exfoliated graphite oxide

Assignee: The Trustees of Princeton University
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Quick Facts
Patent No.
US 7,658,901
App. No.
11/249,404
Granted
Feb 9, 2010
Kind
B2
Abstract

A modified graphite oxide material contains a thermally exfoliated graphite oxide with a surface area of from about 300 m 2 /g to 2600 m 2 /g, wherein the thermally exfoliated graphite oxide displays no signature of the original graphite and/or graphite oxide, as determined by X-ray diffraction.

Claims (61)

1. A modified graphite oxide material, comprising:

a thermally exfoliated graphite oxide having a surface area of from about 500 m 2 /g to 2600 m 2 /g,

wherein said thermally exfoliated graphite oxide is obtained from heating graphite oxide at a temperature of from 300 to 2000° C.

2. The modified graphite oxide material as claimed in claim 1 , wherein said thermally exfoliated graphite oxide has a bulk density of from about 40 kg/m 3 to 0.1 kg/m 3 .

3. The modified graphite oxide material as claimed in claim 1 , wherein said thermally exfoliated graphite oxide has a C/O ratio, after high temperature expansion, of from about 60/40 to 95/5.

4. The modified graphite oxide material as claimed in claim 3 , wherein said thermally exfoliated graphite oxide has a C/O ratio, after high temperature expansion, of from about 65/35 to 85/15.

5. A thermally exfoliated graphite oxide produced by a process, comprising:

(a) oxidizing graphite thereby obtaining graphite oxide with spatially expanded graphene interlayers; and

(b) heating the graphite oxide at a temperature of from 300 to 2000° C. to cause decomposition and expansion of the graphite oxide;

wherein said thermally exfoliated graphite oxide has a surface area of from about 500 m 2 /g to 2600 m 2 /g.

6. The thermally exfoliated graphite oxide as claimed in claim 5 , wherein the oxidizing of the graphite results in substantially complete intercalation and oxidation of graphite.

7. The thermally exfoliated graphite oxide as claimed in claim 5 , which further comprises removing acids and salts from the graphene interlayers prior to heating the graphite oxide.

8. The thermally exfoliated graphite oxide as claimed in claim 5 , which further comprises drying the graphite oxide to remove excess water and/or solvent, prior to heating the graphite oxide.

9. The thermally exfoliated graphite oxide as claimed in claim 5 , wherein said thermally exfoliated graphite oxide has a bulk density of from about 40 kg/m 3 to 0.1 kg/m 3 .

10. The thermally exfoliated graphite oxide as claimed in claim 5 , wherein said thermally exfoliated graphite oxide has a C/O ratio of from about 60/40 to 95/5.

11. A method for manufacturing a thermally exfoliated graphite oxide, comprising:

(a) oxidizing graphite thereby obtaining graphite oxide with spatially expanded graphene interlayers; and

(b) heating the graphite oxide at a temperature of from 300 to 2000° C. to cause decomposition and expansion of the graphite oxide;

wherein said thermally exfoliated graphite oxide has a surface area of from about 400 m 2 /g to 2600 m 2 /g.

12. The method as claimed in claim 11 , wherein the oxidizing of the graphite results in substantially complete intercalation and oxidation of graphite.

13. The method as claimed in claim 11 , which further comprises removing acids and salts from the graphene interlayers prior to heating the graphite oxide.

14. The method as claimed in claim 11 , which further comprises drying the graphite oxide to remove excess water and/or solvent, prior to heating the graphite oxide.

15. The method as claimed in claim 11 , wherein said thermally exfoliated graphite oxide has a bulk density of from about 40 kg/m 3 to 0.1 kg/m 3 .

16. The method as claimed in claim 11 , wherein said thermally exfoliated graphite oxide has a C/O ratio of from about 60/40 to 95/5.

17. The modified graphite oxide material as claimed in claim 1 , wherein the thermally exfoliated graphite oxide has an X-ray diffraction pattern in which the area under the diffraction peak between 2θ=12.5 and 14.5° is less than 15 percent of the total area under the diffraction peak between 2θ=9 and 21°.

18. The modified graphite oxide material as claimed in claim 1 , wherein the thermally exfoliated graphite oxide is obtained from heating graphite oxide at a rate of at least 120° C./min.

19. The modified graphite oxide material as claimed in claim 1 , wherein the thermally exfoliated graphite oxide is obtained from heating graphite oxide at a rate of at least 2000° C./min.

20. The modified graphite oxide material as claimed in claim 1 , wherein the heating is at a temperature of from 700 to 2000° C.

21. The modified graphite oxide material as claimed in claim 1 , wherein the heating is at a temperature of from 900 to 2000° C.

22. The modified graphite oxide material as claimed in claim 1 , wherein the thermally exfoliated graphite oxide has a surface area of from 600 m 2 /g to 2600 m 2 /g.

23. The modified graphite oxide material as claimed in claim 1 , wherein the thermally exfoliated graphite oxide has a surface area of from 800 m 2 /g to 2600 m 2 /g.

24. The modified graphite oxide material as claimed in claim 1 , wherein the graphite oxide is heated for between 1 second and 5 minutes.

25. The modified graphite oxide material as claimed in claim 1 , wherein the graphite oxide is heated for between 1 second and 1 minute.

26. The modified graphite oxide material as claimed in claim 1 , wherein the graphite oxide is heated for between a fraction of a second and about 1 second.

27. The modified graphite oxide material as claimed in claim 1 , wherein the graphite oxide is heated for between 1 second and 10 seconds.

28. The modified graphite oxide material as claimed in claim 1 , wherein said thermally exfoliated graphite oxide displays no signature of graphite and/or graphite oxide, as determined by X-ray diffraction.

29. The thermally exfoliated graphite oxide as claimed in claim 5 , having an X-ray diffraction pattern in which the area under the diffraction peak between 2θ=12.5 and 14.5° is less than 15 percent of the total area under the diffraction peak between 2θ=9 and 21°.

30. The thermally exfoliated graphite oxide as claimed in claim 5 , wherein the thermally exfoliated graphite oxide is obtained from heating graphite oxide at a rate of at least 120° C./min.

31. The thermally exfoliated graphite oxide as claimed in claim 5 , wherein the thermally exfoliated graphite oxide is obtained from heating graphite oxide at a rate of at least 2000° C./min.

32. The thermally exfoliated graphite oxide as claimed in claim 5 , wherein the heating is at a temperature of from 700 to 2000° C.

33. The thermally exfoliated graphite oxide as claimed in claim 5 , wherein the heating is at a temperature of from 900 to 2000° C.

34. The thermally exfoliated graphite oxide as claimed in claim 5 , wherein the thermally exfoliated graphite oxide has a surface area of from 600 m 2 /g to 2600 m 2 /g.

35. The thermally exfoliated graphite oxide as claimed in claim 5 , wherein the thermally exfoliated graphite oxide has a surface area of from 800 m 2 /g to 2600 m 2 /g.

36. The thermally exfoliated graphite oxide as claimed in claim 5 , wherein the graphite oxide is heated for between 1 second and 5 minutes.

37. The thermally exfoliated graphite oxide as claimed in claim 5 , wherein the graphite oxide is heated for between 1 second and 1 minute.

38. The thermally exfoliated graphite oxide as claimed in claim 5 , wherein the graphite oxide is heated for between 1 second and 10 seconds.

39. The thermally exfoliated graphite oxide as claimed in claim 5 , wherein said thermally exfoliated graphite oxide displays no signature of graphite and/or graphite oxide, as determined by X-ray diffraction.

40. The thermally exfoliated graphite oxide as claimed in claim 5 , wherein the graphite oxide is heated for between a fraction of a second and about 1 second.

41. The method as claimed in claim 11 , having an X-ray diffraction pattern in which the area under the diffraction peak between 2θ=12.5 and 14.5° is less than 15 percent of the total area under the diffraction peak between 2θ=9 and 21°.

42. The method as claimed in claim 11 , wherein the thermally exfoliated graphite oxide is obtained from heating graphite oxide at a rate of at least 120° C./min.

43. The method as claimed in claim 11 , wherein the thermally exfoliated graphite oxide is obtained from heating graphite oxide at a rate of at least 2000° C./min.

44. The method as claimed in claim 11 , wherein the heating is at a temperature of from 700 to 2000° C.

45. The method as claimed in claim 11 , wherein the heating is at a temperature of from 900 to 2000° C.

46. The method as claimed in claim 11 , wherein the thermally exfoliated graphite oxide has a surface area of from 500 m 2 /g to 2600 m 2 /g.

47. The method as claimed in claim 11 , wherein the thermally exfoliated graphite oxide has a surface area of from 600 m 2 /g to 2600 m 2 /g.

48. The method as claimed in claim 11 , wherein the thermally exfoliated graphite oxide has a surface area of from 800 m 2 /g to 2600 m 2 /g.

49. The method as claimed in claim 11 , wherein the graphite oxide is heated for between 1 second and 5 minutes.

50. The method as claimed in claim 11 , wherein the graphite oxide is heated for between 1 second and 1 minute.

51. The method as claimed in claim 11 , wherein the graphite oxide is heated for between 1 second and 10 seconds.

52. The method as claimed in claim 11 , wherein the graphite oxide is heated for between a fraction of a second and about 1 second.

53. The method as claimed in claim 13 , wherein said thermally exfoliated graphite oxide displays no signature of graphite and/or graphite oxide, as determined by X-ray diffraction.

Assignments (6)
CONFIRMATORY LICENSE Recorded Dec 22, 2010
From: PRINCETON UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 025549/0073 →
CONFIRMATORY LICENSE Recorded May 19, 2010
From: PRINCETON UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 024410/0155 →
CONFIRMATORY LICENSE Recorded May 19, 2010
From: PRINCETON UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 024410/0372 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 9, 2009
From: PRINCETON UNIVERSITY
To: THE TRUSTEES OF PRINCETON UNIVERSITY
Reel/Frame 023626/0204 →
LICENSE Recorded Dec 3, 2008
From: PRINCETON UNIVERSITY
To: UNITED STATES OF AMERICA AS REPRESENTED BY THE ADMINISTRATOR OF THE NATIONAL AERONAUTICS AND SPACE ADMINISTRATION
Reel/Frame 021922/0925 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 31, 2006
From: PRUD'HOMME, ROBERT K.; AKSAY, ILHAN A.; ADAMSON, DOUGLAS; ABDALA, AHMED
To: PRINCETON UNIVERSITY
Reel/Frame 017516/0653 →
Continuity (1)
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