IP Library Granted Patent US 9,309,124
Granted Patent B2
US 9,309,124 · App. 13/806,713 · Granted Apr 12, 2016

Methods of forming graphene by graphite exfoliation

Inventors: Kian Ping Loh (Singapore, SG); Junzhong Wang (Singaore, SG)
Assignee: National University of Singapore
C01B31/0469B01J21/185B82Y30/00B82Y40/00C01B31/0476H01L31/0324H01L31/035209H01L31/035218H01L31/072H01L51/0002H01L51/4213H01M4/5825H01M4/625H01M4/663H01M4/926Y02E10/50Y10S977/842Y10S977/892Y10T156/10Y10T436/143333
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Quick Facts
Patent No.
US 9,309,124
App. No.
13/806,713
Granted
Apr 12, 2016
Kind
B2
Abstract

Methods of forming graphene by graphite exfoliation, wherein the methods include: providing a graphite sample having atomic layers of carbon; introducing a salt and a solvent into the space between the atomic layers; expanding the space between the atomic layers using organic molecules and ions from the solvent and the salt; and separating the atomic layers using a driving force to form one or more sheets of graphene; the graphene produced by the methods can be used to form solar cells, to perform DNA analysis, and for other electrical, optical and biological applications.

Claims (42)

1. A method of forming graphene, comprising:

providing a graphite sample having atomic layers of carbon with spaces in between;

immersing the graphite sample in an electrolytic solution of propylene carbonate and lithium perchlorate;

performing electrolysis on the immersed graphite sample to introduce organic complexes of lithium ions and propylene carbonate into the spaces between the atomic layers to form intercalated graphite;

subjecting the intercalated graphite to a thermal treatment that expands the space between the atomic layers to form expanded graphite; and

separating the atomic layers using sonication to form one or more sheets of graphene.

2. The method of claim 1 , including forming the graphene as one or more flakes of graphene or one or more sheets of graphene derivatives.

3. The method of claim 1 , wherein the graphite sample is selected from the group of graphite samples comprising: natural graphite, graphite minerals, synthetic graphite, highly oriented pyrolytic graphite (HOPG), graphite fiber, graphite rods, and graphite powder.

4. The method of claim 1 , further comprising:

combining the graphene with quantum dots to form a heterojunction configured to function as an active component in a photovoltaic device.

5. The method of claim 4 , wherein said combining includes performing at least one of:

a sol-gel process, a hot-injection process, a chemical vapor deposition process, a nanocluster deposition process, and a sputtering process.

6. The method of claim 4 , wherein said combining includes asymmetric deposition of different nanocrystals on difference sides of the one or more graphene sheets.

7. The method of claim 6 , further comprising:

providing a hydrophobic/hydrophilic solution environment with the graphene as a surfactant interface;

providing hydrophobic and hydrophilic precursors so as to form at least one of nanocrystals, particles and polymer; and

depositing at least one of the nanocrystals, particles and polymer on the surfactant interface.

8. The method of claim 4 , including providing the quantum dots as chalcogenide semiconductor nanocrystals.

9. The method of claim 1 , further comprising dispersing the one or more graphene sheets in an organic solvent.

10. The method of claim 1 , further comprising forming providing on opposite sides of the one or more sheets of graphene different nano-metals or semiconductor nanocrystals to form a graphene-based asymmetric heterojunction.

11. The method of claim 10 , further comprising forming the graphene-based asymmetric heterojunction as CdTe/graphene/PbS-TiO 2 or CdSe/graphene/PbS-TiO 2 .

12. The method of claim 1 , further comprising:

applying the graphene to a flexible, non-conducting substrate to form a flexible, conducting substrate.

13. A method of forming graphene from a graphite sample comprising a lattice of carbon atoms that define atomic layers and a layer spacing, comprising:

intercalating propylene carbonate and lithium perchlorate into the carbon atom lattice via direct-current electrolysis of a 30 to 50 mg/ml solution of the lithium perchlorate in the propylene carbonate at a voltage of 15V+/−5V to form intercalated graphite;

expanding the layer spacing by subjecting the intercalated graphite to a thermal process to form expanded graphite; and

mechanically exfoliating one or more carbon atomic layers from the expanded graphite to form the graphene.

14. The method of claim 13 , including forming the graphene as one or more flakes of graphene or one or more sheets of graphene derivatives.

15. The method of claim 13 , further comprising:

employing the graphene in a bioanalytical technique involving biomolecules to selectively extract or pre-concentrate the biomolecules.

16. The method of claim 15 , further comprising:

using the selectively extracted or pre-concentrated biomolecules as a substrate for SELDI for directly analyzing the biomolecules without mixing with an organic matrix.

17. The method of claim 13 , where the biomolecules include at least one of: one or more proteins, DNA and RNA.

18. The method of claim 13 , further comprising combining the graphene with chalcogenide semiconductor nanocrystals to form a heterojunction.

19. The method of claim 13 , further comprising forming a photovoltaic device from the graphene by:

using the graphene, forming a solar cell active layer comprising a graphene/nanocrystal junction, the solar cell active layer having first and second sides;

forming an anode on the first side of the solar cell active layer; and

forming a cathode on the second side of the solar cell active layer.

20. The method of claim 1 , wherein performing the electrolysis includes employing two electrodes, wherein the graphite sample is employed as one of the electrodes and a graphite rod is used as the other electrode.

21. The method of claim 1 , wherein the thermal treatment includes heating the intercalated graphite using a flow of a heated inert gas.

22. The method of claim 1 , wherein the electrolytic solution contains 30-50 mg/ml of the lithium perchlorate.

23. The method of claim 13 , wherein the thermal process includes heating the intercalated graphite using a flow of a heated inert gas.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 21, 2012
From: LOH, KIAN PING; WANG, JUNZHONG
To: NATIONAL UNIVERSITY OF SINGAPORE
Reel/Frame 029522/0769 →
Continuity (2)
Provisional Application 61398468 · Jun 25, 2010
Related Publication 20130102084A1 · Apr 25, 2013