Supercritical fluid process for producing nano graphene platelets
View Patent ↗The present invention provides a process for producing pristine or non-oxidized nano graphene platelets (NGPs) that are highly conductive. The process comprises: (i) subjecting a graphitic material to a supercritical fluid at a first temperature and a first pressure for a first period of time in a pressure vessel and then (ii) rapidly depressurizing the fluid at a fluid release rate sufficient for effecting exfoliation of the graphitic material to obtain the NGP material. Conductive NGPs can be used as a conductive additive in transparent electrodes for solar cells or flat panel displays (e.g., to replace expensive indium-tin oxide), battery and supercapacitor electrodes, and nanocomposite for electromagnetic wave interference (EMI) shielding and static charge dissipation, etc.
1. A process for producing a nano graphene platelet (NGP) material, said process comprising: (i) subjecting a graphitic material to a supercritical fluid at a first temperature and a first pressure for a first period of time in a pressure vessel, wherein said supercritical fluid contains no coating agent solubilized therein and no intercalating agent or oxidizing agent is used in the process, and said graphitic material comprises no previously intercalated graphite and said graphitic material is selected from the group consisting of natural graphite, artificial graphite, graphite oxide, graphite fluoride, graphite fiber, carbon fiber, carbon nano-fiber, carbon nano-tube, soft carbon, hard carbon, and combinations thereof; and then (ii) rapidly depressurizing said fluid at a fluid release rate sufficient for effecting exfoliation of said graphitic material to obtain said NGP material.
2. The process as set forth in claim 1 wherein said supercritical fluid comprises a fluid selected from carbon dioxide, water, water oxidation, hydrogen peroxide (H 2 O 2 ), methane, ethane, ethylene, ozone, sulfonic group (SO 3 ), or a combination thereof.
3. The process as set forth in claim 1 further comprising a procedure of repeating step (i) and step (ii) that includes (a) subjecting said NGP material to a supercritical fluid at a second temperature and a second pressure for a second period of time in a pressure vessel and then (b) rapidly depressurizing said fluid at a fluid release rate sufficient for effecting further exfoliation of said NGP material.
4. The process as set forth in claim 3 wherein said second temperature differs from said first temperature or said second pressure differs from said first pressure.
5. The process as set forth in claim 1 wherein said supercritical fluid contains a surfactant or dispersing agent dissolved therein.
6. The process as set forth in claim 5 further comprising a procedure of repeating step (i) and step (ii) that includes (a) subjecting said NGP material to a supercritical fluid at a second temperature and a second pressure for a second period of time in a pressure vessel and then (b) rapidly depressurizing said fluid at a fluid release rate sufficient for effecting further exfoliation of said NGP material.
7. The process as set forth in claim 6 wherein said second temperature differs from said first temperature or said second pressure differs from said first pressure.
8. The process as set forth in claim 1 wherein said supercritical fluid contains a curing agent dissolved therein and the process further comprises mixing said nano graphene material with a thermosetting resin.
9. The process as set forth in claim 1 wherein said supercritical fluid contains a curing agent dissolved therein and the process further comprises a procedure of repeating step (i) and step (ii) and a procedure of mixing said graphene material with a resin.
10. The process as set forth in claim 1 wherein said nano graphene platelet material, when formed into a thin film with a thickness no greater than 100 nm, exhibits an electrical conductivity of at least 100 S/cm.
11. The process as set forth in claim 1 wherein said nano graphene platelet material, when formed into a thin film with a thickness no greater than 100 nm, exhibits an electrical conductivity of at least 1,000 S/cm.
12. The process as set forth in claim 1 wherein said nano graphene material has a specific surface area of approximately from 300 m 2 /g to 2,600 m 2 /g.
13. The process as set forth in claim 1 wherein said nano graphene platelet material comprises single-layer graphene.
14. The process as set forth in claim 1 , further comprising imparting a chemical group to said nano graphene material in said pressure vessel.
15. The process as set forth in claim 1 , wherein said supercritical fluid comprises a reactive chemical group.
16. The process as set forth in claim 1 , wherein said supercritical fluid comprises a reactive chemical group and a surfactant.