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Method for preparing fluorescent graphene quantum dots by solvothermal method

A graphene quantum dot, solvothermal technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of low yield, high cost, and complicated preparation

Inactive Publication Date: 2012-09-12
JILIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to prepare loaded down with trivial details for existing method, the shortcoming that cost is high, and yield is low, provides a kind of graphene quantum dot that uses graphene oxide as raw material, one-step solvothermal method prepares the graphene quantum dot of strong green fluorescence, further through effective Separation by column chromatography to prepare fluorescent graphene quantum dots with controllable oxidation degree, so that the surface oxidation degree and fluorescence emission peak position of graphene quantum dots can be adjusted

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  • Method for preparing fluorescent graphene quantum dots by solvothermal method
  • Method for preparing fluorescent graphene quantum dots by solvothermal method
  • Method for preparing fluorescent graphene quantum dots by solvothermal method

Examples

Experimental program
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Effect test

Embodiment 1

[0033] 1: Preparation of graphene oxide

[0034] 8 grams of graphite powder (Aldrich, figure 1a) join in the concentrated sulfuric acid of 30 milliliters mass fractions 98% (500 milliliters there-necked bottles) that dissolves 10 gram potassium persulfate, 10 gram phosphorus pentoxides of 80 ℃ (500 milliliters there-necked bottles); Place cooling after mechanical stirring 6 hours, use a large amount of Dilute (slowly) with deionized water, filter, and wash until neutral; then the product is dried at room temperature to obtain pre-oxidized graphite powder. The pre-oxidized graphite powder is added to 184 milliliters of mass fraction 98% concentrated sulfuric acid (500 milliliters there-necked bottle) of 0 ℃, carry out mechanical stirring (350 revolutions per minute); Add 4 grams of sodium nitrate again, then slowly add 24 grams Potassium permanganate in fine powder form, the speed is slow to ensure that the temperature of the system does not exceed 5°C; after stirring at low t...

Embodiment 2

[0040] 1: The preparation of graphene oxide is as described in Example 1.

[0041] 2: Preparation of green fluorescent graphene quantum dots

[0042] 100 milligrams of graphene oxide powders were dispersed into 10 milliliters of N,N-dimethylformamide (DMF), then the dispersion was ultrasonically (120W, 100kHz) after 30 minutes, transferred to a polytetrafluoroethylene reactor, The reaction was carried out at 200 degrees Celsius for 10 hours; after the reaction, the supernatant was taken, dried by rotary evaporation, and graphene quantum dots with strong green fluorescence properties were obtained, with a mass of 1.6 grams.

[0043] 3: Preparation of fluorescent graphene quantum dots with controllable oxidation degree

[0044] The dried graphene quantum dots were subjected to two-step gradient column chromatography (the stationary phase was silica gel). The first phase developer is a 2:1 mixture of dichloromethane and methanol, and the second phase developer is deionized wate...

Embodiment 3

[0046] 1: The preparation of graphene oxide is as described in Example 1.

[0047] 2: Preparation of green fluorescent graphene quantum dots

[0048] 270 milligrams of graphene oxide powders were dispersed into 10 milliliters of N,N-dimethylformamide (DMF), and then the dispersion was ultrasonically (120W, 100kHz) after 30 minutes, transferred to a polytetrafluoroethylene reactor, The reaction was carried out at 200 degrees Celsius for 10 hours; after the reaction, the supernatant was taken, dried by rotary evaporation, and graphene quantum dots with strong green fluorescence properties were obtained, with a mass of 7.32 grams.

[0049] 3: Preparation of fluorescent graphene quantum dots with controllable oxidation degree

[0050] The dried graphene quantum dots were subjected to two-step gradient column chromatography (the stationary phase was silica gel). The first phase developer is a 2:1 mixture of dichloromethane and methanol, and the second phase developer is deionized...

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Abstract

The invention belongs to the technical field of the preparation of graphene quantum dots (GQDs), and particularly relates to a method for preparing fluorescent graphene quantum dots with controllable oxidation degree and fluorescence by a solvothermal method. According to the technical scheme, the method comprises the following steps of: 1, preparing graphene oxide; 2, preparing green fluorescent graphene quantum dots by a single-step method starting from the graphene oxide; and 3, preparing the fluorescent graphene quantum dots with the controllable oxidation degree by a column chromatographic separation method. According to the method, the sizes and surface oxidation degree of the graphene quantum dots can be controlled under the synthetic condition, so that the fluorescent properties and surface chemical characteristics of the graphene quantum dots are controlled. The prepared graphene quantum dots are high in chemical stability and biocompatibility, low in biotoxicity, and high in property of applicable upconversion fluorescence, matt and the like and bleaching performance. By the excellent properties, the graphene quantum dots have a wide application range in aspects of biological imaging, photovoltaic devices and sensors, and are novel promising fluorescent nano materials.

Description

technical field [0001] The invention belongs to the technical field of preparation of graphene quantum dots (graphene quantum dots, GQDs), and specifically relates to a method of firstly preparing graphene quantum dots with strong green fluorescence, and then separating them by column chromatography to prepare a controllable oxidation degree and controllable fluorescence. A method for fluorescent graphene quantum dots. Background technique [0002] Graphene has very outstanding properties in thermal conductivity, mechanics, electricity, etc., and has received widespread attention and preliminary applications. However, relatively little attention has been paid to quantum-sized graphene (or graphene quantum dots). Graphene quantum dots have good fluorescence properties, and its fluorescence properties are determined by both quantum size and surface defects. Graphene quantum dots are part of the fluorescent carbon nanomaterials. Such materials include fullerenes, carbon nano...

Claims

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Application Information

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IPC IPC(8): C09K11/65
Inventor 杨柏朱守俊张俊虎李波刘学张国彦李云峰
Owner JILIN UNIV
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