Preparation method of graphene uniform dispersion

A technology of uniform dispersion and graphene, applied in the direction of graphene, nano-carbon, etc., can solve the problems of complicated film transfer process, high raw material price, complicated process, etc., and achieve the effect of good peeling, high conductivity and low cost.

Active Publication Date: 2012-07-18
常熟三爱富氟源新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the use of strong oxidants such as oleum, nitric acid, and potassium permanganate in the oxidation stage, and the use of toxic, flammable and explosive strong reducing agents such as hydrazine hydrate, metal sodium and potassium, hydroquinone, and sodium borohydride in the reduction stage, this This method will encounter serious problems such as wastewater treatment, fire and explosion protection in the process of large-scale production, and at the same time, the complex process and high raw material prices will also make the production cost face challenges
The CVD method can prepare single-layer or low-layer graphene materials in a large area (centimeter scale), which has great application potential in device manufacturing, but the size of the graphene film is still limited by the transition metal substrate (Cu, Ni, Ru etc.), and the film transfer process is complex, how to maintain the stability of product performance will be the key to mass manufacturing of devices

Method used

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  • Preparation method of graphene uniform dispersion
  • Preparation method of graphene uniform dispersion
  • Preparation method of graphene uniform dispersion

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 1g of expandable graphite powder, add 1000mL 0.2g / L polysorbate-80 aqueous solution, heat the autoclave to 200℃, keep the stirring speed at 200rpm for hydrothermal insulation treatment for 6 hours, then centrifuge the slurry at 1000rpm for 20min, The obtained upper layer solution is the graphene dispersion. The dispersion was allowed to stand for 2 hours at room temperature without sedimentation, indicating good stability. figure 1 , 2 The 002 and 004 peaks are the characteristic peaks of graphitization. The intensity of the 002 and 004 peaks of graphene is much lower than that of graphite, indicating that the number of effective exfoliated layers of graphite is reduced; the 001 characteristic peak of graphite oxide does not appear at 10.6° in the XRD graph of graphene It shows that the degree of oxidation is small and the conjugate structure on the surface is less damaged.

Embodiment 2

[0023] Take 10g of high-temperature pyrolytic graphite powder, add 1000mL 2g / L sodium dodecylbenzene sulfonate aqueous solution, heat the autoclave to 160℃, keep the stirring speed 180rpm for hydrothermal insulation treatment for 10 hours, then centrifuge the slurry at 1500rpm After 40 minutes of separation, the upper layer solution obtained is the graphene dispersion, and the dispersion is allowed to stand at room temperature for 2 hours without sedimentation, indicating good stability. The XRD pattern of the obtained product is similar to that of Example 1. The intensity of the 002 and 004 peaks of graphene is relatively lower than that of graphite, and the 001 characteristic peak of graphite oxide does not appear at 10.6°.

Embodiment 3

[0025] Take 100g expandable graphite powder and add it to 1000mL 20g / L polyether P-123 aqueous solution, heat the autoclave to 180℃, keep the stirring speed 160rpm for hydrothermal treatment for 16 hours, then centrifuge the slurry at 2000rpm for 30min to obtain the upper layer solution It is a graphene dispersion, and it is allowed to stand for 2 hours at room temperature without sedimentation, indicating that the dispersion is stable. The XRD pattern of the obtained product is similar to that of Example 1. The intensity of the 002 and 004 peaks of graphene is relatively lower than that of graphite, and the 001 characteristic peak of graphite oxide does not appear at 10.6°.

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Abstract

The invention relates to a preparation method of graphene uniform dispersion, belonging to the technical field of new nano materials. The preparation method comprises the following steps of: (1) preparing aqueous surfactant solution with the concentration of 0.2-20g / L; (2) mixing raw graphite powder with the aqueous surfactant solution according to the concentration of 1-100g / L, forming suspension and adding the suspension into a high-pressure reactor with strirring; (3) adjusting the rotating speed of the high-pressure reactor to be 50-300rpm and the temperature in the reactor to be 100-300 DEG C, carrying out heat preservation treatment on the raw graphite powder for 5-24 hours and then taking out paste; (4) carrying out 1000-2000rpm centrifugation on the paste for 15-45 minutes, and obtaining supernatant solution which is the dispersion with one-layer and multilayer graphene. The preparation method has the advantages that the aqueous surfactant solution used in the preparation process can be recycled without exhaust emission; the used materials are non-corrosive, non-toxic, non-flammable and non-explosive products; the process can not cause large damage to the protogenic conjugated structure of the graphene; and the low cost can be realized, and the graphene dispersion with excellent dispersity and stability can be prepared.

Description

Technical field [0001] The invention relates to the technical field of nano new materials, in particular to a method for preparing a graphene uniform dispersion. Background technique [0002] Since the discovery of graphene in 2004, it has been generally favored by researchers from the fields of physics and materials. Graphene is a two-dimensional honeycomb lattice structure carbonaceous material composed of a single layer of carbon atoms closely packed. Although graphene is only one layer of carbon atoms thick and is the thinnest of the known materials, it is very strong and hard. Graphene is also the most conductive material currently known. In addition, graphene has many excellent properties, such as high thermal conductivity, huge specific surface area and so on. Due to the special properties of graphene, it has broad application prospects in electronics, optics, magnetism, biomedicine, sensors, and energy storage. In order to apply graphene to the above-mentioned fields,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/19
Inventor 何光裕马凯陈海群施健席海涛李丹孙小强汪信
Owner 常熟三爱富氟源新材料有限公司
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