Preparation method of high-conductivity graphene powder

A technology of graphene powder and high conductivity, applied in graphene, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of uncontrollable number of graphene layers, uncontrollable size, expensive price, etc., achieve high yield, The effect of low defect rate and simple feeding

Active Publication Date: 2016-07-13
江苏超电新能源科技发展有限公司
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Problems solved by technology

[0008] The purpose of the present invention is to disclose a method for preparing high-conductivity graphene powder, reduce the production cost of graphene powder, and solve the problem of uncontrollable number of graphene layers, uncontrollable size, many defects, high price, etc. problems, and shorten the process flow, improve the preparation efficiency, and be suitable for large-scale production

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preparation example Construction

[0045] Such as figure 1 Shown, the preparation method of highly conductive graphene powder comprises the following steps:

[0046] First perform step S1, disperse the raw material grade graphite in the mixed solution containing the intercalation agent and the oxidizing agent, and stir evenly;

[0047] Then perform step S2, place in a pressure vessel and keep stirring for a certain period of time, and pass inert gas during the process of keeping pressure and stirring;

[0048] Then perform step S3, extract the upper intercalation agent after the purification operation, and mechanically peel off the single-layer graphene oxide solution from the lower product;

[0049] Then perform step S4, after drying the single-layer graphene oxide solution through a powder drying process, re-dissolving the single-layer graphene oxide powder in the solvent to form a low-concentration single-layer graphene oxide solution;

[0050] Then perform step S5, add a reducing agent, and stir and react...

Embodiment 1

[0058] Mix 1.0 g of 1000-mesh flake graphite (natural graphite) with 3.5 g of potassium permanganate, add it into a 100 mL pressure vessel, and add a magnetic rotor into the pressure vessel. 30 mL of concentrated sulfuric acid (concentration: 98 wt%) at 0°C was added.

[0059] Put the autoclave into the autoclave, and seal the autoclave. A magnetic stirrer is arranged below the autoclave. Argon gas was introduced into the autoclave until the pressure reached 50 bar and the pressure was maintained. Turn on the magnetic stirrer and stir with the magnetic rotor for 5 min, so that the reactants are fully mixed. Then the reaction kettle was reacted at 5°C for 48h, and the pressure kettle was opened after the pressure was released. The obtained reaction product was placed in a centrifuge and centrifuged at a speed of 5000rmp for 5min. The intercalation agent in the upper layer was recovered as a clear liquid, and the muddy product in the lower layer was poured into 50mL of deioni...

Embodiment 2

[0063] Mix 1.0g of 5000 mesh artificial graphite with 3.0g of ammonium persulfate and 1.0g of phosphorus pentoxide, add it into a 100mL pressure vessel, and add a magnetic rotor into the pressure vessel. 10 mL of concentrated sulfuric acid (concentration: 98 wt%) at 0°C was added.

[0064] Put the autoclave into the autoclave, and seal the autoclave. A magnetic stirrer is arranged below the autoclave. Introduce argon until the pressure reaches 100 bar and maintain the pressure. Turn on the magnetic stirrer and stir with the magnetic rotor for 5 min, so that the reactants are fully mixed. Then the reaction kettle was reacted at 0°C for 24h, and the pressure kettle was opened after the pressure was released. Centrifuge at 5000rmp for 5min in a centrifuge. The intercalation agent whose upper layer was clarified liquid was recovered and used, and the muddy product of the lower layer was poured into 50 mL deionized water for dilution, and the clear liquid was removed by centrif...

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Abstract

The invention provides a preparation method of high-conductivity graphene powder. The preparation method comprises the following steps: S1, dispersing raw material level graphite in a mixed solution containing an intercalator and an oxidizing agent, and performing uniform stirring so as to obtain a new solution; S2, placing the new solution in a pressure vessel, introducing inert gas, and performing pressure maintaining and stirring; S3, performing purification operation so as to extract an upper layer intercalator, and stripping out a single-layer oxidized graphene solution from lower-layer products in a mechanical manner; S4, performing drying treatment through a powder drying technology, and then dissolving the single-layer oxidized graphene powder in a solvent again so as to form a low-concentration single-layer oxidized graphene solution; S5, adding a reducing agent, and performing a stirring reaction at 0-50 DEG C for a certain time so as to obtain a single-layer graphene solution; S6, performing drying treatment and heat treatment on the single-layer graphene solution according to the powder drying technology so as to obtain the high-conductivity graphene powder. The preparation method disclosed by the invention has the advantages that the prepared graphene has few structural defects and is good in conductivity and high in yield; the preparation process is simple and convenient to operate, the cost is low, and the large-scale production is easy to realize.

Description

technical field [0001] The invention relates to the technical field of graphene preparation, in particular to a technical method for preparing high-conductivity graphene powder. Background technique [0002] Graphene is made of sp 2 The hexagonal honeycomb-shaped two-dimensional crystal material composed of carbon is only one carbon atom thick. The difference between it and the traditional graphite material is that graphene is a two-dimensional material. This special structure endows graphene with excellent electrical properties (charge mobility of 250,000 cm 2 / V.s), thermal (thermal conductivity 5300W / m.K), mechanical (Young's modulus 1.0TPa) and other properties have received extensive attention from researchers since their discovery in 2004. Graphene has broad application prospects in composite materials, energy storage materials, solar cells, sensors and other fields, and is expected to replace silicon materials in the semiconductor field. In order to realize the com...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
CPCC01B2204/22C01P2004/04
Inventor 王云峰
Owner 江苏超电新能源科技发展有限公司
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