CN113880067B - Preparation method of porous carbon super-structure material - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 44
- 239000000463 material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 36
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229920000642 polymer Polymers 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 17
- WQOWBWVMZPPPGX-UHFFFAOYSA-N 2,6-diaminoanthracene-9,10-dione Chemical compound NC1=CC=C2C(=O)C3=CC(N)=CC=C3C(=O)C2=C1 WQOWBWVMZPPPGX-UHFFFAOYSA-N 0.000 claims abstract description 12
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- 238000003763 carbonization Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- ZVCDLGYNFYZZOK-UHFFFAOYSA-M sodium cyanate Chemical compound [Na]OC#N ZVCDLGYNFYZZOK-UHFFFAOYSA-M 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims 2
- 229910052786 argon Inorganic materials 0.000 claims 1
- 239000001307 helium Substances 0.000 claims 1
- 229910052734 helium Inorganic materials 0.000 claims 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 4
- 230000005540 biological transmission Effects 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 230000004913 activation Effects 0.000 abstract description 2
- 238000010534 nucleophilic substitution reaction Methods 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 230000001360 synchronised effect Effects 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 9
- 239000007772 electrode material Substances 0.000 description 8
- 239000003990 capacitor Substances 0.000 description 6
- 238000004146 energy storage Methods 0.000 description 5
- 102000020897 Formins Human genes 0.000 description 4
- 108091022623 Formins Proteins 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 4
- 238000010000 carbonizing Methods 0.000 description 4
- 125000004122 cyclic group Chemical group 0.000 description 4
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000001493 electron microscopy Methods 0.000 description 3
- 125000005842 heteroatom Chemical group 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 229920002239 polyacrylonitrile Polymers 0.000 description 3
- 238000002336 sorption--desorption measurement Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000011852 carbon nanoparticle Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000003541 multi-stage reaction Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- 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
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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
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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
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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
- H01G11/84—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
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- 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
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Abstract
The invention relates to a preparation method of a porous carbon super-structure material. Belonging to the technical field of material preparation science. Cyanuric chloride and 2, 6-diaminoanthraquinone are selected to generate nucleophilic substitution reaction in acetonitrile solvent to generate polymer precursor, and the porous carbon super-structure material is prepared after synchronous carbonization/chemical activation. The preparation process is simple, complex and harsh experimental conditions are not needed, the prepared carbon super-structure material has ultrahigh specific surface area, a hierarchical porous structure and nitrogen and oxygen heteroatoms, the characteristics enhance the interface wettability of the carbon super-structure material, an ion rapid transmission channel is provided, and a remarkable Faraday reaction can be generated to contribute to pseudo capacitance.
Description
Technical Field
The invention relates to a preparation method of a porous carbon super-structure material, and belongs to the technical field of material preparation.
Background
In order to solve the problems of global fossil fuel depletion and environmental deterioration, development of sustainable and efficient energy storage technologies and devices has become an urgent need. The carbon-based super capacitor is used as an energy storage device with the most development prospect, and has the advantages of high charging and discharging speed, high power density, long service life and the like, so that the carbon-based super capacitor is widely applied to the fields of digital cameras, all-electric automobiles, pulse lasers and the like in recent years. The electrode material is a key component of the supercapacitor, and among various electrode materials, carbon materials are widely used due to the outstanding advantages of high conductivity, stable chemical properties, environmental friendliness, adjustable pore structure parameters, adjustable morphology and the like. In order to improve the energy storage performance of supercapacitors, much research has been devoted to developing advanced carbon electrode materials.
The carbon super-structure material is a novel carbon material, has a regular three-dimensional structure, can inherit the basic properties of a unit construct of the carbon super-structure material, and has the advantages of being exquisite in surface structure, developed in internal pores, high in mechanical strength, rich in heteroatom content, good in thermal stability, stable in chemical property, high in electron conduction rate and the like, and has wide application prospects in the fields of energy storage, catalyst carrier drug transmission, photoelectric devices and the like. The invention relates to a material with a carbon super structure, a preparation method and application thereof (Chinese invention patent, application number 201910890355.5) and reports the preparation of the carbon super structure and the application thereof in the field of energy storage. However, preparing carbon materials with a super-structural morphology is challenging. To date, only a few synthetic methods have been reported for carbon superstructures. These methods typically require multi-step reactions and cumbersome assembly processes, or complex processes involving complex template use and subsequent etching steps to prepare the polymer precursors, greatly limiting practical applications. For example, the invention entitled "a novel polyacrylonitrile system for the preparation of multifunctional carbon patterns and other superstructures" (chinese patent application No. 201980048681. X) provides a method for making a nanostructured carbon superstructure shape of polyacrylonitrile, which is prepared by: the method comprises the steps of forming a polymer precursor in a polyacrylonitrile super-structure shape by using monomer acrylonitrile and initiator azodiisobutyronitrile to carry out free radical polymerization in an organic solvent, and carbonizing the polymer precursor at a high temperature to obtain the super-structure carbon material. However, this method involves the use of the explosive reagent azobisisobutyronitrile, which is harmful to the human body and pollutes the environment; the internal pressure of the reactor increases rapidly during the polymerization process, and the requirements on the reactor are high. Therefore, a simple and efficient preparation method of the carbon super-structure material is urgent to develop.
Disclosure of Invention
The invention aims to disclose a preparation method of a porous carbon super-structure material. The carbon super-structure material prepared by the method has the advantages of exquisite surface structure, high specific surface, developed internal pores, rich heteroatom content, good thermal stability and the like, and can be used as an ideal super-capacitor electrode material.
In order to achieve the purpose, the invention selects cyanuric chloride and 2, 6-diaminoanthraquinone to generate nucleophilic substitution reaction in acetonitrile solvent to generate polymer precursor, and the porous carbon super-structure material is prepared after synchronous carbonization/chemical activation. The preparation method is simple in process and does not need complex and harsh experimental conditions, and the prepared carbon super-structure material has ultrahigh specific surface area, hierarchical porous structure and nitrogen and oxygen heteroatoms. These features enhance carbon electrode interface wettability, provide ion fast transport channels to achieve high rate performance, generate significant faraday reactions to contribute pseudocapacitance, which when used as supercapacitor electrode materials, exhibit excellent specific capacitance, significant rate performance, and superior cycling stability.
The specific preparation process comprises the following steps:
according to the following steps of 1:0.9 to 3.9: sequentially weighing cyanuric chloride, 2, 6-diaminoanthraquinone and acetonitrile according to the mass ratio of 50-200, dissolving cyanuric chloride and 2, 6-diaminoanthraquinone in acetonitrile, uniformly mixing, reacting for 360min at 30-80 ℃ at the stirring speed of 300-800 r/min, filtering, washing with ethanol, drying to obtain a polymer precursor, and mixing the polymer precursor with sodium cyanate according to the mass ratio of 1: mixing at a mass ratio of 0.5-3, placing in a tube furnace, protecting with inert gas, and keeping at 2-20deg.C for min -1 Heating to 600-1000 ℃ for carbonization, keeping the temperature for 2-3 hours, and naturally cooling to room temperature to obtain the porous carbon super-structure material.
The invention has the following advantages:
1. compared with the prior art, the invention has simple process, does not need templates and complex and harsh experimental conditions and high-pressure equipment.
2. The polymer precursor synthesized in the invention has the function of 'all-in-one', simultaneously serves as a carbon source, a nitrogen source and an oxygen source, and can effectively and uniformly introduce hetero atoms into a porous carbon super-structure material framework, thereby enhancing the surface wettability when the polymer precursor is used as an electrode material, improving the transmission and diffusion kinetics of electrolyte ions in a material pore canal, and endowing the electrode material with excellent electrochemical performance.
3. The porous carbon super-structure material prepared by the invention is formed by stacking laminated structures embedded by nano particles, and has huge specific surface area (1431-1993 m 2 g -1 ) The unique micro/mesoporous structure (concentrated at 0.54, 0.82, 1.28 and 2-10 nm), and rich nitrogen and oxygen heteroatoms (9.76-10.22/4.85-5.66 wt.%) are used as electrode materials of super capacitor, and the analysis test shows that the specific capacitance reaches more than 400F/g when the super capacitor is charged and discharged under 1A/g, the capacity retention rate after 1000000 times of cyclic charge and discharge is more than 90%, and the super capacitor has high specific capacitance and excellent cyclic stability.
Drawings
FIG. 1 is a scanning electron microscope image of a porous carbon superstructures material prepared in example 1 of the present invention.
Fig. 2 is a nitrogen adsorption/desorption isotherm of the porous carbon superstructure material prepared in example 1 of the present invention.
FIG. 3 is a graph showing the pore size distribution of the porous carbon superstructure material prepared in example 1 of the present invention.
FIG. 4 is a scanning electron microscope image of the porous carbon superstructure material prepared in example 2 of the present invention.
Fig. 5 is a nitrogen adsorption/desorption isotherm of the porous carbon superstructure material prepared in example 2 of the present invention.
FIG. 6 is a graph showing pore size distribution of the porous carbon superstructure material prepared in example 2 of the present invention.
FIG. 7 is a scanning electron microscope image of the porous carbon superstructure material prepared in example 3 of the present invention.
Fig. 8 is a nitrogen adsorption/desorption isotherm of the porous carbon superstructure material prepared in example 3 of the present invention.
FIG. 9 is a graph showing pore size distribution of the porous carbon superstructure material prepared in example 3 of the present invention.
Detailed Description
Example 1
According to the following steps of 1:2: sequentially weighing cyanuric chloride, 2, 6-diaminoanthraquinone and acetonitrile according to the mass ratio of 79, dissolving cyanuric chloride and 2, 6-diaminoanthraquinone in acetonitrile, uniformly mixing, stirring at a stirring speed of 500 revolutions per minute,the reaction was carried out at 70℃for 120min. Filtering, washing with ethanol and drying to obtain a polymer precursor, mixing the polymer precursor with sodium cyanate at a ratio of 1: mixing at a mass ratio of 0.5, placing in a tube furnace, protecting with inert gas, and standing at 2deg.C for min -1 Heating to 700 ℃ at a heating rate, carbonizing, keeping the temperature for 3 hours, and naturally cooling to room temperature to obtain the porous carbon super-structure material.
Please refer to fig. 1: the product obtained in example 1 was visible by electron microscopy: stacked by carbon nanoparticle-intercalated layered structure with 1866m 2 g -1 The unique micro/meso pore structure was concentrated at 0.54, 0.82, 1.28 and 2.73nm (fig. 3), and rich nitrogen and oxygen heteroatoms (10.87/5.66 wt.%).
Example 2
According to the following steps of 1:2.9:158, sequentially weighing cyanuric chloride, 2, 6-diaminoanthraquinone and acetonitrile according to the mass ratio, dissolving cyanuric chloride and 2, 6-diaminoanthraquinone in acetonitrile, uniformly mixing, and reacting for 120min at 70 ℃ at the stirring speed of 500 revolutions per minute. Filtering, washing with ethanol and drying to obtain a polymer precursor, mixing the polymer precursor with sodium cyanate at a ratio of 1:1, and placing in a tube furnace under the protection of inert gas at 5 ℃ for min -1 Heating to 800 ℃ at a heating rate, carbonizing, keeping the temperature for 2 hours, and naturally cooling to room temperature to obtain the porous carbon super-structure material.
Please refer to fig. 4: the product obtained in example 2 was visible by electron microscopy: stacked by carbon nanoparticle-intercalated layered structure with 1431m 2 g -1 The unique micro/meso pore structure was concentrated at 0.54, 0.82, 1.28 and 2.73nm (fig. 6), and rich nitrogen and oxygen heteroatoms (9.76/4.85 wt.%).
Example 3
According to the following steps of 1:1.5:158, sequentially weighing cyanuric chloride, 2, 6-diaminoanthraquinone and acetonitrile according to the mass ratio, dissolving cyanuric chloride and 2, 6-diaminoanthraquinone in acetonitrile, uniformly mixing, and reacting for 120min at 70 ℃ under the stirring speed of 350 revolutions per minute. Filtering, washing with ethanol and drying to obtain a polymer precursor, mixing the polymer precursor with sodium cyanate at a ratio of 1:1, mixing and placingIn a tube furnace, inert gas is used for protecting the tube furnace at 3 ℃ for min -1 Heating to 700 ℃ at a heating rate, carbonizing, keeping the temperature for 2 hours, and naturally cooling to room temperature to obtain the porous carbon super-structure material.
Please refer to fig. 7: the product obtained in example 3 was visible by electron microscopy: stacked from a layered structure with carbon nanoparticles intercalated with 1993m 2 g -1 The unique micro/meso pore structure was concentrated at 0.54, 0.82, 1.28 and 2-10nm (fig. 9), and rich nitrogen and oxygen heteroatoms (10.22/5.04 wt.%).
Example 4
Weighing the porous carbon superstructure material obtained in the example 1 or 2 or 3 according to the mass ratio: 60wt% polytetrafluoroethylene emulsion (purchased from Shanghai Sanyi Fu New Material Co., ltd.): graphite=8:1:1, after mixing uniformly, placing in an oven for drying, pressing the dried sample on foam nickel (purchased from Changsha Yuan New Material Co., ltd.) under a pressure of 20MPa, and vacuum drying at 100deg.C for 24 hours to prepare an electrode sheet. The electrode slice is used as a working electrode, and the concentration of the electrode slice is 1mol/LH 2 SO 4 Electrochemical performance was tested in solution. When the sample electrode (working electrode) was charged and discharged at 1.0A/g, the specific capacitance (of examples 1, 2 and 3) was 400F/g or more, and the capacity retention rate after 1000000 times of cyclic charging and discharging was 90% or more, showing high specific capacitance and superior cyclic stability.
All the raw materials are commercial reagent grade products.
Claims (1)
1. A preparation method of a porous carbon super-structure material is characterized by comprising the following steps: according to cyanuric chloride: 2, 6-diaminoanthraquinone: acetonitrile = 1:0.9 to 3.9: weighing 50-200 mass ratio, dissolving cyanuric chloride and 2, 6-diaminoanthraquinone in acetonitrile, uniformly mixing, reacting for 360min at 30-80 ℃ at the stirring speed of 300-800 rpm, filtering, washing with ethanol, drying to obtain a polymer precursor, and then preparing the polymer precursor according to the following steps: sodium cyanate = 1: weighing and mixing the materials according to the mass ratio of 0.5-3, placing the materials into a tube furnace, and protecting the materials by inert gas according to the temperature of 2-20 ℃ for min- 1 Heating to 600-1000 ℃ for carbonization,keeping the temperature for 2-3 h, naturally cooling to room temperature to obtain the porous carbon super-structure material;
the inert gas is one of nitrogen, argon and helium;
all the raw materials are commercial reagent grade products.
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| CN108766775B (en) * | 2018-05-25 | 2019-05-28 | 常州大学 | A kind of preparation method and applications of ultralow temperature high capacity supercapacitor |
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| WO2016175879A1 (en) * | 2015-04-30 | 2016-11-03 | The Board Of Trustees Of The Leland Stanford Junior University | Microporous/mesoporous carbon |
| CN108033436A (en) * | 2018-01-09 | 2018-05-15 | 西北师范大学 | A kind of preparation method based on organic covalently nitrogen-doped porous carbon material of frame |
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Non-Patent Citations (1)
| Title |
|---|
| Ziyang Zhou et al.."Highly active N,O-doped hierarchical porous carbons for high-energy supercapacitors".《Chinese Chemical Letters》.2020,第31卷1226-1230. * |
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