# US 9,434,664 B2 · Preparation method for edge-fluorinated graphite via mechanic-chemical process

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- Number: US 9,434,664 B2
- Document ID: US9434664B2
- Status: Granted
- Kind: B2
- Application number: 14/605,716
- Filed: 2015-01-26
- Published: 2015-07-30
- Granted: 2016-09-06
- Earliest claimed: 2014-01-27
- Assignees: Unist (Ulsan National Institute of Science and Technology)
- Applicants: Unist Academy-Industry Research Corporation
- Inventors: Jong-Beom Baek; In-Yup Jeon
- Web page: https://patentgrep.com/patent/US9434664B2

## CPC

- C07C 17/02: to unsaturated hydrocarbons
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- B82Y 40/00: Manufacture or treatment of nanostructures
- C01B 32/10: Carbon fluorides, e.g. [CF]nor [C2F]n (graphite intercalation thereof C01B32/22)
- C01B 32/184: Preparation
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}

## Abstract

Disclosed is a method for producing edge-functionalized graphite or graphene with fluoro groups. According to the method, graphite is pulverized into smaller pieces and is then allowed to react with a surrounding material containing fluorine or a fluorocarbon compound. The method enables the production of graphite or graphene functionalized with fluoro groups, which could not be achieved by conventional mechanochemical methods. In addition, the method is carried out in a very simple and economical manner and is suitable for large-scale production.

## Claims

### Claim 1

A method for producing edge-functionalized graphite or graphene with fluoro groups, comprising (i) mechanically pulverizing graphite under an inert atmosphere in a closed container; (ii) then, evacuating the inert atmosphere, and (iii) reacting the pulverized graphite with fluorine or a fluorocarbon compound at a pressure of 2 to 20 bar, wherein the fluorocarbon compound is trifluoromethane, tetrafluoromethane, trifluoroethane, tetrafluoroethane, chlorotrifluoroethane, dichlorodifluoroethane, pentafluoroethane, hexafluoroethane or a mixture thereof.

### Claim 2 (depends on 1)

The method according to claim 1, wherein the pulverization of graphite and the reaction with fluorine or a fluorocarbon compound are carried out in an atmosphere isolated from the external environment.

### Claim 3 (depends on 1)

The method according to claim 1, wherein step (iii) further comprises introducing an inert gas and the pulverized graphite is allowed to react with a mixture of the fluorine or fluorocarbon compound in the presence of the inert gas.

### Claim 4 (depends on 1)

The method according to claim 1, wherein the inert atmosphere is created by at least one inert gas selected from the group consisting of argon, helium, and neon.

### Claim 5 (depends on 1)

The method according to claim 1, wherein the graphite is pulverized at a rate of 100 to 10,000 rpm for 1 to 100 hours.

### Claim 6 (depends on 1)

The method according to claim 1, wherein the pulverized graphite is allowed to react with the fluorine or fluorocarbon compound for 1 to 100 hours.

### Claim 7 (depends on 1)

The method according to claim 1, wherein the pulverized graphite is 50 nm or more in average diameter.

### Claim 8 (depends on 1)

The method according to claim 1, wherein the fluoro groups are present in an amount of 0.01 to 50% by weight, based on the total weight of the edge-functionalized graphite.

### Claim 9 (depends on 1)

The method according to claim 1, wherein the edge-functionalized graphite or graphene with fluoro groups is a graphene nanoplate having a laminate structure of 1 to 20 graphene sheets.

### Claim 10 (depends on 1)

The method according to claim 1, comprising reacting the pulverized graphite with fluorine or a fluorocarbon compound at a pressure of 2 to 15 bar.