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Graphene material and preparation method thereof

A graphene and graphite technology, applied in the field of graphene materials and their preparation, can solve the problems of difficult peeling, limited graphene performance, low graphene monolayer rate, etc., achieve high monolayer rate, reduce peeling difficulty, improve The effect of preparation safety

Inactive Publication Date: 2014-08-27
OCEANS KING LIGHTING SCI&TECH CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In recent years, there have been studies (such as patents 201210249137.1, 201210135363.7) to suspend graphite powder or carbon nanotubes in ionic liquids, and then stir or ultrasonically or extrude to prepare graphene materials with good dispersibility, but due to graphite powder or The structure of carbon nanotubes is relatively compact, and it is difficult to peel off. The graphene monolayer ratio prepared by this method is low, and the performance of graphene is limited.

Method used

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  • Graphene material and preparation method thereof
  • Graphene material and preparation method thereof

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preparation example Construction

[0027] A kind of preparation method of graphene material, comprises the steps:

[0028] (1) Under an inert gas atmosphere, mix graphite and alkali metal in a molar ratio of 1 to 5:1 and put it into a sealed container, vacuumize to 10-1000Pa, and then heat-treat at 200-1000°C for 12- 120 hours, obtain alkali metal intercalation graphite;

[0029] (2) Take alkali metal intercalated graphite, add it to the molten ionic liquid according to the ratio of solid-liquid ratio 1g: 10~100mL, stir evenly, put it into an ultrasonic pulverizer, and ultrasonically treat 0.5~100mL at a power of 2~10kW Minutes, obtain graphene suspension;

[0030] (3) Filtrating the graphene suspension, taking the filter residue, washing and filtering with an organic solvent, and then repeatedly washing and filtering with deionized water until the eluate is neutral, and drying the filtrate to obtain a graphene material.

[0031] The inert gas atmosphere is nitrogen, argon or helium.

[0032] The graphite is...

Embodiment 1

[0043] A kind of preparation method of graphene material, comprises the steps:

[0044] (1) In an environment filled with helium, mix natural phosphorus flake graphite and metal potassium at a molar ratio of 5:1, mix well and put it into a heat-resistant glass tube, then seal the heat-resistant glass tube and evacuate to 10Pa, heated to 200°C, and heat-preserved for 12 hours to obtain metallic potassium intercalated graphite;

[0045](2) Select 1-ethyl-3-methylimidazolium bromide (EtMeImBr) as the ionic liquid, melt it in a beaker to obtain 1L of EtMeImBr solvent, maintain the temperature of EtMeImBr solvent at 150°C, add 100g of step (1 ) of the obtained metal potassium intercalated graphite, after stirring evenly, put the beaker into an ultrasonic pulverizer, and ultrasonically treat it with a power of 10kW for 1 minute to obtain a graphene suspension;

[0046] (3) Filter the graphene suspension obtained in step (2), take the filter residue and immerse it in N,N-dimethylpyr...

Embodiment 2

[0049] A kind of preparation method of graphene material, comprises the steps:

[0050] (1) In an environment full of nitrogen, mix artificial graphite and metal lithium at a molar ratio of 2:1, mix well and put it into a heat-resistant glass tube, then seal the heat-resistant glass tube and evacuate to 100Pa, heat To 250°C, heat preservation and heat treatment for 20 hours to obtain metal lithium intercalated graphite;

[0051] (2) Use 1-ethyl-3-methylimidazolium chloride salt (EtMeImCl) as the ionic liquid, melt it in a beaker to obtain 1L of EtMeImCl solvent, maintain the temperature of the EtMeImCl solvent at 180°C, and add 10 g of the step (1 ) the obtained metal lithium intercalated graphite, after stirring evenly, put the beaker into an ultrasonic pulverizer, and ultrasonically treat it with a power of 10kW for 0.5 minutes to obtain a graphene suspension;

[0052] (3) Filter the graphene suspension obtained in step (2), take the filter residue and immerse it in N,N-dim...

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Abstract

The invention discloses a preparation method of a graphene material. The preparation method includes the following steps that (1) after graphite and alkali metal are evenly mixed, vacuumizing and heat treatment are carried out, so that alkali metal intercalation graphite is obtained; (2) the alkali metal intercalation graphite is collected to be added into molten ionic liquid, after even stirring is conducted, the mixture is placed into an ultrasonic pulverizer, ultrasonic treatment is performed, and accordingly graphene suspension liquid is obtained; (3) the graphene suspension liquid is filtered, organic solvent for filtering residues is collected for washing and filtering, then, deionized water is used for conducting repeated washing and filtering until an eluate is neutral, filter objects are dried, and hence the graphene material is obtained. The invention further discloses the graphene material obtained through the preparation method. According to the graphene material and the preparation method thereof, the graphite and the alkali metal are mixed to be subjected to heat treatment first, the alkali metal intercalation graphite is obtained and then is dispersed into the ionic liquid, and after ultrasonic treatment is completed, the graphene material which is complete in laminated structure, high in monolayer rate and good in dispersity can be obtained; the method is simple, cost is low, efficiency is high, and the graphene material and the preparation method thereof are suitable for industrial production.

Description

technical field [0001] The invention relates to the field of graphene synthesis, in particular to a graphene material and a preparation method thereof. Background technique [0002] Graphene is a two-dimensional carbon atom crystal discovered by Andre K. Geim of the University of Manchester in 2004, and won the 2010 Nobel Prize in Physics. Due to its unique structure and good photoelectric properties, graphene has become one of the research hotspots in the fields of carbon materials, nanotechnology and functional materials. At present, the method of preparing graphene materials is mainly redox method, but during the preparation process, the sheet structure of graphene is easily destroyed, and graphene is agglomerated, which seriously affects its electrical and thermal conductivity. How to overcome the above-mentioned technical defects and develop new graphene preparation methods has become one of the current research hotspots in the graphene field. [0003] Ionic liquid re...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/184
Inventor 周明杰王要兵袁新生
Owner OCEANS KING LIGHTING SCI&TECH CO LTD
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