CN112897499A - Method for preparing double-heterogeneous-element-doped porous carbon material by salt template method - Google Patents
Method for preparing double-heterogeneous-element-doped porous carbon material by salt template method Download PDFInfo
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 37
- 150000003839 salts Chemical class 0.000 title claims abstract description 22
- 235000002639 sodium chloride Nutrition 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 20
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical group [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 12
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical group [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims description 6
- 239000001263 FEMA 3042 Substances 0.000 claims description 6
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims description 6
- 150000003841 chloride salts Chemical class 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 6
- 235000011181 potassium carbonates Nutrition 0.000 claims description 6
- 239000001103 potassium chloride Substances 0.000 claims description 6
- 235000011164 potassium chloride Nutrition 0.000 claims description 6
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical group OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims description 6
- 229940033123 tannic acid Drugs 0.000 claims description 6
- 235000015523 tannic acid Nutrition 0.000 claims description 6
- 229920002258 tannic acid Polymers 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea group Chemical group NC(=S)N UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 5
- WZRRRFSJFQTGGB-UHFFFAOYSA-N 1,3,5-triazinane-2,4,6-trithione Chemical compound S=C1NC(=S)NC(=S)N1 WZRRRFSJFQTGGB-UHFFFAOYSA-N 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- UBIJTWDKTYCPMQ-UHFFFAOYSA-N hexachlorophosphazene Chemical compound ClP1(Cl)=NP(Cl)(Cl)=NP(Cl)(Cl)=N1 UBIJTWDKTYCPMQ-UHFFFAOYSA-N 0.000 claims description 3
- 229920001661 Chitosan Polymers 0.000 claims description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 229920000609 methyl cellulose Polymers 0.000 claims description 2
- 239000001923 methylcellulose Substances 0.000 claims description 2
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 2
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 2
- 239000011736 potassium bicarbonate Substances 0.000 claims description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- 239000003990 capacitor Substances 0.000 abstract description 3
- 239000007772 electrode material Substances 0.000 abstract description 3
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 40
- 229910052757 nitrogen Inorganic materials 0.000 description 20
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 17
- 229910052717 sulfur Inorganic materials 0.000 description 17
- 239000011593 sulfur Substances 0.000 description 17
- 239000002002 slurry Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 6
- 239000002033 PVDF binder Substances 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 238000010000 carbonizing Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 239000011888 foil Substances 0.000 description 4
- 239000003365 glass fiber Substances 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 4
- 229960001763 zinc sulfate Drugs 0.000 description 4
- 229910000368 zinc sulfate Inorganic materials 0.000 description 4
- 239000012300 argon atmosphere Substances 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
Images
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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
- 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)
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- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention relates to a method for preparing a double-heterogeneous element doped porous carbon material by a salt template method. When the material is used as a capacitive electrode material of a zinc ion hybrid capacitor, the high specific surface area of the material can provide electric double layer capacitance, and the doped heterogeneous elements can provide pseudo capacitance and increase charge storage of the porous carbon material. At 0.5A g‑1At a current density of up to 75mAh g‑1(ii) a At 10A g‑1Current density of 5000 cycles still having 50mAh g‑1Exhibits excellent large current cycle performance.
Description
Technical Field
The invention belongs to the field of porous material preparation, and relates to a method for preparing a double-heterogeneous element doped porous carbon material by a salt template method.
Background
The porous carbon material has the advantages of low price, easy obtaining, simple preparation, high specific surface area, high porosity, high conductivity and the like, can be widely applied to the fields of energy storage and conversion, adsorbents, gas storage, catalyst carriers and the like, and is paid more and more attention by researchers. The porous carbon material prepared by the method has double-layer capacitance provided by developed pores and pseudo capacitance introduced by heterogeneous elements. In addition, the doping of the heterogeneous elements can improve the conductivity and the surface characteristics of the material, thereby being beneficial to improving the electrochemical performance of the porous carbon material.
Considering that the preparation process of the porous carbon material is relatively complicated, and the specific surface area is difficult to reach 2000m2 g-1. Therefore, the porous carbon material with high specific surface area and double heterogeneous element doping is designed, the long cycle life is realized under the high current density, and the method has important significance for the research of the electrode material of the hybrid capacitor.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a method for preparing a double-heterogeneous element doped porous carbon material by a salt template method.
Technical scheme
A method for preparing a double-heterogeneous element doped porous carbon material by a salt template method is characterized by comprising the following steps:
step 1: dissolving a carbon source, a heterogeneous element doping source and a salt template into deionized water at a mass ratio of 1: 0.5-1: 1-20 to obtain a uniformly mixed solution; the mass ratio of the carbon source to the chloride salt is 1: 1-1: 20;
step 2: and (3) after freeze drying the mixed solution, firstly heating to 250-550 ℃ and preserving heat for 1-5 hours at the heating rate of 0.5-30 ℃/min under the inert atmosphere, and then heating to 600-1200 ℃ and preserving heat for 1-5 hours to obtain the double-heterogeneous-element-doped porous carbon material.
Chloride salt in the salt template: the mass ratio of the carbonate or the bicarbonate is 1: 1-1: 10.
The carbon source is tannic acid, glucose, sucrose, starch, methylcellulose or chitosan.
The heterogeneous element doping source is thiourea, trithiocyanuric acid or hexachlorocyclotriphosphazene.
The chloride salt in the salt template is potassium chloride, sodium chloride or zinc chloride.
The carbonate or bicarbonate in the salt template is potassium carbonate, potassium bicarbonate, sodium carbonate or sodium bicarbonate.
Advantageous effects
According to the method for preparing the double-heterogeneous-element-doped porous carbon material by the salt template method, the carbon source, the heterogeneous element doping source and the salt template are mixed, freeze-dried and subjected to simple carbonization treatment, so that the double-heterogeneous-element-doped porous carbon material can be obtained, the preparation process is simple and efficient, and the obtained porous carbon material is developed in pores and excellent in conductivity. When the material is used as a capacitive electrode material of a zinc ion hybrid capacitor, the high specific surface area of the material can provide electric double layer capacitance, and the doped heterogeneous elements can provide pseudo capacitance and increase charge storage of the porous carbon material. At 0.5A g-1At a current density of up to 75mAh g-1(ii) a At 10A g-1Current density of 5000 cycles still having 50mAh g-1Exhibits excellent large current cycle performance.
Drawings
Fig. 1 is a scanning electron microscope image of the nitrogen/sulfur co-doped porous carbon material prepared in example 1 of the method of the present invention.
Fig. 2 is an X-ray photoelectron spectrum of the nitrogen/sulfur co-doped porous carbon material prepared in example 1 of the method of the present invention.
Fig. 3 is a nitrogen adsorption/desorption curve and a pore size distribution diagram of the nitrogen/sulfur co-doped porous carbon material prepared in example 1 of the method of the present invention.
Fig. 4 is a rate performance test chart of the nitrogen/sulfur co-doped porous carbon material prepared in embodiment 1 of the method of the present invention.
FIG. 5 shows that the nitrogen/sulfur co-doped porous carbon material prepared in example 1 of the present invention is at 10A g-1Cycle performance test chart under the condition.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example 1:
1.2g of tannic acid, 2.4g of trithiocyanuric acid, 1.2g of potassium chloride and 8g of potassium carbonate are dissolved in 30mL of deionized water, and are frozen and dried after being uniformly stirred. And carbonizing the freeze-dried product at high temperature in a tubular furnace, heating to 550 ℃ at the heating rate of 1 ℃/min and preserving heat for 1 hour under the argon atmosphere, heating to 800 ℃ at the heating rate of 3 ℃/min and preserving heat for 1 hour, cooling to room temperature, washing and drying the obtained black powder, and obtaining the nitrogen/sulfur co-doped porous carbon material shown in the attached drawing 1.
Preparing slurry from the obtained nitrogen/sulfur co-doped porous carbon material, conductive carbon black and PVDF according to the mass ratio of 8:1:1, uniformly coating the slurry on an aluminum foil coated with carbon on the surface to serve as a positive electrode, a zinc sheet as a negative electrode, 2mol/L zinc sulfate solution as electrolyte and glass fiber as a diaphragm, and assembling the button cell. The current density was 0.5A g-1The capacity is as high as 75mAh g-1(ii) a The current density rises to 5A g-1Still had 53.7mAh g-1Has excellent rate characteristics. At 10A g-1Current density of 5000 cycles still having 50mAh g-1Exhibits excellent large current cycle performance.
Fig. 1 is a scanning electron microscope image of the nitrogen/sulfur co-doped porous carbon material, and it can be seen that the material has a developed pore structure. Referring to the XPS test of fig. 2, it can be calculated that the nitrogen content is 7.47 at%, the sulfur content is 1.36 at%, and the oxygen content is 3.88 at% in the nitrogen/sulfur co-doped porous carbon material. As can be seen from FIG. 3, the specific surface area of the resulting product was 2180.84m2g-1Pore volume of 1.22cm3 g-1. Fig. 4 is a multiplying power performance test chart of the nitrogen/sulfur co-doped porous carbon material, and it can be seen that the nitrogen/sulfur co-doped porous carbon material has excellent multiplying power characteristics under different current densities: the current density was 0.5A g-1The capacity is as high as 75mAh g-1(ii) a The current density rises to 5A g-1The capacity was 53.7mAh g-1. As shown in FIG. 5, the nitrogen/sulfur co-doped porous carbon material was at 10A g-1Current density of 5000 cycles still having 50mAh g-1Exhibits excellent large current cycle performance.
Example 2:
dissolving 1.2g of tannic acid, 0.6g of trithiocyanuric acid, 1g of potassium chloride and 10g of potassium carbonate in 30mL of deionized water, uniformly stirring, freeze-drying the solution, then carbonizing at high temperature in a tubular furnace, firstly heating to 550 ℃ at the heating rate of 1 ℃/min under the argon atmosphere, preserving heat for 1 hour, then heating to 800 ℃ at the heating rate of 3 ℃/min, preserving heat for 1 hour, then cooling to room temperature, washing and drying the obtained black powder, and obtaining the nitrogen/sulfur co-doped porous carbon material.
Preparing slurry from the obtained nitrogen/sulfur co-doped porous carbon material, conductive carbon black and PVDF according to the mass ratio of 8:1:1, uniformly coating the slurry on an aluminum foil coated with carbon on the surface to serve as a positive electrode, a zinc sheet as a negative electrode, 2mol/L zinc sulfate solution as electrolyte and glass fiber as a diaphragm, and assembling the button cell. When the current density is 0.1A g-1The capacity is 127mAh g-1The current density is increased to 10A g-1The capacity can reach 48mAh g-1At 5A g-1After 10000 cycles of circulation under the current density, the capacity retention rate is 87%.
Example 3:
dissolving 1.2g of tannic acid, 1.2g of thiourea, 1.2g of potassium chloride and 6g of potassium carbonate in 30mL of deionized water, uniformly stirring, freeze-drying the solution, then carbonizing at high temperature in a tubular furnace, firstly heating to 550 ℃, preserving heat for 1 hour under the atmosphere of argon, then heating to 800 ℃, preserving heat for 1 hour, wherein the heating rates are 3 ℃/min, then cooling to room temperature, washing and drying the obtained black powder, and thus obtaining the nitrogen/sulfur co-doped porous carbon material.
Preparing slurry from the obtained nitrogen/sulfur co-doped porous carbon material, conductive carbon black and PVDF according to the mass ratio of 8:1:1, uniformly coating the slurry on an aluminum foil coated with carbon on the surface to serve as a positive electrode, a zinc sheet as a negative electrode, 2mol/L zinc sulfate solution as electrolyte and glass fiber as a diaphragm, and assembling the button cell. When the current density is 0.1A g-1The capacity is as high as 123mAh g-1The current density is increased to 10A g-1The capacity can reach 47mAh g-1At 5A g-1After 10000 cycles of circulation under the current density, the capacity retention rate is 90 percent.
Example 4:
dissolving 1.2g of tannic acid, 1.2g of hexachlorocyclotriphosphazene, 1.2g of potassium chloride and 8g of potassium carbonate in 30mL of deionized water, uniformly stirring, freeze-drying the solution, then carbonizing at high temperature in a tubular furnace, firstly heating to 250 ℃ under the argon atmosphere, preserving heat for 1 hour, then heating to 850 ℃ and preserving heat for 1 hour, wherein the heating rate is 3 ℃/min, then cooling to room temperature, washing and drying the obtained black powder, and thus obtaining the nitrogen/phosphorus co-doped porous carbon material.
Preparing slurry from the obtained nitrogen/phosphorus co-doped porous carbon material, conductive carbon black and PVDF according to the mass ratio of 8:1:1, uniformly coating the slurry on an aluminum foil coated with carbon on the surface to serve as a positive electrode, a zinc sheet as a negative electrode, 2mol/L zinc sulfate solution as electrolyte and glass fiber as a diaphragm, and assembling the button cell. When the current density is 0.1A g-1Time, capacity is 102mAh g-1The current density is raised to 20A g-1The capacity can reach 42mAh g-1At 5A g-1After 10000 cycles of circulation under the current density, the capacity retention rate is 91 percent.
Claims (6)
1. A method for preparing a double-heterogeneous element doped porous carbon material by a salt template method is characterized by comprising the following steps:
step 1: dissolving a carbon source, a heterogeneous element doping source and a salt template into deionized water at a mass ratio of 1: 0.5-1: 1-20 to obtain a uniformly mixed solution; the mass ratio of the carbon source to the chloride salt is 1: 1-1: 20;
step 2: and (3) after freeze drying the mixed solution, firstly heating to 250-550 ℃ and preserving heat for 1-5 hours at the heating rate of 0.5-30 ℃/min under the inert atmosphere, and then heating to 600-1200 ℃ and preserving heat for 1-5 hours to obtain the double-heterogeneous-element-doped porous carbon material.
2. The method for preparing the double heterogeneous element doped porous carbon material by the salt template method according to claim 1, wherein the method comprises the following steps: chloride salt in the salt template: the mass ratio of the carbonate or the bicarbonate is 1: 1-1: 10.
3. The method for preparing the double heterogeneous element doped porous carbon material by the salt template method according to claim 1, wherein the method comprises the following steps: the carbon source is tannic acid, glucose, sucrose, starch, methylcellulose or chitosan.
4. The method for preparing the double heterogeneous element doped porous carbon material by the salt template method according to claim 1, wherein the method comprises the following steps: the heterogeneous element doping source is thiourea, trithiocyanuric acid or hexachlorocyclotriphosphazene.
5. The method for preparing the double heterogeneous element doped porous carbon material by the salt template method according to claim 1, wherein the method comprises the following steps: the chloride salt in the salt template is potassium chloride, sodium chloride or zinc chloride.
6. The method for preparing the double heterogeneous element doped porous carbon material by the salt template method according to claim 1, wherein the method comprises the following steps: the carbonate or bicarbonate in the salt template is potassium carbonate, potassium bicarbonate, sodium carbonate or sodium bicarbonate.
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