Preparation method and application of nitrogen-doped graphene-based carbon aerogel microspheres

A technology of nitrogen-doped graphene and carbon airgel, which is applied in chemical instruments and methods, hybrid/electric double layer capacitor manufacturing, inorganic chemistry, etc., can solve the problems of unsatisfactory wettability and achieve high energy density, The effect of clean appearance and large specific surface area

Inactive Publication Date: 2020-02-21
GUIZHOU MEILING POWER SUPPLY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the wettability with the electrolyte is still unsatisfactory, and the present invention is intended to be applicable to graphene-doped spherical nitrogen-doped carbon aerogels suitable for lithium-ion capacitors, which is different from the battery system applicable to the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] First, take by weighing 15g resorcinol, 8.181g formaldehyde, and measure 50ml of graphene oxide dispersion liquid with a concentration of 0.25mg / ml, wherein the dispersion liquid is a solvent with deionized water, and the aforementioned three substances are placed in a 500ml In the beaker, place it on a magnetic stirrer and stir, after the resorcinol is completely dissolved, add 0.1443g of catalyst anhydrous sodium carbonate, stir in a constant temperature oil bath at 40-60°C for 30-50min, and then add 8.59g of melamine to the beaker. Stir in the above solution until the solution becomes clear, then stir in a constant temperature oil bath at 60°C for 30-50min, then add an appropriate amount of deionized water to make the overall solid content of the graphene-based carbon aerogel become 40%, then, Add the reaction solution to the surfactant stirring system, the surfactant concentration is between 10%-20%, and the magnetic stirring is maintained at 600-800r / min to obtain a...

Embodiment 2

[0048] The graphene-based carbon aerogel microspheres obtained in Example 1 were placed in a planetary ball mill with a rotational speed of 400 r / min and ball-milled for 3-4 h to obtain powdered graphene-based carbon aerogels, which were prepared in a KOH solution (KOH). The mass ratio of GA to GA is 5) under the condition of continuous stirring, slowly add it into the powdered graphene-based carbon aerogel and continue stirring for 10-12 hours. Put it in a tube furnace under nitrogen atmosphere (ventilation rate is 80-100ml / min) at 800-1000°C for constant temperature activation for 3-5h, the heating rate is 3-5°C / min, after cooling to room temperature, take out and mash it , and then immersed in 1mol / L hydrochloric acid solution for 24h. After filtration, use deionized water to wash several times until it is neutral, filter and dry (120 ° C constant temperature drying for 12-24 hours) to obtain spherical carbon aerogel;

[0049] The obtained spherical carbon aerogel has a BE...

Embodiment 3

[0052] The spherical carbon aerogel prepared in Example 2 was heated to 800-1000°C at 3-5°C / min under nitrogen atmosphere, and kept for 1 h; Cool to room temperature under nitrogen protection, and dry to obtain activated nitrogen-doped graphene-based carbon aerogel microspheres; wherein, CO 2 and N 2 The ventilation rate is 100-120ml / min;

[0053] The obtained activated nitrogen-doped graphene-based carbon aerogel microspheres have a BET specific surface area of ​​2435 m in N2 adsorption test 2 / g, the average pore size is 5.80nm;

[0054] The activated nitrogen-doped graphene-based carbon aerogel microspheres were made into lithium ion capacitors, and after 24 hours of storage, the electrochemical performance was tested. The steps are as follows: connect the assembled lithium ion capacitors to a battery tester, Charge to 3.8V at a constant current rate of 5C, then charge at a constant voltage of 3.8V, leave it for 5 minutes, discharge it to 0.1V at a constant current, and ...

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Abstract

The invention relates to the technical fields of gel microsphere preparation and applications, and in particular relates to a preparation method and application of nitrogen-doped graphene-based carbonaerogel microspheres. The method includes the following steps: S1, mixing resorcinol, formaldehyde, catalyst anhydrous sodium carbonate, graphene oxide, melamine and deionized water, performing a reaction to obtain a reaction solution; S2, adding the reaction solution into a surfactant, and performing stirring to obtain a uniformly dispersed red-brown emulsion; S3, performing a sol-gel reaction on the red-brown emulsion, performing aging by using an acetone solution containing trifluoroacetic acid, performing soaking by using acetone, and performing normal-pressure drying to obtain an organicaerogel; S4, performing carbonization to obtain graphene-based carbon aerogel microspheres; S5, performing KOH activation to obtain a spherical carbon aerogel; and S6, performing CO2 activation. Thecarbon aerogel microspheres prepared by the method have a moderate particle size, a higher bulk density and higher porosity, a high effective specific surface area, excellent electrical conductivity,and good wettability with an electrolyte.

Description

technical field [0001] The invention relates to the technical field of preparation and application of gel microspheres, in particular to a preparation method and application of nitrogen-doped graphene-based carbon aerogel microspheres. Background technique [0002] With the development of science and technology and the improvement of living standards, people's demand for energy storage devices in terms of high energy, high power and long cycle life continues to increase. Lithium-ion batteries and supercapacitors both show deficiencies. Lithium-ion batteries have problems such as low power density (less than 500W kg-1), long charging time (1-5h), and poor cycle life (500-2000). , supercapacitors have problems such as low energy density (1-10Wh·kg-1), which limit the application range of lithium-ion batteries and supercapacitors. [0003] Under the above background, in recent years, both the high energy density (150-200Wh·kg-1) characteristics of lithium-ion batteries and the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/348C01B32/336C01B32/318H01G11/24H01G11/32H01G11/34H01G11/36H01G11/44H01G11/50H01G11/84H01G11/86
CPCC01B32/318C01B32/336C01B32/348H01G11/24H01G11/32H01G11/34H01G11/36H01G11/44H01G11/50H01G11/84H01G11/86Y02E60/13
Inventor 陈安国石斌杨程响陈晓涛王庆杰牟钦尧陈铤
Owner GUIZHOU MEILING POWER SUPPLY CO LTD
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