IP Library › Granted Patent US 11,299,671
Granted Patent B2
US 11,299,671 · App. 15/744,852 · Granted Apr 12, 2022

Preparation method for graphene quantum dots with different oxygen contents, graphene quantum dot, and fluorescent material

Inventors: Linde Zhang (Shenzhen, CN); Mingdong Zhang (Shenzhen, CN)
Assignee: Linde Zhang
C09K11/65C01B32/184B82Y20/00B82Y30/00B82Y40/00Y10S977/734Y10S977/774Y10S977/842Y10S977/95
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Quick Facts
Patent No.
US 11,299,671
App. No.
15/744,852
Granted
Apr 12, 2022
Kind
B2
Abstract

The present invention provides a preparation method for graphene quantum dots with different oxygen contents, including the following steps: Step 1: dispersing a graphene oxide in a peroxide solution to obtain a graphene oxide dispersion; Step 2: mixing the graphene oxide dispersion with an alkali liquor, purifying to obtain a graphene quantum dot dry powder; Step 3: loading the graphene quantum dots dry powder on a carrier, performing a gradient elution to obtain a plurality of graphene quantum dots with different oxygen contents. The preparation method for graphene quantum dots can realize the control of oxygen content of the graphene quantum dots. Therefore, the control of the emission wavelength of the product is achieved, which provides a reliable premise for applications of the graphene quantum dots in the fields of LED, cell labeling, etc. In addition, the method provided by the present invention is also simple and easy to operate.

Claims (20)

1. A preparation method for graphene quantum dots with different oxygen contents, comprising following steps:

step 1: dispersing a graphene oxide in a peroxide solution containing hydroxyl radicals to obtain a graphene oxide dispersion;

step 2: mixing the graphene oxide dispersion with an alkali liquor, purifying to obtain a graphenc quantum dot dry powder,

wherein a purifying step comprises reacting the purified product with a reducing agent in a solvent reduce an oxygen content of the graphene quantum dots, and purifying to obtain the graphene quantum dot dry powder, wherein the reducing agent is at least one of potassium borohydride, zinc-hydrochloric acid, iron-acetic acid, lithium aluminum hydride, sodium naphthalene, sodium amalgam, and Raney nickel, and

step 3: loading the graphene quantum dot dry powder on a carrier, performing a gradient elution to obtain a plurality of graphene quantum dots with different oxygen contents.

2. The preparation method for graphene quantum dots with different oxygen contents according to claim 1 , wherein a mass concentration of the graphene oxide in the graphene oxide dispersion is 0.1%-5%; and/or, a mass concentration of the peroxide solution is 3%-30%.

3. The preparation method for graphene quantum dots with different oxygen contents according to claim 1 , wherein the peroxide is at least one selected from the group consisting of hydrogen peroxide, ammonium persulfate, sodium persulfate, potassium hydrogen persulfate, sodium perborate, dibenzoyl peroxide and dilauroyl peroxide.

4. The preparation method for graphene quantum dots with different oxygen contents according to claim 1 , wherein the gradient elution in step 3 includes performing the gradient elution using a vacuum liquid chromatography or a column chromatography.

5. The preparation method for graphene quantum dots with different oxygen contents according to claim 4 , wherein an eluent used for the gradient elution includes a first polar solvent and a second polar solvent, wherein a polarity of the first polar solvent is greater than that of the second polar solvent, wherein the first polar solvent is one or more selected from the group consisting of water, methanol, ethanol, ethylene glycol, hydrochloric acid-methanol solution, tetrahydrofuran, formic acid, acetic acid, acetonitrile, N, N-dimethylformamide, diethyl. ether, acetone and nitromethane, wherein the second polar solvent is one or more selected from the group consisting of cyclohexane, n-hexane, petroleum ether, ethyl acetate, dimethyl carbonate, dichloromethane, trichloromethane and carbon tetrachloride.

6. The preparation method for graphene quantum dots with different oxvaen contents according to claim 1 , wherein the dots produced have an emission wavelength is 550 nm-750 nm.

7. The preparation method for graphene quantum dots with different oxygen contents according to claim 2 , wherein the gradient elution in step 3 includes performing the gradient elution using a vacuum liquid chromatography or a column chromatography.

8. The preparation method for graphene quantum dots with different oxygen contents according to claim 3 , wherein the gradient elution in step 3 includes performing the gradient elution using a vacuum liquid chromatography or a column chromatography.

9. A preparation method for graphene quantum dots with different oxygen contents, comprising:

a step of converting a graphene oxide to a graphene quantum dot powder and a step of purifying the graphene quantum dot powder,

wherein the step for converting a graphene oxide to a graphene quantum dot consists of:

step 1: dispersing a graphene oxide in a peroxide solution containing hydroxyl radicals to obtain a graphene oxide dispersion;

step 2: mixing the graphene oxide dispersion with an alkali liquor, purifying to obtain a graphene quantum dot dry powder,

wherein the step of purifying the graphene quantum dot powder comprises:

step 3: reacting the purified product with a reducing agent in a solvent reduce an oxygen content of the graphene quantum dots, and purifying to obtain the graphene quantum dot dry powder, wherein the reducing agent is at least one of: potassium borohydride, zinc-hydrochloric acid, iron-acetic acid, lithium aluminum hydride, sodium naphthalene, sodium amalgam, and Raney nickel, and

step 4: loading the graphene quantum dot dry powder on a carrier, performing a gradient elution to obtain a plurality of graphene quantum dots with different oxygen contents.

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 20, 2026
From: CARBON NANO ENGINEERING SYSTEMS CO., LTD.
To: HUNAN YUANCHANG NEW MATERIAL TECHNOLOGY CO., LTD.
Reel/Frame 075415/0829 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 1, 2025
From: HUBEI HIGHLAND GRAPHENE TECHNOLOGY CO., LTD.
To: CARBON NANO ENGINEERING SYSTEMS CO., LTD.
Reel/Frame 071904/0322 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 14, 2022
From: ZHANG, LINDE
To: HUBEI HIGHLAND GRAPHENE TECHNOLOGY CO., LTD.
Reel/Frame 059605/0354 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 15, 2018
From: ZHANG, LINDE; ZHANG, MINGDONG
To: ZHANG, LINDE
Reel/Frame 045073/0420 →
Priority Claims (1)
CN 201510528994.9 · Aug 25, 2015 · national
Continuity (1)
Related Publication 20180230379A1 · Aug 16, 2018