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Preparation method of three-dimensional hierarchical porous nitrogen-doped graphene and product

A nitrogen-doped graphene, hierarchical porous technology, applied in graphene, chemical instruments and methods, nano-carbon, etc., can solve problems affecting the performance of porous graphene, save template costs and process steps, have a wide range of sources, maintain The effect of internal topography

Active Publication Date: 2016-07-06
湖北虹润高科新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The template method is the most commonly used method to prepare porous graphene. However, the porous structure formed by this method is at the expense of a hard template, and the residual template greatly affects the performance of porous graphene.

Method used

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  • Preparation method of three-dimensional hierarchical porous nitrogen-doped graphene and product
  • Preparation method of three-dimensional hierarchical porous nitrogen-doped graphene and product
  • Preparation method of three-dimensional hierarchical porous nitrogen-doped graphene and product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] 1) Taking duckweed (its microstructure as figure 1 As shown in the figure, it can be seen from the figure that the duckweed itself contains a three-dimensional porous structure) as a raw material, wash the duckweed, soak it in ethanol solution for 48 hours, and then take it out; then place it in a tube furnace for carbonization at 1000°C under an argon atmosphere , keep warm for 2h, at 2℃·min -1 heating rate heating;

[0048] 2) Weigh 5g of the sample in step 3), put it into 10g of concentrated sulfuric acid, and then add 5g of NaNO 3 Solid and 20g KMnO 4 The solid was placed in a water bath at 30°C and stirred for 30 minutes, then an excess of 30 g K was added 2 CO 3 Continue to stir the solid for 30 minutes, and then fully dry it in a common drying oven;

[0049] 3) Place the consolidated block obtained in step 2) in a tube furnace, and activate it by raising the temperature to 700°C under an inert gas protective atmosphere. The activation holding time is 1h, and...

Embodiment 2

[0054] 1) Wash the straw, soak it in ethanol solution for 52 hours, take it out, and then place it in a tube furnace for carbonization at 900°C under an argon atmosphere. -1 heating rate heating;

[0055] 2) Weigh 5g of the sample in step 1), and add 7.5g of NaNO to 15g of concentrated sulfuric acid 3 Solid and 25g KMnO 4 The solid was placed in a water bath at 20°C and stirred for 20 minutes, then an excess of 55 g K was added 2 CO 3 Continue to stir the solid for 40 minutes, and then fully dry it in a common drying oven;

[0056] 3) Put the consolidated block obtained in step 2) in a tube furnace, and activate it by raising the temperature to 800°C under an inert gas protective atmosphere. The activation holding time is 1.5h, and the heating rate is 7°C·min -1 ;

[0057] 4) Grinding the product obtained in step 3) to 0.5MH 2 SO 4 Pickling at room temperature for 4 hours, suction filtration, and washing with water until neutral;

[0058] 5) The sample obtained in step...

Embodiment 3

[0061] 1) Wash the peanut shells, soak them in ethanol solution for 56 hours, take them out, and place them in a tube furnace for carbonization at 1100°C under a nitrogen atmosphere. -1 heating rate heating;

[0062] 2) Weigh 5g of the sample in step 1), and add 10g of NaNO to 10g of concentrated sulfuric acid 3 Solid and 28g KMnO 4 The solid was placed in a water bath at 40°C and stirred for 40 minutes, then an excess of 40 g K was added 2 CO 3 Continue to stir the solid for 20 minutes, and then fully dry it in an ordinary drying oven;

[0063] 3) Put the consolidated block obtained in step 2) in a tube furnace, and activate it by raising the temperature to 900°C under an inert gas protective atmosphere. The activation holding time is 2h, and the heating rate is 6°C·min-1 ;

[0064] 4) Grinding the product obtained in step 3) to 0.5MH 2 SO 4 Pickling at room temperature for 8 hours, suction filtration, and washing with water until neutral;

[0065] 5) The sample obtain...

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Abstract

The invention discloses a preparation method of three-dimensional hierarchical porous nitrogen-doped graphene and the product, and belongs to the field of graphene preparation.The preparation method comprises the steps that a biomass material which is most common in the natural world is selected as a raw material and taken as a solid carbon source, a nitrogen source and a synthesizing template simultaneously, gradient dewatering processing is firstly performed, then carbonization and pre-expansion processing is performed, the processed biomass material is mixed with a K2CO3 solution, high-temperature activation is performed, freeze-drying is performed, and then the three-dimensional hierarchical porous nitrogen-doped graphene is obtained.The obtained graphene has a hierarchical pore structure comprising macropores, mesopores and micropores, the nitrogen-doped content is 2.5 at.%-7.5 at.%, and the specific surface area reaches up to 1300 m<2> / g or above.The preparation method has the advantages that the preparation technology is simple and the prepared graphene is excellent in performance and shows the very good oxygen reduction activity in the electro-catalysis field.

Description

technical field [0001] The invention belongs to the field of graphene preparation, and more specifically relates to a preparation method and product of three-dimensional hierarchical porous nitrogen-doped graphene. Background technique [0002] Graphene is a two-dimensional allotrope of carbon, which combines many excellent properties such as high carrier mobility, good light transmission, high thermal conductivity, high mechanical strength and high electrochemical stability. extensive attention. Among them, the most important thing is the electrical properties exhibited by the unique electronic structure of graphene, such as electron ballistic transport at room temperature, anomalous quantum Hall effect and quantum tunneling effect. However, the energy band gap of intrinsic graphene is zero, showing semi-metallicity, resulting in no switching behavior of devices made of graphene, which greatly limits its application in electronic and optoelectronic devices. [0003] In or...

Claims

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Application Information

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IPC IPC(8): C01B31/04
CPCC01B2204/22C01B2204/32C01P2002/80C01P2002/82C01P2002/85C01P2004/04C01P2006/17
Inventor 黄云辉张建胡培
Owner 湖北虹润高科新材料有限公司
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