IP Library Granted Patent US 9,902,866
Granted Patent B2
US 9,902,866 · App. 14/756,304 · Granted Feb 27, 2018

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); Bok Y. Ahn (Cambridge, MA); Jennifer A. Lewis (Cambridge, MA)
Assignees: Northwestern University; President and Fellows of Harvard College
C09D11/38B41J2/01B41M5/0023C01B32/19C09D11/14C09D11/322C09D11/36C09D11/52H01L51/0005C01P2006/32H01L51/0045
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Quick Facts
Patent No.
US 9,902,866
App. No.
14/756,304
Granted
Feb 27, 2018
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 (34)

1. A method of preparing an inkjet printed 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 precursor composition comprising graphene and a said ethyl cellulose;

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

contacting said solid graphene-ethyl cellulose precursor composition with a hydrophobic fluid component, to provide a graphene ink composition;

inkjet printing said graphene ink composition on a substrate; and

photonic annealing said graphene ink composition.

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

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

4. The method of claim 1 wherein said graphene ink composition has a graphene concentration of greater than about 3 mg/mL.

5. The method of claim 4 wherein said graphene ink composition has a graphene concentration of about 20 mg/mL.

6. The method of claim 5 wherein said graphene ink has a solids content of about 4% w/v.

7. The method of claim 6 wherein said graphene ink composition has a viscosity of about 8-15 mPa·sec.

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

9. A method of preparing an inkjet printed 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 to provide a precursor composition comprising graphene and a said ethyl cellulose;

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

contacting said graphene-ethyl cellulose precursor composition with a hydrophobic fluid component, to provide a graphene ink composition comprising a graphene concentration greater than about 3 mg/mL;

inkjet printing said graphene ink composition on a substrate; and

photonic annealing said graphene ink composition.

10. The method of claim 9 wherein said hydrophobic fluid comprises a component selected from terpenes, terpine alcohols and combinations thereof.

11. The method of claim 9 wherein said hydrophobic fluid component comprises a terpineol and cyclohexanone.

12. The method of claim 9 wherein said graphene ink composition has a graphene ink concentration of about 20 mg/mL.

13. The method of claim 12 wherein said graphene ink has a solids content of about 4% w/v.

14. The method of claim 13 wherein said graphene ink composition has a viscosity of about 8-15 mPa·sec.

15. The method of claim 9 wherein said exfoliating comprises shear mixing said graphene source material and said medium.

16. A method of using photonic annealing to prepare a graphene ink composite, said method comprising:

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

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

contacting said graphene-ethyl cellulose precursor composition with a hydrophobic fluid component, to provide a graphene ink composition comprising a solids content of about 4% w/v, a graphene concentration of about 20 mg/mL and a viscosity of about 8-about 15 mPa·sec;

inkjet printing said graphene ink composition on a substrate to provide a graphene-substrate composite; and

photonic annealing said graphene ink composition to provide a graphene ink composition comprising a decomposition product of a said ethyl cellulose.

17. The method of claim 16 wherein said hydrophobic fluid component comprises a terpineol and cyclohexanone.

18. The method of claim 16 wherein said precursor composition comprises about 50% wt. graphene and about 50% wt. a said ethyl cellulose.

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 19, 2016
From: AHN, BOK YEOP; LEWIS, JENNIFER A.
To: PRESIDENT AND FELLOWS OF HARVARD COLLEGE
Reel/Frame 039483/0317 →
CONFIRMATORY LICENSE Recorded Mar 18, 2016
From: NORTHWESTERN UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 038177/0564 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 13, 2016
From: HERSAM, MARK C.; SECOR, ETHAN B.; LIANG, YU TENG; PRABHUMIRASHI, PRADYUMNA L.; PUNTAMBEKAR, KANAN P.; GEIER, MICHAEL L.
To: NORTHWESTERN UNIVERSITY
Reel/Frame 037475/0549 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 13, 2016
From: AHN, BOK YEOP; LEWIS, JENNIFER A.
To: PRESIDENT AND FELLOWS OF HARVARD COLLEGE
Reel/Frame 037475/0918 →
Continuity (4)
Continuation In Part 14121097 · Jul 30, 2014
Continuation In Part 13453608 · Apr 23, 2012
Provisional Application 61478361 · Apr 22, 2011
Related Publication 20170081537A1 · Mar 23, 2017