Method for Manufacturing Nano-Graphene Sheets

• US 20150158729A1
• Filed: 06/12/2014
• Published: 06/11/2015
• Est. Priority Date: 12/11/2013
• Status: Abandoned Application

• Current Assignee: Enerage Inc.
• Original Assignee: Enerage Inc.
• Inventors: HSIEH, Cheng-Yu, WU, Mark Y, LIN, Geng-Wei, YEH, Ping-Yun, CHEN, Tsung-Han
• Application Number:
  US14/303,409
• Publication Number:
  US 20150158729A1
• Time in Patent Office: Days
• US Class Current: 1/1
• CPC Class Codes: C01B 2204/32 Size or surface area
• CPC Class Codes: C01B 32/192 starting from graphitic oxides

Abstract

A method for manufacturing nano-graphene sheets, includes: intercalating and oxidizing a graphite material to form a graphite oxide by mixing the graphite material with an intercalation agent and oxidant; contacting the graphite oxide with a heat source to thermally flake the graphite oxide to nano-graphite sheets; suspending the nano-graphite sheets in a liquid medium and applying a mechanical shear force larger than 5,000 psi to mechanically flake the nano-graphite sheets for reducing the lateral size and thickness to form a nano-graphene suspension solution; separating the nano-graphene sheets from the nano-graphene suspension solution and drying the nano-graphene sheets; and finally reducing and heat treating the nano-graphene sheets to lower the oxygen content to less than 3 wt % and decrease the crystal defects.

Claims

1. A method for manufacturing nano-graphene sheets, comprising steps of:

intercalating and oxidizing a graphite material to form a graphite oxide by mixing the graphite material with at least one intercalation agent and at least one oxidant;

contacting the graphite oxide with a heat source to thermally flake the graphite oxide to a plurality of nano-graphite sheets;

suspending the nano-graphite sheets in a liquid medium and applying a mechanical shear force to mechanically flake the nano-graphite sheets such that a lateral size and a thickness of the nano-graphite sheets are reduced to form a nano-graphene suspension solution;

separating the nano-graphene sheets from the nano-graphene suspension solution and drying the nano-graphene sheets;

placing the nano-graphene sheets into a reductant atmosphere and heating up to a heat treatment temperature to reduce an oxygen content of the nano-graphene sheets so as to decrease crystal defects.

2. The method as claimed in claim 1, wherein the graphite material is selected from a group consisting of at least one of natural graphite, expanded graphite, artificial graphite, graphite fiber, carbon nano-tube and mesophase carbon micro-bead.

3. The method as claimed in claim 1, wherein the intercalation agent is selected from a group consisting of at least one of sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, phosphoric anhydride and carboxylic acid.

4. The method as claimed in claim 1, wherein the oxidant consists of at least one of potassium permanganate and perchloric acid.

5. The method as claimed in claim 1, wherein the intercalation agent is in a range of 500 to 3000 wt % of the graphite material, the oxidant is in a range of 100 to 1000 wt % of the graphite material, and the graphite oxide has a density less than a density of the graphite material.

6. The method as claimed in claim 1, wherein the heat source is provided with temperature within a range of 500 to 1300°

C., and a period of time of contacting with the heat source is less than 3 minutes.

7. The method as claimed in claim 1, wherein the liquid medium consists of at least one of water and organic solvent.

8. The method as claimed in claim 7, wherein the liquid medium further consists of a dispersant.

9. The method as claimed in claim 1, wherein the reductant atmosphere consists of at least one of hydrogen (H₂), ammonia (NH₃) and carbon monoxide (CO), a temperature of the heat treatment is 500-1200°

C., and the heat treatment takes 30-120 minutes.

10. The method as claimed in claim 1, wherein the liquid medium is deionized water and/or an organic solvent, the shear force is generated by at least one of ultrasonication, high speed mixing, normal pressure homogenizer, planet bead milling, and high pressure homogenizer, and the mechanical shear force is larger than 5,000 psi.

11. The method as claimed in claim 1, wherein the nano-graphene sheet has an oxygen content less than 3 wt %, a carbon content larger than 95 wt %, an average particle size less than 30 gm, and a specific surface area larger than 15 m²/g.