CN113120897A - Method for preparing nitrogen-doped microporous carbon electrode material by solvent-free method - Google Patents

Method for preparing nitrogen-doped microporous carbon electrode material by solvent-free method Download PDF

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CN113120897A
CN113120897A CN202110330986.9A CN202110330986A CN113120897A CN 113120897 A CN113120897 A CN 113120897A CN 202110330986 A CN202110330986 A CN 202110330986A CN 113120897 A CN113120897 A CN 113120897A
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nitrogen
electrode material
microporous carbon
carbon electrode
doped microporous
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CN113120897B (en
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任鹏刚
孙爱月
戴忠
靳彦岭
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Xian University of Technology
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    • Y02E60/13—Energy storage using capacitors

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Abstract

The invention discloses a method for preparing a nitrogen-doped microporous carbon electrode material by a solvent-free method, which comprises the following steps: firstly, dissolving potassium phenolate and urotropine in deionized water, then adding uniformly dispersed silicon dioxide aqueous solution, stirring, drying, reacting for 12 hours at 160 ℃, then mixing and grinding an organic polymer precursor and polytetrafluoroethylene particles, placing the mixture in a tubular furnace for pyrolysis reaction, finally washing the product with dilute hydrochloric acid and deionized water, and drying to obtain the nitrogen-doped microporous carbon electrode material. The method disclosed by the invention is used for preparing the nitrogen-doped microporous carbon electrode material with rich nitrogen content by using a polymerization-assisted one-step template activation method, no additional activating agent or template removing step is needed, the yield is high, the preparation is simple, and the method has good universality. The prepared nitrogen-doped microporous carbon used as an electrode has high specific capacity which is about 270-410F/g. The retention after 10000 cycles of cycling was close to 92.3%.

Description

Method for preparing nitrogen-doped microporous carbon electrode material by solvent-free method
Technical Field
The invention belongs to the technical field of electrode material preparation, and particularly relates to a method for preparing a nitrogen-doped microporous carbon electrode material by a solvent-free method.
Background
Supercapacitors, particularly electric double layer supercapacitor EDLCs, have a higher power density than lithium batteries and the like>10kW·kg-1Longer cycle life of over 105One circulationAnd higher reliability, and thus has attracted a wide range of attention from scientists. Whether academic research or practical research, carbon-based materials are simple to prepare and widely available, and for example, activated carbon, carbon tubes and graphene-like materials are widely used as electrode materials of EDLC systems due to their low cost and perfect physicochemical properties. However, conventional carbon-based supercapacitors still have poor specific capacitance performance and relatively low energy density in certain industrial areas such as consumer electronics, electric vehicles and smart devices. Thus, there remains a need to precisely tailor the structure of carbon microspheres, such as morphology, composition and pore structure, to improve the performance of electric double layer supercapacitors. Although some efforts are currently made to improve the performance of the heteroatom-doped porous carbon of the supercapacitor, research shows that the performance can be improved by doping the heteroatom to improve the pseudocapacitance, and the green and low-cost synthesis of novel heteroatom-rich porous carbon still remains a great challenge.
Disclosure of Invention
The invention aims to provide a method for preparing a nitrogen-doped microporous carbon electrode material by a solvent-free method, which solves the problem of low heteroatom content of a capacitor electrode material in the prior art.
The technical scheme adopted by the invention is that the method for preparing the nitrogen-doped microporous carbon electrode material by a solvent-free method is implemented according to the following steps:
step 1, dissolving potassium phenolate and urotropine in deionized water, uniformly mixing, adding a uniformly dispersed silicon dioxide aqueous solution, and stirring to obtain a mixed solution;
step 2, drying the mixed solution obtained in the step 1, and reacting the dried mixture at 160 ℃ for 12h to obtain an organic polymer precursor embedded in the silicon dioxide particles;
step 3, mixing the organic polymer precursor obtained in the step 2 with polytetrafluoroethylene particles, grinding the mixture to uniformly mix the mixture, and then placing the mixture in a tubular furnace for pyrolysis reaction;
and 4, washing the product obtained in the step 3 with dilute hydrochloric acid, then washing with deionized water until the pH value is neutral, and drying to obtain the nitrogen-doped microporous carbon electrode material.
The present invention is also characterized in that,
in the step 1, the mass ratio of the potassium phenoxide to the urotropine to the silicon dioxide aqueous solution is 2.5: 1: 1; the stirring time is 1-2 h.
In the step 2, the drying temperature is 60-80 ℃, and the drying time is 20-24 h.
In step 3, the mass ratio of the organic polymer precursor to the polytetrafluoroethylene particles is 1: 3; the grinding time is 20min-40 min.
In step 3, the pyrolysis reaction conditions are as follows: introducing nitrogen at the speed of 100-200 mL/s, heating to 700-900 ℃ at the speed of 5 ℃/min, preserving heat for 2h, and cooling to room temperature.
In the step 4, the drying temperature is 60-80 ℃, and the drying time is 20-24 h.
The beneficial effect of the invention is that,
the method disclosed by the invention is used for preparing the nitrogen-doped microporous carbon electrode material with rich nitrogen content by using a polymerization-assisted one-step template activation method, no additional activating agent or template removing step is needed, the yield is high, the preparation is simple, and the method has good universality. The prepared electrode material has large specific surface area of 3368m2The pore distribution is uniform and is 0.8-2nm, the chemical property is stable, the structural morphology is controllable, and the like; the prepared nitrogen-doped microporous carbon used as an electrode has high specific capacity which is about 270-410F/g. The retention rate after 10000 cycles of circulation is close to 92.3%, and the electrode material has good circulation stability and other excellent electrochemical properties.
Drawings
Fig. 1 is an SEM image of a nitrogen-doped microporous carbon electrode material prepared in example 1 of the present invention;
FIG. 2 is a TEM image of a nitrogen-doped microporous carbon electrode material prepared in example 1 of the present invention;
FIG. 3 is a graph showing cyclic voltammetry characteristics of nitrogen-doped microporous carbon electrode materials prepared in examples 1 to 3 of the present invention;
fig. 4 is a graph showing the relationship between the specific capacitance and the current density of the nitrogen-doped microporous carbon electrode material prepared in examples 1 to 3 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a method for preparing a nitrogen-doped microporous carbon electrode material by a solvent-free method, which is implemented by the following steps:
step 1, dissolving potassium phenolate and urotropine in deionized water, uniformly mixing, adding a uniformly dispersed silicon dioxide aqueous solution, and stirring for 1-2 hours to obtain a mixed solution;
the mass ratio of the potassium phenolate to the urotropine to the aqueous solution of silicon dioxide is 2.5: 1: 1;
the mass fraction of the silicon dioxide aqueous solution is 3.2-7.7%;
step 2, drying the mixed solution obtained in the step 1, and reacting the dried mixture at 160 ℃ for 12h to obtain an organic polymer precursor embedded in the silicon dioxide particles;
the drying temperature is 60-80 ℃, and the drying time is 20-24 h;
step 3, mixing the organic polymer precursor obtained in the step 2 with polytetrafluoroethylene particles, grinding the mixture to uniformly mix the mixture, and then placing the mixture in a tubular furnace for pyrolysis reaction;
the mass ratio of the organic polymer precursor to the polytetrafluoroethylene particles is 1: 3;
grinding for 20-40 min;
the pyrolysis reaction conditions are as follows: introducing nitrogen at the speed of 100-200 mL/s, heating to 700-900 ℃ at the speed of 5 ℃/min, preserving heat for 2h, and cooling to room temperature;
step 4, washing the product obtained in the step 3 with dilute hydrochloric acid for 6-9 times, then washing with deionized water until the pH value is neutral, and drying to obtain the nitrogen-doped microporous carbon electrode material;
the concentration of the dilute hydrochloric acid is 1mol/L, the drying temperature is 60-80 ℃, and the drying time is 20-24 h.
Example 1
The invention relates to a method for preparing a nitrogen-doped microporous carbon electrode material by a solvent-free method, which is implemented by the following steps:
step 1, dissolving potassium phenolate and urotropine in deionized water, uniformly mixing, adding a uniformly dispersed silicon dioxide aqueous solution, and stirring for 1 hour to obtain a mixed solution;
the mass ratio of the potassium phenolate to the urotropine to the aqueous solution of silicon dioxide is 2.5: 1: 1;
the mass fraction of the aqueous silica solution was 7.7%;
step 2, drying the mixed solution obtained in the step 1, and reacting the dried mixture at 160 ℃ for 12h to obtain an organic polymer precursor embedded in the silicon dioxide particles;
the drying temperature is 80 ℃, and the drying time is 24 hours;
step 3, mixing the organic polymer precursor obtained in the step 2 with polytetrafluoroethylene particles, grinding the mixture to uniformly mix the mixture, and then placing the mixture in a tubular furnace for pyrolysis reaction;
the mass ratio of the organic polymer precursor to the polytetrafluoroethylene particles is 1: 3;
grinding for 20 min;
the pyrolysis reaction conditions are as follows: introducing nitrogen at the rate of 150mL/s, heating to 800 ℃ at the rate of 5 ℃/min, preserving heat for 2h, and cooling to room temperature;
step 4, washing the product obtained in the step 3 with dilute hydrochloric acid for 6 times, then washing with deionized water until the pH value is neutral, and drying to obtain a nitrogen-doped microporous carbon electrode material, which is marked as NOPC-800;
the concentration of the dilute hydrochloric acid is 1mol/L, the drying temperature is 60 ℃, and the drying time is 12 h.
Scanning electron microscope and transmission electron microscope of the nitrogen-doped microporous carbon electrode material are shown in fig. 1 and 2, the morphology and pore structure of the composite material are represented by the Scanning Electron Microscope (SEM) and the Transmission Electron Microscope (TEM), and a spongy three-dimensional structure with a plurality of irregular cotton-like pores appears on the surface of the material. The TEM images clearly show that the obtained porous carbon is amorphous and has a rich wormhole-like pore structure.
Example 2
The invention relates to a method for preparing a nitrogen-doped microporous carbon electrode material by a solvent-free method, which is implemented by the following steps:
step 1, dissolving potassium phenolate and urotropine in deionized water, uniformly mixing, adding a uniformly dispersed silicon dioxide aqueous solution, and stirring for 1.5 hours to obtain a mixed solution;
the mass ratio of the potassium phenolate to the urotropine to the aqueous solution of silicon dioxide is 2.5: 1: 1;
the mass fraction of the aqueous silica solution was 3.2%;
step 2, drying the mixed solution obtained in the step 1, and reacting the dried mixture at 160 ℃ for 12h to obtain an organic polymer precursor embedded in the silicon dioxide particles;
the drying temperature is 60 ℃, and the drying time is 20 hours;
step 3, mixing the organic polymer precursor obtained in the step 2 with polytetrafluoroethylene particles, grinding the mixture to uniformly mix the mixture, and then placing the mixture in a tubular furnace for pyrolysis reaction;
the mass ratio of the organic polymer precursor to the polytetrafluoroethylene particles is 1: 3;
grinding for 25 min;
the pyrolysis reaction conditions are as follows: introducing nitrogen at the speed of 100mL/s, heating to 700 ℃ at the speed of 5 ℃/min, preserving heat for 2h, and cooling to room temperature;
step 4, washing the product obtained in the step 3 with dilute hydrochloric acid for 9 times, then washing with deionized water until the pH value is neutral, and drying to obtain a nitrogen-doped microporous carbon electrode material, which is marked as NOPC-700;
the concentration of the dilute hydrochloric acid is 1mol/L, the drying temperature is 70 ℃, and the drying time is 20 h.
Example 3
The invention relates to a method for preparing a nitrogen-doped microporous carbon electrode material by a solvent-free method, which is implemented by the following steps:
step 1, dissolving potassium phenolate and urotropine in deionized water, uniformly mixing, adding a uniformly dispersed silicon dioxide aqueous solution, and stirring for 2 hours to obtain a mixed solution;
the mass ratio of the potassium phenolate to the urotropine to the aqueous solution of silicon dioxide is 2.5: 1: 1;
the mass concentration of the silica aqueous solution was 5%;
step 2, drying the mixed solution obtained in the step 1, and reacting the dried mixture at 160 ℃ for 12h to obtain an organic polymer precursor embedded in the silicon dioxide particles;
the drying temperature is 75 ℃, and the drying time is 24 hours;
step 3, mixing the organic polymer precursor obtained in the step 2 with polytetrafluoroethylene particles, grinding the mixture to uniformly mix the mixture, and then placing the mixture in a tubular furnace for pyrolysis reaction;
the mass ratio of the organic polymer precursor to the polytetrafluoroethylene particles is 1: 3;
grinding for 40 min;
the pyrolysis reaction conditions are as follows: introducing nitrogen at the rate of 150mL/s, heating to 900 ℃ at the rate of 5 ℃/min, preserving heat for 2h, and cooling to room temperature;
step 4, washing the product obtained in the step 3 with dilute hydrochloric acid for 6-9 times, then washing with deionized water until the pH value is neutral, and drying to obtain a nitrogen-doped microporous carbon electrode material, which is marked as NOPC-900;
the concentration of the dilute hydrochloric acid is 1mol/L, the drying temperature is 60 ℃, and the drying time is 24 h.
The nitrogen-doped microporous carbon electrode materials prepared in examples 1-3 were tested for their performance in a three-electrode system, wherein: the prepared nitrogen-doped microporous carbon is used as a working electrode, a platinum sheet is used as a counter electrode, and an Hg/HgO electrode is used as a reference electrode. The assembled device is used for performance tests of cyclic voltammetry, impedance, constant current charge and discharge, cyclic stability and the like by using a coster electrochemical workstation. Fig. 3 and 4 are graphs of cyclic voltammetry characteristics and specific capacity variation with current density, respectively, and thus it can be known that the electrode material has good supercapacitor characteristics, and the cyclic voltammetry characteristics maintain a good rectangular shape at a high scan rate. And the capacity retention rate after 10000 cycles of circulation is close to 93 percent.

Claims (6)

1. A method for preparing a nitrogen-doped microporous carbon electrode material by a solvent-free method is characterized by comprising the following steps:
step 1, dissolving potassium phenolate and urotropine in deionized water, uniformly mixing, adding a uniformly dispersed silicon dioxide aqueous solution, and stirring to obtain a mixed solution;
step 2, drying the mixed solution obtained in the step 1, and reacting the dried mixture at 160 ℃ for 12h to obtain an organic polymer precursor embedded in the silicon dioxide particles;
step 3, mixing the organic polymer precursor obtained in the step 2 with polytetrafluoroethylene particles, grinding the mixture to uniformly mix the mixture, and then placing the mixture in a tubular furnace for pyrolysis reaction;
and 4, washing the product obtained in the step 3 with dilute hydrochloric acid, then washing with deionized water until the pH value is neutral, and drying to obtain the nitrogen-doped microporous carbon electrode material.
2. The method for preparing the nitrogen-doped microporous carbon electrode material by the solvent-free method according to claim 1, wherein in the step 1, the mass ratio of the potassium phenoxide to the urotropine to the aqueous solution of silicon dioxide is 2.5: 1: 1; the stirring time is 1-2 h.
3. The method for preparing the nitrogen-doped microporous carbon electrode material according to the claim 1, wherein in the step 2, the drying temperature is 60-80 ℃ and the drying time is 20-24 h.
4. The method for preparing the nitrogen-doped microporous carbon electrode material by the solvent-free method according to claim 1, wherein in the step 3, the mass ratio of the organic polymer precursor to the polytetrafluoroethylene particles is 1: 3; the grinding time is 20min-40 min.
5. The method for preparing the nitrogen-doped microporous carbon electrode material by the solvent-free method according to claim 1, wherein in the step 3, the pyrolysis reaction conditions are as follows: introducing nitrogen at the speed of 100-200 mL/s, heating to 700-900 ℃ at the speed of 5 ℃/min, preserving heat for 2h, and cooling to room temperature.
6. The method for preparing the nitrogen-doped microporous carbon electrode material according to the claim 1, wherein in the step 4, the drying temperature is 60-80 ℃ and the drying time is 20-24 h.
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