CN112885615A - Preparation method of porous nitrogen-doped carbon electrode material - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000007772 electrode material Substances 0.000 title claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000843 powder Substances 0.000 claims abstract description 41
- 241000219000 Populus Species 0.000 claims abstract description 29
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 33
- 238000010438 heat treatment Methods 0.000 claims description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000012153 distilled water Substances 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 11
- 235000012239 silicon dioxide Nutrition 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- 230000003213 activating effect Effects 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 238000010000 carbonizing Methods 0.000 claims description 4
- 239000000839 emulsion Substances 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 150000002829 nitrogen Chemical class 0.000 claims description 4
- -1 Polytetrafluoroethylene Polymers 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical compound [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 claims description 2
- 239000012190 activator Substances 0.000 claims description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 239000002023 wood Substances 0.000 claims description 2
- 235000013339 cereals Nutrition 0.000 claims 1
- 238000005485 electric heating Methods 0.000 claims 1
- 235000013312 flour Nutrition 0.000 claims 1
- 239000000741 silica gel Substances 0.000 claims 1
- 229910002027 silica gel Inorganic materials 0.000 claims 1
- 239000003575 carbonaceous material Substances 0.000 abstract description 12
- 239000003990 capacitor Substances 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000001351 cycling effect Effects 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 8
- 238000002484 cyclic voltammetry Methods 0.000 description 5
- 238000004146 energy storage Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000007605 air drying Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 1
- 229960004424 carbon dioxide Drugs 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 238000007600 charging Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010277 constant-current charging Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910021508 nickel(II) hydroxide Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000001932 seasonal effect Effects 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention relates to a preparation method of a nitrogen-doped porous carbon material, in particular to a method for preparing a nitrogen-doped porous carbon material by taking poplar powder as a carbon source, and also relates to application and electrochemical performance of the nitrogen-doped porous carbon material in an electrochemical capacitor. The preparation method has rich raw material sources, is convenient and cheap, and is an effective way for preparing the nitrogen-doped porous carbon material. The preparation steps are simple, the reaction conditions are mild, the operation and control are easy, and the prepared nitrogen-doped porous carbon has large specific surface area and high specific capacitance. The specific surface area of the electrode material of the super capacitor prepared under the better condition can reach 1800 m2g‑1The nitrogen content can reach 5%, and the cycling stability is good, so the composite material is a relatively ideal electrode material of an electrochemical capacitor.
Description
Technical Field
The invention relates to a preparation method of a nitrogen-doped porous carbon material, in particular to a method for preparing a nitrogen-doped porous carbon material by taking poplar powder as a raw material, and also relates to application and electrochemical performance of the nitrogen-doped porous carbon material in a super capacitor.
Background
The development and utilization of renewable energy have important implications for solving the energy crisis and environmental problems of the current human society. Solar energy, wind energy, water and electricity and the like are environment-friendly renewable energy sources. However, this type of energy has seasonal, regional and discontinuous characteristics, which make them not directly applicable to industry and daily life, and they must be stored for use. The energy storage problem is therefore a key and focus problem for energy utilization today. In addition, with the rapid advance of portable terminals and wearable electronic technologies, the update of energy storage devices is also urgently needed. Currently, commercial energy storage devices include secondary storage batteries such as lead-acid batteries, nickel-cadmium batteries, nickel-hydrogen batteries, lithium ion batteries, and the like. The storage battery has the advantage of high energy density and can be repeatedly used. However, the conventional storage battery has low power density and cannot meet the requirement of high-power electric equipment, so that an energy storage device with high power density is needed to solve the problem. Electrochemical capacitors (supercapacitors) have the advantages of high power density, long cycle life, low preparation cost, good safety and the like, and have been widely paid attention to the research in the field of energy storage. The electrode material and the electrolyte are important for the performance of the electrochemical capacitor, are key parts for measuring the performance of the capacitor, and determine the energy density, the power density, the cycling stability and the like of the capacitor. The electrode materials of the super capacitor mainly comprise the following types: carbon materials (e.g., activated carbon, graphene, carbon fiber, etc.); metal oxides (e.g. RuO)2，MnO2，Ni(OH)2Etc.). Porous carbon has the characteristics of low cost, wide source, large specific surface area, excellent electrochemical performance and the like, and is widely concerned by researchers. But the mass and volume energy density of the porous carbon are low, and the specific capacitance and energy of the porous carbon are improvedThe density is generally increased by increasing the specific surface area of the porous carbon. But the increase of the specific surface area can cause the reduction of the conductivity of the material and increase the internal resistance of the super capacitor; by introducing nitrogen element into the porous carbon, the wettability between the surface of the porous carbon material and electrolyte can be increased, pseudo-capacitance reaction is increased, and the specific capacitance of the porous carbon is improved. Therefore, the method for preparing the nitrogen-doped carbon material of the supercapacitor electrode by using poplar powder as a carbon source and a nitrogen source and adopting nano silicon dioxide as a template is provided, and the prepared nitrogen-doped porous carbon has large specific surface area and high specific capacitance.
Disclosure of Invention
The invention relates to a preparation method of nitrogen-doped carbon, in particular to a method for preparing a nitrogen-doped carbon material by taking poplar powder as a raw material.
A method for preparing a supercapacitor electrode nitrogen-doped carbon material by taking poplar powder as a raw material and providing a carbon source and a nitrogen source is characterized by comprising the following steps of:
1, dispersing quantitative poplar powder into quantitative distilled water, adding the quantitative poplar powder into quantitative silica sol, stirring for 30-60min at 60 ℃, cooling to room temperature, carrying out forced air drying at 50 ℃ for 24 hours to obtain a poplar powder/silicon dioxide mixture, and grinding a sample into powder for later use; the performance indexes of the poplar wood powder are as follows: the color is white or milk white; the water content is less than 15 percent; the PH value is 4.0-6.0; the performance indexes of the used silica sol are as follows: the grain diameter is 4-20 nm; the content is 10 percent; the proportion of the powder to the silica sol solution is as follows: the mass ratio of the m poplar powder to the m silica sol is 1: 2-6, and the preferred mass ratio is 1: 4; the using proportion of the poplar powder and the distilled water is as follows: the mass ratio of the m poplar powder to the m distilled water is 1: 10-30, and the preferred ratio is 1: 20;
2. placing a poplar powder/silicon dioxide mixture sample in a quartz boat, carbonizing under the protection of nitrogen, heating to 600-900 ℃ at a heating rate of 3-10 ℃/min, carbonizing for 1-3 hours, cooling along with the furnace under the protection of nitrogen, cooling to room temperature, placing the obtained product in a quantitative 3mol/L KOH solution, soaking for 2 hours at 70 ℃, washing with distilled water until the pH value is 7, and drying for 12 hours at 80 ℃ to obtain nitrogen-doped porous Carbon (CN); wherein the preferred heating rate is 2 ℃/min, the preferred carbonization temperature is 850 ℃, and the preferred carbonization time is 2 hours;
3. the obtained nitrogen-doped porous carbon (C & N) and an activating agent are uniformly mixed, placed in a tube furnace for activation under the protection of nitrogen, the heating rate is 3-10 ℃/min, and the temperature is raised to 600-900 ℃ for heat preservation for 1 h. Then furnace cooling is carried out under the protection of nitrogen, the obtained sample is neutralized by 6mol/L hydrochloric acid after being cooled to room temperature, then the sample is washed by distilled water until the pH value is 7, and the sample is dried for 12 hours at 80 ℃ to obtain activated nitrogen doped porous carbon (CNAC); the activating agent is one or a mixture of more of potassium hydroxide, lithium hydroxide, sodium hydroxide, lithium carbonate, sodium carbonate and potassium carbonate, and the mass ratio of the nitrogen-doped porous carbon to the activating agent is 1: 1-5; wherein, the better activator is potassium hydroxide, the better mass ratio of the nitrogen-doped porous carbon to the potassium hydroxide is 1: 2.5, the better heating rate is 3 ℃/min, and the better activation temperature is 800 ℃;
4. mixing the prepared nitrogen-doped porous carbon (CN or CNAC), conductive carbon black and Polytetrafluoroethylene (PTFE) emulsion according to the mass ratio of 80: 10, coating the mixture on a foamed nickel mesh current collector with the thickness of 1 mm, coating the mixture with the area of 2 multiplied by 2cm, and pressing the mixture for 15 to 60 seconds under the pressure of 15MPa by a tablet press; and drying the pressed electrode at 80 ℃ for 12h, cooling to room temperature, soaking the electrode in 6mol/L KOH solution for 12h, and performing Cyclic Voltammetry (CV) and constant current charging and discharging (GCD) tests.
The specific embodiment adopted by the invention is as follows:
the invention is further described with reference to specific embodiments, without limiting the scope of protection. At the same time
The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Embodiment 1: dispersing 5 g poplar powder in 100 ml distilled water, adding into 18 g silica sol, stirring at 60 deg.C for 35min, cooling to room temperature, 50 deg.CAnd (3) performing forced air drying for 24 hours to obtain a poplar powder/silicon dioxide mixture, grinding a sample into powder, placing the powder in a tubular furnace, heating to 800 ℃ for heat preservation for 2 hours at the heating rate of 5 ℃/min under the protection of nitrogen. Placing the obtained product in 3mol/L KOH solution, soaking at 80 deg.C for 2h, washing to neutrality, drying at 80 deg.C for 12h to obtain nitrogen-doped porous Carbon (CN), and measuring the specific surface area of the nitrogen-doped porous carbon to be 720 m by specific surface tester2g-1The nitrogen content was 5.4% as measured by X-ray photoelectron spectroscopy (XPS). Mixing the obtained nitrogen-doped porous Carbon (CN), conductive carbon black and binder PTFE emulsion at a ratio of 80: 10, and coating on a 2cm × 1cm nickel net with a coating area of 1cm2. After soaking in 6M KOH solution for 12h, cyclic voltammetry curve and constant current charge and discharge tests are carried out. Figure 1 exhibits double layer capacitance behavior; the electrical curves are approximately symmetrical to the corresponding charging curves, indicating that the CN electrode has better electrochemical reversibility (fig. 2).
Embodiment 2:
dispersing 5 g of poplar powder in 100 ml of distilled water, adding 18 g of silica sol, stirring for 35min at 60 ℃, cooling to room temperature, blowing and drying for 24 h at 50 ℃ to obtain a poplar powder/silicon dioxide mixture, grinding a sample into powder, placing the powder in a tubular furnace, heating to 800 ℃ at a heating rate of 5 ℃/min under the protection of nitrogen, and keeping the temperature for 2 h. Uniformly mixing the obtained nitrogen-doped porous carbon and KOH according to the mass ratio of 1: 2, placing the mixture in a tubular furnace for nitrogen protection at the heating rate of 5 ℃/min, heating to 80 ℃, and preserving heat for 1 h. The obtained sample is washed to be neutral by hydrochloric acid and dried for 12h at 80 ℃ to obtain the nitrogen-doped porous carbon (CNAC). The specific surface area of the nitrogen-doped porous carbon is 1900 m measured by a specific surface tester2g-1The nitrogen content was 4.2% as measured by X-ray photoelectron spectroscopy (XPS). Mixing the obtained CNAC with conductive carbon black and binder PTFE emulsion at a ratio of 80: 10, and coating on 2cm × 1cm nickel net with a coating area of 1cm2. And soaking in 6M KOH solution for 12h, and testing the electrochemical performance of the electrode. All discharge curves were approximately symmetrical to the corresponding charge curves, indicating that the CNAC electrodes have good electrochemical reversibility (fig. 3); performance ofDouble layer capacitance behavior (figure 4); has higher specific capacity and excellent cycling stability. The performance of the activated carbon material is obviously better than that of an unactivated material, and the CV curve is closer to a rectangle. And the charge-discharge rate performance is better.
Embodiment 3:
dispersing 5 g of poplar powder in 120 ml of distilled water, adding 25 g of silica sol, stirring for 35min at 60 ℃, cooling to room temperature, blowing and drying for 24 h at 50 ℃ to obtain a poplar powder/silicon dioxide mixture, grinding a sample into powder, placing the powder in a tubular furnace, heating to 800 ℃ at a heating rate of 5 ℃/min under the protection of nitrogen, and keeping the temperature for 2 h. Uniformly mixing the obtained nitrogen-doped porous carbon and potassium carbonate according to the mass ratio of 1: 4, placing the mixture in a tubular furnace for nitrogen protection, heating to 800 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 1 h. Washing the obtained sample with hydrochloric acid to neutrality, drying at 80 deg.C for 12h to obtain nitrogen-doped porous carbon (CNAC3), and determining the specific surface area of the nitrogen-doped porous carbon to 1720 m by specific surface tester2g-1The nitrogen content was measured by X-ray photoelectron spectroscopy (XPS) to be 6.2%.
Embodiment 4:
dispersing 5 g poplar powder in 80 ml distilled water, adding 10 g silica sol, stirring at 60 deg.c
And cooling to room temperature for 45min, carrying out forced air drying at 50 ℃ for 24 h to obtain a poplar powder/silicon dioxide mixture, grinding the sample into powder, placing the powder in a tube furnace, heating to 800 ℃ at a heating rate of 5 ℃/min under the protection of nitrogen, and keeping the temperature for 2 h. Uniformly mixing the obtained nitrogen-doped porous carbon and sodium hydroxide according to the mass ratio of 1: 3, placing the mixture in a tubular furnace for nitrogen protection, heating to 800 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 1 h. Washing the obtained sample with hydrochloric acid to neutrality, drying at 80 deg.C for 12h to obtain nitrogen-doped porous carbon (CNAC4), and determining the specific surface area of nitrogen-doped porous carbon to 1930 m by specific surface tester2g-1The nitrogen content was measured by X-ray photoelectron spectroscopy (XPS) to be 5.3%.
Drawings
Illustration of the drawings:
FIG. 1 is a graph showing charge and discharge curves of nitrogen-doped Carbon (CN) at different current densities
FIG. 2. Cyclic voltammograms of nitrogen-doped Carbon (CN) at different scan rates
FIG. 3 shows charge and discharge curves of activated nitrogen doped carbon (CNAC) at different current densities
FIG. 4 cyclic voltammograms of activated nitrogen doped carbon (CNAC) at different scan rates
Claims (7)
1. A preparation method of a porous nitrogen-doped carbon electrode material is characterized by comprising the following steps of dispersing quantitative poplar powder into quantitative distilled water, adding the quantitative poplar powder into quantitative silica sol, stirring the mixture for 30-60min at 50 ℃, cooling the mixture to room temperature, drying the mixture for 24 hours by blowing air at 50 ℃ to obtain poplar powder/silicon dioxide mixture, grinding a sample into fine powder, placing the fine powder into a quartz boat, carbonizing the sample under the protection of nitrogen at the heating rate of 3-10 ℃/min, heating the sample to 600-900 ℃, carbonizing the sample for 1-4 hours, cooling the sample to room temperature along with a furnace, soaking the obtained product in 200 ml of 2-6mol/L KOH solution at 70 ℃ for 4 hours to remove a silicon dioxide template, repeatedly washing the obtained product with distilled water until the pH value is 7-8, drying the obtained product for 12 hours at 80 ℃ to obtain nitrogen-doped carbon, uniformly mixing the prepared nitrogen-doped carbon and an activating agent, activating under the protection of nitrogen, heating up to 600-900 ℃ at the heating rate of 3-10 ℃/min, and keeping the temperature for 2 h; and then furnace cooling is carried out under the protection of nitrogen, the obtained sample is neutralized by 3mol/L hydrochloric acid after being cooled to room temperature, the obtained sample is washed by distilled water until the pH value is 7, and the obtained product is dried for 12 hours at 80 ℃ to obtain the activated nitrogen doped porous carbon.
2. The method according to claim 1, wherein the poplar wood flour has the following properties: the color is white or milk white powder; the water content is less than 15 percent; the PH value is 4.0-6.0; the total nitrogen content (N)% is 10-15%.
3. The process according to claim 1, wherein the silica sol has the following properties: the grain diameter is 4-20 nm; the content is 10 percent.
4. The method according to claim 1, wherein the poplar powder and the silica gel solution are used in a ratio of: the mass ratio of the m poplar powder to the m silica sol is 1: 2-6.
5. The method according to claim 1, wherein the poplar powder and the distilled water are used in a ratio of: the mass ratio of the m poplar powder to the m distilled water is 1: 10-30.
6. The process according to claim 1, wherein the activating agent is one or a mixture of potassium hydroxide, lithium hydroxide, sodium hydroxide, lithium carbonate, sodium carbonate and potassium carbonate; the mass ratio of the nitrogen-doped porous carbon to the activator is 1: 1-5.
7. The nitrogen-doped porous carbon prepared according to the claim 1, conductive carbon black and Polytetrafluoroethylene (PTFE) emulsion are mixed according to the mass ratio of 80: 10, the mixture is coated on a foamed nickel mesh current collector with the thickness of 1 mm, the coating area is 2 x 2cm, the mixture is pressed for 60 seconds by a tablet press under the pressure of 15MPa, and then the mixture is placed in an electric heating air blast drying oven to be dried for 12 hours at the temperature of 80 ℃ and cooled to the room temperature, and the electrode material for the supercapacitor is prepared.
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| US20090220775A1 (en) * | 2006-05-02 | 2009-09-03 | Fumio Kurosaki | Macroporous Carbon Material and Mesoporous Carbon Material Starting from Wood Material, Method for Producing them, and Porous Metal Carbon Material and Method for Producing it |
| CN107777685A (en) * | 2017-09-30 | 2018-03-09 | 浙江农林大学 | The method that Carbon-based supercapacitor electrode material is prepared using wood powder as raw material |
| CN110436457A (en) * | 2019-07-29 | 2019-11-12 | 聊城大学 | A kind of preparation method of supercapacitor N doping porous carbon electrode material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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