A kind of preparation method of ultra-thin graphene powder and its prepared product

A graphene powder and graphene technology, applied in the field of preparation of ultra-thin graphene powder, can solve the problems of complex process, incomplete peeling, low graphene yield, etc., and achieve a green and simple preparation method and simple and easy equipment and process. The effect of easy industrial production

Active Publication Date: 2021-05-21
武汉低维材料研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the graphene prepared by these traditional methods generally has thick sheets, incomplete exfoliation, damaged internal structure, many defects, and low electrical conductivity.
Moreover, the graphene prepared by the above existing technologies has a low yield, requires the use of toxic and harmful reagents, requires high equipment, and complicated processes, and is not suitable for mass production, which greatly limits its application.

Method used

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  • A kind of preparation method of ultra-thin graphene powder and its prepared product
  • A kind of preparation method of ultra-thin graphene powder and its prepared product
  • A kind of preparation method of ultra-thin graphene powder and its prepared product

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Embodiment 1

[0033] A kind of preparation method of ultra-thin graphene powder of the present embodiment, described method specifically comprises the following steps:

[0034] (1) Using a graphite rod as a working electrode, add a 5V DC voltage to the sodium sulfate electrolyte, electrolyze for 6 hours, then undergo solid-liquid separation, ultrasonic dispersion, washing, and drying to obtain a graphene precursor;

[0035] (2) Dissolving the above-mentioned graphene precursor in N-methylformamide, the proportioning of the graphene precursor and N-methylformamide is 10g / L, and the resulting solution is placed in an ultrasonic cleaning machine for ultrasonic 3h, The ultrasonic temperature is 30°C, the ultrasonic power is 500W, the solution after ultrasonic treatment is suction filtered, and the filtered solid is put into the autoclave;

[0036] (3) After the temperature in the autoclave reaches 25°C, pump carbon dioxide into the autoclave, and treat for 2 hours after the pressure in the auto...

Embodiment 2

[0040] A kind of preparation method of ultra-thin graphene powder of the present embodiment, described method specifically comprises the following steps:

[0041] (1) Using a graphite rod as a working electrode, add a 5V DC voltage to the sodium sulfate electrolyte, electrolyze for 8 hours, and then undergo solid-liquid separation, ultrasonic dispersion, washing, and drying to finally obtain a graphene precursor;

[0042] (2) The above-mentioned graphene precursor is dissolved in N, in N-dimethylformamide, the proportioning of graphene precursor and N, N-dimethylformamide is 40g / L, the gained solution is placed in ultrasonic Ultrasound in the cleaning machine for 2 hours, the ultrasonic temperature is 35 ° C, the ultrasonic power is 800 W, the solution after ultrasonic treatment is suction filtered, and the filtered solid is put into the autoclave;

[0043] (3) After the temperature in the autoclave reaches 25°C, pump carbon dioxide into the autoclave, and treat for 3 hours af...

Embodiment 3

[0047] A kind of preparation method of ultra-thin graphene powder of the present embodiment, described method specifically comprises the following steps:

[0048](1) Using a graphite rod as a working electrode, add a 6V DC voltage to the potassium sulfate electrolyte, electrolyze for 5 hours, then undergo solid-liquid separation, ultrasonic dispersion, washing, and drying to finally obtain a graphene precursor;

[0049] (2) Dissolve the above-mentioned graphene precursor in acetamide, the proportion of graphene precursor and acetamide is 30g / L, put the resulting solution in an ultrasonic cleaner for 4 hours, the ultrasonic temperature is 40°C, and the ultrasonic power 500W, suction filter the solution after ultrasonic treatment, filter out the solid and put it into the autoclave;

[0050] (3) After the temperature in the autoclave reaches 30°C, pump carbon dioxide into the autoclave, and treat for 4 hours after the pressure in the autoclave reaches 20 MPa;

[0051] (4) Decrea...

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Abstract

The invention discloses a preparation method of ultra-thin graphene powder and a product thereof, belonging to the technical field of graphene preparation. The method of the present invention specifically comprises the following steps: first, a graphite rod is used as a working electrode, a DC voltage is added to the electrolytic solution, electrolysis is performed, and a graphene precursor is obtained through post-treatment; then the graphene precursor is dissolved and ultrasonically filtered, The filtered solid is placed in an autoclave for treatment for a period of time, and then the pressure is quickly reduced to reduce the pressure in the autoclave to normal pressure. Finally, the obtained product is repeatedly washed and dried by centrifugation, and the ultra-thin graphene powder is prepared. The present invention combines the advantages of the electrochemical method and carbon dioxide, and the entire stripping process maintains the internal crystal structure of graphene to the greatest extent. The thickness of the prepared ultra-thin graphene is only 1-5nm, and the sheets are uniform and continuous. With few defects and high electrical conductivity, it has broad application prospects in the fields of electronic components, catalysis and new energy.

Description

technical field [0001] The invention belongs to the technical field of graphene preparation, and in particular relates to a method for preparing ultra-thin graphene powder and a prepared product thereof. Background technique [0002] Graphene is a carbon atom with sp 2 A two-dimensional crystal material with a hexagonal honeycomb structure formed by hybridization. Since it was discovered by a professor at the University of Manchester in 2004, it has attracted great attention from relevant scholars all over the world. As a new material, graphene has excellent performance in light, electricity, heat, force, etc., and has great application potential. It has good prospects in new energy, electronic information, intelligent sensing, aerospace, and military equipment. The preparation of graphene is the premise of basic research and the key to industrial application. Therefore, how to obtain large quantities of high-quality graphene has become the research goal of many scholars....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B1/135C01B32/19
Inventor 常海欣李刚辉郭辉
Owner 武汉低维材料研究院有限公司
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