IP Library Granted Patent US 10,427,941
Granted Patent B2
US 10,427,941 · App. 16/104,251 · Granted Oct 1, 2019

Direct ultrasonication production of graphene sheets from coke or coal

Inventors: Aruna Zhamu (Springboro, OH); Bor Z. Jang (Centerville, OH)
Assignee: Nanotek Instruments, Inc.
C01B32/19C09D7/61C09D11/52C09D171/02C09K5/14H01B1/24C08K3/04
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Quick Facts
Patent No.
US 10,427,941
App. No.
16/104,251
Granted
Oct 1, 2019
Kind
B2
Abstract

Provided is a method of producing isolated graphene sheets from a supply of coke or coal powder containing therein domains of hexagonal carbon atoms and/or hexagonal carbon atomic interlayers. The method comprises: (a) dispersing particles of the coke or coal powder in a liquid medium containing therein an optional surfactant or dispersing agent to produce a suspension or slurry, wherein the coke or coal powder is selected from petroleum coke, coal-derived coke, mesophase coke, synthetic coke, leonardite, anthracite, lignite coal, bituminous coal, or natural coal mineral powder, or a combination thereof; and (b) exposing the suspension or slurry to ultrasonication at an energy level for a sufficient length of time to produce the isolated graphene sheets.

Claims (12)

1. A method of producing a isolated graphene sheets-containing ink composition, said method comprising:

a) dispersing particles of said coke or coal powder in a liquid medium containing therein a surfactant or dispersing agent to produce a suspension and containing no oxidant or acid, wherein said coke or coal powder is selected from the group consisting of petroleum coke, coal-derived coke, mesophase coke, synthetic coke, leonardite, anthracite, lignite coal, bituminous coal, or natural coal mineral powder, and combinations thereof; and

b) exposing said suspension to ultrasonication at an energy level for a sufficient length of time to produce said isolated graphene sheets in said liquid medium

c) adding a property modifier or chemical species to produce said isolated graphene sheets-containing ink composition, wherein said addition can occur before, during or after exposing said suspension to ultrasonication.

2. The method of claim 1 wherein said step of ultrasonication has a time from 5 minutes to 2 hours.

3. The method of claim 1 further comprising a mechanical shearing treatment selected from air milling, air jet milling, wet milling, ball milling, rotating blade shearing, or a combination thereof.

4. The method of claim 1 further comprising a step of spraying said isolated graphene sheets-containing ink composition onto a solid surface to form a wet film, and drying said wet film, to form a dried graphene film.

5. The method of claim 1 further comprising a step of coating said isolated graphene sheets-containing ink composition onto a solid surface to form a wet film having aligned graphene sheets, and drying said wet film, to form a dried graphene film.

6. The method of claim 5 further comprising a step of heat treating said dried graphene film at a temperature from 100° C. to 3,200° C.

7. The method of claim 5 further comprising a step of compression.

8. The method of claim 1 wherein said liquid medium is selected from the group consisting of water, organic solvents, alcohols, monomers, oligomers, and resins.

9. The method of claim 1 wherein said property modifier or chemical species is selected from the group consisting of anionic surfactants, nonionic surfactants, cationic surfactants, amphoteric surfactants, silicone surfactants, fluoro-surfactants, polymeric surfactants, sodium hexametaphosphate, sodium lignosulfonate, poly (sodium 4-styrene sulfonate), sodium dodecylsulfate, sodium sulfate, sodium phosphate, sodium sulfonate, melamine, ammonium sulfate, sodium dodecyl sulfate, sodium (ethylenediamine), tetraalkylammonium, ammonia, carbamide, hexamethylenetetramine, organic amine, pyrene, 1-pyrenecarboxylic acid, 1-pyrenebutyric acid, 1-pyrenamine, poly(sodium-4-styrene sulfonate), and combinations thereof.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 20, 2019
From: NANOTEK INSTRUMENTS, INC.
To: GLOBAL GRAPHENE GROUP, INC.
Reel/Frame 050444/0315 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 11, 2018
From: ZHAMU, ARUNA; JANG, BOR Z
To: NANOTEK INSTRUMENTS, INC.
Reel/Frame 046835/0096 →