Low-temperature method of producing nano-scaled graphene platelets and their nanocomposites
View Patent ↗A method of exfoliating a layered material to produce separated nano-scaled platelets having a thickness smaller than 100 nm. The method comprises: (a) providing a graphite intercalation compound comprising a layered graphite containing expandable species residing in an interlayer space of the layered graphite; (b) exposing the graphite intercalation compound to an exfoliation temperature lower than 650° C. for a duration of time sufficient to at least partially exfoliate the layered graphite without incurring a significant level of oxidation; and (c) subjecting the at least partially exfoliated graphite to a mechanical shearing treatment to produce separated platelets. The method can further include a step of dispersing the platelets in a polymer or monomer solution or suspension as a precursor step to nanocomposite fabrication.
1. A method of exfoliating a layered material to produce separated nano-scaled platelets having a thickness smaller than 100 nm, said method comprising:
a) providing an acid-intercalated graphite compound;
b) exposing said graphite intercalation compound to an exfoliation temperature lower than 600° C. for a duration of time sufficient to at least partially exfoliate said layered graphite; and
c) subjecting said at least partially exfoliated graphite to a mechanical shearing treatment to produce said separated nano-scaled platelets.
2. The method of claim 1 wherein said exfoliation temperature is lower than 350° C.
3. The method of claim 1 wherein said mechanical shearing treatment comprises air milling, ball milling, rotating blade shearing, ultrasonication, or a combination thereof.
4. The method of claim 1 wherein said mechanical shearing treatment comprises mixing said at least partially exfoliated graphite in a liquid medium which is subjected to ultrasonication or rotating blade shearing for further exfoliating and separating said graphite to produce the platelets and for dispersing said platelets in said liquid medium.
5. The method of claim 1 wherein said platelets have a thickness smaller than 10 nm.
6. The method of claim 1 wherein said step (b) comprises exfoliating said graphite in a protective gas atmosphere.
7. The method of claim 1 wherein said layered graphite comprises natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite oxide, graphite fluoride, graphite or carbon fiber, carbon nano-fiber, or a combination thereof.
8. The method of claim 1 wherein said step (b) comprises placing said graphite intercalation compound in a heated zone of a furnace or subjecting said intercalation compound to microwave or dielectric heating.
9. The method of claim 1 further including a step of dispersing said platelets in a liquid to form a suspension or in a monomer- or polymer-containing liquid medium to form a nanocomposite precursor suspension.
10. The method of claim 9 further including a step of converting said suspension to a mat or paper, or converting said nanocomposite precursor suspension to a nanocomposite solid.
11. The method of claim 1 further including steps of mixing said platelets with a monomer or polymer to form a mixture and converting said mixture to obtain a nanocomposite solid.
12. The method of claim 9 wherein said platelets comprise graphite oxide or graphite fluoride platelets and said method further includes a step of partially or totally reducing said graphite oxide or graphite fluoride after the formation of said suspension.
13. A method of exfoliating a layered material to produce separated nano-scaled platelets having a thickness smaller than 100 nm, said method comprising:
a) providing an acid-intercalated graphite compound;
b) exposing said intercalated compound to a first exfoliation temperature for a duration of time sufficient to partially exfoliate said layered material without inducing oxidation or a chemical reaction; and
c) subjecting said partially exfoliated material to a mechanical shearing treatment at a second temperature lower than the first temperature to produce said separated nano-scaled platelets.
14. The method of claim 13 wherein said mechanical shearing treatment comprises air milling, ball milling, rotating blade shearing, ultrasonication, or a combination thereof.
15. The method of claim 13 wherein said mechanical shearing treatment comprises mixing said partially exfoliated material in a liquid medium which is subjected to ultrasonication or rotating blade shearing for further exfoliating and separating said material to produce the platelets and for dispersing said platelets in said liquid medium.
16. The method of claim 13 further including a step of dispersing said platelets in a liquid to form a suspension or in a monomer- or polymer-containing liquid medium to form a nanocomposite precursor suspension.
17. The method of claim 16 further including a step of converting said suspension to a mat or paper, or converting said nanocomposite precursor suspension to a nanocomposite solid.
18. The method of claim 13 further including steps of mixing said platelets with a monomer or polymer to form a mixture and converting said mixture to obtain a nanocomposite solid.
19. A method of exfoliating a layered material to produce flexible graphite sheets, said method comprising:
a) providing an acid-intercalated graphite compound;
b) exposing said graphite intercalation compound to an exfoliation temperature lower than 600° C. for a duration of time sufficient to partially exfoliate said layered graphite;
c) subjecting said partially exfoliated graphite to a mechanical shearing treatment to further exfoliate said layered graphite; and
d) re-compressing said further exfoliated graphite to obtain flexible graphite sheets.
20. The method of claim 19 wherein said exfoliation temperature is lower than 350° C.
21. The method of claim 19 wherein said mechanical shearing treatment comprises air milling, ball milling, rotating blade shearing, ultrasonication, or a combination thereof.