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Macro preparation method of micropore-rich nitrogen-doped yolk-eggshell structure carbon microspheres

A technology of nitrogen doping and carbon microspheres, applied in the field of electrochemical energy storage, can solve the problem of low energy density, achieve excellent rate performance, improve electrical conductivity and electrochemical performance, and achieve low cost effects

Active Publication Date: 2020-08-28
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As an electrode material for supercapacitors, in addition to the advantages of adjustable shape, good conductivity, good stability, high power density, and low cost, porous carbon also has a fatal disadvantage: low energy density.

Method used

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  • Macro preparation method of micropore-rich nitrogen-doped yolk-eggshell structure carbon microspheres
  • Macro preparation method of micropore-rich nitrogen-doped yolk-eggshell structure carbon microspheres
  • Macro preparation method of micropore-rich nitrogen-doped yolk-eggshell structure carbon microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046]1) Dissolve 0.33g of m-aminophenol and evenly disperse in 30mL of water, add 1mL of vinyltrimethoxysilane dropwise, then add 1mL of ammonia water and stir the organosilane hydrolysis reaction for 5h, the solution is uniform off-white; add 456μL of formaldehyde solution while stirring The phenolic resin was condensed for 5 hours, and the solution was gray-black after the reaction. Centrifuge, wash, and dry to obtain core-shell microspheres of silicone@phenolic resin.

[0047] 2) Carbonize the dried sample above at 800°C for 3 hours in a tube furnace under an argon atmosphere, remove the silicon template with 10 wt% hydrofluoric acid, activate (carbon material / potassium hydroxide = 0.25) and wash to obtain micro-rich Porous nitrogen-doped egg yolk@eggshell structured carbon microspheres.

[0048] Take the microporous nitrogen-doped egg yolk@eggshell carbon microspheres obtained in this example as an example. Its synthesis mechanism is as attached figure 1 shown. First,...

Embodiment 2

[0056] 1) Dissolve 0.33g m-aminophenol and evenly disperse in 30mL water, add 1mL vinyltrimethoxysilane dropwise, then add 1mL ammonia water and stir the organosilane hydrolysis reaction for 5h, the solution is uniform off-white; add 456μL formaldehyde solution while stirring The phenolic resin was condensed for 5 hours, and the solution was gray-black after the reaction. Centrifuge, wash, and dry to obtain core-shell microspheres of silicone@phenolic resin.

[0057] 2) Carbonize the dried sample above at 700°C for 3 hours in a tube furnace under an argon atmosphere, remove the silicon template with 10 wt% hydrofluoric acid, activate (carbon material / potassium hydroxide = 0.25) and wash to obtain microbe-rich Porous nitrogen-doped egg yolk@eggshell structured carbon microspheres.

[0058] For the microporous nitrogen-doped carbon microspheres (YCS700-A) obtained in this example, the mass ratio of the active material, acetylene black, and PTFE is 80:10:10. The active material...

Embodiment 3

[0063] 1) Dissolve 0.33g m-aminophenol and evenly disperse in 30mL water, add 1mL vinyltrimethoxysilane dropwise, then add 1mL ammonia water and stir the organosilane hydrolysis reaction for 5h, the solution is uniform off-white; add 456μL formaldehyde solution while stirring The phenolic resin was condensed for 5 hours, and the solution was gray-black after the reaction. Centrifuge, wash, and dry to obtain core-shell microspheres of silicone@phenolic resin.

[0064] 2) Carbonize the dried sample above at 900°C for 3 hours in a tube furnace under an argon atmosphere, remove the silicon template with 10wt% hydrofluoric acid, activate (carbon material / potassium hydroxide = 0.25) and wash to obtain micro-rich Porous nitrogen-doped egg yolk@eggshell structured carbon microspheres.

[0065] Use the microporous nitrogen-doped carbon microspheres (YCS900-A) obtained in this example. The mass ratio of active material, acetylene black, and PTFE is 80:10:10. The active material, acet...

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Abstract

The invention relates to a macro preparation method of micropore-rich nitrogen-doped yolk-eggshell structure carbon microspheres. The macro preparation method comprises the following steps: 1) dissolving a phenol source in deionized water, adjusting the solution to be weakly alkaline, adding organosilane for hydrolysis to obtain an organosilicone core, then adding an aldehyde source for condensation polymerization to form a coating shell layer, centrifuging, washing and drying to obtain organosilicone-phenolic resin core-shell structure microspheres; and 2) carbonizing the product in the step1) in an inert atmosphere, removing the silicon template, and activating to obtain the micropore-rich nitrogen-doped yolk-eggshell structure carbon microspheres. Compared with the prior art, the method has the following advantages: the synthesis process is simple and green, and the cost is low; the obtained carbon microspheres have high micropore content and high carbon residue and are suitable for industrial application; the pore size distribution of the carbon microspheres is highly matched with the ion size of the EMIMBF4 electrolyte, and the electrode / electrolyte system shows high specificcapacity, high energy density and excellent rate capability when being applied to a supercapacitor.

Description

technical field [0001] The invention belongs to the field of electrochemical energy storage, and in particular relates to a method for macro-preparing microporous nitrogen-doped egg yolk@eggshell structured carbon microspheres that can be applied to supercapacitor electrode materials. Background technique [0002] Porous carbon is a common industrial raw material, widely used as supercapacitor electrode material and secondary battery anode material. As an electrode material for supercapacitors, in addition to the advantages of adjustable morphology, good conductivity, good stability, high power density, and low cost, porous carbon also has a fatal shortcoming: low energy density. Improving the energy density of supercapacitors can start from two aspects: increasing the specific capacity of porous carbon materials and increasing the voltage window: increasing the specific capacity of porous carbon materials can be achieved from four aspects: increasing the specific surface ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/318C01B32/348H01G11/24H01G11/26H01G11/34
CPCC01B32/318C01B32/348H01G11/24H01G11/26H01G11/34Y02E60/13
Inventor 周亮李欣媛麦立强蔡聪聪
Owner WUHAN UNIV OF TECH
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