Microwave system and method for graphene production

Patent metadata

Field	Value
Publication number	US-10822239-B2
Application number	US-201715491714-A
Country	US
Kind code	B2
Filing date	Apr 19, 2017
Priority date	Apr 19, 2017
Publication date	Nov 3, 2020
Grant date	Nov 3, 2020

Abstract

Provided is a method of producing graphene from a microwave-expandable un-exfoliated graphite or graphitic carbon, comprising: (a) feeding a powder of the microwave-expandable material onto a non-metallic solid substrate, wherein the powder is in a ribbon shape having a first ribbon width and a first ribbon thickness; (b) moving the ribbon-shape powder into a microwave applicator chamber containing a microwave power zone having a microwave application width (no less than the first ribbon width) and a microwave penetration depth (no less than the first ribbon thickness) so that the entire ribbon-shape powder receives and absorbs microwave power with a sufficient power level for a sufficient length of time to exfoliate and separate the powder for producing graphene sheets; and (c) moving the graphene sheets out of the microwave chamber, cooling the graphene sheets, and collecting the graphene sheets in a collector container or for a subsequent use.

First claim

The invention claimed is:

1. A method of producing graphene from a microwave-expandable un-exfoliated graphite or graphitic carbon, said method comprising:
(a) supplying and feeding a powder of said microwave-expandable un-exfoliated graphite or graphitic carbon onto a non-metallic solid substrate surface, wherein said powder is in a substantially ribbon shape having a first ribbon width and a first ribbon thickness, wherein said powder of microwave-expandable un-exfoliated graphite or graphitic carbon further contains 0.1% to 20% by weight of a dielectric heating promoter selected from water, polar organic molecule, or a combination thereof;
(b) moving said ribbon-shape powder into a microwave applicator chamber containing a microwave power zone having a microwave application width and a microwave penetration depth, wherein said microwave application width is no less than said first ribbon width and said microwave penetration depth is no less than said first ribbon thickness so that the entire ribbon-shape powder receives and absorbs microwave power with a sufficient power level for a sufficient length of time to exfoliate and separate said microwave-expandable un-exfoliated graphite or graphitic carbon for producing graphene sheets that occupy an expanded volume having a second width, greater than said first ribbon width, and a second thickness, greater than said first ribbon thickness; and
(c) moving said graphene sheets out of said microwave chamber, cooling said graphene sheets, and collecting said graphene sheets.

2. The method of claim 1 wherein said microwave-expandable un-exfoliated graphite or graphitic carbon is selected from intercalated natural graphite, oxidized natural graphite, fluorinated natural graphite, intercalated synthetic graphite, oxidized synthetic graphite, fluorinated synthetic graphite, intercalated amorphous graphite, oxidized amorphous graphite, fluorinated amorphous graphite, intercalated highly oriented pyrolytic graphite (HOPG), oxidized HOPG, fluorinated HOPG, intercalated meso-carbon micro-bead, oxidized meso-carbon micro-bead, fluorinated meso-phase carbon, intercalated needle coke, oxidized needle coke, fluorinated needle coke, intercalated carbon or graphite fiber, oxidized carbon or graphite fiber, fluorinated carbon or graphite fiber, intercalated carbon nano-fiber, oxidized carbon nano-fiber, fluorinated carbon nano-fiber, nitrogenated graphite, chlorinated graphite, brominated graphite, iodized graphite, or a combination thereof.

3. The method of claim 1 wherein a residence time for said microwave-expandable un-exfoliated graphite or graphitic carbon in said microwave power zone is from 10 seconds to 5 minutes.

4. The method of claim 1 wherein said residence time is from 30 seconds to 3 minutes.

5. The method of claim 1 wherein said first ribbon width is selected from the range of 1 mm to 10 cm and said first ribbon thickness is from 10 nm to 3.8 cm.

6. The method of claim 1 wherein said first ribbon width is selected from the range of 5 mm to 5 cm and said first ribbon thickness is from 1 μm to 2.5 cm.

7. The method of claim 1 wherein said first ribbon width is selected from the range of 1 cm to 3 cm and said first ribbon thickness is from 0.1 mm to 1.0 cm.

8. The method of claim 1 wherein said powder of microwave-expandable un-exfoliated graphite or graphitic carbon is fed and moved into microwave application chamber in a continuous or intermittent manner.

9. The method of claim 1 , wherein said graphene sheets are subjected to a mechanical shearing treatment to produce smaller graphene sheets.

10. The method of claim 9 , wherein said mechanical shearing treatment comprises using air milling, air jet milling, ball milling, rotating-blade mechanical shearing, ultrasonication, cavitation, or a combination thereof.

11. The method of claim 1 wherein said graphene contains single-layer graphene sheets.

12. The method of claim 1 wherein said graphene contains at least 80% single-layer graphene sheets.

13. The method of claim 1 wherein said graphene contains pristine graphene, oxidized graphene with less than 5% oxygen content by weight, graphene fluoride, graphene fluoride with less than 5% fluorine by weight, graphene with a carbon content no less than 95% by weight, or functionalized graphene.

14. A method of producing graphene from a microwave-expandable un-exfoliated graphite or graphitic carbon, said method comprising:
(a) supplying and feeding a powder of said microwave-expandable un-exfoliated graphite or graphitic carbon onto a non-metallic solid substrate surface, wherein said powder is in a substantially ribbon shape having a first ribbon width and a first ribbon thickness;
(b) moving said ribbon-shape powder into a microwave applicator chamber containing a microwave power zone having a microwave application width and a microwave penetration depth, wherein said microwave application width is no less than said first ribbon width and said microwave penetration depth is no less than said first ribbon thickness so that the entire ribbon-shape powder receives and absorbs microwave power with a sufficient power level for a sufficient length of time to exfoliate and separate said microwave-expandable un-exfoliated graphite or graphitic carbon for producing graphene sheets that occupy an expanded volume having a second width, greater than said first ribbon width, and a second thickness, greater than said first ribbon thickness, wherein a ratio of said second width to said first ribbon width is from 3 to 300; and
(c) moving said graphene sheets out of said microwave chamber, cooling said graphene sheets, and collecting said graphene sheets.

15. A method of producing graphene from a microwave-expandable un-exfoliated graphite or graphitic carbon, said method comprising: (a) supplying and feeding a volume of the microwave-expandable un-exfoliated graphite or graphitic carbon powder onto a solid substrate surface, wherein the powder volume has a maximum width and a maximum thickness, wherein the microwave-expandable un-exfoliated graphite or graphitic carbon powder further contains a dielectric heating promoter selected from water, polar organic molecule, or a combination thereof; (b) moving the powder into a microwave applicator chamber containing a microwave power zone having a microwave application width and a microwave penetration depth, wherein the microwave application width is no less than the maximum width of the powder volume and the microwave penetration depth is no less than the maximum thickness of the powder volume so that the entire powder volume receives and absorbs microwave power with a sufficient power level for a sufficient length of time to exfoliate and separate the microwave-expandable un-exfoliated graphite or graphitic carbon into graphene sheets that occupy an expanded volume having a second width, greater than the maximum width, and a second thickness, greater than the maximum thickness; and (c) moving the graphene sheets out of the microwave chamber, cooling the graphene sheets, and collecting the graphene sheets.

Assignees

• Nanotek Instruments Inc
• Global Graphene Group Inc

Inventors

• Lin Yi-Jun
• Zhamu Aruna
• Jang Bor Z

Classifications

• C01B32/225

  Expansion; Exfoliation · CPC title

• C01B32/184 Primary

  Preparation · CPC title

• B01J2219/1239

  Means for feeding and evacuation · CPC title

• B01J2219/1218

  Multiple reactors · CPC title

• B01J2219/0879

  Solid · CPC title