Preparation method of graphene

Patent metadata

Field	Value
Publication number	US-9950930-B2
Application number	US-201415039655-A
Country	US
Kind code	B2
Filing date	Dec 24, 2014
Priority date	Dec 26, 2013
Publication date	Apr 24, 2018
Grant date	Apr 24, 2018

Abstract

Disclosed herein is a preparation method of graphene, capable of preparing graphene having a smaller thickness and a large area, and with reduced defect generation, by a simplified process. The preparation method of graphene includes forming dispersion including a carbon-based material including unoxidized graphite, and a dispersant; and continuously passing the dispersion through a high pressure homogenizer including an inlet, an outlet, and a micro-channel for connection between the inlet and the outlet, having a diameter in a micrometer scale, wherein the carbon-based material is exfoliated, as the material is passed through the micro-channel under application of a shear force, thereby forming graphene having a thickness in nanoscale.

First claim

The invention claimed is:

1. A preparation method of graphene, the preparation method comprising:
forming a dispersion including a carbon-based material including unoxidized graphite, and a dispersant; and
continuously passing the dispersion through a high pressure homogenizer including an inlet, an outlet, and a micro-channel for connection between the inlet and the outlet, having a diameter in a micrometer scale,
wherein the carbon-based material is exfoliated, as the material is passed through the micro-channel under application of a shear force, thereby forming graphene having a thickness in nanoscale, and
wherein the dispersant includes a mixture of a plurality of polyaromatic hydrocarbon oxides, including polyaromatic hydrocarbon oxides having a molecular weight of 300 to 1000, said dispersant being present in an amount of at least 60% by weight.

2. The preparation method of claim 1 , wherein the unoxidized graphite has an element ratio of oxygen to carbon (O/C atomic ratio) of 5% or less, as measured by elemental analysis measurement by combustion or XPS analysis (X-ray photoelectron spectrometry analysis).

3. The preparation method of claim 1 , wherein the unoxidized graphite includes planar graphite.

4. The method of claim 1 , wherein the dispersion is dispersion in which the carbon-based material and the dispersant are dissolved or dispersed in an aqueous solvent or a polar organic solvent.

5. The preparation method of claim 1 , wherein the dispersant has an oxygen content of 12 to 50% by weight, based on a total element content, when the plural kinds of polyaromatic hydrocarbon oxides contained in the dispersant are subjected to elemental analysis.

6. The preparation method of claim 1 , wherein the polyaromatic hydrocarbon oxides contained in the dispersant has a structure where one or more oxygen-containing functional groups are bonded to an aromatic hydrocarbon containing 5 to 30 benzene rings.

7. The preparation method of claim 6 , wherein the aromatic hydrocarbon has 7 to 20 benzene rings in the structure.

8. The preparation method of claim 1 , wherein the micro-channel has a diameter of 10 to 800 μm.

9. The preparation method of claim 1 , wherein the dispersion is introduced to the inlet of the high pressure homogenizer under application of pressure of 100 to 3000 bar to be passed through the micro-channel.

10. The preparation method of claim 1 , wherein the graphene includes a graphene flake having a thickness of 0.3 to 50 nm.

11. The preparation method of claim 9 , wherein the graphene flake has a diameter of 0.1 to 10 μm, and a diameter/thickness ratio of 50 to 6000.

12. The preparation method of claim 1 , further comprising recovering graphene flakes from dispersion of the graphene flakes, and drying the graphene flakes.

13. The preparation method of claim 12 , wherein the recovering proceeds by centrifugation, vacuum filtration or pressure filtration.

14. The preparation method of claim 12 , wherein the drying proceeds by vacuum drying at a temperature of 30 to 200° C.

Assignees

• Lg Chemical Ltd

Inventors

• Yoo Kwang Hyun
• Sohn Kwon Nam
• Kwon Won Jong
• Lee Kil Sun

Classifications

• C01P2002/82

  by IR- or Raman-data · CPC title

• C01P2004/24

  Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer · CPC title

• C01B32/184 Primary

  Preparation · CPC title

• C01B32/19 Primary

  by exfoliation · CPC title

• C01P2002/85

  by XPS, EDX or EDAX data · CPC title