One-step synthesis of graphene quantum dots

Patent metadata

Field	Value
Publication number	US-9505623-B1
Application number	US-201514747332-A
Country	US
Kind code	B1
Filing date	Jun 23, 2015
Priority date	Jun 24, 2014
Publication date	Nov 29, 2016
Grant date	Nov 29, 2016

Abstract

Methods of making graphene quantums dots are provided. The methods can produce graphene quantum dots with a monodisperse size distribution. The graphene quantum dots are produced, via one-pot synthesis, from a graphene source and a strong oxidizing mixture at an elevated temperature. The strong oxidizing mixture can contain one or more permanganates and one or more oxidizing acids. Exemplary permanganates include sodium permanganate, potassium permanganate, and calcium permanganate. Exemplary oxidizing acids include nitric acid and sulfuric acid. The graphene quantum dots can have an average particle size of between about 1 nm and 20 nm and a monodisperse size distribution. For example, the size distribution can have a span about 1 or less and/or a coefficient of variance of about 0.5 or less. About 40% or more of the graphene quantum dots can have a diameter within ±5 nm of the average particle size of the graphene quantum dots.

First claim

We claim:

1. A method of making graphene quantum dots (GQDs) comprising:
combining a graphene source with a strong oxidizing mixture to form a combination; and
heating the combination to an elevated temperature with respect to room temperature to produce the GQDs,
wherein the strong oxidizing mixture comprises an oxidizing agent selected from the group consisting of a permanganate, a hexafluoromanganate, a persulfate, a chromate, Fenton's reagent, an oxidizing acid, and a combination thereof.

2. The method of claim 1 , wherein the graphene source is selected from the group consisting of graphite, carbon black, and combinations thereof.

3. The method of claim 1 , wherein the oxidizing mixture comprises a permanganate selected from the group consisting of potassium permanganate, ammonium permanganate, calcium permanganate, sodium permanganate, and silver permanganate.

4. The method of claim 1 , wherein the strong oxidizing mixture comprises a persulfate selected from the group consisting of sodium peroxomonosulfate, sodium persulfate, potassium peroxymonosulfate, and ammonium persulfate.

5. The method of claim 1 , wherein the strong oxidizing mixture comprises an oxidizing acid selected from the group consisting of nitric acid, perchloric acid, chloric acid, chromic acid, and sulfuric acid.

6. The method of claim 1 , wherein the oxidizing mixture comprises three or more oxidizing agents.

7. The method of claim 1 , wherein the oxidizing mixture comprises at least one permanganate and at least one oxidizing acid.

8. The method of claim 1 , wherein the oxidizing mixture comprises potassium permanganate, nitric acid, and sulfuric acid.

9. The method of claim 1 , wherein the elevated temperature is 100° C. to 200° C.

10. The method of claim 1 , wherein the GQDs have an average diameter of between 2.0 nm and 10.0 nm.

11. The method of claim 1 , wherein the GQDs have a monodisperse particle distribution.

12. The method of claim 1 , wherein the heating is for a period of time of 2 hours or less.

13. The method of claim 1 , wherein the strong oxidizing mixture comprises one or more oxidizing agents having a standard electrode potential between 1.0 V and 2.5 V.

14. A method of making graphene quantum dots (GQDs) comprising:
combining a graphene source with a strong oxidizing mixture to form a combination; and
heating the combination to an elevated temperature with respect to room temperature to produce the GQDs,
wherein the oxidizing mixture comprises three or more oxidizing agents.

15. The method of claim 14 , wherein the graphene source is selected from the group consisting of graphite, carbon black, and combinations thereof.

16. The method of claim 14 , wherein the oxidizing mixture comprises a permanganate selected from the group consisting of potassium permanganate, ammonium permanganate, calcium permanganate, sodium permanganate, and silver permanganate.

17. The method of claim 14 , wherein the strong oxidizing mixture comprises a persulfate selected from the group consisting of sodium peroxomonosulfate, sodium persulfate, potassium peroxymonosulfate, and ammonium persulfate.

18. The method of claim 14 , wherein the strong oxidizing mixture comprises an oxidizing acid selected from the group consisting of nitric acid, perchloric acid, chloric acid, chromic acid, and sulfuric acid.

19. The method of claim 14 , wherein the oxidizing mixture comprises at least one permanganate and at least one oxidizing acid.

20. The method of claim 14 , wherein the oxidizing mixture comprises potassium permanganate, nitric acid, and sulfuric acid.

21. The method of claim 14 , wherein the elevated temperature is 100° C. to 200° C.

22. The method of claim 14 , wherein the GQDs have an average diameter of between 2.0 nm and 10.0 nm.

23. The method of claim 14 , wherein the GQDs have a monodisperse particle distribution.

24. The method of claim 14 , wherein the heating is for a period of time of 2 hours or less.

25. The method of claim 14 , wherein the strong oxidizing mixture comprises one or more oxidizing agents having a standard electrode potential between 1.0 V and 2.5 V.

Assignees

• Qin Yiru
• Zhou shu-feng
• Univ South Florida

Inventors

• Qin Yiru
• Zhou shu-feng

Classifications

• C09K11/65 Primary

  containing carbon (in organic compounds C09K11/06) · CPC title

• B82Y40/00

  Manufacture or treatment of nanostructures · CPC title

• Y10S977/774

  Exhibiting three-dimensional carrier confinement, e.g. quantum dots · CPC title

• C01B31/0446 Primary

  Chemistry & Metallurgy · mapped topic

• B82Y5/00

  Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery · CPC title