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Graphene quantum dot and preparation method thereof

A technology of graphene quantum dots and graphene, applied in chemical instruments and methods, nanotechnology, nano-optics, etc., to achieve the effect of enriching oxygen-containing functional groups and good water solubility

Inactive Publication Date: 2018-08-03
HUBEI UNIV FOR NATITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no report on how to obtain GQDs with a uniform oxygen-to-carbon ratio

Method used

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  • Graphene quantum dot and preparation method thereof
  • Graphene quantum dot and preparation method thereof
  • Graphene quantum dot and preparation method thereof

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preparation example Construction

[0019] According to the preparation method of graphene quantum dots in the present invention, the method comprises that under oxidation reaction conditions, graphene is oxidized in an oxidation solution to obtain graphene quantum dots, wherein the oxidation solution contains H 2 SO 4 and HNO 3 , the H in the oxidation solution 2 SO 4 The concentration is 10-14mol / L, and H 2 SO 4 with HNO 3 The molar ratio is 1:0.20-0.45.

[0020] Preferably, the H 2 SO 4 with HNO 3 The molar ratio is 0.25-0.45; more preferably, the H 2 SO 4 with HNO 3 The molar ratio is 1:0.31-0.44.

[0021] Preferably, the H in the oxidation solution 2 SO 4 The concentration is 12-14mol / L, and H 2 SO 4 with HNO 3 The molar ratio is 1:0.30-0.35.

[0022] According to the present invention, in order to better control the oxidation degree of the obtained graphene quantum dots, the HNO in the oxidation solution 3 The concentration is 2.0-6.0mol / L, preferably 3.0-4.5mol / L, more preferably 4.0-4....

Embodiment 1

[0034] containing H 2 SO 4 and HNO 3 10mL of oxidation solution (where H 2 SO 4 The concentration is 13.25mol / L, HNO 3 10 mg of graphene was added into a three-necked flask with a concentration of 4.03 mol / L, and the reaction was carried out under uniform stirring for 120 min, and the temperature was controlled at 80°C. The system eventually turned dark brown. Then, 250 mL of deionized water was added to the reaction system to terminate the reaction, and NaOH was added in an ice bath to neutralize the pH value to 7.0. Salts in solution were removed by dialysis using a dialysis bag with a molecular weight cut-off of 1 kDa. After the dialysate is concentrated by a rotary evaporator, it is separated by ultrafiltration tubes with a molecular weight cut-off of 100, 50, 30, 10, and 3KDa to obtain molecular weights of (50-100kDa), (30-50kDa), (10- 30kDa), (3-10kDa) and <3kDa GQDs, respectively marked as 1-GQDs@(50-100k), 1-GQDs@(30-50k), 1-GQDs@(10-30k), 1-GQDs @(3-10k) and 1...

Embodiment 2

[0036] Graphene quantum dots are prepared according to the method of Example 1, the difference is that H 2 SO 4 The concentration is 12.88mol / L, HNO 3 The concentration is 4.32mol / L.

[0037] Prepared graphene quantum dots 2-GQDs@(50-100k), 2-GQDs@(30-50k), 2-GQDs@(10-30k), 2-GQDs@(3-10k) and 2-GQDs@ (<3k).

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Abstract

The invention relates to the field of quantum dot preparation, and discloses a preparation method of a graphene quantum dot. The method is characterized in that graphene undergoes an oxidation reaction in an oxidizing solution under an oxidation reaction condition to obtain the graphene quantum dot, wherein the oxidizing solution contains H2SO4 and HNO3, the concentration of H2SO4 in the oxidizingsolution is 10-14 mol / L, and a molar ratio of H2SO4 to HNO3 is 1:(0.20-0.45). The graphene quantum dot obtained by the preparation method has a uniform oxygen-to-carbon ratio and spectrally controllable properties, and is suitable for bioimaging, multicolor labeling and construction of fluorescent and electrochemiluminescent biosensors.

Description

technical field [0001] The invention relates to the field of quantum dot preparation, in particular to a graphene quantum dot and a preparation method thereof. Background technique [0002] Graphene is a zero-bandgap two-dimensional nanomaterial composed of graphite with a single-layer flake structure. Opening the energy band of graphene will facilitate its application in optical and electronic devices. Graphene quantum dots (GQDs) are homologous materials of graphene. By controlling the particle size and shape, the energy band energy of GQDs can be adjusted from 0eV to ~6eV (benzene ring). Therefore, GQDs, a zero-site carbon nanomaterial, has received extensive attention. The preparation methods of GQDs mainly include chemical oxidation, electrochemical etching, microwave radiation, free radical oxidation and so on. The preparation methods of GQDs are increasing, however, the methods that can control the surface state of GQDs still need to be developed. Among them, the c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/65B82Y20/00B82Y40/00
CPCB82Y20/00B82Y40/00C09K11/65
Inventor 齐宝平尚冰冰张升晖
Owner HUBEI UNIV FOR NATITIES
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