IP Library Granted Patent US 9,834,693
Granted Patent B2
US 9,834,693 · App. 14/121,097 · Granted Dec 5, 2017

Methods for preparation of concentrated graphene ink compositions and related composite materials

Inventors: Mark C. Hersam (Wilmette, IL); Yu Teng Liang (Chicago, IL); Ethan B. Secor (Evanston, IL); Pradyumna L. Prabhumirashi (Chicago, IL); Kanan P. Puntambekar (Chicago, IL); Michael L. Geier (Chicago, IL)
Assignee: Northwestern University
C09D11/38C09D11/14C09D11/52H01B1/24Y10T428/31721Y10T428/31786
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Quick Facts
Patent No.
US 9,834,693
App. No.
14/121,097
Granted
Dec 5, 2017
Kind
B2
Abstract

A rapid, scalable methodology for graphene dispersion and concentration with a polymer-organic solvent medium, as can be utilized without centrifugation, to enhance graphene concentration.

Claims (24)

1. A method of using a cellulosic polymer for preparing a concentrated graphene medium, said method comprising:

exfoliating a graphene source material with a medium comprising an organic solvent at least partially miscible with water and a dispersing agent comprising a cellulosic polymer, said dispersing agent at least partially soluble in said organic solvent;

contacting at least a portion of said exfoliated graphene medium with an aqueous medium to concentrate exfoliated graphene in a solid composition comprising graphene and a said cellulosic polymer;

isolating said solid composition from said exfoliating and said aqueous media; and

contacting said solid graphene composition with a hydrophobic fluid component.

2. The method of claim 1 wherein said cellulosic polymer comprises an ethyl cellulose.

3. The method of claim 1 wherein said organic solvent is selected from C 2 - C 5 alcohols, esters, amides, ethers and ketones and combinations thereof.

4. The method of claim 3 wherein said organic solvent is selected from ethanol and dimethylformamide.

5. The method of claim 1 wherein said hydrophobic fluid component comprises a component selected from terpenes, terpene alcohols and combinations thereof.

6. The method of claim 1 wherein said hydrophobic fluid component comprises a terpineol and cyclohexanone.

7. The method of claim 1 wherein said graphene source material is graphite.

8. The method of claim 1 comprising deposition of said graphene composition on a substrate.

9. The method of claim 8 wherein said graphene composition is annealed.

10. The method of claim 9 wherein said graphene composition is photoannealed.

11. The method of claim 1 wherein said exfoliation comprises shear mixing said graphene source material and said medium.

12. The method of claim 11 wherein said organic solvent is selected from C 2 - C 5 alcohols, esters, amides, ethers and ketones and combinations thereof; and said dispersing agent comprises an ethyl cellulose.

13. A method of preparing a graphene ink composition, said method comprising:

exfoliating a graphene source material with a medium comprising an organic solvent selected from ethanol and dimethylformamide, and an ethyl cellulose;

contacting at least a portion of said exfoliated graphene medium with an aqueous medium to concentrate exfoliated graphene and ethyl cellulose in a solid composition comprising graphene and said ethyl cellulose;

isolating said solid composition from said exfoliating and said aqueous media; and

contacting said solid graphene ethyl cellulose composition with a hydrophobic fluid component to provide a graphene ink composition.

14. The method of claim 13 wherein said exfoliating comprises shear mixing said graphene source material and said medium.

15. The method of claim 13 comprising printing said graphene ink composition on a substrate.

16. The method of claim 15 wherein said graphene ink composition is photoannealed.

Assignments (2)
CONFIRMATORY LICENSE Recorded Oct 1, 2015
From: NORTHWESTERN UNIVERSITY
To: NAVY, SECRETARY OF THE UNITED STATES OF AMERICA
Reel/Frame 036737/0461 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 3, 2014
From: HERSAM, MARK C.; SECOR, ETHAN B.; PRABHUMIRASHI, PRADYUMNA L.; PUNTAMBEKAR, KANAN P.; GEIER, MICHAEL L.; LIANG, YU TENG
To: NORTHWESTERN UNIVERSITY
Reel/Frame 034091/0657 →
Continuity (4)
Continuation In Part 13453608 · Apr 23, 2012
Provisional Application 61861257 · Aug 1, 2013
Provisional Application 61478361 · Apr 22, 2011
Related Publication 20150072162A1 · Mar 12, 2015