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A kind of preparation method of three-dimensional nitrogen-doped graphene/coox composite material

A nitrogen-doped graphene and composite material technology is applied in the field of preparation of three-dimensional nitrogen-doped graphene/CoOx composite nanomaterials. Effect

Inactive Publication Date: 2017-10-24
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The experimental steps are relatively cumbersome, and the lithium storage performance of the material obtained by this preparation method under high current density still needs to be improved (400 mAhg -1 at 1 Ag -1 )

Method used

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  • A kind of preparation method of three-dimensional nitrogen-doped graphene/coox composite material
  • A kind of preparation method of three-dimensional nitrogen-doped graphene/coox composite material
  • A kind of preparation method of three-dimensional nitrogen-doped graphene/coox composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Nitrogen-doped graphene / CoO x The preparation steps of the composite material are as follows:

[0029] A. Preparation of Graphene Oxide (GO)

[0030] a. Weigh 10g of graphite powder and 7.5g of sodium nitrate in a 2L round bottom beaker, and mechanically stir vigorously. Slowly add 300mL of concentrated sulfuric acid, and after stirring for 0.5h, slowly add 40g of potassium permanganate (completely added in 2 hours). When the magnetic stirrer was stirred until the next day, the mixture in the flask turned brown and had a thick character, and then changed to a mechanical stirrer for about five days.

[0031] b. Slowly add 1L of deionized water into the beaker. Since this process will release a lot of heat, the speed must be controlled when the dilution is first started. After dilution, the mixture turns into a tan liquid. Slowly add 60ml of 30% hydrogen peroxide while stirring to neutralize the unreacted potassium permanganate. At the same time, a large number of bubb...

Embodiment 2

[0040] The difference between this example and Example 1 is: the surfactant is F127, and the addition amount is 1mg / ml; the temperature is raised to 600°C at a rate of 2°C / min under a nitrogen atmosphere; the material is used as a cathode catalyst for the fuel cell oxygen reduction reaction.

Embodiment 3

[0042] e. Heat up the 3D cobalt phthalocyanine / surfactant CTAB / graphene airgel obtained in B (c) above to 800°C at a rate of 2°C / min in a nitrogen atmosphere, keep it for 2h, and wait for the temperature to drop to 400°C ℃, stop the nitrogen flow, change to the air, keep the sample for 20 minutes, and then cool the sample rapidly to obtain a three-dimensional nitrogen-doped graphene / CoO x nanocomposites, and the obtained cobalt is Co 3 o 4 as the main form (3D nitrogen-doped graphene / CoO x -2); The material can be used as a negative electrode catalyst for lithium-ion batteries.

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Abstract

The invention relates to a method for preparing a three-dimensional nitrogen-doped graphene / CoOx composite material, and belongs to the technical field of functional materials. The method comprises the main processes of: by taking phthalonitrile as a nitrogen-containing precursor, cobalt acetate as a transition metal precursor, and graphene oxide prepared by the Hummers method as a carbon carrier, adding a surface active agent and carrying out solvent-thermal-technology one-step in-situ coordination, assembling, freeze drying and calcination treatment to obtain the three-dimensional structured nitrogen-doped graphene / CoOx composite nano material. In comparison with the prior art, the three-dimensional nitrogen-doped graphene / CoOx composite material prepared by the invention has the advantages that particles are homogeneous and do not agglomerate; in addition, more electron transmission channels exit because of mesopores left after the surface active agent is removed, the impedance is reduced, and the electrochemical property of the material is improved.

Description

technical field [0001] The present invention relates to three-dimensional nitrogen-doped graphene / CoO x The invention relates to a method for preparing composite nanomaterials, which belongs to the technical field of functional materials. The main process of the method of the present invention is: using phthalonitrile as a nitrogen-containing precursor, cobalt acetate as a transition metal precursor, and graphene as a carbon carrier, adding a surfactant and recombining in situ in one step through solvothermal technology, and finally obtaining Three-dimensional nitrogen-doped graphene / CoO x composite nanomaterials. Background technique [0002] Graphene is a carbon material with a two-dimensional honeycomb structure formed by a single layer of carbon atoms, and has excellent mechanical and electrical properties. At the same time, graphene has a high specific surface area and can be used as a carrier material for nanomaterials. Yeager and co-workers proposed that nitrogen-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/52H01M4/587B82Y30/00
CPCB82Y30/00H01M4/139H01M4/362H01M4/52H01M4/88H01M4/90Y02E60/10Y02E60/50
Inventor 刘瑞丽邢霞吴东清刘少卿徐培敏
Owner SHANGHAI UNIV
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