CN113120878A - Preparation method of N, B co-doped carbon-based supercapacitor electrode material - Google Patents
Preparation method of N, B co-doped carbon-based supercapacitor electrode material Download PDFInfo
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- CN113120878A CN113120878A CN202110419102.7A CN202110419102A CN113120878A CN 113120878 A CN113120878 A CN 113120878A CN 202110419102 A CN202110419102 A CN 202110419102A CN 113120878 A CN113120878 A CN 113120878A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 25
- 239000007772 electrode material Substances 0.000 title claims abstract description 18
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229920001661 Chitosan Polymers 0.000 claims abstract description 35
- 239000003990 capacitor Substances 0.000 claims abstract description 17
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004327 boric acid Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000004964 aerogel Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002019 doping agent Substances 0.000 claims abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 36
- 239000000843 powder Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 10
- 239000003575 carbonaceous material Substances 0.000 claims description 10
- 239000004246 zinc acetate Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000010335 hydrothermal treatment Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003792 electrolyte Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000003763 carbonization Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 125000005842 heteroatom Chemical group 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 241000238557 Decapoda Species 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 241000195493 Cryptophyta Species 0.000 description 1
- OVRNDRQMDRJTHS-FMDGEEDCSA-N N-acetyl-beta-D-glucosamine Chemical group CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O OVRNDRQMDRJTHS-FMDGEEDCSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- MSWZFWKMSRAUBD-UHFFFAOYSA-N beta-D-galactosamine Natural products NC1C(O)OC(CO)C(O)C1O MSWZFWKMSRAUBD-UHFFFAOYSA-N 0.000 description 1
- MSWZFWKMSRAUBD-QZABAPFNSA-N beta-D-glucosamine Chemical compound N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O MSWZFWKMSRAUBD-QZABAPFNSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
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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
- C01B32/05—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, 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
-
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
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- 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)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention belongs to the technical field of supercapacitor electrode materials, and relates to a preparation method of an N, B co-doped carbon-based supercapacitor electrode material. Chitosan is used as a nitrogen-containing carbon source, and boric acid is used as a doping agent. The preparation of the high-performance B and N co-doped hierarchical porous carbon double-electrode-layer capacitor electrode material is realized through the processes of Zn-chitosan aerogel preparation, high-temperature heat treatment, hydrothermal doping B treatment and the like. The invention uses cheap and renewable chitosan as the nitrogen-containing carbon source, and solves the problem of high cost of the electrode material of the commercial electric double-layer capacitor. By designing the B and N co-doped hierarchical porous carbon structure, the problem that the specific capacity of the electrode material of the commercial double electric layer capacitor is low is solved, and the wide application of the double electric layer capacitor is facilitated.
Description
Technical Field
The invention belongs to the technical field of supercapacitor electrode materials, and relates to a preparation method of an N, B co-doped carbon-based supercapacitor electrode material.
Background
The super capacitor has the advantages of high power capacity, excellent safety, stable cyclability and the like. The electric double layer capacitor stores energy by adsorbing electrolyte ions through an interface between an electrode and an electrolyte, and has the advantages of high charging efficiency, high response speed, long service life, wide working temperature range and the like, thereby being widely applied to many fields. Common EDLC electrode materials today include activated carbon and graphene. Porous carbon materials generally exhibit excellent rate and cycle performance due to high specific surface area and abundant porosity.
However, most activated carbon-based supercapacitors face two bottlenecks: low specific capacitance and high cost. Such as YP50F, available from clony, japan, with a capacitance of 28F g-1The price is as high as 20 yuan/g. Modification of the carbon-based electric double layer capacitor electrode material generally includes introducing heteroatoms for doping, constructing a hierarchical porous structure and the like. Heteroatom doping can significantly reduce the adsorption free energy of gibbs, thereby increasing energy and power density. Co-doping can further improve charge storage capability due to synergistic effects between the dopants. Meanwhile, the heteroatom in the carbon skeleton can not only enhance the electronic conductivity, but also improve the electrolyte wettability of the carbon material. The hierarchical porous structure plays an important role in improving the electrode material of the super capacitor. The micropores can provide a high specific surface area to the electrode, which is very helpful for improving charge storage capacity. While the mesopores and macropores can act as ion buffer reservoirs to shorten the diffusion length of the ions. Therefore, how to prepare the heteroatom-doped hierarchical porous structure carbon-based electrode material becomes a research hotspot at present.
Disclosure of Invention
In order to solve the above situation, the invention uses chitosan as a nitrogen-containing carbon source and uses boric acid as a doping agent. The preparation of the high-performance B and N co-doped hierarchical porous carbon double-electrode-layer capacitor electrode material is realized through the processes of Zn-chitosan aerogel preparation, high-temperature heat treatment, hydrothermal doping B treatment and the like. Mainly comprises the following steps:
dissolving acetic acid in deionized water to prepare an acetic acid solution. Then stirring the prepared acetic acid solution, slowly adding chitosan powder, and stirring until clear sol is obtained.
And (2) dissolving certain zinc acetate in deionized water to obtain a zinc acetate solution. And slowly adding the obtained solution into the chitosan sol, and stirring to prepare the Zn-chitosan sol.
And (3) placing the prepared Zn-chitosan sol into a freeze dryer, and setting a program to freeze and prepare the Zn-chitosan aerogel at a low temperature for a certain time.
And (4) putting the Zn-chitosan aerogel into a tubular carbonization furnace, and performing high-temperature heat treatment to obtain the N-doped hierarchical porous carbon.
And (5) grinding the prepared N-doped hierarchical porous carbon into powder, placing the powder into deionized water, stirring and dispersing the powder, and adding boric acid powder to fully dissolve boric acid.
And (6) placing the boric acid-N doped porous carbon solution in the lining of a polytetrafluoroethylene hydrothermal kettle, and carrying out high-temperature hydrothermal treatment.
And (7) carrying out suction filtration on the solution after hydrothermal treatment to neutrality, washing with ethanol, and drying the obtained powder in a constant-temperature air-blast drying oven for a certain time to obtain the N and B co-doped hierarchical porous carbon material.
The concentration of the acetic acid solution prepared in the step (1) can be between 1 and 2 percent, the preparation volume is between 40 and 50mL, and the mass of the added chitosan is between 1 and 1.5 g.
The mass ratio of the zinc acetate to the chitosan in the step (2) is controlled to be 2: 1-8: 1.
In the step (3), the freeze-drying temperature is controlled at-90 ℃, the vacuum degree of a freeze dryer is controlled at-0.08-0.1 MPa, and the freeze-drying time is controlled between 36h and 48 h.
And (4) controlling the temperature rise rate of the tubular resistance furnace in the step (4) to be 5 ℃/min, controlling the temperature to be 910-1000 ℃, and keeping the temperature for 2-4 h. The cooling rate is controlled between 500 ℃ and 1000 ℃, and the temperature is naturally cooled below 500 ℃.
The specific surface area of the N-doped hierarchical porous carbon prepared in the step (5) is 500-1000 m2 g-1The mass ratio of the added boric acid to the added boric acid is controlled to be 2: 1-4: 1, and the stirring time is controlled to be 12-24 hours.
The temperature of hydrothermal treatment in the step (6) is controlled to be between 6 and 12 hours, and the temperature of hydrothermal treatment is controlled to be between 150 and 160 ℃.
And (7) controlling the temperature of the constant-temperature blast drying box to be 80-100 ℃ and controlling the drying time to be 12-24 h.
The prepared N, B doped hierarchical porous carbon material is tested by a symmetrical capacitor assembled by 6M KOH electrolyte, and the specific capacitance value is 0.5F g-1Condition 170F g-1The voltage window can be expanded to 0-1.25V, and the energy density can reach 9.57Wh kg-1。
The invention has the following advantages:
(1) chitosan is a low cost natural polymer material derived from algae, shrimp shells, crabs, and other amphibians. The chitosan molecule is formed by D-glucosamine and N-acetyl-D-glucosamine units through beta- (1 → 4) glycosidic bonds, contains a large number of nitrogen-containing groups, and can be used as a self-doping nitrogen-containing carbon source.
(2) A large number of nitrogen-containing groups of chitosan molecules are coordinated with metal Zn to form Zn-chitosan aerogel, and the metal template is removed without acid washing through high-temperature heat treatment at the temperature higher than the boiling point temperature (>907 ℃) of Zn, so that the N-doped hierarchical porous carbon material is prepared in one step.
(3) The doping of B can keep the catalytic decomposition activity of the carbon material to water, and effectively expand the voltage window of the aqueous double-layer capacitor. The N and B codoping synergy also improves the energy density of the double-electric-layer capacitor.
Detailed Description
The present invention is illustrated by way of specific examples, but is not intended to be limited thereto.
Example 1:
1g of acetic acid is dissolved in deionized water to prepare a 1% acetic acid solution, and the acetic acid is uniformly dispersed by stirring. 20ml of 1% acetic acid solution was placed in a magnetic stirrer at 500r/min, and 1g of chitosan powder was slowly added thereto, thereby forming chitosan gel. 5g of zinc acetate was dissolved in 20g of deionized water and stirred continuously to dissolve it completely. And slowly adding the zinc acetate solution into the chitosan gel, and stirring to obtain clear Zn-chitosan sol. The Zn-chitosan gel was frozen in a refrigerator overnight. And (3) putting the frozen Zn-chitosan gel into a freeze dryer, setting the vacuum degree to be-0.1 MPa and the freezing temperature to be-90 ℃, and freezing for 40 hours to obtain the Zn-chitosan aerogel. And (3) placing the obtained Zn-chitosan aerogel in a tubular resistance furnace, setting the heating rate of the heating furnace to be 5 ℃/min, controlling the temperature to be 1000 ℃, and keeping the temperature for 2 h. The cooling rate is controlled between 500 ℃ and 1000 ℃, and the temperature is naturally cooled below 500 ℃. The obtained N-doped graded porous carbon powder was collected and ground, 0.1g of which was dispersed in 50ml of deionized water, and then 0.2g of boric acid was added to the solution and stirred for 24 hours to be sufficiently dissolved. The solution was placed in a 100ml teflon liner and hydrothermal treated at 160 ℃ for 12 h. And (3) performing suction filtration and water washing on the hydrothermal solution to neutral and ethanol washing, and placing the obtained suction filtration product in a constant-temperature air-blast drying oven for heat preservation for 12 hours at the temperature of 80 ℃ to obtain the N and B co-doped graded porous carbon double-electrode-layer capacitor electrode material.
Example 2:
the mass of zinc acetate was changed to 2g, and the other conditions were the same as in example 1 to obtain 632m2 g-1The N-doped graded porous carbon material is obtained in the next step, and the N and B co-doped graded porous carbon double-electrode-layer capacitor electrode material is obtained.
Example 3:
zinc acetate mass was changed to 8g, and other conditions were the same as in example 1 to obtain 582m2 g-1The N-doped graded porous carbon material is obtained in the next step, and the N and B co-doped graded porous carbon double-electrode-layer capacitor electrode material is obtained.
Claims (9)
1. The invention uses chitosan as nitrogen-containing carbon source and boric acid as dopant. The preparation of the high-performance B and N co-doped hierarchical porous carbon double-electrode-layer capacitor electrode material is realized through the processes of Zn-chitosan aerogel preparation, high-temperature heat treatment, hydrothermal doping B treatment and the like. Mainly comprises the following steps:
dissolving acetic acid in deionized water to prepare an acetic acid solution. Then stirring the prepared acetic acid solution, slowly adding chitosan powder, and stirring until clear sol is obtained.
And (2) dissolving certain zinc acetate in deionized water to obtain a zinc acetate solution. And slowly adding the obtained solution into the chitosan sol, and stirring to prepare the Zn-chitosan sol.
And (3) placing the prepared Zn-chitosan sol into a freeze dryer, and setting a program to freeze and prepare the Zn-chitosan aerogel at a low temperature for a certain time.
And (4) putting the Zn-chitosan aerogel into a tubular carbonization furnace, and performing high-temperature heat treatment to obtain the N-doped hierarchical porous carbon.
And (5) grinding the prepared N-doped hierarchical porous carbon into powder, placing the powder into deionized water, stirring and dispersing the powder, and adding boric acid powder to fully dissolve boric acid.
And (6) placing the boric acid-N doped porous carbon solution in the lining of a polytetrafluoroethylene hydrothermal kettle, and carrying out high-temperature hydrothermal treatment.
And (7) carrying out suction filtration on the solution after hydrothermal treatment to neutrality, washing with ethanol, and drying the obtained powder in a constant-temperature air-blast drying oven for a certain time to obtain the N and B co-doped hierarchical porous carbon material.
2. The method according to claim 1, wherein the concentration of the acetic acid solution prepared in the step (1) is 1-2%, the preparation volume is 40-50 mL, and the mass of the added chitosan is 1-1.5 g.
3. The method according to claim 1, wherein the mass ratio of zinc acetate to chitosan in step (2) is controlled to be between 2:1 and 8: 1.
4. The method according to claim 1, wherein the temperature of the freeze-drying in the step (3) is controlled at-90 ℃, the vacuum degree of the freeze-dryer is controlled at-0.08-0.1 MPa, and the freeze-drying time is controlled between 36h and 48 h.
5. The method according to claim 1, wherein the temperature rise rate of the tubular resistance furnace in the step (4) is 5 ℃/min, the temperature is controlled to be 910-1000 ℃, and the heat preservation time is 2-4 h. The cooling rate is controlled between 500 ℃ and 1000 ℃, and the temperature is naturally cooled below 500 ℃.
6. The method according to claim 1, wherein the specific surface area of the N-doped hierarchical porous carbon prepared in the step (5) is 600 to 1000m2g-1The mass ratio of the added boric acid to the added boric acid is controlled to be 2: 1-4: 1, and the stirring time is controlled to be 12-24 hours.
7. The method according to claim 1, wherein the temperature of the hydrothermal treatment in the step (6) is controlled to be between 6 and 12 hours, and the temperature of the hydrothermal treatment is controlled to be between 150 and 160 ℃.
8. The method according to claim 1, wherein in the step (7), the temperature of the constant-temperature air-blast drying box is controlled to be 80-100 ℃, and the drying time is controlled to be 12-24 hours.
9. The method according to any one of claims 1 to 8, wherein the prepared N, B doped hierarchical porous carbon material is tested in a symmetrical capacitor assembled with 6M KOH electrolyte and has a specific capacitance value of 0.5F g-1Under the condition of 150-170F g-1The voltage window can be expanded to 0-1.25V, and the energy density can reach 8-9.57 Wh kg-1。
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Cited By (1)
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| CN115124020A (en) * | 2022-06-22 | 2022-09-30 | 江南大学 | Boron-nitrogen co-doped carbon material with hierarchical holes and preparation method and application thereof |
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