CN110164705B - Novel cobalt-iron-based supercapacitor electrode material and preparation method thereof - Google Patents
Novel cobalt-iron-based supercapacitor electrode material and preparation method thereof Download PDFInfo
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- 239000007772 electrode material Substances 0.000 title claims abstract description 56
- FQMNUIZEFUVPNU-UHFFFAOYSA-N cobalt iron Chemical compound [Fe].[Co].[Co] FQMNUIZEFUVPNU-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 49
- 239000008367 deionised water Substances 0.000 claims description 39
- 229910021641 deionized water Inorganic materials 0.000 claims description 39
- 239000011259 mixed solution Substances 0.000 claims description 38
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 28
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 claims description 26
- 229910021577 Iron(II) chloride Inorganic materials 0.000 claims description 26
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 26
- 238000010992 reflux Methods 0.000 claims description 23
- YSWBFLWKAIRHEI-UHFFFAOYSA-N 4,5-dimethyl-1h-imidazole Chemical compound CC=1N=CNC=1C YSWBFLWKAIRHEI-UHFFFAOYSA-N 0.000 claims description 20
- 229910020598 Co Fe Inorganic materials 0.000 claims description 20
- 229910002519 Co-Fe Inorganic materials 0.000 claims description 20
- 239000013078 crystal Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 239000012046 mixed solvent Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000002086 nanomaterial Substances 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 10
- 239000013543 active substance Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 7
- 239000003990 capacitor Substances 0.000 abstract description 4
- 239000011149 active material Substances 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000012983 electrochemical energy storage Methods 0.000 abstract description 2
- 239000008204 material by function Substances 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 31
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 239000002135 nanosheet Substances 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910017709 Ni Co Inorganic materials 0.000 description 1
- 229910003267 Ni-Co Inorganic materials 0.000 description 1
- 229910003262 Ni‐Co Inorganic materials 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229940075397 calomel Drugs 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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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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- 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
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Abstract
The invention provides a novel cobalt-iron-based supercapacitor electrode material and a preparation method thereof, and the novel ultrathin hexagonal supercapacitor electrode material obtained by the method has good electrochemical energy storage capacity, high specific capacitance, good circulation stability and non-toxic and environment-friendly performance; the high-efficiency and light electrode material has wide application prospect in the technical field of novel nanometer functional materials and electrode materials of super capacitors; the prepared composite electrode material has the characteristics of ultralight (the active material mass is less than 2mg), ultrathin (the thickness is less than 100nm) and ultrahigh specific capacitance (1000F/g).
Description
Technical Field
The utility model relates to a material science technical field especially relates to a novel cobalt iron base ultracapacitor system electrode material and preparation method thereof.
Background
Electrochemical pseudocapacitors, also known as supercapacitors, have the advantages of high power density, short charging time, long cycle life, green environmental protection, and the like, and are one of the most promising energy storage devices in modern electronic products. But practical application of supercapacitors is hindered by the lack of suitable cost of high performance electrode materials. Over the past few decades, various electrode materials, including carbonaceous materials, conductive polymers and transition metal oxides, have been used for supercapacitor electrode materials. However, since the energy density of the carbon material is low, the conductive polymer has poor cyclicity in long-term charge/discharge, so that the application of the two materials in an energy storage device is limited; transition metal oxides are ideal electrode materials because they undergo a fast reversible faradaic redox reaction at the electrode/electrolyte interface, but their wide commercialization is limited by their low conductivity.
At present, most of electrode materials for preparing the super capacitor are single metal oxides, and have the defects of low rate capability, low cycling stability and the like, and due to the addition of the second metal in the double metal oxides, a plurality of metal species form a complex microstructure and a mutual synergistic effect, so that higher electrochemical activity can be expressed, and the defects of the single metal oxides are avoided. The current common method for preparing the electrode material of the super capacitor is an efficient reflux method, the preparation process is simple, the process is green and environment-friendly, and the capacitance property of the electrode material is excellent.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a novel cobalt iron base ultracapacitor system electrode material with super high specific capacitance and good cycling stability, and a simple process, convenient operation and the novel cobalt iron base ultracapacitor system electrode material of environmental protection and preparation method thereof.
In order to achieve the above object, the utility model provides a novel cobalt iron base supercapacitor electrode material, novel cobalt iron base supercapacitor electrode material is two-dimentional lamellar structure, and the shape is slice regular hexagon.
Preferably, the side length of the novel cobalt-iron-based supercapacitor electrode material is 1-2 um.
Preferably, the active substance of the novel cobalt-iron-based supercapacitor electrode material is less than 2mg, the thickness of the novel cobalt-iron-based supercapacitor electrode material is less than 100nm, the capacitance of the novel cobalt-iron-based supercapacitor electrode material is more than 1000F/g, and the active substance is a cobalt-iron-based bimetallic nano material.
The invention also provides a preparation method of the novel cobalt-iron-based supercapacitor electrode material, which comprises the following steps:
step 1: introducing nitrogen into the deionized water;
step 2: taking CoCl2·6H2O crystal and FeCl2·4H2Placing the O crystal into a part of mixed solvent of the deionized water and the absolute ethyl alcohol to form a first mixed solution;
and step 3: dissolving dimethyl imidazole into the other part of mixed solvent of the deionized water and the absolute ethyl alcohol to form a second mixed solution;
and 4, step 4: placing the first mixed solution in a beaker and refluxing;
and 5: stirring and heating the first mixed solution;
step 6: slowly adding the second mixed solution to the first mixed solution to form a third mixed solution;
and 7: refluxing the third mixed solution;
and 8: and sequentially carrying out centrifugation, washing and drying on the third mixed solution to obtain the novel cobalt-iron-based supercapacitor electrode material.
Preferably, in step 1, 100ml of deionized water is purged with nitrogen for 30min to remove some CO from the water3 2-。
Preferably, in step 2, the CoCl2·6H2O and FeCl2·4H2The material ratio of O is 1.189 g: 0.3168g, mixing and dissolving the mixture into a mixed solvent of 40-50 ml of the deionized water and 10-0 ml of the absolute ethyl alcohol, and fully stirring.
Preferably, in the step 3, 2.46 to 9.84g of the dimethylimidazole is dissolved in 40 to 50ml of the mixed solvent of the deionized water and 10 to 0ml of the absolute ethyl alcohol, and the mixture is fully stirred.
Preferably, in step 4, the first mixed solution is placed in a three-neck flask and refluxed under an atmosphere of nitrogen.
Preferably, in step 5, the first mixed solution is stirred and heated to 90 ℃.
Preferably, in the step 7, the third mixed solution is refluxed for 5 to 10 hours at 90 ℃ in a nitrogen atmosphere.
Preferably, in step 8, the novel cobalt-iron-based supercapacitor electrode material is a hexagonal Co-Fe nano material.
Compared with the prior art, the utility model has the advantages that: the novel ultrathin hexagonal supercapacitor electrode material has good electrochemical energy storage capacity, high specific capacitance, good circulation stability and non-toxic and environment-friendly performance; the high-efficiency and light electrode material has wide application prospect in the technical field of novel nanometer functional materials and electrode materials of super capacitors; the prepared composite electrode material has the characteristics of ultralight (the active material mass is less than 2mg), ultrathin (the thickness is less than 100nm) and ultrahigh specific capacitance (1000F/g).
Drawings
Fig. 1 is an SEM image of the novel cobalt-iron based supercapacitor electrode material obtained in example 1.
Fig. 2 is an SEM image of the novel cobalt-iron based supercapacitor electrode material obtained in example 5.
FIG. 3 is a cyclic voltammogram of a Co-Fe electrode material.
FIG. 4 is a constant current charge and discharge curve of the Co-Fe electrode material.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention will be further described below.
The invention provides a novel cobalt-iron-based supercapacitor electrode material which is of a two-dimensional layered structure and is in the shape of a sheet regular hexagon.
Preferably, the side length of the novel cobalt-iron-based supercapacitor electrode material is 1-2 um.
Preferably, the active substance of the novel cobalt-iron-based supercapacitor electrode material is less than 2mg, the thickness of the novel cobalt-iron-based supercapacitor electrode material is less than 100nm, the capacitance of the novel cobalt-iron-based supercapacitor electrode material is more than 1000F/g, and the active substance is a cobalt-iron-based bimetallic nano material.
The invention also provides a preparation method of the novel cobalt-iron-based supercapacitor electrode material, which comprises the following steps:
step 1: introducing nitrogen into the deionized water;
step 2: taking CoCl2·6H2O crystal and FeCl2·4H2Placing the O crystal into a part of mixed solvent of deionized water and absolute ethyl alcohol to form a first mixed solution;
and step 3: dissolving dimethyl imidazole into the other part of mixed solvent of deionized water and absolute ethyl alcohol to form a second mixed solution;
and 4, step 4: placing the first mixed solution in a beaker and refluxing;
and 5: stirring and heating the first mixed solution;
step 6: slowly adding the second mixed solution into the first mixed solution to form a third mixed solution;
and 7: refluxing the third mixed solution;
and 8: and sequentially carrying out centrifugation, washing and drying on the third mixed solution to obtain the novel cobalt-iron-based supercapacitor electrode material.
In this example, in step 1, 100ml of deionized water was purged with nitrogen for 30min to remove some CO from the water3 2-。
In this example, in step 2, CoCl2·6H2O and FeCl2·4H2The material ratio of O is 1.189 g: 0.3168g, mixing and dissolving in a mixed solvent of 40-50 ml of deionized water and 10-0 ml of absolute ethyl alcohol, and fully stirring.
In this embodiment, in step 3, 2.46 to 9.84g of dimethylimidazole is dissolved in a mixed solvent of 40 to 50ml of deionized water and 10 to 0ml of anhydrous ethanol, and the mixture is fully stirred.
In this example, in step 4, the first mixed solution was placed in a three-necked flask and refluxed under an atmosphere of nitrogen gas.
In this example, in step 5, the first mixed solution was stirred and heated to 90 ℃.
In this embodiment, in step 7, the third mixed solution is refluxed for 5 to 10 hours at 90 ℃ under a nitrogen atmosphere.
In this embodiment, in step 8, the novel cobalt-iron-based supercapacitor electrode material is a hexagonal Co-Fe nanomaterial, and the Co-Fe-based two-dimensional nanosheet is prepared by using an efficient backflow method, and has the advantages of ultrahigh specific capacitance, good cycle stability and the like.
The invention will be further elucidated by means of specific examples:
example 1
A novel method for preparing a novel cobalt-iron-based supercapacitor electrode material comprises the following steps:
1. introducing nitrogen into 100ml of deionized water for 30min to remove CO in water3 2-;
2. Taking CoCl2·6H2O crystal and FeCl2·4H2O crystals, CoCl2·6H2O and FeCl2·4H2The material ratio of O is 1.189 g: 0.3168g, mixing and adding into 50ml of deionized water, and fully stirring to obtain a pink solution;
3. adding 2.46g of dimethylimidazole into 50ml of deionized water, and fully stirring to obtain a white solution;
4. adding CoCl2·6H2O and FeCl2·4H2Transferring the pink solution obtained by mixing the O into a three-neck flask, refluxing in the nitrogen atmosphere, violently stirring and heating to 90 ℃, then adding the dimethyl imidazole solution into the three-neck flask, and efficiently refluxing for 5 hours in the nitrogen atmosphere at 90 ℃;
5. after the reaction is finished, cooling to room temperature, centrifuging, washing and drying to obtain the hexagonal Co-Fe-based nano material; as shown in fig. 1.
Example 2
1. Introducing nitrogen into 100ml of deionized water for 30min to remove CO in water3 2-;
2. Taking CoCl2·6H2O crystal and FeCl2·4H2O crystals, CoCl2·6H2O and FeCl2·4H2The material ratio of O is 1.189 g: 0.3168g, mixing and adding into a mixed solvent of 45ml of deionized water and 5ml of absolute ethyl alcohol, and fully stirring to obtain a pink solution;
3. adding 2.46g of dimethyl imidazole into a mixed solvent of 45ml of deionized water and 5ml of absolute ethyl alcohol, and fully stirring to obtain a white solution;
4. adding CoCl2·6H2O and FeCl2·4H2Transferring the pink solution obtained by mixing the O into a three-neck flask, refluxing in the nitrogen atmosphere, violently stirring and heating to 90 ℃, then adding the dimethyl imidazole solution into the three-neck flask, and efficiently refluxing for 5 hours in the nitrogen atmosphere at 90 ℃;
5. after the reaction is finished, cooling to room temperature, centrifuging, washing and drying to obtain the hexagonal Co-Fe-based nano material;
example 3
1. Introducing nitrogen into 100ml of deionized water for 30min to remove CO in water3 2-;
2. Taking CoCl2·6H2O crystal and FeCl2·4H2O crystals, CoCl2·6H2O and FeCl2·4H2The material ratio of O is 1.189 g: 0.3168g, mixing and adding into a mixed solution of 40ml of deionized water and 10ml of absolute ethyl alcohol, and fully stirring to obtain a pink solution;
3. adding 2.46g of dimethyl imidazole into a mixed solution of 40ml of deionized water and 10ml of absolute ethyl alcohol, and fully stirring to obtain a white solution;
4. adding CoCl2·6H2O and FeCl2·4H2Transferring the pink solution obtained by mixing the O into a three-neck flask, refluxing in the nitrogen atmosphere, violently stirring and heating to 90 ℃, then adding the dimethyl imidazole solution into the three-neck flask, and efficiently refluxing for 5 hours in the nitrogen atmosphere at 90 ℃;
5. after the reaction is finished, cooling to room temperature, centrifuging, washing and drying to obtain a hexagonal Co-Fe-based nanosheet electrode material;
example 4
1. Introducing nitrogen into 100ml of deionized water for 30min to remove CO in water3 2-;
2. Taking CoCl2·6H2O crystal and FeCl2·4H2O crystals, CoCl2·6H2O and FeCl2·4H2The material ratio of O is 1.189 g: 0.3168g, mixing and adding into 50ml of deionized water, and fully stirring to obtain a pink solution;
3. adding 4.92g of dimethyl imidazole into 50ml of deionized water, and fully stirring to obtain a white solution;
4. adding CoCl2·6H2O and FeCl2·4H2Transferring the pink solution obtained by mixing the O into a three-neck flask, refluxing in the nitrogen atmosphere, violently stirring and heating to 90 ℃, then adding the dimethyl imidazole solution into the three-neck flask, and efficiently refluxing for 5 hours in the nitrogen atmosphere at 90 ℃;
5. after the reaction is finished, cooling to room temperature, centrifuging, washing and drying to obtain the hexagonal Co-Fe-based nano material;
example 5
1. Introducing nitrogen into 100ml of deionized water for 30min to remove CO in water3 2-;
2. Taking CoCl2·6H2O crystal and FeCl2·4H2O crystals, CoCl2·6H2O and FeCl2·4H2The material ratio of O is 1.189 g: 0.3168g, mixing and adding into 50ml of deionized water, and fully stirring to obtain a pink solution;
3. adding 9.84g of dimethylimidazole into 50ml of deionized water, and fully stirring to obtain a white solution;
4. adding CoCl2·6H2O and FeCl2·4H2Transferring the pink solution obtained by mixing the O into a three-neck flask, refluxing in the nitrogen atmosphere, violently stirring and heating to 90 ℃, then adding the dimethyl imidazole solution into the three-neck flask, and efficiently refluxing for 5 hours in the nitrogen atmosphere at 90 ℃;
5. after the reaction is finished, cooling to room temperature, centrifuging, washing and drying to obtain the hexagonal Co-Fe-based nano material;
example 6
1. Introducing nitrogen into 100ml of deionized water for 30min to remove CO in water3 2-;
2. Taking CoCl2·6H2O crystal and FeCl2·4H2O crystals, CoCl2·6H2O and FeCl2·4H2The material ratio of O is 1.189 g: 0.3168g, mixing and adding into 50ml of deionized water, and fully stirring to obtain a pink solution;
3. adding 2.46g of dimethylimidazole into 50ml of deionized water, and fully stirring to obtain a white solution;
4. adding CoCl2·6H2O and FeCl2·4H2Transferring the pink solution obtained by O mixing into a three-neck flask, refluxing under nitrogen atmosphere, vigorously stirring and heating to 90 ℃, and then adding the dimethyl imidazole solution into the three-neck flaskIn a bottle, efficiently refluxing for 10h at 90 ℃ in a nitrogen atmosphere;
5. after the reaction is finished, cooling to room temperature, centrifuging, washing and drying to obtain a hexagonal Co-Fe-based nanosheet electrode material;
example 7
1. Introducing nitrogen into 100ml of deionized water for 30min to remove CO in water3 2-;
2. Taking CoCl2·6H2O and FeCl2·4H2The material ratio of O is 1.189 g: 0.3168g, mixing and adding into 50ml of deionized water, and fully stirring to obtain a pink solution;
3. adding 4.92g of dimethyl imidazole into 50ml of deionized water, and fully stirring to obtain a white solution;
4. adding CoCl2·6H2O and FeCl2·4H2Transferring the pink solution obtained by mixing the O into a three-neck flask, suspending 1 x 1cm of foamed nickel into the solution by using a rope, refluxing in the nitrogen atmosphere, violently stirring and heating to 90 ℃, then adding the dimethyl imidazole solution into the three-neck flask, and efficiently refluxing for 5 hours in the nitrogen atmosphere at 90 ℃;
5. after the reaction is finished and the temperature is cooled to room temperature, taking out the foamed nickel, and washing and drying the foamed nickel to obtain the hexagonal Co-Fe-based nanosheet electrode material as shown in FIG. 2;
example 8
Preparing a Co-Fe electrode slice: mixing the Co-Fe-based nano material prepared in the example 1, acetylene black and a binder according to the mass ratio of 7:2:1, adding a proper amount of absolute ethyl alcohol, grinding into uniform slurry, coating the uniform slurry on a 1 x 2cm foam nickel sheet, drying in vacuum at 80 ℃ for 1h, taking out, compacting under the pressure of 10MPa, and continuously drying in vacuum for 12h to obtain the Co-Fe electrode sheet.
And assembling the prepared Co-Fe-based electrode slice into a standard three-electrode for electrochemical performance test, wherein a platinum electrode is a counter electrode, a calomel electrode is a reference electrode, and electrolyte is 6 MKOH. As can be seen from FIG. 3, the cyclic voltammetry is closed and has distinct oxidation peak and reduction peak, which indicates that the Co-Fe electrode material of the present invention has good pseudocapacitance, and in addition, as the scanning speed increases, the oxidation peak moves towards the more positive potential and the oxidation peak moves towards the more negative potential, which indicates that the Co-Fe electrode material has polarization phenomenon under the condition of high scanning speed. Calculated by using a constant current charge-discharge curve in fig. 4, the specific capacity of the Co-Fe electrode material is 1000F/g at a current density of 1A/g, which is significantly higher than that of Ni-Co prepared by a conventional hydrothermal method (CN106057482, the specific capacity is about 600F/g at a current density of 1A/g), where C is It/mV, C is the specific capacity, I is the current, t is the discharge time, m is the active material mass, and V is the voltage range.
The above description is only for the preferred embodiment of the present invention, and does not limit the present invention. Any technical personnel who belongs to the technical field, in the scope that does not deviate from the technical scheme of the utility model, to the technical scheme and the technical content that the utility model discloses expose do the change such as the equivalent replacement of any form or modification, all belong to the content that does not break away from the technical scheme of the utility model, still belong to within the scope of protection of the utility model.
Claims (1)
1. A novel cobalt-iron-based supercapacitor electrode material is characterized in that the novel cobalt-iron-based supercapacitor electrode material is of a two-dimensional layered structure and is in the shape of a flaky regular hexagon;
the side length of the novel cobalt-iron-based supercapacitor electrode material is 1-2 um;
the novel cobalt-iron-based supercapacitor electrode material has an active substance less than 2mg, a thickness less than 100nm and a capacitance greater than 1000F/g, and the active substance is a cobalt-iron-based bimetallic nano material;
the preparation method of the novel cobalt-iron-based supercapacitor electrode material comprises the following steps:
step 1: introducing nitrogen into the deionized water;
step 2: taking CoCl2∙6H2O crystal and FeCl2∙4H2Placing the O crystal into a part of mixed solvent of the deionized water and the absolute ethyl alcohol to form a first mixed solution;
and step 3: dissolving dimethyl imidazole into the other part of mixed solvent of the deionized water and the absolute ethyl alcohol to form a second mixed solution;
and 4, step 4: placing the first mixed solution in a beaker and refluxing;
and 5: stirring and heating the first mixed solution;
step 6: slowly adding the second mixed solution to the first mixed solution to form a third mixed solution;
and 7: refluxing the third mixed solution;
and 8: sequentially centrifuging, washing and drying the third mixed solution to obtain a novel cobalt-iron-based supercapacitor electrode material;
in step 1, 100ml of deionized water was purged with nitrogen for 30min to remove some CO from the water3 2-;
In step 2, the CoCl2∙6H2O and FeCl2∙4H2The material ratio of O is 1.189 g: 0.3168g, mixing and dissolving the mixture into a mixed solvent of 40-50 ml of the deionized water and 10-0 ml of the absolute ethyl alcohol, and fully stirring;
in the step 3, 2.46-9.84 g of the dimethyl imidazole is dissolved in 40-50 ml of the mixed solvent of the deionized water and 10-0 ml of the absolute ethyl alcohol, and the mixture is fully stirred;
in step 4, placing the first mixed solution into a three-neck flask, and refluxing under the atmosphere of nitrogen;
in step 5, stirring and heating the first mixed solution to 90 ℃;
in the step 7, refluxing the third mixed solution for 5-10 h in a nitrogen atmosphere at 90 ℃;
in step 8, the novel cobalt-iron-based supercapacitor electrode material is a hexagonal Co-Fe nano material.
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Effective date of registration: 20231211 Address after: 231300 Xiazhuang Group, Baijiagang Village, Chunqiu Township, Shucheng County, Lu'an City, Anhui Province Patentee after: Wang Liang Address before: 200093 No. 516, military road, Shanghai, Yangpu District Patentee before: University of Shanghai for Science and Technology |