CN110517900B - Preparation method of nitrogen-doped low-temperature carbon nanofiber electrode material for supercapacitor - Google Patents
Preparation method of nitrogen-doped low-temperature carbon nanofiber electrode material for supercapacitor Download PDFInfo
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- 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
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Abstract
The invention discloses a preparation method of a nitrogen-doped low-temperature carbon nanofiber electrode material for a supercapacitor. The low-temperature carbon nanofiber in the electrode material has a developed micropore and mesoporous structure, can adsorb a large amount of electrolyte ions, has high specific capacity, and the nitrogen-containing functional groups doped on the surface of the carbon fiber material improve the wettability of the material and increase the utilization rate of the specific surface area, change the local charge density and improve the conductivity, and the nitrogen-containing functional groups can also perform redox reaction to generate pseudo capacitance and further improve the capacitance performance. The electrode material has high specific capacity, excellent rate performance and cycling stability, simple and easy synthetic process, no need of electrostatic spinning, low cost, high yield and good application prospect in the super capacitor.
Description
Technical Field
The invention belongs to the technical field of super capacitors, and particularly relates to a preparation method of a nitrogen-doped low-temperature carbon nanofiber electrode material for a super capacitor.
Background
Because of the increasing shortage of non-renewable energy sources such as petroleum, and the pollution of tail gas generated by burning petroleum to the environment is becoming serious. Researchers in various countries around the world are looking for new energy devices that clean energy and utilize energy more efficiently. The super capacitor as a novel energy storage device has the characteristics of large specific capacity, high power density, long cycle life, wide operating temperature, environmental friendliness and the like, is widely applied to the fields of electronics, energy, transportation, aerospace and national defense, and has become a focus of attention of global researchers.
Compared with conventional batteries, supercapacitors have high power density but low energy density, and it remains a challenge to develop high energy density, low cost electrode materials and their better applications in supercapacitors. How to improve the energy density characteristics has been the focus. From E =1/2CV2It is known that the improvement of the energy density of the capacitor can be started from the improvement of the capacitance (C) of the electrode material, and therefore, further research and further development of the electrode material are requiredAnd (5) development. The carbon material has the characteristics of high specific surface area, controllable pore structure, high electric conductivity, thermal conductivity and the like, and the activated carbon has simple preparation process, wide and easy raw material sources, and wide application in the fields of electrochemical energy storage, adsorption, catalysis and the like.
At present, the capacitance of the activated carbon is improved mainly by increasing the specific surface area of the activated carbon. For example, patent CN201510004277.6 discloses a method for preparing porous carbon, which comprises reacting polycarboxylic acid and diamine or acetic anhydride and diamine as reactants in a metal salt solution to form a three-dimensional network prepolymer, and performing heat treatment to obtain porous carbon, wherein the specific surface area of the prepared porous carbon is 300-450 m/g, and the specific capacitance is 189F/g at a current density of 0.1A/g, which is poor in electrochemical performance, because the porous carbon has a larger specific surface area but contributes to ultra-fine micropores with undersized pore diameters, and the capacitor mainly depends on electrolyte ions entering pores of activated carbon to form an electric double layer for storing charges, and the electrolyte ions are difficult to enter the ultra-fine micropores, and the surface areas corresponding to the micropores become ineffective surface areas, resulting in a lower specific capacitance.
The carbon nanofiber has good physical properties and chemical properties, such as large specific surface area, high mechanical strength and Young modulus, and the electric and heat conducting properties of the carbon nanofiber are comparable to those of graphite, so that the carbon nanofiber has a huge application prospect in flexible wearable energy storage devices. For example, the invention patent CN201910010104.3 discloses a self-supporting flexible supercapacitor electrode material and a preparation method thereof, firstly, a mixed solution of polyphosphazene and a polymer is prepared, then, the mixed solution is used for preparing a polymer/polyphosphazene nanofiber membrane by an electrostatic spinning method, the obtained polymer/polyphosphazene nanofiber membrane is subjected to high-temperature carbonization and potassium hydroxide activation processes to obtain a nitrogen-phosphorus-doped self-supporting flexible carbon nanofiber membrane, and the specific capacitance can reach 176F/g; angew chem.int.Ed.,2012,51,5101-5105 discloses that Te nano-wires are used as templates, hydrothermal reaction is carried out in glucose solution at 180 ℃ to obtain carbon nano-fibers, wherein the Te nano-wire templates need to be etched and removed at the later stage, and when the carbon nano-fibers are assembled into a super capacitor electrode material, the specific capacity of the super capacitor electrode material is 202F/g under the current density of 1A/g; J.mater. chem.A.2013, 1,9449-9455 discloses that a phenolic resin is used as a precursor, and SiO is used as2The mesoporous carbon nanofiber is synthesized by the hard template in a hydrothermal mode, and the specific capacity of the mesoporous carbon nanofiber is 276F/g under the current density of 0.5A g. However, the method has complex synthetic process, large energy consumption and high cost, is not suitable for large-scale popularization, and has low specific capacity and low energy density when being used as a super capacitor electrode material, thereby limiting the practical application of the method.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a nitrogen-doped low-temperature carbon nanofiber electrode material for a supercapacitor, and solves the problems of low specific capacitance, low energy density of the capacitor, complex synthesis process, high energy consumption and high cost of the conventional electrode material.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of a nitrogen-doped low-temperature carbon nanofiber electrode material for a supercapacitor comprises the following steps:
1) placing a catalyst in a heating pipe, heating to 240-280 ℃ under the nitrogen atmosphere, introducing a carbon source gas, and cooling to room temperature under the protection of nitrogen after the reaction is finished to obtain low-temperature carbon nanofibers;
2) mixing the low-temperature carbon nanofiber obtained in the step 1) with strong base, activating at high temperature under the protection of nitrogen, cooling to room temperature after the reaction is finished, and performing suction filtration, washing and drying to obtain activated carbon nanofiber;
3) mixing the activated carbon nanofiber obtained in the step 2) with a nitrogen-containing polymer, then placing the mixture in a heating pipe, sintering the mixture in a nitrogen atmosphere, cooling to room temperature after the reaction is finished, then placing the sintered product in a strong acid solution for acidification, and then performing suction filtration, washing and drying to obtain the nitrogen-doped low-temperature carbon nanofiber electrode material.
Further, the catalyst is nickel powder, copper tartrate or ferrous tartrate.
Further, the carbon source is one or more of methane, ethylene, acetylene and propylene.
Further, the mass ratio of the low-temperature carbon nanofibers to the strong base is 1:1 to 3.
Further, the activation temperature is 700-900 ℃, and the activation time is 1-2 h.
Further, the ratio of carbon to nitrogen in the activated carbon nanofibers and the nitrogen-containing polymer is 1-3: 1.
Further, the nitrogen-containing polymer is at least one compound of polyaniline, amino acid, melamine, chitosan or polyacrylamide. Therefore, the nitrogen content is high, and meanwhile, the nitrogen-containing polymer can generate partial carbon to be fully utilized to improve the specific capacitance, so that the energy density of the capacitor is effectively improved.
Further, the sintering temperature is 600-800 ℃, and the sintering time is 1-2 h.
Further, the strong acid is concentrated nitric acid, and the acidification time is 1-2 h.
The invention also provides a lithium battery, which comprises the nitrogen-doped low-temperature carbon nanofiber electrode material for the supercapacitor prepared by the method.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the nitrogen-doped low-temperature carbon nanofiber electrode material prepared by the invention, the low-temperature carbon nanofiber is prepared by adopting a low-temperature deposition method, and the obtained low-temperature carbon nanofiber has the characteristic of a spiral structure (mainly comprising amorphous carbon and a plurality of fullerene interlamination inclusion bodies), so that the structure is favorable for full contact of electrolyte ions and the electrode material, the electrolyte ions can be effectively transmitted in the whole electrode, and the storage of charges is increased. In addition, the structure not only can enable the carbon fiber to have the advantages of larger specific surface area, smaller density, good heat conduction and electric conductivity and the like, but also enables the nano-scale graphite sheet layer to be twisted due to the spiral, and microcracks are generated to form defects while the graphite sheet layer is spiral, so that the specific surface area is greatly improved, the electrochemical performance is good, and the specific capacitance is further improved. And then, under the action of strong alkali, the surface of the carbon nano fiber is subjected to high-temperature activation, and the high-temperature activation is performed relative to the normal temperature, so that deep etching is favorably realized, superfine micropores are avoided, the material performance is fully exerted and utilized, the specific surface area of the low-temperature carbon nano fiber is improved through etching, the surface activity of the low-temperature carbon nano fiber is activated through acidification, the later nitrogen doping amount is favorably improved, the pseudo capacitance is further provided, and the energy density of the capacitor can be effectively improved.
2. In the nitrogen-doped low-temperature carbon nanofiber electrode material obtained by the invention, the low-temperature carbon nanofiber has a developed micropore and mesoporous structure, can adsorb a large amount of electrolyte ions, has high specific capacity, and the nitrogen-containing functional groups doped on the surface of the carbon nanofiber material can improve the wettability of the material, increase the utilization rate of the specific surface area, change the local charge density, improve the conductivity, and can also perform redox reaction to generate pseudo capacitance so as to further improve the capacitance performance. The electrode material prepared by the invention has a specific capacitance value of 257.02F/g under the current density of 1A/g, and is improved by 20% compared with the gas specific capacity of carbon nanofibers which are not doped with nitrogen, even under the heavy current density of 50A/g, the specific capacitance can still maintain 168.77F/g and 65.66%, and the electrode material has high specific capacity, excellent rate capability and cycling stability, which are attributed to the fact that the specific surface area of the carbon nanofibers is larger, and the surface porosity of the carbon nanofibers is increased by the etching of strong base on the surfaces of the carbon nanofibers in the activation process, so that a stable interface film is formed between electrolyte and an electrode, ions can be transferred in or out in a reversible manner on the interface, and the electrode material has good structural stability and better practical applicability, and has good application prospect when being used as the electrode material of a super capacitor.
3. The invention has simple and easy operation of the synthesis process, no need of electrostatic spinning, low cost, high yield, low temperature in the chemical deposition reaction process, low energy consumption, no need of subsequent treatment procedures and more suitability for industrial popularization.
Drawings
FIG. 1 is an SEM image of activated carbon nanofibers prepared according to the present invention;
FIG. 2 is a Raman spectrum of the nitrogen-doped low-temperature carbon nanofiber electrode material prepared in examples 1 to 3;
FIG. 3 is a comparison of electrochemical properties of the nitrogen-doped low-temperature carbon nanofiber electrode materials prepared in examples 1-3; FIG. a is a GCD curve at a current density of 1A/g, and FIG. b is a specific capacitance at a current density of 1A/g.
Detailed Description
The present invention will be described in further detail with reference to the following specific embodiments and the accompanying drawings. The experimental procedures are not specifically described in the following examples, and are carried out in a conventional manner using reagents which are generally commercially available.
Preparation method of nitrogen-doped low-temperature carbon nanofiber electrode material for supercapacitor
Example 1
1) Putting a powder catalyst copper tartrate in a quartz boat, uniformly paving, putting the quartz boat in a heating tube, heating to 240 ℃ under the protection of high-purity nitrogen, introducing acetylene, keeping the temperature for 1h, cooling to room temperature under the protection of nitrogen after the reaction is finished, and taking out a sample to obtain the low-temperature carbon nanofiber.
2) Accurately weighing the low-temperature carbon nanofibers obtained in the step 1) and KOH according to the mass ratio of 1:1, heating to 800 ℃ under the protection of high-purity nitrogen, activating for 1h, adding a large amount of distilled water, filtering through a sand core funnel to obtain a precipitate, repeatedly cleaning the precipitate with distilled water and absolute ethyl alcohol until the solution is neutral, and finally drying in a vacuum drying oven at 80 ℃ to obtain the activated carbon nanofibers.
3) Putting the activated carbon nanofiber obtained in the step 2) and the melamine nitrogenous polymer into a quartz boat according to the nitrogen-carbon ratio of 1:1, putting the quartz boat into a heating tube, introducing nitrogen, removing air in the tube, heating to 600 ℃, preserving heat for 1h, cooling to room temperature after the reaction is finished, and taking out a sample to obtain a precursor.
4) Transferring the precursor prepared in the step 3) into a beaker, carrying out acidification treatment for 2h by using a proper amount of concentrated nitric acid, finally filtering through a sand core funnel to obtain a precipitate, then repeatedly cleaning the precipitate by using distilled water and absolute ethyl alcohol until the solution is neutral, and then drying in a vacuum drying oven at 80 ℃ to obtain the high-purity nitrogen-doped low-temperature carbon nanofiber.
Example 2
1) Putting a powder catalyst copper tartrate in a quartz boat, uniformly paving, putting the quartz boat in a heating tube, heating to 260 ℃ under the protection of high-purity nitrogen, introducing acetylene, keeping the temperature for 1h, cooling to room temperature under the protection of nitrogen after the reaction is finished, and taking out a sample to obtain the low-temperature carbon nanofiber.
2) Accurately weighing the low-temperature carbon nanofibers obtained in the step 1) and KOH according to the mass ratio of 1:2, heating to 800 ℃ under the protection of high-purity nitrogen, activating for 3 hours, adding a large amount of distilled water, filtering through a sand core funnel to obtain a precipitate, repeatedly cleaning the precipitate with distilled water and absolute ethyl alcohol until the solution is neutral, and finally drying in a vacuum drying oven at 80 ℃ to obtain the activated carbon nanofibers.
3) Putting the activated carbon nanofiber obtained in the step 2) and the melamine nitrogenous polymer into a quartz boat according to the nitrogen-carbon ratio of 2:1, putting the quartz boat into a heating tube, introducing nitrogen, removing air in the tube, heating to 800 ℃, preserving heat for 1h, cooling to room temperature after the reaction is finished, and taking out a sample to obtain a precursor.
4) Transferring the precursor prepared in the step 3) into a beaker, carrying out acidification treatment for 2h by using a proper amount of concentrated nitric acid, finally filtering through a sand core funnel to obtain a precipitate, then repeatedly cleaning the precipitate by using distilled water and absolute ethyl alcohol until the solution is neutral, and then drying in a vacuum drying oven at 80 ℃ to obtain the high-purity nitrogen-doped low-temperature carbon nanofiber.
Example 3
1) Putting a powder catalyst copper tartrate in a quartz boat, uniformly paving, putting the quartz boat in a heating tube, heating to 280 ℃ under the protection of high-purity nitrogen, introducing acetylene, keeping the temperature for 1h, cooling to room temperature under the protection of nitrogen after the reaction is finished, and taking out a sample to obtain the low-temperature carbon nanofiber.
2) Accurately weighing the low-temperature carbon nanofibers obtained in the step 1) and KOH according to the mass ratio of 1:3, heating to 800 ℃ under the protection of high-purity nitrogen, activating for 2 hours, adding a large amount of distilled water, filtering through a sand core funnel to obtain a precipitate, repeatedly cleaning the precipitate with distilled water and absolute ethyl alcohol until the solution is neutral, and finally drying in a vacuum drying oven at 80 ℃ to obtain the activated carbon nanofibers.
3) Putting the activated carbon nanofiber obtained in the step 2) and the melamine nitrogenous polymer into a quartz boat according to the nitrogen-carbon ratio of 3:1, putting the quartz boat into a heating tube, introducing nitrogen, removing air in the tube, heating to 700 ℃, preserving heat for 1h, cooling to room temperature after the reaction is finished, and taking out a sample to obtain a precursor.
4) Transferring the precursor prepared in the step 3) into a beaker, carrying out acidification treatment for 2h by using a proper amount of concentrated nitric acid, finally filtering through a sand core funnel to obtain a precipitate, then repeatedly cleaning the precipitate by using distilled water and absolute ethyl alcohol until the solution is neutral, and then drying in a vacuum drying oven at 80 ℃ to obtain the high-purity nitrogen-doped low-temperature carbon nanofiber.
Comparative example 1
The reaction temperature in step 1) was 700 ℃ and the other steps were the same as in example 1.
Comparative example 2
The nitrogen-containing polymer in step 3) was replaced with ammonia gas, and the other steps were the same as in example 1.
Second, performance verification
1. The nitrogen-doped carbon nanofibers prepared in examples 1 to 3 and comparative examples 1 to 2 were subjected to specific capacitance analysis at different current densities.
TABLE 1 specific capacitance of different N-doped carbon nanofibers at different current densities
| 1 A·g-1 | 10 A·g-1 | 50 A· |
1~10 A·g-1Retention rate | 1~50 A·g-1Retention rate | |
| CNF | 214.85 | 175 | 135 | 81.45 % | 62.83 % |
| Example 1 | 232.6 | 203.88 | 161.01 | 87.65 % | 69.22 % |
| Example 2 | 257.02 | 221.6 | 168.77 | 86.22 % | 65.66 % |
| Example 3 | 244.44 | 196.82 | 99.8 | 80.52 % | 40.91 % |
| Comparative example 1 | 231.50 | 156.40 | - | 65.85 % | - |
| Comparative example 2 | 180.00 | 140.00 | - | 77.78% | - |
Note: "-" indicates none.
As can be seen from Table 1, compared with a comparative example, the specific capacitance value of the nitrogen-doped low-temperature nano spiral carbon fiber electrode material obtained by the invention can reach 257.02F/g at a current density of 1A/g, the capacity of the electrode material is improved by 20% compared with that of a low-temperature Carbon Nanofiber (CNF) without nitrogen doping, and even at a high current density of 50A/g, the specific capacitance can still retain 168.77F/g-65.66% is kept, and the carbon nanofiber has high specific capacity, excellent multiplying power performance and circulation stability, mainly because the low-temperature carbon nanofiber has a spiral structure and a developed micropore and mesoporous structure, can adsorb a large amount of electrolyte ions, and has high specific capacity, and the nitrogen-containing functional groups doped on the surface of the carbon fiber material by using melamine can improve the wettability of the material and increase the utilization rate of the specific surface area, and can also change the local charge density and improve the conductivity, and the nitrogen-containing functional groups can also carry out redox reaction to generate pseudo capacitance, thereby further improving the capacitance performance.
2. The activated carbon nanofibers prepared according to the present invention were observed under a scanning electron microscope, and the results are shown in fig. 1.
As can be seen from the figure, the carbon nanofibers have smooth surfaces and uniform diameter distribution, and are prepared by a chemical vapor deposition method at a low temperature, and part of the carbon nanofibers have a micro-spiral structure, so that electrolyte ions can be in full contact with electrode materials, the electrolyte ions can be effectively transmitted in the whole electrode, the storage capacity of charges is increased, and the specific capacity of the supercapacitor is further improved.
3. The results of raman spectroscopy analysis of the nitrogen-doped low-temperature carbon nanofibers prepared in examples 1 to 3 are shown in fig. 2.
As can be seen from FIG. 2, the D peak appears at 1320 cm-1~1350 cm-1G peak appears at 1560 cm-1~1590 cm-1In the meantime. Through observation and analysis, doping nitrogen can effectively increase I of carbon fiberDValue and IGValue, but as the nitrogen to carbon ratio increases, I of the carbon fiberDThe value will increase continuously, but IGThe value is continuously reduced, which is beneficial to improving the degree of graphite lattice defects, thereby improving the conductivity of the material.
4. The nitrogen-doped low-temperature carbon nanofibers prepared in examples 1 to 3 were subjected to electrochemical test analysis, and the results are shown in fig. 3.
As can be seen from FIG. 3, the specific capacitance of the material subjected to nitrogen doping is greatly improved, wherein the specific capacitance is higher when the nitrogen-carbon ratio is 2: 1. The reason is that after the nitrogen atoms are doped into the graphite crystal lattice, the graphite crystal lattice defects are increased, the density of the graphite crystal lattice defects is improved, the graphite crystal lattice defects serve as electron donors to obviously improve the conductivity of the carbon fibers, but when the defects reach a certain degree, the defects can block the migration of electrons in the material, and the defects have a larger influence on the comparative capacitance.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (2)
1. A preparation method of a nitrogen-doped low-temperature carbon nanofiber electrode material for a supercapacitor is characterized by comprising the following steps:
1) putting a powder catalyst copper tartrate in a quartz boat, uniformly paving, putting the quartz boat in a heating tube, heating to 240 ℃ under the protection of high-purity nitrogen, introducing acetylene, keeping the temperature for 1h, cooling to room temperature under the protection of nitrogen after the reaction is finished, and taking out a sample to obtain low-temperature carbon nanofiber;
2) accurately weighing the low-temperature carbon nanofibers obtained in the step 1) and KOH according to the mass ratio of 1:1, heating to 800 ℃ under the protection of high-purity nitrogen, activating for 1h, adding a large amount of distilled water, filtering through a sand core funnel to obtain a precipitate, repeatedly cleaning the precipitate with distilled water and absolute ethyl alcohol until the solution is neutral, and finally drying in a vacuum drying oven at 80 ℃ to obtain activated carbon nanofibers;
3) putting the activated carbon nanofiber obtained in the step 2) and the melamine nitrogenous polymer into a quartz boat according to the nitrogen-carbon ratio of 1:1, putting the quartz boat into a heating tube, introducing nitrogen, removing air in the tube, heating to 600 ℃, preserving heat for 1h, cooling to room temperature after the reaction is finished, and taking out a sample to obtain a precursor;
4) transferring the precursor prepared in the step 3) into a beaker, carrying out acidification treatment for 2h by using a proper amount of concentrated nitric acid, finally filtering through a sand core funnel to obtain a precipitate, then repeatedly cleaning the precipitate by using distilled water and absolute ethyl alcohol until the solution is neutral, and then drying in a vacuum drying oven at 80 ℃ to obtain the high-purity nitrogen-doped low-temperature carbon nanofiber.
2. A capacitor comprising the nitrogen-doped low-temperature carbon nanofiber electrode material for the supercapacitor prepared by the method of claim 1.
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