IP Library Granted Patent US 10,099,929
Granted Patent B2
US 10,099,929 · App. 14/771,293 · Granted Oct 16, 2018

Method of producing a graphene material

Inventor: Iti Srivastava (Rocky River, OH)
Assignee: NeoGraf Solutions, LLC
C01B31/0469C01B32/184C01B32/19C01B2204/04
View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 10,099,929
App. No.
14/771,293
Granted
Oct 16, 2018
Kind
B2
Abstract

A method of producing graphene powder includes the heat treatment of a graphitizable polymer film to at least 2000 degrees C. to form a heat treated film having a substantially turbostratic graphitic structure. The heat treated film is then sheared along a plane substantially parallel to a major surface of the heat treated film to form a particulate having a thickness less than 100 nanometers.

Claims (24)

1. A method of producing a graphene powder comprising:

heat treating to between 2000 degrees C. and 2600 degrees C. a graphitizable polymer film having a thickness from between about 10 microns to about 200 microns thereby forming a heat treated film having a turbostratic graphitic structure of stacks of aligned graphene planes of between 5 graphene layers to 200 graphene layers, wherein the stacks are unaligned; and

shearing the heat treated film along a plane parallel to a major surface of the heat treated film to delaminate the graphene planes within the stacks and separate the unaligned stacks thereby forming a particulate wherein said particulate has a thickness less than about 100 nanometers and said shearing is not ball milling.

2. The method according to claim 1 wherein said heat treating is to at least 2200 degrees C.

3. The method according to claim 1 wherein said graphitizable polymer selected from the group consisting of polyphenylenoxadiazoles (POD), polybenzothiazole (PBT), polybenzohisthiazole (PBBT), polybenzooxazole (PBO), polybenzobisoxazole (PBBO), aromatic potyimides (PI), aromatic polyamides (PA), polyphenylenbenzoimidazole (PBI), polyphenylenebenzobisimidazole (PPBI), polythiazole (PT), poly-p-phenylenevinylene (PPV) or mixtures thereof.

4. The method according to claim 1 wherein said graphitizable polymer film is from between 10 and 100 microns thick.

5. The: method according to claim 4 wherein said, graphitizable polymer film is less than about 75 microns thick.

6. The method according to claim 1 wherein said particulate has a thickness less than about 25 nanometers.

7. The method according claim 1 wherein said shearing comprises mechanical shearing using a centrifugal mill.

8. The method according to claim 7 wherein said shearing occurs between a rotor and a fixed ring sleeve.

9. The method according to claim 1 wherein said heat treated film exhibits an ( 002 ) peak d-spacing from between about 3.3500 Å to about 3.4300 Å.

10. The method according to claim 1 wherein said heat treated film exhibits an ( 002 ) peak d-spacing greater than about 3.3500 Å.

11. The method according to claim 1 wherein said heat treated film exhibits a crystal size Le from between about 50 Å to about 600 Å.

12. The method according to claim 1 wherein the thickness comprises no more than 75 nanometers.

13. The method according to claim l wherein said shearing includes a blade contacting the heat treated film in a direction parallel to a major surface of the heat treated film.

14. A method of producing a graphene powder comprising:

heat treating to between 2000 degrees C. and 2600 degrees C. a graphitizable polymer film having a thickness from between about 10 microns to about 200 microns thereby forming a heat treated film having a turbostratic graphitic structure of stacks of aligned graphene planes of between 5 graphene layers to 200 graphene layers, wherein the stacks are unaligned; and

shearing the heat treated film along a plane parallel to a major surface of the heat treated film to delaminate the graphene planes within the stacks and separate the unaligned stacks thereby forming a particulate wherein said particulate has a thickness less than about 1000 nanometers and said shearing is not ball milling.

15. method of claim 14 wherein the particulate thickness comprises no more than 250 nanometers.

16. The method of claim 14 wherein the graphitizable polymer film is formed from a precursor film having a thickness comprising from about 25 microns to about 75 microns.

17. The method according claim 14 wherein said shearing comprises mechanical shearing using a centrifugal mill.

18. The method according to claim 17 wherein said shearing occurs between a rotor and a fixed ring sleeve.

19. The method according to claim 14 wherein said heat treated film exhibits a crystal size Le from between about 50 Å to about 600 Å.

20. The method according to claim 14 wherein said shearing includes a blade contacting the heat treated film in a direction parallel to a major surface of the heat treated film.

Assignments (9)
RELEASE OF SECURITY INTEREST Recorded Feb 1, 2023
From: WELLS FARGO BANK, NATIONAL ASSOCIATION
To: NEOGRAF SOLUTIONS, LLC
Reel/Frame 062972/0634 →
SECURITY INTEREST Recorded Jan 31, 2023
From: NEOGRAF SOLUTIONS, LLC
To: GLADSTONE CAPITAL CORPORATION
Reel/Frame 062571/0858 →
SECURITY INTEREST Recorded Jan 31, 2023
From: NEOGRAF SOLUTIONS, LLC
To: GCG INVESTORS V, L.P., AS AGENT
Reel/Frame 062568/0036 →
SECURITY AGREEMENT Recorded Sep 13, 2017
From: NEOGRAF SOLUTIONS, LLC
To: WELLS FARGO BANK, NATIONAL ASSOCIATION
Reel/Frame 043843/0582 →
CHANGE OF NAME Recorded Jul 26, 2017
From: ADVANCED ENERGY TECHNOLOGIES LLC
To: NEOGRAF SOLUTIONS, LLC
Reel/Frame 043336/0472 →
RELEASE OF SECURITY INTERESTS RECORDED AT REEL/FRAMES 013463/0360, 024678/0830, 014357/0075, AND 035839/0754 Recorded Jul 6, 2017
From: JPMORGAN CHASE BANK, N.A., AS COLLATERAL AGENT FKA MORGAN GUARANTY TRUST COMPANY OF NEW YORK
To: ADVANCED ENERGY TECHNOLOGIES LLC AS ASSIGNEE OF GRAFTECH INTERNATIONAL HOLDINGS INC. FKA ADVANCED ENERGY TECHNOLOGY INC. FKA GRAFTECH INC.
Reel/Frame 043099/0502 →
CORRECTIVE ASSIGNMENT TO CORRECT THE INCORRECT APPL. NO. 14/771,229 PREVIOUSLY RECORDED AT REEL: 040647 FRAME: 0534. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT. Recorded Jun 21, 2017
From: GRAFTECH INTERNATIONAL HOLDINGS INC.
To: ADVANCED ENERGY TECHNOLOGIES LLC
Reel/Frame 042938/0856 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 18, 2016
From: GRAFTECH INTERNATIONAL HOLDINGS INC.
To: ADVANCED ENERGY TECHNOLOGIES LLC
Reel/Frame 040647/0534 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 28, 2015
From: SRIVASTAVA, ITI
To: GRAFTECH INTERNATIONAL HOLDINGS, INC.
Reel/Frame 036447/0046 →
Continuity (2)
Provisional Application 61834610 · Jun 13, 2013
Related Publication 20160002046A1 · Jan 7, 2016