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Three-dimensional microstructural self-supporting flexible porous carbon film as well as preparation method and application thereof

A microstructure, self-supporting technology, applied in the field of porous carbon materials, can solve the problems of hindering electrolyte ions from entering the internal pores, specific surface area cannot participate in charge storage, capacitive performance limitations, etc., and achieves controllable carbon network density, small network diameter, The effect of high specific surface area

Active Publication Date: 2019-11-12
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Commercial porous carbon has a large specific surface area to provide abundant active sites for charge accumulation and storage of electrical energy. However, the existence of numerous closed pores and irregular pores seriously hinders the electrolyte ions from entering the internal pores during charge and discharge. The surface area cannot participate in charge storage, and its low conductivity also limits its capacitive performance.

Method used

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  • Three-dimensional microstructural self-supporting flexible porous carbon film as well as preparation method and application thereof
  • Three-dimensional microstructural self-supporting flexible porous carbon film as well as preparation method and application thereof
  • Three-dimensional microstructural self-supporting flexible porous carbon film as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0035] 1. According to the molar ratio of resorcinol: formaldehyde: sodium carbonate is 50:100:1, and the mass ratio of resorcinol: water is 1:20, mix resorcinol, formaldehyde, sodium carbonate and water After stirring for 1 minute, react at 45°C for 1 hour to obtain a prepolymer solution;

[0036] 2. Add 20 milliliters of 1.8 g / L iminodiacetic acid solution to the pre-polymerization liquid, and after standing at room temperature for 20 minutes, the filter paper absorbs water until the dehydration is 80%, and puts it into an autoclave at 115° C. for 0.5 days to obtain the reaction intermediate product A.

[0037] 3. Put the reaction intermediate product A in tert-butanol, soak it at 25°C for 1 day to obtain the reaction product B, freeze-dry the reaction product B at -20°C for 1 day, and then pre-carbonize the obtained product B at 600°C for 1 hour , after soaking in nickel nitrate-tert-butanol solution (mass ratio of nickel nitrate and tert-butanol 1:20) solution and freeze-d...

Embodiment 2

[0040] 1. According to the molar ratio of resorcinol: formaldehyde: sodium carbonate is 50:100:1, and the mass ratio of resorcinol: water is 1:20, mix resorcinol, formaldehyde, sodium carbonate and water Stir for 1 minute after mixing, and react for 1 hour at 45°C to obtain a prepolymer solution;

[0041] 2. Add 20 milliliters of 1.8 g / L iminodiacetic acid solution to the pre-polymerization solution, dehydrate it by 90%, put it in an autoclave at 115° C. for 0.5 days, and obtain the reaction intermediate product A.

[0042] 3. After the reaction product A is frozen in liquid nitrogen, freeze-dry at -20°C for 1 day, and the resulting product is pre-carbonized at 600°C for 1 hour, soaked in nickel nitrate-tert-butanol (the mass ratio of nickel nitrate and tert-butanol is 1 :10) solution and freeze-drying at -20°C to obtain product B, which is carbonized at 950°C to obtain a three-dimensional microstructure self-supporting flexible porous carbon film.

[0043] Figure 4 Scannin...

Embodiment 3

[0045] 1. According to the molar ratio of resorcinol: formaldehyde: sodium carbonate is 50:100:1, the mass ratio of phenolic monomer: water is 1:20, the resorcinol, formaldehyde, sodium carbonate and water After mixing, stir for 1 minute, and react at 45°C for 2 hours to obtain a prepolymer solution;

[0046] 2. Add 40 ml of 1.8 g / L iminodiacetic acid solution to the pre-polymerization solution, dehydrate it by 90%, put it in an autoclave at 115°C for 0.5 days, and obtain the reaction intermediate product A;

[0047] 3. Put the reaction intermediate product A into tert-butanol containing 20 wt% of water (after mixing water and tert-butanol, water accounts for 20% in the solution), soak at 25°C for 1 day to obtain reaction product B;

[0048] 4. The reaction product B was freeze-dried at -20°C for 1 day after being frozen in liquid nitrogen, and the resulting product was pre-carbonized at 600°C for 1 hour, soaked in nickel nitrate-tert-butanol (mass ratio 1:10) solution and Afte...

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Abstract

The invention belongs to the technical field of porous carbon materials, and discloses a three-dimensional microstructural self-supporting flexible porous carbon film and a preparation method and application thereof. The preparation method of the three-dimensional microstructural self-supporting flexible porous carbon film comprises the following steps: mixing a phenol monomer, an aldehyde monomer, an alkaline catalyst and water, performing stirring, and performing a reaction at 25-45 DEG C to obtain a prepolymer solution; adding an acidic solution into the prepolymer solution, allowing the mixed solution to stand, performing dehydration to loss 60-90% of water, placing the dehydrated product at 110-130 DEG C, putting the obtained product into an alcohol solvent, and performing soaking at25-60 DEG C; and performing freeze drying on the obtained reaction product at -20 DEG C to 0 DEG C, performing carbonization on the product at 600 DEG C, performing soaking in a softening solution, performing freeze drying, and finally performing carbonization treatment on the obtained product at 700-1000 DEG C to obtain the product. The three-dimensional microstructural self-supporting flexible porous carbon film prepared by the method has the characteristics of a high specific surface area, certain flexibility, a controllable carbon network density and a small network diameter, and can be applied to the field of sodium ion batteries.

Description

technical field [0001] The invention belongs to the technical field of porous carbon materials, and more specifically relates to a three-dimensional microstructure self-supporting flexible porous carbon film and its preparation method and application. Background technique [0002] Porous materials organically integrate the characteristics of materials with different scale pore structures. For example, the high specific surface of micropores and mesoporous surfaces can provide sufficient modification sites, and the surface properties can be adjusted through chemical and physical treatments, so that the materials have new properties. Chemical properties; macropores allow material molecules to easily reach active sites. These properties make porous materials widely used in catalysis, adsorption, loading, energy storage and conversion, sensing, and biomedicine. [0003] The conductivity of porous carbon materials is poor. It can be improved by doping heteroatoms such as nitroge...

Claims

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Application Information

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IPC IPC(8): C01B32/05H01M4/587H01M10/054
CPCC01B32/05H01M4/587H01M10/054Y02E60/10
Inventor 李娜吴序豪李宽杨桥刘星
Owner GUANGDONG UNIV OF TECH