IP Library Granted Patent US 8,734,683
Granted Patent B2
US 8,734,683 · App. 13/306,540 · Granted May 27, 2014

Graphene nano-sheets and methods for making the same

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Quick Facts
Patent No.
US 8,734,683
App. No.
13/306,540
Granted
May 27, 2014
Kind
B2
Abstract

Various embodiments provide materials and methods for forming a graphene product by vacuum induction heating expandable graphite. The graphene product can include graphene nano-sheets with high purity and uniform thickness. The graphene nano-sheets can contain carbon of more than about 99% by weight. The graphene nano-sheets can be exfoliated or dispersed within a matrix of a semiconducting polymer to form a graphene-containing composite.

Claims (25)

1. A method of making graphene nano-sheets, comprising:

placing an expandable graphite within a chamber;

applying vacuum to the chamber, such that a vacuum pressure in the chamber ranges from about 10 −1 mbar to about 10 −7 mbar in the chamber;

applying an electric current to induction heat the expandable graphite within the chamber under the vacuum to form an expanded graphite; and

exfoliating the expanded graphite in a solvent to form one or more graphene nano-sheets dispersed in the solvent.

2. The method of claim 1 , further comprising expanding the expandable graphite by about 200% to about 1000% by volume within the chamber to form the expanded graphite.

3. The method of claim 1 , wherein the expandable graphite is heated to a temperature ranging from about 500° C. to about 1100° C.

4. The method of claim 3 , wherein the expandable graphite is heated at the temperature for a time length ranging from about 1 second to about 5 minutes.

5. The method of claim 1 , wherein the expandable graphite comprises an intercalation agent.

6. The method of claim 5 , wherein the intercalation agent is selected from the group consisting of halogens, alkali metals, sulfate, nitrate, acids, metal halides, and combinations thereof.

7. A method of making a graphene product comprising:

placing expandable graphite within a chamber, the expandable graphite comprising an intercalation agent capable of producing thermal expansion;

applying vacuum to the chamber, wherein a vacuum pressure ranges from about 10 −1 mbar to about 10 −7 mbar in the chamber;

applying an electric current to induction heat the expandable graphite under the vacuum to form expanded graphite; and

exfoliating the expanded graphite in a solvent to forms one or more graphene nano-sheets dispersed in the solvent.

8. The method of claim 7 , wherein the electric current is applied to reach a heating temperature ranging from 500° C. to about 1100° C.

9. The method of claim 7 , wherein each of the one or more graphene nano-sheets is formed to have an average thickness ranging from about 0.3 nm to about 15 nm.

10. The method of claim 7 , wherein the one or more graphene nano-sheets are substantially free of impurity species comprising S, N, Cl, O atoms, or their combinations.

11. The method of claim 7 , wherein the one or more graphene nano-sheets comprise carbon of at least about 99% by weight.

12. The method of claim 7 , wherein the step of exfoliating the expanded graphite comprises sonicating the expanded graphite to form the one or more graphene nano-sheets in the solvent.

13. The method of claim 7 , wherein the solvent comprises toluene, chiorotoluene, chlorobenzene, dichlorobenzene, xylene, mesitylene, chloroethane, chloromethane, dimethylformamide (DMF), N-Methyl-2-pyrrolidone (NMP), or combinations thereof.

14. The method of claim 7 , wherein the step of exfoliating the expanded graphite is carried out in a presence of a conjugated polymer.

15. The method of claim 14 , wherein the conjugated polymer comprises a polythiophene.

16. The method of claim 14 , further comprising coating the graphene dispersion on a substrate to form a graphene-containing composite comprising the one or more graphene nano-sheets dispersed in a matrix of the conjugated polymer.

17. The method of claim 14 , wherein the one or more graphene nano-sheets are present in an, amount ranging from about 0.001% to about 5.0% by weight of a total of the one or more graphene nano-sheets and the conjugate polymer.

Assignments (9)
SECOND LIEN NOTES PATENT SECURITY AGREEMENT Recorded Jul 2, 2025
From: XEROX CORPORATION
To: U.S. BANK TRUST COMPANY, NATIONAL ASSOCIATION, AS COLLATERAL AGENT
Reel/Frame 071785/0550 →
FIRST LIEN NOTES PATENT SECURITY AGREEMENT Recorded Apr 11, 2025
From: XEROX CORPORATION
To: U.S. BANK TRUST COMPANY, NATIONAL ASSOCIATION, AS COLLATERAL AGENT
Reel/Frame 070824/0001 →
SECURITY INTEREST Recorded Feb 13, 2024
From: XEROX CORPORATION
To: CITIBANK, N.A., AS COLLATERAL AGENT
Reel/Frame 066741/0001 →
TERMINATION AND RELEASE OF SECURITY INTEREST IN PATENTS RECORDED AT RF 064760/0389 Recorded Feb 13, 2024
From: CITIBANK, N.A., AS COLLATERAL AGENT
To: XEROX CORPORATION
Reel/Frame 068261/0001 →
SECURITY INTEREST Recorded Nov 20, 2023
From: XEROX CORPORATION
To: JEFFERIES FINANCE LLC, AS COLLATERAL AGENT
Reel/Frame 065628/0019 →
SECURITY INTEREST Recorded Jun 22, 2023
From: XEROX CORPORATION
To: CITIBANK, N.A., AS COLLATERAL AGENT
Reel/Frame 064760/0389 →
RELEASE OF SECURITY INTEREST IN PATENTS AT R/F 062740/0214 Recorded May 18, 2023
From: CITIBANK, N.A., AS AGENT
To: XEROX CORPORATION
Reel/Frame 063694/0122 →
SECURITY INTEREST Recorded Nov 10, 2022
From: XEROX CORPORATION
To: CITIBANK, N.A., AS AGENT
Reel/Frame 062740/0214 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 29, 2011
From: WU, YILIANG; GARDNER, SANDRA J
To: XEROX CORPORATION
Reel/Frame 027290/0231 →