CN112331490A - Preparation method of supercapacitor electrode material - Google Patents
Preparation method of supercapacitor electrode material Download PDFInfo
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- CN112331490A CN112331490A CN202011153692.5A CN202011153692A CN112331490A CN 112331490 A CN112331490 A CN 112331490A CN 202011153692 A CN202011153692 A CN 202011153692A CN 112331490 A CN112331490 A CN 112331490A
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- 239000007772 electrode material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 58
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 239000000243 solution Substances 0.000 claims abstract description 24
- OYFRNYNHAZOYNF-UHFFFAOYSA-N 2,5-dihydroxyterephthalic acid Chemical compound OC(=O)C1=CC(O)=C(C(O)=O)C=C1O OYFRNYNHAZOYNF-UHFFFAOYSA-N 0.000 claims abstract description 22
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 238000004090 dissolution Methods 0.000 claims abstract description 12
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims abstract description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 235000019441 ethanol Nutrition 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 7
- 229940110728 nitrogen / oxygen Drugs 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 239000012046 mixed solvent Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 238000003860 storage Methods 0.000 abstract description 4
- 230000005611 electricity Effects 0.000 abstract description 2
- 239000006260 foam Substances 0.000 abstract 3
- 239000000203 mixture Substances 0.000 description 15
- 239000012621 metal-organic framework Substances 0.000 description 7
- 239000003990 capacitor Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229920001940 conductive polymer Polymers 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 239000013099 nickel-based metal-organic framework Substances 0.000 description 2
- 239000013110 organic ligand Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000013114 Co-MOF-74 Substances 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013246 bimetallic metal–organic framework Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229940075397 calomel Drugs 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000013265 porous functional material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 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
- H01G11/84—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
-
- 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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, 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
-
- 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)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a preparation method of a supercapacitor electrode material, which comprises the steps of putting foam nickel with a certain thickness into an ultrasonic machine by using acetone, dilute hydrochloric acid, deionized water and ethanol as solvents in sequence, carrying out ultrasonic treatment for 10min respectively, taking out the foam nickel and putting the foam nickel into a vacuum drying oven for drying; adding cobalt nitrate and zinc nitrate into N, N-dimethylacetamide, carrying out ultrasonic full dissolution, then adding 2, 5-dihydroxyterephthalic acid into another solvent, carrying out ultrasonic dissolution, uniformly mixing the two solutions, then transferring the two solutions into a high-pressure reaction kettle, putting foamed nickel into the mixed solution of the high-pressure reaction kettle, standing, then covering the reaction kettle, placing the reaction kettle in an oven, cooling, taking out the foamed nickel, washing the foamed nickel with absolute ethyl alcohol, placing the obtained product in a tubular furnace, introducing mixed gas, roasting the obtained product at a high temperature for a period of time, and cooling to obtain the electrode material. The electrode material has higher specific capacity, namely has excellent electricity storage performance.
Description
Technical Field
The invention belongs to the technical field of electrode materials of a super capacitor, and particularly relates to a preparation method of an electrode material of a super capacitor.
Background
The electrochemical super capacitor is a novel energy storage device, generally called super capacitor, and has the characteristics of rapid storage capacity, high power density, long cycle life and the like. The charge storage and capacitance of supercapacitors are largely dependent on the electrode materials, which are mainly carbon materials, conducting polymers and transition metal oxy/sulfides. The carbon-based electrode material has the main advantages of excellent conductivity, good chemical stability and thermal stability, wide range of applications and low cost; the conductive polymer material has the advantages of high conductivity, higher specific capacitance, low price, simple preparation and the like. In recent years, metal organic framework materials are also used in supercapacitor electrode materials.
The Metal Organic Frameworks (MOFs) are a novel porous functional material, and are formed by self-assembly of metal ions or metal clusters and organic ligands through coordination bonds. The metal organic framework material has the advantages of high specific surface area, easy synthesis, regular and adjustable pore structure, high porosity, ordered porous structure, exposed active sites, diversity of chemical compositions of organic ligands and metal nodes, and extremely easily-controllable functionality and chemical properties. However, the direct use of MOFs as supercapacitor electrode materials is very limited, and the existing MOFs materials as supercapacitor electrode materials have the defects of low specific capacity, poor conductivity, poor stability and the like, and researchers have conducted extensive research on them.
Documents J.Yang, C.ZHEN, P.Xiong, Y.Li and M.Wei, Zn-doped Ni-MOF material with a high performance, J.Mater.chem.A,2014,2,19005 report that flower-shaped microspheres are prepared by doping Zn ions in Ni-MOF in a hydrothermal method, and the specific capacitance of the microspheres can reach 1620F/g when the specific capacitance is 0.25A/g. Chinese patent document CN110085446A discloses a preparation method of an in-situ Ni-doped Co-MOF-74 supercapacitor electrode material, wherein the specific capacitance can reach 510F/g and 640F/g under the conditions of current density of 1A/g and current density of 10A/g.
Disclosure of Invention
The invention aims to provide a preparation method of a super capacitor electrode material, which comprises the following steps:
s1: and (3) current collector substrate treatment: pressing foamed nickel with the thickness of 1-1.2 mm into a round shape with the diameter of 7.5mm by using a tablet press, then sequentially using acetone, dilute hydrochloric acid, deionized water and ethanol as solvents, putting the solvents into an ultrasonic machine, performing ultrasonic treatment for 10min respectively, taking the obtained product out, and putting the obtained product into a vacuum drying oven for drying; the step is mainly to achieve the purpose of removing impurities, organic matters and an oxide layer on the surface of the foamed nickel.
S2: adding cobalt nitrate and zinc nitrate into N, N-dimethylacetamide, and carrying out ultrasonic full dissolution, wherein the molar ratio of the cobalt nitrate to the zinc nitrate is 1: 0.76-0.92, so as to obtain a solution I; then adding 2, 5-dihydroxy terephthalic acid into the solvent A, carrying out ultrasonic dissolution to obtain a solution II, uniformly mixing the solution I and the solution II, and then transferring into a high-pressure reaction kettle.
S3: putting the foamed nickel in the step S1 into a high-pressure reaction kettle mixed solution, standing for 3-5 min, then covering the reaction kettle, putting the reaction kettle into an oven, reacting for 20-30 h at 120-150 ℃, cooling, and taking out the foamed nickel, wherein the bimetal rod-shaped MOF synthesized by hydrothermal synthesis in the step S is arranged on a foamed nickel substrate; and then washing the electrode material with absolute ethyl alcohol for 3-5 times, placing the electrode material in a tubular furnace, introducing mixed gas, baking the electrode material for 3-6 hours at 480-500 ℃, and cooling to obtain the electrode material.
Preferably, the solvent a is a mixed solvent of absolute ethyl alcohol and deionized water.
Preferably, the volume ratio of the N, N-dimethylacetamide to the absolute ethyl alcohol to the deionized water is 17mL to 15 mL to 17mL to 3 mL to 5 mL.
Preferably, the mass ratio of the cobalt nitrate and zinc nitrate mixed metal salt to the 2, 5-dihydroxy terephthalic acid is 1g: 0.26-0.32 g.
Preferably, the content ratio of the mixed gas in the step S3 is 75%: 25% nitrogen/oxygen.
The invention has the following beneficial effects:
the electrode material of the super capacitor prepared by the invention adopts a hydrothermal synthesis method to synthesize a cobalt/zinc bimetallic metal organic framework material on a foamed nickel current collector substrate according to the proportion of added metal salt, and then adopts the electrode material obtained by baking in the mixed nitrogen/oxygen atmosphere.
Drawings
FIG. 1 is an XRD pattern of an electrode material prepared in example 1 of the present invention;
fig. 2 is a TEM spectrum of the electrode material prepared in example 1 of the present invention.
Detailed Description
The following examples are provided for the purpose of illustration, and the present invention is not limited to the following examples.
Example 1
A preparation method of a supercapacitor electrode material specifically comprises the following steps:
s1: and (3) current collector substrate treatment: pressing foamed nickel with the thickness of 1mm into a circle with the diameter of 7.5mm by using a tablet press, then sequentially using acetone, dilute hydrochloric acid, deionized water and ethanol as solvents, putting the mixture into an ultrasonic machine for ultrasonic treatment for 10min respectively, taking the mixture out, and putting the mixture into a vacuum drying oven for drying; the step is mainly to achieve the purpose of removing impurities, organic matters and an oxide layer on the surface of the foamed nickel.
S2: adding cobalt nitrate and zinc nitrate into N, N-dimethylacetamide, and carrying out ultrasonic full dissolution, wherein the molar ratio of the cobalt nitrate to the zinc nitrate is 1:0.76, so as to obtain a solution I; then adding 2, 5-dihydroxyterephthalic acid into a mixed solvent of absolute ethyl alcohol and deionized water, carrying out ultrasonic dissolution to obtain a solution II, uniformly mixing the solution I and the solution II, and then transferring the mixture into a high-pressure reaction kettle, wherein the volume ratio of N, N-dimethylacetamide to absolute ethyl alcohol to deionized water is 17:15:3, and the mass ratio of cobalt nitrate to zinc nitrate mixed metal salt to 2, 5-dihydroxyterephthalic acid is 1: 0.26.
S3: putting the foamed nickel in the step S1 into the mixed solution of the high-pressure reaction kettle, standing for 3min, covering the reaction kettle, putting the reaction kettle into an oven, reacting for 20h at 120 ℃, cooling, taking out the foamed nickel, washing for 3 times by using absolute ethyl alcohol, putting the foamed nickel into a tube furnace, and introducing the mixture with the content ratio of 75%: and (3) calcining 25% of nitrogen/oxygen mixed gas at 480 ℃ for 3 hours, and cooling to obtain the electrode material.
Example 2
A preparation method of a supercapacitor electrode material specifically comprises the following steps:
s1: and (3) current collector substrate treatment: pressing foamed nickel with the thickness of 1.2mm into a round shape with the diameter of 7.5mm by using a tablet press, then sequentially using acetone, dilute hydrochloric acid, deionized water and ethanol as solvents, putting the mixture into an ultrasonic machine for ultrasonic treatment for 10min respectively, taking the mixture out, and putting the mixture into a vacuum drying oven for drying; the step is mainly to achieve the purpose of removing impurities, organic matters and an oxide layer on the surface of the foamed nickel.
S2: adding cobalt nitrate and zinc nitrate into N, N-dimethylacetamide, and carrying out ultrasonic full dissolution, wherein the molar ratio of the cobalt nitrate to the zinc nitrate is 1:0.92, so as to obtain a solution I; then adding 2, 5-dihydroxyterephthalic acid into a mixed solvent of absolute ethyl alcohol and deionized water, carrying out ultrasonic dissolution to obtain a solution II, uniformly mixing the solution I and the solution II, and then transferring the mixture into a high-pressure reaction kettle, wherein the volume ratio of N, N-dimethylacetamide to absolute ethyl alcohol to deionized water is 17:17:5, and the mass ratio of cobalt nitrate to zinc nitrate mixed metal salt to 2, 5-dihydroxyterephthalic acid is 1: 0.32.
S3: putting the foamed nickel in the step S1 into the mixed solution of the high-pressure reaction kettle, standing for 5min, covering the reaction kettle, putting the reaction kettle into an oven, reacting for 30h at 150 ℃, cooling, taking out the foamed nickel, washing for 5 times by using absolute ethyl alcohol, putting the obtained product into a tube furnace, and introducing the solution with the content ratio of 75%: 25% of nitrogen/oxygen mixed gas, baking for 6 hours at 500 ℃, and cooling to obtain the electrode material.
Example 3
A preparation method of a supercapacitor electrode material specifically comprises the following steps:
s1: and (3) current collector substrate treatment: pressing foamed nickel with the thickness of 1.1mm into a round shape with the diameter of 7.5mm by using a tablet press, then sequentially using acetone, dilute hydrochloric acid, deionized water and ethanol as solvents, putting the mixture into an ultrasonic machine for ultrasonic treatment for 10min respectively, taking the mixture out, and putting the mixture into a vacuum drying oven for drying; the step is mainly to achieve the purpose of removing impurities, organic matters and an oxide layer on the surface of the foamed nickel.
S2: adding cobalt nitrate and zinc nitrate into N, N-dimethylacetamide, and carrying out ultrasonic full dissolution, wherein the molar ratio of the cobalt nitrate to the zinc nitrate is 1:0.86, so as to obtain a solution I; then adding 2, 5-dihydroxyterephthalic acid into a mixed solvent of absolute ethyl alcohol and deionized water, carrying out ultrasonic dissolution to obtain a solution II, uniformly mixing the solution I and the solution II, and then transferring the mixture into a high-pressure reaction kettle, wherein the volume ratio of N, N-dimethylacetamide to absolute ethyl alcohol to deionized water is 17:16:4, and the mass ratio of cobalt nitrate to zinc nitrate mixed metal salt to 2, 5-dihydroxyterephthalic acid is 1: 0.3.
S3: putting the foamed nickel in the step S1 into the mixed solution of the high-pressure reaction kettle, standing for 4min, covering the reaction kettle, putting the reaction kettle into an oven, reacting for 26h at 140 ℃, cooling, taking out the foamed nickel, washing for 4 times by using absolute ethyl alcohol, putting the foamed nickel into a tube furnace, and introducing the mixture with the content ratio of 75%: 25% of nitrogen/oxygen mixed gas, baking for 5 hours at 490 ℃, and cooling to obtain the electrode material.
Comparative example 1
The supercapacitor electrode material was prepared according to the method described in example 3 of chinese patent document CN 110085446A.
Performance test experiments:
the electrode materials prepared in examples 1-3 and comparative example 1 were used as working electrodes respectively, electrochemical tests were performed at room temperature, in a three-electrode system, the reference electrode was a calomel electrode, the counter electrode was a platinum sheet electrode, the electrolyte was 6mol/L KOH solution, the test system was CHI660E electrochemical workstation, the specific capacitance was tested under the conditions of current density of 1A/g, 5A/g and 10A/g, and the test results are shown in Table 1,
the electrode materials prepared in examples 1 to 3 and comparative example 1 were used as working electrodes, respectively, and the specific capacitance C of the electrode material was measured at a current density of 1A/g0And then after 1000 cycles, the electrode materials of examples 1 to 3 and comparative example 1 were tested for specific capacitance C1Using the formula: w ═ C0-C1)/C0X 100%, calculating the capacity retention rate, wherein the electrode materials prepared in examples 1-3 and comparative example 1The capacity retention rates are respectively maintained at 86.4%, 85.2%, 86.6% and 61.2%, which shows that the electrode material has better cycling stability.
TABLE 1 test results
As can be seen from Table 1, the specific capacitances of the electrode materials prepared in examples 1 to 3 are respectively about 960F/g, 985F/g, 1003F/g and 1123F/g under the conditions of current densities of 1A/g, 5A/g and 10A/g, and compared with the specific capacitances of the electrode material prepared in comparative example 1 of 510F/g, 535F/g, 586F/g and 640F/g under the same conditions, the electrode material provided by the invention has higher specific capacity, namely has more excellent electricity storage performance.
Claims (5)
1. A preparation method of a supercapacitor electrode material is characterized by comprising the following steps:
s1: and (3) current collector substrate treatment: pressing foamed nickel with the thickness of 1-1.2 mm into a round shape with the diameter of 7.5mm by using a tablet press, then sequentially using acetone, dilute hydrochloric acid, deionized water and ethanol as solvents, putting the solvents into an ultrasonic machine, performing ultrasonic treatment for 10min respectively, taking the obtained product out, and putting the obtained product into a vacuum drying oven for drying;
s2: adding cobalt nitrate and zinc nitrate into N, N-dimethylacetamide, and carrying out ultrasonic full dissolution, wherein the molar ratio of the cobalt nitrate to the zinc nitrate is 1: 0.76-0.92, so as to obtain a solution I; then adding 2, 5-dihydroxy terephthalic acid into the solvent A, carrying out ultrasonic dissolution to obtain a solution II, uniformly mixing the solution I and the solution II, and then transferring into a high-pressure reaction kettle;
s3: and (4) placing the foamed nickel in the step S1 into the mixed solution of the high-pressure reaction kettle, standing for 3-5 min, covering the reaction kettle, placing the reaction kettle in an oven, reacting for 20-30 h at 120-150 ℃, cooling, taking out the foamed nickel, washing for 3-5 times with absolute ethyl alcohol, placing the reaction kettle in a tubular furnace, introducing mixed gas, baking for 3-6 h at 480-500 ℃, and cooling to obtain the electrode material.
2. The method for preparing the electrode material of the supercapacitor according to claim 1, wherein the solvent A is a mixed solvent of absolute ethyl alcohol and deionized water.
3. The preparation method of the electrode material of the supercapacitor, according to claim 1, wherein the volume ratio of the N, N-dimethylacetamide, the absolute ethyl alcohol and the deionized water is 17mL: 15-17 mL: 3-5 mL.
4. The preparation method of the electrode material of the supercapacitor as claimed in claim 1, wherein the mass ratio of the cobalt nitrate and zinc nitrate mixed metal salt to the 2, 5-dihydroxyterephthalic acid is 1g: 0.26-0.32 g.
5. The method for preparing the electrode material of the supercapacitor according to claim 1, wherein the mixed gas in the step S3 is 75%: 25% nitrogen/oxygen.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116682675A (en) * | 2023-06-27 | 2023-09-01 | 南华大学 | Preparation method of composite material for super capacitor |
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| CN116682675A (en) * | 2023-06-27 | 2023-09-01 | 南华大学 | Preparation method of composite material for super capacitor |
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