A kind of preparation method of graphene quantum dot

A graphene quantum dot and expanded graphite technology, which is applied in the field of preparation of high-quality graphene quantum dots, can solve the problems of harsh preparation conditions, difficult separation and purification, complicated operation, etc., and achieves clear process and principle, simple and controllable operation. , the effect of high specific surface area

Active Publication Date: 2020-01-10
SHANGHAI SPACE PRECISION MACHINERY RES INST
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  • Application Information

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Problems solved by technology

This type of method has good water solubility due to the easy introduction of various hydrophilic groups during the reaction process, and can achieve relatively precise control of the shape and size of GQDs, but the operation is cumbersome and time-consuming, and the separation and purification are difficult and the yield is low.
In addition, there are some more special methods, such as ruthenium-catalyzed fullerene cage opening method, laser cutting method, combustion method and diamond blade cutting graphite method, etc., which are limited due to harsh preparation conditions, complicated operation and low yield.

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  • A kind of preparation method of graphene quantum dot
  • A kind of preparation method of graphene quantum dot
  • A kind of preparation method of graphene quantum dot

Examples

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Embodiment 1

[0038] This embodiment relates to a preparation method of low-temperature expanded graphite, specifically:

[0039] One, prepare the mixed acid of sulfuric acid and nitric acid, control the massfraction of sulfuric acid wherein is 70%, the massfraction of nitric acid is 68%;

[0040] 2. Add natural flake graphite to the mixed acid of sulfuric acid and nitric acid, and drop in potassium permanganate to control the ratio of natural flake graphite, mixed acid of sulfuric acid and nitric acid, and potassium permanganate to be 1g: 3mL: 0.11g, at 80 ℃ for constant temperature water bath reaction;

[0041] 3. Deacidify the reaction solution, wash it with water until the pH value is 6-7, dry it to constant weight, and undergo high-temperature instantaneous expansion treatment at 300-600° C. to obtain low-temperature expanded graphite.

[0042] The TEM and Raman spectrograms of the transmission electron micrographs of the low-temperature expanded graphite prepared in this embodiment a...

Embodiment 2

[0044] The present embodiment relates to a kind of preparation method of graphene quantum dot, specifically:

[0045] One, utilizing the weakly oxidized low-temperature expanded graphite prepared in Example 1;

[0046] 2. Fully mix 40mL of SDS aqueous solution with a concentration of 1.5mg / mL and 20mg of expanded graphite powder, stir evenly, and use a pulsed ultrasonic wave with a power of 800W to conduct controllable ultrasonic treatment on the mixed solution for 4 hours to obtain a dark black solution.

[0047] 3. Separation and purification of the dark black solution after treatment, including high-speed centrifugation (8000rpm, 10min, keep the supernatant), vacuum filtration (Φ0.22μm PTFE filter membrane, keep the filtered solution), deionization Water dialysis treatment (MWCO=8000-14000Da, 24h), that is, a transparent light gray graphene quantum dot solution is prepared.

[0048] The graphene quantum dots prepared by the method have a concentrated size of about 35nm, a co...

Embodiment 3

[0050] The present embodiment relates to a kind of preparation method of graphene quantum dot, specifically:

[0051] One, utilizing the weakly oxidized low-temperature expanded graphite prepared in Example 1;

[0052] 2. Fully mix 40mL of SDS aqueous solution with a concentration of 1.5mg / mL and 20mg of expanded graphite powder, stir evenly, and use a pulsed ultrasonic wave with a power of 1000W to conduct controllable ultrasonic treatment on the mixed solution for 4 hours to obtain a deep black solution.

[0053] 3. Separation and purification of the dark black solution after treatment, including high-speed centrifugation (8000rpm, 10min, keep the supernatant), vacuum filtration (Φ0.22μm PTFE filter membrane, keep the filtered solution), deionization Water dialysis treatment (MWCO=8000-14000Da, 24h), that is, a transparent light gray graphene quantum dot solution is prepared.

[0054] The graphene quantum dots prepared by the method have a concentrated size of about 18 nm, ...

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Abstract

The invention provides a preparation method for a graphene quantum dot. The preparation method comprises the following steps: preparing low-temperature expanded graphite; dispersing the low-temperature expanded graphite in a sodium dodecyl sulfate aqueous solution, carrying out ultrasonic treatment and centrifuging treatment, and subjecting a supernatant to filtering so as to obtain a transparentlight-black solution; and subjecting the transparent light-black solution to dialysis in deionized water, and removing impurities which are soluble in sodium dodecyl sulfate so as to obtain a transparent light-gray graphene quantum dot solution. The preparation method for the graphene quantum dot provided by the invention has the advantages of clear process and principle, simple and controllable operation, economy, high efficiency, sustainability, high product yield and high product quality through intercalation-stripping-dispersion treatment to an expanded graphene raw material by combinationof high-power ultrasonic wave in an SDS solution.

Description

technical field [0001] The invention relates to a method for preparing high-quality graphene quantum dots, belonging to the technical field of nanomaterials and their preparation. Background technique [0002] As a new quasi-zero-dimensional carbon material quantum dot, graphene quantum dots (Graphene QuantumDots, GQDs) are essentially single-layer or few-layer nanographene with a two-dimensional size of several nanometers to tens of nanometers (strictly and diameter<10nm, number of layers<10 layers), has a very high specific surface area, and its unique properties are jointly determined by graphene and quantum dots: it not only has the excellent electrical and thermal conductivity of graphene materials, but also has quantum confinement effects and edge The unique properties brought about by the effect. On the one hand, the major difficulty in research lies in the fact that the large-scale, high-quality and controllable preparation of GQDs has not been effectively res...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/19B82Y40/00
CPCB82Y40/00C01B2204/04C01B2204/32C01P2002/82C01P2004/03C01P2004/04
Inventor 曾柏栋李邦盛张旭亮王宝兵张诗禹晋玺周扬
Owner SHANGHAI SPACE PRECISION MACHINERY RES INST
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