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Method for preparing three-dimensional microporous graphene totally without participation of solution

A solution-free, graphene-free technology, applied in the field of inorganic synthesis, can solve problems such as affecting electrical conductivity and thermal conductivity, large impact on waste liquid environment, and graphene structure damage, and achieves the effects of simple operation, large-scale preparation, and low equipment requirements.

Inactive Publication Date: 2016-01-20
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of three-dimensional graphene by solvent self-assembly will introduce a large number of defects and functional groups, which will seriously affect the electrical and thermal conductivity; the preparation of three-dimensional graphene by chemical vapor deposition requires solution etching to remove the template, which will damage the structure of graphene and the waste liquid will be harmful to the Great environmental impact

Method used

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  • Method for preparing three-dimensional microporous graphene totally without participation of solution
  • Method for preparing three-dimensional microporous graphene totally without participation of solution
  • Method for preparing three-dimensional microporous graphene totally without participation of solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1, copper powder is used as catalyst growth three-dimensional graphene

[0030] First of all, the preparation work before the reaction: take a certain amount of copper powder and spread it in the ceramic boat, place the ceramic boat in the temperature zone of the tube furnace, turn on the vacuum pump to pump the internal pressure of the quartz tube to 5×10 -3 Below Torr, close the gas outlet valve, feed the argon gas with a flow rate of 400 milliliters per minute through the flowmeter to rush the air pressure back to normal pressure, continue feeding argon gas to exhaust the air (at this time, until the reaction is over, the gas outlet valve is opened to maintain normal pressure) pressure environment), the temperature of the tube furnace was raised to 1000 °C at a rate of 50 °C / min.

[0031] Next, the reaction stage: ①template preparation; turn off the argon gas, and change it into 200 ml per minute of hydrogen gas to reduce and anneal the copper powder for 2...

Embodiment 2

[0032] Embodiment 2, copper powder is used as catalyst growth three-dimensional graphene

[0033] The preparation method is basically the same as in Example 1, the difference is: in the ② growth material process in the reaction stage, alcohol vapor is introduced in the form of argon bubbling alcohol, and hydrogen is introduced at the same time, and the ratio of hydrogen to argon is 10 / 50 ml Every minute, the mixed gas is used as the carbon source.

Embodiment 3

[0034] Embodiment 3, copper powder is used as catalyst to grow three-dimensional graphene

[0035] The preparation method is basically the same as in Example 1, except for: ② growing material process in the reaction stage. After preparing a three-dimensional microporous network copper template (such as figure 1 ), take it out and immerse it in the anisole solution dissolved in polymethyl methacrylate, then put it into the quartz tube, and directly enter the furnace temperature zone of 1000 degrees Celsius under the atmosphere of argon (the tube furnace can be moved flexibly). React for 20 minutes to prepare graphene.

[0036] 2. Transition metal compounds as catalyst precursors

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Abstract

The invention specifically provides a method for preparing three-dimensional microporous graphene totally without participation of a solution, which belongs to the technical field of inorganic synthesis. The method employs chemical vapor deposition and uses elemental transition metal powder or a compound containing a transition metal element as a catalyst so as to prepare a porous metal catalyst skeleton through high temperature reduction; then chemical vapor deposition is used for growing of graphene so as to obtain three-dimensional graphene with the catalyst skeleton; and a template is removed through direct evaporation at a high temperature under vacuum so as to obtain three-dimensional graphene. The method is simple and convenient to operate, and the obtained graphene can completely copy the shape of the template, which enables the designing space of the shape of a material to be great; no solution participates in the whole process of preparation, elimination of waste liquid is not needed, and the method is friendly to environment and can realize rapid and large-scale preparation of high-quality three-dimensional graphene; and the prepared three-dimensional graphene has the advantages of a small gap, great density and the like and has extensive application prospects in fields like spatial heat conduction, electric conduction, medicine, energy and catalyst carriers.

Description

technical field [0001] The invention belongs to the technical field of inorganic synthesis, and specifically relates to a method for preparing three-dimensional microporous graphene without the participation of a solution in the whole process. Background technique [0002] Graphene is a two-dimensional carbon material with only a single atomic layer thickness, which has excellent mechanical properties, high electrical conductivity, thermal conductivity and large specific surface area. Since graphene was discovered, there have been four main methods for preparing graphene; mechanical exfoliation, solvent (redox) method, epitaxial growth, and chemical vapor deposition. The commonly used method is the solvent method, which will introduce a large number of defects and functional groups to the preparation of graphene, which greatly reduces the conductivity of graphene; the chemical vapor deposition method belongs to the bottom-up growth of graphene, and the graphene prepared by t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 魏大程夏冬云郑保忠李孟林
Owner FUDAN UNIV
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