CN115995348A - Three-dimensional electrode material applied to super capacitor and preparation method thereof - Google Patents
Three-dimensional electrode material applied to super capacitor and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of new energy materials, and discloses a three-dimensional electrode material applied to a supercapacitor and a preparation method thereof, wherein the three-dimensional electrode material comprises a nitrogen-containing doped three-dimensional graphite-like material and active brilliant blue KN-R, wherein the nitrogen-containing doped three-dimensional graphite-like material is prepared by taking fructose and dicyandiamide as raw materials to prepare a premix, then soaking melamine sponge in the premix, and finally preparing the nitrogen-containing doped three-dimensional graphite-like material through high-temperature pyrolysis, and the nitrogen-containing doped three-dimensional graphite-like material has higher specific surface area and excellent electrochemical properties such as conductivity and the like; the active brilliant blue KN-R and the nitrogen-doped three-dimensional graphite-like material are combined by a solvothermal method under the pi-pi stacking effect of the active brilliant blue KN-R and the nitrogen-doped three-dimensional graphite-like material, and the prepared three-dimensional electrode material has good conductivity, excellent specific capacitance performance and strong cycling stability, and is beneficial to realizing application in the electrode material of the super capacitor.
Description
Technical Field
The invention relates to the technical field of new energy materials, in particular to a three-dimensional electrode material applied to a supercapacitor and a preparation method thereof.
Background
Under the background of the increasing global energy consumption, the continuous exhaustion of fossil energy and the increasing environmental pollution, the strong development of clean energy is becoming the mainstream, therefore, the energy storage and conversion device is applied in large scale, the super capacitor is more and more researched with high power density and excellent cycle stability, the super capacitor is mainly divided into an electric double layer capacitor and a Faraday capacitor according to the difference of energy storage mechanism, the electrode materials used by different types of capacitors are different, the electric double layer capacitor is mainly used for realizing electric energy storage by orderly separating double layer charges between carbon electrode materials such as active carbon, graphene or carbon nano tube and electrolyte, the Faraday capacitor is mainly used for storing electric energy by generating oxidation-reduction reaction on electrode materials such as organic compounds, metal oxides or conductive polymers, the electrode materials of the electric double layer capacitor and the electrode materials of the Faraday capacitor are compounded, and the electrode materials of the capacitor with high energy density are prepared by the synergistic effect among the electrode materials of the super capacitor, and one of the main directions of research in the research field of super capacitor in recent years.
The invention patent in China with the application number of CN201610768005.8 discloses a nickel hydroxide/graphene nanocomposite and a preparation method thereof, a supercapacitor electrode and a supercapacitor, wherein the nickel hydroxide/graphene nanocomposite which is flaky and three-dimensional porous is prepared by a hydrothermal method, the electrode material not only has the high cycle life, high power density and high stability of an electric double layer capacitor, but also has the high specific capacitance characteristic of a Faraday capacitor, so that the supercapacitor has excellent comprehensive performance, but the production and storage cost of metal elements such as nickel and the like are higher, and nickel belongs to heavy metal elements, and heavy metal pollution is inevitably caused by large-scale use, so that the environment protection is not facilitated, and therefore, the development of a novel electrode material which can combine the excellent performance of the electric double layer capacitor and the Faraday capacitor, has lower cost and can not cause heavy metal environment pollution is particularly important.
Disclosure of Invention
The invention aims to provide a three-dimensional electrode material applied to a supercapacitor and a preparation method thereof, and solves the problems of lower specific capacitance and poor cycling stability of the traditional supercapacitor electrode material.
The three-dimensional electrode material applied to the supercapacitor comprises the following raw materials in parts by weight: 10-20 parts of nitrogen-containing doped three-dimensional graphite-like material and 10-20 parts of active brilliant blue KN-R;
the preparation method of the nitrogen-containing doped three-dimensional graphite-like material comprises the following steps:
s1: adding fructose and dicyandiamide into purified water, uniformly mixing, and preserving heat for 1-2 hours at the temperature of 70-80 ℃ to obtain a premix;
s2: immersing melamine sponge into the premix prepared in the step S1, transferring the melamine sponge into a freeze dryer, and freeze-drying for 24-48 hours to obtain a precursor;
s3: and (3) placing the precursor prepared in the step (S2) in a tube furnace, raising the temperature to perform high-temperature solid-phase reaction, and grinding and crushing the material after the material is cooled to room temperature to obtain the nitrogen-doped three-dimensional graphite-like material.
Further, in the step S1, the mass ratio of the fructose to the dicyandiamide is 0.1-0.2:1.
Further, in step S2, the melamine sponge has a density of 8kg/m 3 -10kg/m 3 。
Further, in the step S2, the volume ratio of the melamine sponge to the premix is 1:1-3.
Further, in the step S3, the temperature is raised to 500-600 ℃ at a heating rate of 1-5 ℃/min during the solid phase reaction, the temperature is kept for 1-2h, the temperature is continuously raised to 700-800 ℃, and the temperature is kept for 1-2h.
According to the technical scheme, after fructose and dicyandiamide are mixed to form the premix, fructose and dicyandiamide can flow into pores of melamine sponge in an infiltration mode, after freeze drying, fructose and dicyandiamide components in the premix can be locked into the melamine sponge, the melamine sponge can be subjected to polycondensation in a high-temperature environment to form a three-dimensional interconnected carbon nitride frame, dicyandiamide can form lamellar carbon nitride in the high-temperature environment and exist in the three-dimensional interconnected carbon nitride frame, the lamellar carbon nitride can provide a template for an aromatic carbon intermediate product generated by interaction of hydroxyl groups and other functional groups in the fructose, growth of the aromatic carbon intermediate is facilitated, after the temperature is further improved, the lamellar carbon nitride is pyrolyzed, and can be simultaneously doped into the aromatic carbon intermediate as a nitrogen source, and a three-dimensional structure with pore morphology is formed in the aromatic carbon intermediate along with an impact expansion effect generated by gas release, so that the nitrogen-containing doped three-dimensional graphite-like material is finally formed.
The preparation method of the three-dimensional electrode material applied to the super capacitor comprises the following steps:
SS1: adding active brilliant blue KN-R into N, N-dimethylformamide, stirring uniformly, adding a nitrogen-containing doped three-dimensional graphite-like material, and performing ultrasonic dispersion to obtain uniform dispersion;
SS2: and (3) placing the dispersion liquid into a reaction kettle, placing the reaction kettle into an oven, raising the temperature to perform reaction, pouring out materials after the reaction is finished, centrifugally separating a solid product, washing the solid product by using purified water and ethanol, and placing the solid product into a vacuum drying oven to perform drying to obtain the nitrogen-doped three-dimensional graphite-like material loaded with active brilliant blue KN-R, namely the three-dimensional electrode material.
According to the technical scheme, the nitrogen-doped three-dimensional graphite-like material is taken as a framework, and the active brilliant blue KN-R structure contains a plurality of conjugated benzene ring structures, so that the active brilliant blue KN-R can be adsorbed on the surface of the nitrogen-doped three-dimensional graphite-like material framework through stronger pi-pi stacking effect by using a solvothermal method, oxidation-reduction reaction can be carried out on the active brilliant blue KN-R, and the electric double layer capacitance characteristic of the three-dimensional graphite-like material is matched, so that the organic combination of the electric double layer capacitor electrode material and the Faraday capacitor electrode material is realized, and the three-dimensional electrode material is prepared.
Further, in step SS1, the ultrasonic frequency is set to be 60-80kHz and the ultrasonic time is set to be 20-30min during ultrasonic dispersion.
Further, in the step SS2, the temperature of the reaction is 170-180 ℃ and the time is 6-18h.
The invention has the beneficial effects that: the three-dimensional conductive network of the nitrogen-doped three-dimensional graphite-like material prepared by the method is beneficial to electron transmission and electrolyte ion diffusion, can show more excellent electric double layer capacitance performance, has rich pore structures, is beneficial to exposing more electrochemical active energy storage sites on the surface on one hand, and is beneficial to loading more active brilliant blue KN-R molecules on the other hand due to the pore structures, so that more redox active sites are generated, more pseudo-capacitance is provided, and meanwhile, active defect structures such as pyridine nitrogen, graphite nitrogen, pyrrole nitrogen and the like can be formed in a matrix due to the doping of nitrogen elements in the three-dimensional graphite-like material, so that the conductivity, the specific capacitance and the other electrochemical activities of the three-dimensional graphite-like material are further improved.
According to the invention, the nitrogen-doped three-dimensional graphite-like material is taken as a framework, the active brilliant blue KN-R molecules are adsorbed on the surface of the nitrogen-doped three-dimensional graphite-like material through the stronger pi-pi stacking effect, the stronger stacking effect can enable the active brilliant blue KN-R molecules to have stronger interaction with the nitrogen-doped three-dimensional graphite-like material, the nitrogen-doped three-dimensional graphite-like material has higher specific surface area and excellent conductivity, a channel can be provided for charge transmission and transfer, the active brilliant blue KN-R molecules can realize faster redox reversible reaction, meanwhile, the active brilliant blue KN-R molecules can play a certain blocking effect, the nitrogen-doped three-dimensional graphite-like material can be prevented from mutually agglomerating, the negative influence on the electrochemical performance of the electrode material is caused, in addition, the active brilliant blue KN-R molecules contain benzene sulfonic acid groups, the hydrophilicity of the electrode material is improved, the electrolyte is facilitated, the utilization rate of the electrode material is improved, and the prepared electrode material has stable structure and stronger cycle stability.
Of course, it is not necessary for any one product to practice the invention to achieve all of the advantages set forth above at the same time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a thermogravimetric analysis diagram of the nitrogen-containing doped three-dimensional graphite-like material and the three-dimensional electrode material prepared in inventive examples 1-3;
FIG. 2 is a scanning electron microscope image of the nitrogen-doped three-dimensional graphite-like material prepared in example 1 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The three-dimensional electrode material applied to the supercapacitor comprises the following raw materials in parts by weight: 10 parts of nitrogen-containing doped three-dimensional graphite-like material and 10 parts of reactive brilliant blue KN-R;
the preparation method of the three-dimensional electrode material applied to the super capacitor comprises the following steps:
SS1: adding active brilliant blue KN-R into N, N-dimethylformamide, stirring uniformly, adding a nitrogen-containing doped three-dimensional graphite-like material, and performing ultrasonic dispersion for 20min at ultrasonic frequency of 60kHz to obtain uniform dispersion;
SS2: placing the dispersion liquid into a reaction kettle, placing the reaction kettle into an oven, raising the temperature to 170 ℃, reacting for 6 hours, pouring out materials after the reaction is finished, centrifugally separating a solid product, washing the solid product by using purified water and ethanol, and placing the solid product into a vacuum drying oven for drying to obtain a nitrogen-doped three-dimensional graphite-like material loaded with active brilliant blue KN-R, namely a three-dimensional electrode material;
the thermal gravimetric analysis was performed on the nitrogen-doped three-dimensional graphite-like material and the three-dimensional electrode material by using a BOS-TGA101 thermal gravimetric analyzer, and the test result is shown in FIG. 1, and as can be seen from FIG. 1, the active brilliant blue KN-R load of the three-dimensional electrode material is 19.1%.
The preparation method of the nitrogen-containing doped three-dimensional graphite-like material comprises the following steps:
s1: adding 0.15g of fructose and 1g of dicyandiamide into the purified water, uniformly mixing, and preserving the temperature for 2 hours at 70 ℃ to obtain a premix;
s2: immersing the melamine sponge into the premix prepared in the step S1, transferring the melamine sponge into a freeze dryer, and freeze-drying for 24 hours to obtain a precursor, wherein the density of the melamine sponge is 10kg/m3, and the volume ratio of the melamine sponge to the premix is 1:2;
s3: placing the precursor prepared in the step S2 into a tube furnace, heating to 500 ℃ at a heating rate of 3 ℃/min, preserving heat for 2 hours, continuously heating to 800 ℃, preserving heat for 2 hours, cooling the material to room temperature, and grinding and crushing to obtain the nitrogen-doped three-dimensional graphite-like material;
characterization is carried out by using a MX2600FE type scanning electron microscope, the result is shown in figure 2, and as can be seen from figure 2, the nitrogen-containing doped three-dimensional graphite-like material has a three-dimensional structure with rich pores; the specific surface area of the nitrogenous doped three-dimensional graphite-like material is 1529.7m tested by using an FBT-9 full-automatic specific surface area analyzer 2 G, exhibiting a large specific surface area; the conductivity of the nitrogen-doped three-dimensional graphite-like material is tested to be 151.9S/m by using an HFD-8100A-300KG conductivity tester, and the nitrogen-doped three-dimensional graphite-like material shows excellent conductivity.
Example 2
The three-dimensional electrode material applied to the supercapacitor comprises the following raw materials in parts by weight: 15 parts of nitrogen-containing doped three-dimensional graphite-like material and 18 parts of reactive brilliant blue KN-R;
the preparation method of the three-dimensional electrode material applied to the super capacitor comprises the following steps:
SS1: adding active brilliant blue KN-R into N, N-dimethylformamide, stirring uniformly, adding a nitrogen-containing doped three-dimensional graphite-like material, and performing ultrasonic dispersion at an ultrasonic frequency of 70kHz for 25min to obtain a uniform dispersion;
SS2: placing the dispersion liquid into a reaction kettle, placing the reaction kettle into an oven, raising the temperature to 175 ℃ for reaction for 12 hours, pouring out materials after the reaction is finished, centrifugally separating a solid product, washing the solid product by using purified water and ethanol, and placing the solid product into a vacuum drying oven for drying to obtain a nitrogen-doped three-dimensional graphite-like material loaded with active brilliant blue KN-R, namely a three-dimensional electrode material; the three-dimensional electrode material was also subjected to thermogravimetric analysis, and as can be seen from fig. 1, the active brilliant blue KN-R loading amount of the three-dimensional electrode material was 24.7%.
The preparation method of the nitrogen-doped three-dimensional graphite-like material is the same as in example 1.
Example 3
The three-dimensional electrode material applied to the supercapacitor comprises the following raw materials in parts by weight: 20 parts of nitrogen-containing doped three-dimensional graphite-like material and 20 parts of reactive brilliant blue KN-R;
the preparation method of the three-dimensional electrode material applied to the super capacitor comprises the following steps:
SS1: adding active brilliant blue KN-R into N, N-dimethylformamide, stirring uniformly, adding a nitrogen-containing doped three-dimensional graphite-like material, and performing ultrasonic dispersion for 30min at ultrasonic frequency of 80kHz to obtain uniform dispersion;
SS2: placing the dispersion liquid into a reaction kettle, placing the reaction kettle into an oven, raising the temperature to 180 ℃ for reaction for 18 hours, pouring out materials after the reaction is finished, centrifugally separating a solid product, washing the solid product by using purified water and ethanol, and placing the solid product into a vacuum drying oven for drying to obtain a nitrogen-doped three-dimensional graphite-like material loaded with active brilliant blue KN-R, namely a three-dimensional electrode material; the three-dimensional electrode material was also subjected to thermogravimetric analysis, and as can be seen from fig. 1, the active brilliant blue KN-R loading amount of the three-dimensional electrode material was 21.3%.
The preparation method of the nitrogen-doped three-dimensional graphite-like material is the same as in example 1.
Comparative example 1
The electrode material applied to the supercapacitor comprises the following raw materials in parts by weight: 15 parts of graphene and 15 parts of active brilliant blue KN-R;
the preparation method of the electrode material applied to the super capacitor comprises the following steps:
SS1: adding active brilliant blue KN-R into N, N-dimethylformamide, stirring uniformly, adding graphene, and performing ultrasonic dispersion at an ultrasonic frequency of 70kHz for 25min to obtain uniform dispersion;
SS2: and (3) placing the dispersion liquid into a reaction kettle, placing the reaction kettle into an oven, raising the temperature to 175 ℃, reacting for 12 hours, pouring out materials after the reaction is finished, centrifugally separating a solid product, washing the solid product by using purified water and ethanol, and placing the solid product into a vacuum drying oven for drying to obtain the graphene material loaded with the active brilliant blue KN-R, namely the electrode material.
Performance detection
The electrode materials prepared in the examples 1 to 3 and the comparative example 1 of the present invention were subjected to electrochemical performance test by using a three-electrode system, wherein the working electrode was prepared by dissolving an electrode material, acetylene black and polytetrafluoroethylene in a mass ratio of 8:1:1 with ethanol, grinding and mixing, coating the mixture on foam nickel of 1cm×1cm, drying and compacting the mixture, forming an inclusion calomel electrode as a reference electrode, a platinum sheet as a counter electrode, and 1mol/L H 2 SO 4 For the electrolyte composition of the three-electrode system, the specific capacitance of the three-electrode system at a current density of 1A/g and the capacitance retention after 10000 cycles were tested using a CHI760D electrochemical workstation, and the test results are shown in the following table:
as can be seen from the above table, the electrode materials prepared in examples 1 to 3 of the present invention have higher specific capacitance values, and meanwhile, the electrode material prepared in comparative example 1 has higher capacitance retention rate and shows good cycle stability, while the electrode material prepared in comparative example 1 uses graphene as a matrix, and has lower specific capacitance value, poorer capacitance retention rate and better cycle stability, presumably because the specific surface area of graphene is limited, more reactive brilliant blue KN-R molecules cannot be adsorbed, and thus, the specific capacitance is poorer.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (8)
1. The three-dimensional electrode material applied to the super capacitor is characterized by comprising the following raw materials in parts by weight: 10-20 parts of nitrogen-containing doped three-dimensional graphite-like material and 10-20 parts of active brilliant blue KN-R;
the preparation method of the nitrogen-containing doped three-dimensional graphite-like material comprises the following steps:
s1: adding fructose and dicyandiamide into purified water, uniformly mixing, and preserving heat for 1-2 hours at the temperature of 70-80 ℃ to obtain a premix;
s2: immersing melamine sponge into the premix prepared in the step S1, transferring the melamine sponge into a freeze dryer, and freeze-drying for 24-48 hours to obtain a precursor;
s3: and (3) placing the precursor prepared in the step (S2) in a tube furnace, raising the temperature to perform high-temperature solid-phase reaction, and grinding and crushing the material after the material is cooled to room temperature to obtain the nitrogen-doped three-dimensional graphite-like material.
2. The three-dimensional electrode material for super capacitor according to claim 1, wherein in step S1, the mass ratio of fructose to dicyandiamide is 0.1-0.2:1.
3. The three-dimensional electrode material for super capacitor according to claim 1, wherein in step S2, the melamine sponge has a density of 8kg/m 3 -10kg/m 3 。
4. The three-dimensional electrode material for super capacitor according to claim 1, wherein in step S2, the volume ratio of melamine sponge to premix is 1:1-3.
5. The three-dimensional electrode material for super capacitor according to claim 1, wherein in step S3, the temperature is raised to 500-600 ℃ at a temperature raising rate of 1-5 ℃/min, the temperature is kept for 1-2h, the temperature is continuously raised to 700-800 ℃, and the temperature is kept for 1-2h.
6. The three-dimensional electrode material applied to the super capacitor according to claim 1, wherein the preparation method of the three-dimensional electrode material comprises the following steps:
SS1: adding active brilliant blue KN-R into N, N-dimethylformamide, stirring uniformly, adding a nitrogen-containing doped three-dimensional graphite-like material, and performing ultrasonic dispersion to obtain uniform dispersion;
SS2: and (3) placing the dispersion liquid into a reaction kettle, placing the reaction kettle into an oven, raising the temperature to perform reaction, pouring out materials after the reaction is finished, centrifugally separating a solid product, washing the solid product by using purified water and ethanol, and placing the solid product into a vacuum drying oven to perform drying to obtain the nitrogen-doped three-dimensional graphite-like material loaded with active brilliant blue KN-R, namely the three-dimensional electrode material.
7. The three-dimensional electrode material for super capacitor according to claim 6, wherein in step SS1, the ultrasonic frequency is set to 60-80kHz and the ultrasonic time is set to 20-30min during the ultrasonic dispersion.
8. The three-dimensional electrode material for super capacitor as claimed in claim 6, wherein in step SS2, the reaction temperature is 170-180 ℃ and the reaction time is 6-18h.
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