CN107934933B - Preparation method of two-dimensional nitrogen-doped porous carbon material for supercapacitor electrode - Google Patents
Preparation method of two-dimensional nitrogen-doped porous carbon material for supercapacitor electrode Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
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- H01G11/32—Carbon-based
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
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Abstract
The invention belongs to the technical field of material preparation, and relates to a preparation method of a two-dimensional nitrogen-doped porous carbon material for a supercapacitor electrode. The method comprises the following steps of carrying out hydrothermal reaction at a certain temperature by using two-dimensional graphene oxide as a template, biomass sugar as a carbon source and amino acid as a nitrogen source to prepare the nitrogen-modified hydrothermal carbon. And mixing the prepared hydrothermal carbon with potassium hydroxide in a certain proportion, and then activating at high temperature to obtain the two-dimensional nitrogen-doped porous carbon material. The invention has the advantages that: the raw materials are rich, the price is low, and the preparation method is simple; the graphene oxide is used as a two-dimensional structure template, a template agent does not need to be removed, pollution is reduced, and the method has the advantages of environmental friendliness and the like; the amino acid and the biomass saccharide react under the hydrothermal condition to carry out nitrogen doping, so that the doping amount of nitrogen elements is increased; the construction of the two-dimensional structure and the introduction of nitrogen elements improve the electrochemical performance of the prepared two-dimensional nitrogen-doped porous carbon material.
Description
Technical Field
The invention belongs to the technical field of material preparation, and relates to a preparation method of a two-dimensional nitrogen-doped porous carbon material for a supercapacitor electrode.
Background
With the gradual depletion of traditional fossil fuels, the development and application of sustainable energy becomes a core problem to be paid attention to and urgently solved all over the world. The super capacitor attracts more and more attention of scientists and industrial researchers as an electrochemical energy storage device with excellent electrochemical characteristics and environmental friendliness. The porous carbon material is a novel carbon material widely applied, has the advantages of simple and easily obtained raw materials, good chemical stability and larger specific surface area, can be used as a capacitor electrode material, and has poorer rate capability due to the influence of the pore structure and the micro-morphology. Due to the unique structure of the two-dimensional porous carbon material, the ion transmission channel can be shortened, and the rate performance can be improved, so that a plurality of methods are developed to prepare the two-dimensional porous carbon material. The template method is a common method for preparing two-dimensional porous carbon, and common templates comprise nano metal salts, silicon dioxide and the like. For example, the army of the Hamburg university successfully prepares a two-dimensional porous material by using a magnesium oxide template (Fan Zhuangjun, et al, adv. energy Mater.2012,2, 419-424). However, the synthesis conditions of the template are harsh and high in cost, and the removal of the template requires a large amount of acid or alkali washing, which brings about a serious problem of environmental pollution. The graphene is a two-dimensional material with excellent physical and chemical properties, and has a good two-dimensional guiding effect in material preparation. The carbon material with a two-dimensional structure can be prepared by compounding the template agent and the carbon source, and the template agent graphene does not need to be removed. When the graphene is used as a capacitor material, the graphene in the two-dimensional porous carbon material can obviously improve the electrochemical performance of the carbon material.
In order to further improve the electrochemical performance of the porous carbon material, the pseudo-capacitance can be improved by introducing nitrogen atoms into the carbon material. The method is commonly carried out by simply mechanically mixing the prepared porous carbon material with nitrogen-containing precursors such as urea and melamine, and then carrying out high-temperature treatment to obtain the nitrogen-doped porous carbon, for example, the patent with the application number of 201710009138.1 discloses a method for preparing the nitrogen-doped porous carbon by mechanically mixing the melamine serving as a nitrogen source with the carbon-containing precursors and then carrying out high-temperature treatment. However, simple mechanical mixing affects the amount of nitrogen incorporated, and multiple high temperature treatments add to the process complexity.
Disclosure of Invention
The invention provides a preparation method of a two-dimensional nitrogen-doped porous carbon material for a supercapacitor electrode.
The invention is realized by the following technical scheme. Preparing a biomass saccharide aqueous solution with a certain concentration, adding a certain amount of amino acid and graphene oxide, wherein the amino group of the amino acid can perform Maillard reaction with the carbonyl group of the saccharide at a high temperature to play a nitrogen fixation role. And then activating the obtained hydrothermal carbon material with potassium hydroxide in a certain proportion at high temperature to prepare the two-dimensional nitrogen-doped porous carbon material.
The technical scheme of the invention is as follows:
a preparation method of a two-dimensional nitrogen-doped porous carbon material for a supercapacitor electrode comprises the following steps:
(a) preparing 0.025-0.1 g/mL of biomass saccharide aqueous solution, adding graphene oxide according to the mass ratio of the biomass saccharide to the graphene oxide of 1: 0.01-1: 0.05, adding amino acid according to the mass ratio of the biomass saccharide to the amino acid of 1: 0.5-1: 2, putting the mixture into a hydrothermal kettle, reacting for 6-24 hours at the temperature of 150-180 ℃, washing with deionized water after the reaction is finished, and drying at the temperature of 80 ℃ to obtain hydrothermal carbon;
(b) taking the hydrothermal carbon prepared in the step (a) as a raw material, mixing the hydrothermal carbon and potassium hydroxide according to a mass ratio of 1: 1-1: 4, raising the temperature to 600-800 ℃ at a speed of 1-5 ℃/min, reacting for 2-4 h, washing to be neutral by using deionized water, and drying at 80 ℃ for 12h to obtain the two-dimensional nitrogen-doped porous carbon material.
The biomass sugar is fructose, glucose or sucrose.
The amino acid is lysine, glutamic acid, serine or arginine.
The graphene oxide is prepared by a Hummers' method.
The invention has the beneficial effects that: 1) the raw materials are rich, the price is low, and the preparation method is simple; 2) the graphene oxide is used as a two-dimensional structure template, a template agent does not need to be removed, pollution is reduced, and the method has the advantages of environmental friendliness and the like; 3) the amino acid and the biomass saccharide react under the hydrothermal condition to carry out nitrogen doping, so that the doping amount of nitrogen elements is increased; 4) the construction of the two-dimensional structure and the introduction of nitrogen elements improve the electrochemical performance of the prepared two-dimensional nitrogen-doped porous carbon material as a capacitor electrode.
Drawings
Fig. 1 is a transmission photograph of example 1.
FIG. 2 is a transmission photograph of example 6.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
Example 1
Dissolving 1g of fructose in 40ml of deionized water, adding 800mg of lysine and 10mg of graphene oxide, uniformly stirring, putting into a hydrothermal kettle, reacting at 160 ℃ for 12 hours, washing with deionized water, and drying at 80 ℃ for 12 hours.
Mixing the obtained hydrothermal carbon and potassium hydroxide according to the mass ratio of 1:2, then placing the mixture into a tubular furnace, heating to 600 ℃ at the speed of 5 ℃/min under the argon atmosphere, keeping the temperature for 2h, cooling to room temperature, washing the mixture to be neutral by using deionized water, and drying the mixture for 12h at the temperature of 80 ℃ to obtain the two-dimensional nitrogen-doped porous carbon material. The nitrogen content was 6.7 wt.% and the specific surface area was 917m as measured by elemental analysis2/g。
The specific capacitance of the material can reach 301F/g under the condition of 0.5A/g by three-electrode test. Under the test of 1A/g, 2A/g, 5A/g and 10A/g, the specific capacitance is 287, 272, 259 and 242F/g, and the multiplying power retention is more than 80 percent.
Example 2
Dissolving 4g of sucrose in 40ml of deionized water, adding 2mg of serine and 40mg of graphene oxide, uniformly stirring, putting into a hydrothermal kettle, reacting at 180 ℃ for 12h, washing with deionized water, and drying at 80 ℃ for 12 h.
Mixing the obtained waterMixing hot carbon and potassium hydroxide according to the mass ratio of 1:4, then placing the mixture into a tubular furnace, heating the mixture to 800 ℃ at the speed of 2 ℃/min under the argon atmosphere, keeping the temperature for 2h, cooling the mixture to room temperature, washing the product to be neutral by using deionized water, and drying the product for 12h at 80 ℃ to obtain the two-dimensional nitrogen-doped porous carbon material. The nitrogen content is 3.7 wt.% and the specific surface area is 642m by element analysis test2/g
The specific capacitance of the material can reach 243F/g under the condition of 0.5A/g by three-electrode test.
Example 3
Dissolving 2g of glucose in 40ml of deionized water, adding 1.8g of glutamic acid and 40mg of graphene oxide, uniformly stirring, putting into a hydrothermal kettle, reacting for 24 hours at 150 ℃, washing with deionized water, and drying for 12 hours at 80 ℃.
Mixing the obtained hydrothermal carbon and potassium hydroxide according to the mass ratio of 1:2, then placing the mixture into a tubular furnace, heating the mixture to 700 ℃ at the speed of 1 ℃/min under the argon atmosphere, keeping the temperature for 2h, cooling the mixture to room temperature, washing the product to be neutral by using deionized water, and then drying the product for 12h at the temperature of 80 ℃ to obtain the two-dimensional nitrogen-doped porous carbon material. The nitrogen content was 5.1 wt.% as measured by elemental analysis. Specific surface area 784m2/g
The specific capacitance of the material can reach 261F/g under the condition of 0.5A/g by three-electrode test. Under the test conditions of 1A/g, 2A/g, 5A/g and 10A/g, the specific capacitance is 251, 237, 223 and 210F/g, and the rate retentivity is more than 80 percent
Example 4
Dissolving 1g of glucose in 40ml of deionized water, adding 1g of arginine and 20mg of graphene oxide, uniformly stirring, putting into a hydrothermal kettle for reaction at 180 ℃ for 6h, washing with deionized water, and drying at 80 ℃ for 12 h.
Mixing the obtained hydrothermal carbon and potassium hydroxide according to the mass ratio of 1:1, then placing the mixture into a tubular furnace, heating the mixture to 800 ℃ at the speed of 1 ℃/min under the argon atmosphere, then keeping the temperature for 4 hours, cooling the mixture to room temperature, washing the product to be neutral by using deionized water, and drying the product for 12 hours at the temperature of 80 ℃ to obtain the two-dimensional nitrogen-doped porous carbon material. The nitrogen content was 4.0 wt.% as measured by elemental analysis. Proportion tableArea 708m2/g
Example 5
Dissolving 1g of fructose in 40ml of deionized water, adding 2g of lysine and 50mg of graphene oxide, uniformly stirring, putting into a hydrothermal kettle for reaction at 160 ℃ for 12 hours, washing with deionized water, and drying at 80 ℃ for 12 hours.
Mixing the obtained hydrothermal carbon and potassium hydroxide according to the mass ratio of 1:2, then placing the mixture into a tubular furnace, heating to 600 ℃ at the speed of 5 ℃/min under the argon atmosphere, keeping the temperature for 2h, cooling to room temperature, washing the product to be neutral by using deionized water, and then drying for 12h at 80 ℃ to obtain the two-dimensional nitrogen-doped porous carbon material. The nitrogen content is 7.2 wt.% and the specific surface area is 878m by element analysis test2/g
The specific capacitance of the material can reach 313F/g under the condition of 0.5A/g by three-electrode test. Under the test conditions of 1A/g, 2A/g, 5A/g and 10A/g, the specific capacitance is 305, 295, 283 and 270F/g, and the multiplying power retention is more than 85 percent.
Example 6
Dissolving 1g of fructose in 40ml of deionized water, adding 600mg of serine and 50mg of graphene oxide, uniformly stirring, putting into a hydrothermal kettle for reaction at 160 ℃ for 12 hours, washing with deionized water, and drying at 80 ℃ for 12 hours.
Mixing the obtained hydrothermal carbon and potassium hydroxide according to the mass ratio of 1:2, then placing the mixture into a tubular furnace, heating the mixture to 600 ℃ at the speed of 5 ℃/min under the argon atmosphere, then keeping the temperature for 2h, cooling the mixture to room temperature, washing the product to be neutral by using deionized water, and drying the product for 12h at the temperature of 80 ℃ to obtain the two-dimensional nitrogen-doped porous carbon material. The nitrogen content reaches 5.5 wt.% and the specific surface area is 765m through element analysis test2/g
The specific capacitance of the material can reach 265F/g under the condition of 0.5A/g by three-electrode test. Under the test conditions of 1A/g, 2A/g, 5A/g and 10A/g, the specific capacitance is 256, 244, 230 and 209F/g, and the rate retentivity is over 75 percent
Example 7
Dissolving 1g of fructose in 40ml of deionized water, adding 700mg of lysine and 30mg of graphene oxide, uniformly stirring, putting into a hydrothermal kettle, reacting at 150 ℃ for 24 hours, washing with deionized water, and drying at 80 ℃ for 12 hours.
Mixing the obtained hydrothermal carbon and potassium hydroxide according to the mass ratio of 1:2, then placing the mixture into a tubular furnace, heating to 600 ℃ at the speed of 3 ℃/min under the argon atmosphere, keeping the temperature for 2h, cooling to room temperature, using deionized washing water to neutralize the product, and drying at 80 ℃ for 12h to obtain the two-dimensional nitrogen-doped porous carbon material. The nitrogen content reaches 6.0 wt.% and the specific surface area is 828m by element analysis test2/g
The specific capacitance of the material can reach 277F/g under the condition of 0.5A/g by three-electrode test. Under the test conditions of 1A/g, 2A/g, 5A/g and 10A/g, the specific capacitance is 270, 259, 246 and 230F/g, and the rate retentivity is more than 80 percent.
Example 8
Dissolving 8g of fructose in 80ml of deionized water, adding 4g of lysine and 80mg of graphene oxide, uniformly stirring, putting into a hydrothermal kettle for reaction at 160 ℃ for 12 hours, washing with deionized water, and drying at 80 ℃ for 12 hours.
Mixing the obtained hydrothermal carbon and potassium hydroxide according to the mass ratio of 1:4, then placing the mixture into a tubular furnace, heating to 600 ℃ at the speed of 5 ℃/min under the argon atmosphere, keeping the temperature for 2h, cooling to room temperature, washing the product to be neutral by using deionized water, and then drying for 12h at 80 ℃ to obtain the two-dimensional nitrogen-doped porous carbon material. The nitrogen content reached 4.1 wt.% as measured by elemental analysis. Specific surface area 719m2/g。
Claims (2)
1. A preparation method of a two-dimensional nitrogen-doped porous carbon material for a supercapacitor electrode is characterized by comprising the following steps:
(a) preparing 0.025-0.1 g/mL of biomass saccharide aqueous solution, adding graphene oxide according to the mass ratio of the biomass saccharide to the graphene oxide of 1: 0.01-1: 0.05, adding amino acid according to the mass ratio of the biomass saccharide to the amino acid of 1: 0.5-1: 2, putting the mixture into a hydrothermal kettle, reacting for 6-24 hours at the temperature of 150-180 ℃, washing with deionized water after the reaction is finished, and drying at the temperature of 80 ℃ to obtain hydrothermal carbon; the biomass saccharide is fructose, glucose or sucrose; the amino acid is lysine, glutamic acid, serine or arginine;
(b) taking the hydrothermal carbon prepared in the step (a) as a raw material, mixing the hydrothermal carbon and potassium hydroxide according to a mass ratio of 1: 1-1: 4, raising the temperature to 600-800 ℃ at a speed of 1-5 ℃/min, reacting for 2-4 h, washing to be neutral by using deionized water, and drying at 80 ℃ for 12h to obtain the two-dimensional nitrogen-doped porous carbon material.
2. The method according to claim 1, wherein the graphene oxide is prepared by Hummers' method.
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