Process for producing dispersible nano graphene platelets from oxidized graphite
View Patent ↗The present invention provides a process for producing nano graphene platelets (NGPs) that are dispersible and conducting. The process comprises: (a) preparing a graphite intercalation compound (GIC) or graphite oxide (GO) from a laminar graphite material; (b) exposing the GIC or GO to a first temperature for a first period of time to obtain exfoliated graphite; and (c) exposing the exfoliated graphite to a second temperature in a protective atmosphere for a second period of time to obtain the desired dispersible nano graphene platelet with an oxygen content no greater than 25% by weight, preferably below 20% by weight, further preferably between 5% and 20% by weight. Conductive NGPs can find applications in transparent electrodes for solar cells or flat panel displays, additives for battery and supercapacitor electrodes, conductive nanocomposite for electromagnetic wave interference (EMI) shielding and static charge dissipation, etc.
1. A process for producing a dispersible nano graphene or graphene oxide platelet material, said process comprising:
(a) preparing a graphite intercalation compound (GIC) or graphite oxide (GO) from a laminar graphite material selected from the group consisting of artificial graphite, graphite fluoride, graphite fiber, carbon fiber, carbon nano-fiber, carbon nano-tube, mesophase carbon micro-bead (MCMB) or carbonaceous micro-sphere (CMS), soft carbon, hard carbon, and combinations thereof;
(b) exposing said GIC or GO to a first temperature for a first period of time to obtain exfoliated graphite; and
(c) exposing said exfoliated graphite to a second temperature in a protective atmosphere for a second period of time to obtain said dispersible nano graphene platelet material with an oxygen content no greater than 25% by weight.
2. The process as set forth in claim 1 wherein said protective atmosphere comprises an inert gas, nitrogen, hydrogen, a combination thereof, or vacuum.
3. The process as set forth in claim 1 wherein said second temperature is higher than said first temperature.
4. The process as set forth in claim 1 wherein said oxygen content is below 20% by weight.
5. The process as set forth in claim 1 wherein said oxygen content is below 15% by weight.
6. The process as set forth in claim 1 wherein said oxygen content is between 5% by weight and 20% by weight.
7. The process as set forth in claim 1 wherein said first temperature is between approximately 200° C. and 1,500° C.
8. The process as set forth in claim 1 wherein said first temperature is between approximately 800° C. and 1,300° C.
9. The process as set forth in claim 1 wherein said second temperature is between approximately 800° C. and 1,500° C.
10. The process as set forth in claim 1 wherein said second temperature is at least 1,000° C.
11. The process as set forth in claim 1 wherein said second temperature is at least 1,000° C. and the second period of time is at least 10 minutes.
12. The process as set forth in claim 1 wherein said second temperature is at least 1,100° C. and the second period of time is at least 5 minutes.
13. The process as set forth in claim 1 wherein said second temperature is at least 1,200° C. and the second period of time is at least 2 minutes.
14. The process as set forth in claim 1 wherein said dispersible 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 10 S/cm.
15. The process as set forth in claim 1 wherein said dispersible 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 50 S/cm.
16. The process as set forth in claim 1 wherein said dispersible 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.
17. The process as set forth in claim 1 wherein said dispersible 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 600 S/cm.
18. The process as set forth in claim 1 wherein said nano graphene material has a specific surface area of from approximately 300 m 2 /g to 2,600 m 2 /g.
19. The process as set forth in claim 1 wherein said nano graphene platelet material comprises single-layer graphene.
20. The process as set forth in claim 1 wherein said step of preparing a graphite intercalation compound (GIC) or graphite oxide (GO) comprises subjecting said laminar graphite material to an acid and/or an oxidizer.
21. The process as set forth in claim 1 wherein said step of preparing a graphite intercalation compound (GIC) or graphite oxide (GO) comprises subjecting said laminar graphite material to an acid and/or an oxidizer selected from sulfuric acid, nitric acid, carboxylic acid, sodium or potassium nitrate, potassium permanganate (KMnO 4 ), sodium or potassium chlorate, hydrogen peroxide (H 2 O 2 ), or a combination thereof.
22. The process as set forth in claim 1 , further comprising a step of contacting the nano graphene platelet material obtained in step (c) with a reactant such that a functional group is added to a surface or edge of the nano graphene platelet material.
23. The process as set forth in claim 22 , wherein said functional group is selected from alkyl or aryl silane, alkyl or aralkyl group, hydroxyl group, carboxyl group, amine group, sulfonate group (—SO 3 H), aldehydic group, quinoidal, fluorocarbon, or a combination thereof.