CN111268673A - Preparation method of supercapacitor electrode material taking foamed nickel as template - Google Patents
Preparation method of supercapacitor electrode material taking foamed nickel as template Download PDFInfo
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- CN111268673A CN111268673A CN202010087235.4A CN202010087235A CN111268673A CN 111268673 A CN111268673 A CN 111268673A CN 202010087235 A CN202010087235 A CN 202010087235A CN 111268673 A CN111268673 A CN 111268673A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 127
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 63
- 239000007772 electrode material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 50
- 239000006260 foam Substances 0.000 claims abstract description 39
- 229920001661 Chitosan Polymers 0.000 claims abstract description 31
- 238000001035 drying Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000008367 deionised water Substances 0.000 claims abstract description 23
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 23
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 238000003763 carbonization Methods 0.000 claims abstract description 13
- 229960000583 acetic acid Drugs 0.000 claims abstract description 9
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 101710134784 Agnoprotein Proteins 0.000 claims abstract description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 6
- 238000002791 soaking Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- 238000010000 carbonizing Methods 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 24
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 11
- 229910052709 silver Inorganic materials 0.000 abstract description 8
- 239000004332 silver Substances 0.000 abstract description 8
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- 239000003990 capacitor Substances 0.000 description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 8
- 229910052593 corundum Inorganic materials 0.000 description 8
- 239000010431 corundum Substances 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 description 5
- 238000000967 suction filtration Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000013543 active substance Substances 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000004758 underpotential deposition Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/205—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- 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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- 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
- H01G11/30—Electrodes characterised by their material
-
- 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
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a preparation method of a supercapacitor electrode material taking foam nickel as a template, which comprises the following steps: firstly, mixing glacial acetic acid, deionized water and chitosan, and ultrasonically stirring to obtain a chitosan solution; turning over and drying the foam nickel sheet in a chitosan solution, then putting the foam nickel sheet into a tubular furnace for carbonization, then putting the foam nickel sheet into a nitric acid solution for soaking and washing to obtain a primary untreated carbon material; then the carbon material and AgNO which are not treated preliminarily are mixed3Mixing with deionized water, ultrasonic dispersing, drying, and dissolving in N2The carbonization is carried out under the atmosphere,obtaining the carbon material. In the method, chitosan is used as a carbon source, and simultaneously the chitosan can also be used as a nitrogen source to carry out nitrogen doping on the carbon material, and the specific surface area of the carbon material is improved by using foamed nickel as a template to prepare the carbon material containing a layered microstructure; the surface is coated with silver, so that the conductivity of the carbon material is improved, and the electrochemical performance of the carbon material is enhanced.
Description
Technical Field
The invention belongs to the technical field of electrode material preparation, and particularly relates to a preparation method of a supercapacitor electrode material taking foamed nickel as a template.
Background
Supercapacitors, also known as electrochemical capacitors, are a new type of energy storage device between a battery and a flat capacitor. Supercapacitors have higher energy densities than conventional capacitors, and higher power densities than batteries. In addition, the super capacitor has excellent performances such as high charging and discharging speed, long service life, good safety performance, small pollution and the like, so the super capacitor becomes a novel energy storage device which is concerned all over the world.
The super capacitor can be divided into two types according to an energy storage mechanism, one type adopts electrode materials with high specific surface area, and energy is stored by forming an interface double electric layer electrostatic capacitance between an electrode and electrolyte, namely the double electric layer capacitance; the other type adopts transition metal oxide or macromolecule conducting polymer as electrode material, and the active substance is subjected to underpotential deposition on the surface of the electrode or in a two-dimensional or quasi-two-dimensional space in a bulk phase to generate rapid and reversible chemical adsorption/desorption or oxidation/reduction reaction so as to generate specific capacitance higher than the electric double layer capacitance, namely Faraday pseudo capacitance.
The carbon-based material is widely researched in the application of the super capacitor, and comprises an activated carbon material, graphene and derivatives thereof, a carbon nanotube, template carbon and the like, wherein the energy density of the super capacitor is increased by increasing the specific surface area and the porosity of the carbon-based material and doping heteroatoms. How to improve the conductivity of the carbon material so as to make the carbon material have more excellent electrochemical performance becomes a difficult problem to be solved.
Disclosure of Invention
The invention aims to provide a preparation method of a supercapacitor electrode material taking foamed nickel as a template, which solves the problem of poor electrochemical performance of the capacitor electrode material in the prior art.
The invention adopts the technical scheme that a preparation method of a supercapacitor electrode material taking foam nickel as a template is implemented according to the following steps:
step 1, mixing glacial acetic acid, deionized water and chitosan, and ultrasonically stirring for 1-4h to obtain a chitosan solution;
step 2, turning the foam nickel sheet in the chitosan solution for 10-100 times, and then drying the foam nickel sheet;
step 3, putting the foamed nickel sheet obtained in the step 2 into the chitosan solution again, turning over for 10-100 times, and drying;
step 4, putting the foam nickel sheet obtained in the step 3 into a tubular furnace for carbonization, then soaking the carbonized foam nickel sheet in a nitric acid solution for 6-12h, and finally washing the obtained material with deionized water to be neutral to obtain a primary untreated carbon material;
step 5, mixing the carbon material and AgNO which are not treated in step 43Mixing with deionized water, performing ultrasonic dispersion for 1-4h, and drying to obtain a treated carbon material;
and 6, carbonizing the carbon material treated in the step 5 to obtain the carbon material, namely the supercapacitor electrode material.
The present invention is also characterized in that,
in the step 1, the mass ratio of the glacial acetic acid to the deionized water to the chitosan is 0.5-1: 100: 1-6.
In the step 2, the thickness of the foam nickel sheet is 1-3mm, and the foam nickel sheet is a rectangular foam nickel sheet with the side length of 30-100 mm.
In the step 2 and the step 3, the drying temperature is 50-100 ℃, and the drying time is 2-6 h.
In step 4, the carbonization conditions are as follows: in N2Heating to 1000-1400 ℃ at the speed of 1-5 ℃/min in the atmosphere, preserving the heat for 60-180 min, and cooling to room temperature; n is a radical of2The flow rate of (A) is 40-60 mL/min.
In the step 5, the drying temperature is 50-100 ℃, and the drying time is 24 hours.
In step 5, the carbon material and AgNO which are not treated preliminarily3And deionized water in a mass ratio of 3-50: 1: 10 to 100.
In step 6, the strips are carbonizedThe parts are as follows: in N2Heating to 350-500 ℃ at the speed of 1-10 ℃/min in the atmosphere, preserving the heat for 60-300 min, and cooling to room temperature; n is a radical of2The flow rate of (A) is 40-60 mL/min.
The invention has the beneficial effects that:
in the method, chitosan is used as a carbon source, and simultaneously the chitosan can also be used as a nitrogen source to carry out nitrogen doping on the carbon material, and the specific surface area of the carbon material is improved by using foamed nickel as a template to prepare the carbon material containing a layered microstructure; the effect of improving the specific surface area is achieved by taking the metal Ni as the template, meanwhile, the graphitization degree of the carbon material can be improved by the metal, and the electrochemical performance of the material is further improved. In addition, the carbon material prepared by the method of the invention has the advantages that the surface is coated with silver, so that the conductivity of the carbon material is improved, and the electrochemical performance of the carbon material is enhanced.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of the electrode material ANIC of the super capacitor obtained in example 1 of the present invention;
FIG. 2 is a Scanning Electron Microscope (SEM) image of the electrode material NIC of the supercapacitor obtained in the control group;
FIG. 3 is an X-ray energy spectrum (EDS) diagram of the supercapacitor electrode material obtained in example 3 of the present invention;
FIG. 4 is a constant current charge-discharge test spectrum (GCD) of the electrode material ANIC of the super capacitor obtained in example 1 of the present invention;
fig. 5 is a comparative group of supercapacitor electrode material NIC constant current charge-discharge test spectrogram (GCD);
FIG. 6 is an ANIC Electrochemical Impedance Spectroscopy (EIS) spectrum of the supercapacitor electrode material obtained in example 1 of the present invention;
fig. 7 is an Electrochemical Impedance Spectroscopy (EIS) chart of the electrode material NIC of the supercapacitor obtained from the control group.
Detailed Description
The present invention will be described in detail with reference to the following detailed description and accompanying drawings.
The invention relates to a preparation method of a supercapacitor electrode material taking foamed nickel as a template, which is implemented according to the following steps:
step 1, mixing glacial acetic acid, deionized water and chitosan, and ultrasonically stirring for 1-4h to obtain a chitosan solution;
the mass ratio of the glacial acetic acid to the deionized water to the chitosan is 0.5-1: 100: 1 to 6;
step 2, turning over the foam nickel sheet in the chitosan solution for 10-100 times, and then drying the foam nickel sheet in a forced air oven at the drying temperature of 50-100 ℃ for 2-6 h;
the thickness of the foam nickel sheet is 1-3mm, and the foam nickel sheet is a rectangular foam nickel sheet with the side length of 30-100 mm;
step 3, placing the foamed nickel sheet obtained in the step 2 into the chitosan solution again, turning the foamed nickel sheet for 10-100 times, and placing the foamed nickel sheet into a forced air oven to dry, wherein the drying temperature is 50-100 ℃, and the drying time is 2-6 hours;
step 4, putting the foam nickel sheet obtained in the step 3 into a tubular furnace for carbonization, then soaking the carbonized foam nickel sheet in a nitric acid solution for 6-12h, then carrying out suction filtration, and finally washing the obtained material with deionized water to be neutral to obtain a primary untreated carbon material;
the carbonization conditions are as follows: in N2Heating to 1000-1400 ℃ at the speed of 1-5 ℃/min in the atmosphere, preserving the heat for 60-180 min, and cooling to room temperature; n is a radical of2The flow rate of the water is 40-60 mL/min;
step 5, mixing the carbon material and AgNO which are not treated in step 43Mixing with deionized water, ultrasonically dispersing for 1-4h, and then drying in a forced air oven at 50-100 ℃ for 24h to obtain a treated carbon material;
preliminary untreated carbon material, AgNO3And deionized water in a mass ratio of 3-50: 1: 10 to 100 parts;
step 6, putting the carbon material treated in the step 5 into a tubular furnace for carbonization to obtain a carbon material, namely a super capacitor electrode material;
the carbonization conditions are as follows: in N2Heating to 350-500 ℃ at the speed of 1-10 ℃/min in the atmosphere, preserving the heat for 60-300 min, and cooling to room temperature; n is a radical of2The flow rate of (A) is 40-60 mL/min.
Example 1
First, 6 pieces of nickel foam having a length and a width of 60mm by 40mm were cut out on 3mm thick nickel foam with a blade. Weighing 1ml of glacial acetic acid solution, adding 99ml of deionized water, weighing 2g of chitosan, adding the chitosan into the solution, carrying out ultrasonic stirring for 2 hours, then pouring the chitosan solution into a culture dish, clamping the cut foam nickel sheet by using steel tweezers, repeatedly turning over the foam nickel sheet in the culture dish, drying the foam nickel sheet in a blast oven for 4 hours after the turning over is finished, then putting the dried foam nickel sheet into the culture dish containing the chitosan solution again, repeating the previous step of operation, and drying the foam nickel sheet in the blast oven for 4 hours after the turning over is finished. Transferring the dried sample into a corundum boat, then putting the corundum boat into a tube furnace, setting a temperature rise program, wherein the temperature rise speed is 5 ℃/min, the temperature is raised to 1200 ℃, the temperature is kept for 2h, nitrogen is introduced, and the nitrogen flow rate is 40 ml/min; and after carbonization, putting the product into nitric acid for soaking for 8 hours, then carrying out suction filtration, washing the suction filtration product with deionized water, and washing to be neutral. Then weighing the prepared carbon powder and AgNO3And (3) adding 15: 1, adding 50ml of deionized water, performing ultrasonic dispersion for 2 hours, then placing the mixture into a blast oven for drying for 24 hours, then transferring the dried sample into a corundum boat, then placing the corundum boat into a tubular furnace, introducing nitrogen, setting a heating program at a heating rate of 5 ℃/min and heating to 500 ℃, and keeping the temperature for 3 hours, wherein the nitrogen flow rate is 40 ml/min; cooling and taking out the product; the silver coated carbon material was named ANIC. As a control group, the carbon material without silver coating under the same experimental conditions was named NIC.
Uniformly mixing the obtained carbon material with conductive carbon black and polytetrafluoroethylene dispersion (PTFE), stirring the mixture into slurry by taking an ethanol solvent as a diluent, and mixing active substances according to the mixing ratio: conductive carbon black: PTFE 85:10: 5; uniformly coating the mud mixture on the surface of the foamed nickel under certain pressure, wherein the coating amount is about 2-3mg, and drying. And after drying, assembling two electrodes with similar loads into a sandwich structure by taking Woltmann filter paper as a diaphragm, and performing hot pressing under the pressure of 5MPa to form the supercapacitor.
Fig. 1 is an ANIC scanning electron microscope image, which shows that the surface of the carbon material is successfully coated with the nano silver particles, so that the electrochemical performance of the material is improved, and the surface of the carbon material has a certain micropore and layered structure, so that the specific surface area of the carbon material is increased, and the effect of increasing the electric double layer capacitance is achieved.
Fig. 4 and 5 show GCD curves of ANIC and NIC, respectively, both curves presenting symmetrical isosceles triangles, illustrating that ANIC electrodes have good reversibility in application. The charge-discharge time of the ANIC electrode is obviously longer than that of the NIC electrode, which shows that the AEC has higher specific capacitance by coating silver, the performance of the electrode is improved to a certain extent, and the AEC specific capacitance 76F g is obtained by calculation-148F g above EC-1。
Example 2
First, 6 pieces of nickel foam having a length and a width of 40mm x 40mm were cut out on 3mm thick nickel foam with a blade. Weighing 1ml of glacial acetic acid solution, adding 99ml of deionized water, weighing 2g of chitosan, adding the chitosan into the solution, carrying out ultrasonic stirring for 3 hours, then pouring the chitosan solution into a culture dish, clamping the cut foam nickel sheet by using steel tweezers, repeatedly turning over the foam nickel sheet in the culture dish, drying the foam nickel sheet in a blast oven for 4 hours after the turning over is finished, then putting the dried foam nickel sheet into the culture dish containing the chitosan solution again, repeating the previous step of operation, and drying the foam nickel sheet in the blast oven for 4 hours after the turning over is finished. Transferring the dried sample into a corundum boat, then putting the corundum boat into a tube furnace, setting a temperature rise program, wherein the temperature rise speed is 5 ℃/min, the temperature is raised to 1200 ℃, the temperature is kept for 2h, nitrogen is introduced, and the nitrogen flow rate is 40 ml/min; and after carbonization, putting the product into nitric acid for soaking for 8 hours, then carrying out suction filtration, washing the suction filtration product with deionized water, and washing to be neutral. Then weighing the prepared carbon powder, and adding no AgNO3Adding 50ml of deionized water, placing the mixture into a blast oven for drying for 24 hours, transferring the dried sample into a corundum boat, placing the corundum boat into a tube furnace, introducing nitrogen at the nitrogen flow rate of 40ml/min, setting a temperature rise program, wherein the temperature rise speed is 5 ℃/min, raising the temperature to 500 ℃, and preserving the temperature for 3 hours; the product was taken out after cooling. As a control group, the carbon material without silver coating under the same experimental conditions was named NIC.
Uniformly mixing the obtained carbon material with conductive carbon black and polytetrafluoroethylene dispersion (PTFE), stirring the mixture into slurry by taking an ethanol solvent as a diluent, and mixing active substances according to the mixing ratio: conductive carbon black: and (3) uniformly coating the pasty mixture on the surface of the foamed nickel under certain pressure, wherein the coating amount is about 2-3mg, and drying. And after drying, assembling two electrodes with similar loads into a sandwich structure by taking Woltmann filter paper as a diaphragm, and performing hot pressing under the pressure of 5MPa to form the supercapacitor.
It can be seen from fig. 2 that the carbon material has many micropores distributed over the surface, indicating that the obtained carbon material successfully has a similar structure by using the nickel foam as a template, thereby increasing the electrochemical performance of the material.
Fig. 6 and 7 are ac impedance diagrams of two electrodes fabricated, and in a high frequency region, the intercept of the diagrams on the x axis is called equivalent resistance, including electrolyte resistance, active material, substrate internal resistance, and contact resistance of the active material and a current collector. Meanwhile, the ion transfer capability of the electrode material can be clearly observed through the slope of the image, and the larger the slope is, the larger the ion transfer capability is. The equivalent resistance of ANIC is about 0.3 omega and is less than the equivalent resistance of NIC 2.3 omega, which shows that ANIC has better ion transfer capability. Meanwhile, due to the appearance of a small semicircle image of a high-frequency area caused by the formation of a double electric layer of the electrode and the electrolyte, the diameter of the small semicircle represents the transfer resistance of electrons, and the fact that the diameter of the semicircle of the ANIC is obviously smaller than that of the NIC can be observed, which indicates that the electron transfer resistance of the ANIC is smaller and is more favorable for the rapid passing of the electrons.
Example 3
This example compares to example 2: 2g of chitosan, AgNO mixed with carbon powder3The mass ratio of the carbon powder to the mass increase of (1) is 5:1, the other points are the same as in example 1. Fig. 3 is an EDS diagram of the carbon material, from which the structure of the carbon material surface coated with silver can be seen, and it is obvious that silver and the carbon material are well combined, thereby achieving the purpose of improving the electrochemical performance.
Claims (8)
1. A preparation method of a supercapacitor electrode material taking foamed nickel as a template is characterized by comprising the following steps:
step 1, mixing glacial acetic acid, deionized water and chitosan, and ultrasonically stirring for 1-4h to obtain a chitosan solution;
step 2, turning the foam nickel sheet in the chitosan solution for 10-100 times, and then drying the foam nickel sheet;
step 3, putting the foamed nickel sheet obtained in the step 2 into the chitosan solution again, turning over for 10-100 times, and drying;
step 4, putting the foam nickel sheet obtained in the step 3 into a tubular furnace for carbonization, then soaking the carbonized foam nickel sheet in a nitric acid solution for 6-12h, and finally washing the obtained material with deionized water to be neutral to obtain a primary untreated carbon material;
step 5, mixing the carbon material and AgNO which are not treated in step 43Mixing with deionized water, performing ultrasonic dispersion for 1-4h, and drying to obtain a treated carbon material;
and 6, carbonizing the carbon material treated in the step 5 to obtain the carbon material, namely the supercapacitor electrode material.
2. The method for preparing the supercapacitor electrode material taking the foamed nickel as the template according to claim 1, wherein in the step 1, the mass ratio of the glacial acetic acid to the deionized water to the chitosan is 0.5-1: 100: 1-6.
3. The method for preparing the supercapacitor electrode material taking the foamed nickel as the template in the step 2, wherein the thickness of the foamed nickel sheet is 1-3mm, and the foamed nickel sheet is a rectangular foamed nickel sheet with the side length of 30-100 mm.
4. The method for preparing the supercapacitor electrode material taking the foamed nickel as the template according to claim 1, wherein in the step 2 and the step 3, the drying temperature is 50-100 ℃, and the drying time is 2-6 h.
5. The method for preparing the supercapacitor electrode material taking the foamed nickel as the template according to the claim 1, wherein in the step 4, the carbonization conditions are as follows: in N2In the atmosphereRaising the temperature to 1000-1400 ℃ at the speed of 1-5 ℃/min, preserving the temperature for 60-180 min, and cooling to room temperature; n is a radical of2The flow rate of (A) is 40-60 mL/min.
6. The preparation method of the supercapacitor electrode material taking the foamed nickel as the template according to claim 1, wherein in the step 5, the drying temperature is 50-100 ℃ and the drying time is 24 hours.
7. The method for preparing the supercapacitor electrode material taking the foam nickel as the template according to claim 1, wherein in the step 5, the carbon material and AgNO which are not processed preliminarily are adopted3And deionized water in a mass ratio of 3-50: 1: 10 to 100.
8. The method for preparing the supercapacitor electrode material taking the foamed nickel as the template according to the claim 1, wherein in the step 6, the carbonization conditions are as follows: in N2Heating to 350-500 ℃ at the speed of 1-10 ℃/min in the atmosphere, preserving the heat for 60-300 min, and cooling to room temperature; n is a radical of2The flow rate of (A) is 40-60 mL/min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010087235.4A CN111268673A (en) | 2020-02-11 | 2020-02-11 | Preparation method of supercapacitor electrode material taking foamed nickel as template |
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