CN113675007A - Electrode with good cycle performance, preparation method thereof and super capacitor - Google Patents
Electrode with good cycle performance, preparation method thereof and super capacitor Download PDFInfo
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- CN113675007A CN113675007A CN202110928739.9A CN202110928739A CN113675007A CN 113675007 A CN113675007 A CN 113675007A CN 202110928739 A CN202110928739 A CN 202110928739A CN 113675007 A CN113675007 A CN 113675007A
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- 239000003990 capacitor Substances 0.000 title description 10
- 238000002360 preparation method Methods 0.000 title description 6
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 claims abstract description 26
- 229910002518 CoFe2O4 Inorganic materials 0.000 claims abstract description 25
- 239000000758 substrate Substances 0.000 claims abstract description 18
- 239000011149 active material Substances 0.000 claims abstract description 15
- 229910003321 CoFe Inorganic materials 0.000 claims abstract description 9
- 239000011159 matrix material Substances 0.000 claims abstract description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 68
- 229910052759 nickel Inorganic materials 0.000 claims description 33
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 13
- 238000004070 electrodeposition Methods 0.000 claims description 10
- 239000003792 electrolyte Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 239000002243 precursor Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000006260 foam Substances 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 230000001351 cycling effect Effects 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 4
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 claims description 3
- ZAJAQTYSTDTMCU-UHFFFAOYSA-N 3-aminobenzenesulfonic acid Chemical group NC1=CC=CC(S(O)(=O)=O)=C1 ZAJAQTYSTDTMCU-UHFFFAOYSA-N 0.000 claims description 3
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 claims description 3
- 238000000137 annealing Methods 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 238000010907 mechanical stirring Methods 0.000 claims description 3
- 229910052603 melanterite Inorganic materials 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000004146 energy storage Methods 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Classifications
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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
- H01G11/46—Metal oxides
-
- 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
- H01G11/84—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)
- 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)
Abstract
An electrode with good cycle performance comprises a substrate and an active material, wherein the active material comprises spherical CoFe2O4And PEDOT; spherical CoFe2O4Attached to the substrate, PEDOT coated with spherical CoFe2O4On a substrate. In the present invention, by spherical CoFe2O4The electrode is attached to a matrix, so that the active material obtains a larger specific surface area, the specific capacity of the electrode is high, and the energy storage capacity of the electrode is strong. Meanwhile, the high-conductivity polymer PEDOT is directly deposited on the CoFe with the spherical shape2O4The substrate of (2) allows the electrode to obtain excellent rate performance; PEDOT can also increase the specific capacity of the electrode.
Description
Technical Field
The invention relates to a capacitor, in particular to an electrode with good cycle performance, a preparation method thereof and a super capacitor.
Background
The foamed nickel has excellent electrical conductivity. The mechanical toughness and the acid and alkali resistance are good, so the electrode is often used as a substrate of the electrode. The key factors of the performance of the electrode material of the super capacitor in the super capacitor mainly comprise the composition of the material and the morphology of the material. Therefore, how to design the composition of the material and control its morphology is an important issue in the synthesis of supercapacitor materials. Conventional supercapacitor materials include carbon-based materials, conductive polymers and transition metal oxides. Among them, the transition metal oxide has been widely noticed because of its abundant raw material sources, low cost, high theoretical specific capacitance, etc., but its low conductivity and cycling stability limit its commercial application.
Patent CN111847526A discloses a high-capacity super capacitor, the positive electrode of which is CNT/CoFe2O4/Fe3O4A composite material; but it does not consider CoFe2O4The morphology on the positive electrode leads to a need for further improvement in the cycling performance of supercapacitors.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an electrode material with good cycle performance and high capacity, a preparation method thereof and a super capacitor.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: an electrode with good cycle performance comprises a substrate and an active material, wherein the active material comprises spherical CoFe2O4And PEDOT; the spherical CoFe2O4Attached to a substrate, the PEDOT is covered with spherical CoFe2O4On a substrate.
The electrode with good cycling performance is preferably formed by covering the PEDOT with the spherical CoFe through electrochemical deposition2O4On a substrate.
Preferably, the substrate of the electrode with good cycling performance is foamed nickel.
A preparation method of an electrode with good cycle performance comprises the following steps:
1) cutting the foamed nickel into a preset size, and cleaning;
2) 2 parts by mol of FeSO4·7H2O with 1 molar part by weight of CoCl2·6H2Uniformly mixing O in a mixed solution of 10-20L of ethylene glycol and 10-20L of deionized water under mechanical stirring to obtain a precursor solution; the volumes of the ethylene glycol and the deionized water are the same;
3) adding 1-2L of ammonia water into the precursor solution in the step 2), and then placing the foamed nickel in the step 1 into the precursor solution mixed with the ammonia water; then placing the two materials into an autoclave together, and keeping the two materials in the autoclave at the temperature of 150 ℃ and 180 ℃ for 10-15 h;
4) taking out the foamed nickel, cleaning and drying at the temperature of 80 ℃;
5) annealing the dried foam nickel at the temperature of 250-350 ℃ for 1-3 hours;
6) taking the foamed nickel prepared in the step 5) as an anode, and performing electrochemical deposition in electrolyte by adopting a balanced voltage method, wherein the weight concentration of EDOT in the electrolyte is 0.1-5 wt%; the solvent is aminobenzenesulfonic acid solution; the voltage of the electrochemical deposition is 1.2V, and the time is 150-200S;
7) drying the foamed nickel after the step 6) at the temperature of 60-100 ℃ to obtain the product with the attached CoFe2O4Foamed nickel electrode of/PEDOT active material.
In the above method for preparing an electrode with good cycle performance, preferably, in step 1), the nickel foam is washed and dried, and then soaked in ethanol for 20 minutes to 1 hour.
A super capacitor, the electrode with good cycle performance.
Compared with the prior art, the invention has the advantages that: in the present invention, by spherical CoFe2O4The electrode is attached to a matrix, so that the active material obtains a larger specific surface area, the specific capacity of the electrode is high, and the energy storage capacity of the electrode is strong. Meanwhile, the high-conductivity polymer PEDOT is directly deposited on the CoFe with the spherical shape2O4The substrate of (2) allows the electrode to obtain excellent rate performance; PEDOT can also increase the specific capacity of the electrode.
Drawings
FIG. 1 is an SEM photograph of an electrode in example 1.
FIG. 2 is a graph of specific capacities of the electrodes of example 1 at various current densities.
FIG. 3 is a graph showing the cycle characteristics of the electrode of example 1 under a current density of 1A/g.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments described below.
It should be particularly noted that when an element is referred to as being "fixed to, connected to or communicated with" another element, it can be directly fixed to, connected to or communicated with the other element or indirectly fixed to, connected to or communicated with the other element through other intermediate connecting components.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Example 1
An electrode with good cycle performance comprises a matrix and an active material, wherein the matrix adopts foamed nickel; the active material comprises spherical CoFe2O4And PEDOT; spherical CoFe2O4Attached to the substrate, PEDOT coated with spherical CoFe2O4On a substrate. In this embodiment, PEDOT is coated with spherical CoFe by electrochemical deposition2O4On a substrate.
The embodiment also provides a preparation method of the electrode with good cycle performance, which comprises the following steps:
1) cutting the foamed nickel into a preset size, and cleaning; drying, and soaking in ethanol for 30 min;
2) 2 parts by mol of FeSO4·7H2O with 1 molar part by weight of CoCl2·6H2Mixing O in a mixed solution of 20L of ethylene glycol and 20L of deionized water uniformly under the condition of mechanical stirring to obtain a precursor solution;
3) adding 2L of ammonia water into the precursor solution in the step 2), and then placing the foamed nickel in the step 1 into the precursor solution mixed with the ammonia water; then placing the two into an autoclave together, and keeping the two in the autoclave at the temperature of 150 ℃ and 180 ℃ for 12 hours;
4) taking out the foamed nickel, cleaning and drying at the temperature of 80 ℃;
5) annealing the dried foamed nickel at the temperature of 300 ℃ for 2 hours;
6) taking the foamed nickel prepared in the step 5) as an anode, and performing electrochemical deposition in electrolyte by adopting a balanced voltage method, wherein the weight concentration of EDOT in the electrolyte is 2 wt%; the solvent is aminobenzenesulfonic acid solution; the voltage of the electrochemical deposition is 1.2V, and the time is 200S; in this embodiment, when the electrochemical time reaches 200S, the conductivity of the electrode reaches the maximum value, so the deposition time does not need to exceed 200S, but when the time is too short, too little PEDOT is deposited on the electrode, so that the conductivity is not greatly improved.
7) Drying the foamed nickel after the step 6) at the temperature of 80 ℃ to obtain the attached spherical CoFe2O4Foamed nickel electrode of/PEDOT active material.
In this example, CoFe was grown on the resulting nickel foam2O4Of (2) CoFe2O4The structure of (a) is controlled by the structure directing agent and the ratio of the structure directing agent to the solvent; in this example, deionized water was used as spherical CoFe2O4And the glycol is CoFe2O4A directing agent for the nanoparticles; in this example, the volume ratio of ethylene glycol to deionized water was 1:1, and spherical CoFe was grown just on foamed nickel2O4Nanoparticles.
In the embodiment, the electrochemical deposition of a layer of PEDOT on the surface of the electrode can effectively reduce the resistance of the electrode, and spherical CoFe is adhered in the embodiment2O4The conductivity of the foamed nickel electrode of the PEDOT active material is 1.149 multiplied by 10-3Sm-1(ii) a Whereas the conductivity of a nickel foam electrode with attached spherical CoFe2O4 active material, made in the same way but without electrochemically deposited PEDOT, was 7.75X 10-4 Sm-1。
Fig. 1 shows an SEM image of the electrode in this example. In this example, spherical CoFe was adhered to2O4On the foamed nickel electrodeA layer of colloidal PEDOT film is chemically deposited, so that electrolyte ions can be effectively diffused and rapidly move; in which electrons of PEDOT film species can be rapidly transferred to CoFe2O4The spherical layer, thereby making the transfer path of electrons short. The large area PEDOT jelly-like film on the electrode provides fast electron transfer during charge and discharge, resulting in high specific capacitance, excellent conductivity and long cycle life.
In order to test the performance of the electrode obtained in this example, the test was performed using a three-electrode system with 3mol/L KOH as the electrolyte. As shown in FIG. 2, the electrode of this example is at 1 Ag-1Shows 299.2 mAhg-1High specific capacity of (2). As shown in FIG. 3, at a current density of 1A/g, the specific capacitance of the electrode of this example was maintained at 96% or more after 4000 cycles and at 85% or more after 10,000 cycles.
This example also provides a supercapacitor using NF (nickel foam)/CNT as the cathode, and NF (nickel foam)/CoFe2O4The ball/PEDOT was used as an anode to assemble a hybrid supercapacitor. Wherein, the electrolyte is 3mol/L KOH solution, and the diaphragm adopts cellulose membrane.
The super capacitor obtained in the embodiment has excellent energy power density of 616Wkg-1When the density is 230.4 Whkg-1. In addition, after 2000 cycles, the water-based hybrid supercapacitor has a longer cycle life and a capacity retention rate of 91.3%.
Claims (6)
1. An electrode with good cycle performance is characterized in that: comprises a matrix and an active material, wherein the active material comprises spherical CoFe2O4And PEDOT; the spherical CoFe2O4Attached to a substrate, the PEDOT is covered with spherical CoFe2O4On a substrate.
2. The electrode with good cycle performance as claimed in claim 1, wherein: the PEDOT is covered with the spherical CoFe through electrochemical deposition2O4On a substrate.
3. The electrode with good cycle performance as claimed in claim 1, wherein: the substrate is made of foamed nickel.
4. A method for preparing an electrode having good cycle performance according to any one of claims 1 to 3, wherein: the method comprises the following steps:
1) cutting the foamed nickel into a preset size, and cleaning;
2) 2 parts by mol of FeSO4·7H2O with 1 molar part by weight of CoCl2·6H2Uniformly mixing O in a mixed solution of 10-20L of ethylene glycol and 10-20L of deionized water under mechanical stirring to obtain a precursor solution; the volumes of the ethylene glycol and the deionized water are the same;
3) adding 1-2L of ammonia water into the precursor solution in the step 2), and then placing the foamed nickel in the step 1 into the precursor solution mixed with the ammonia water; then placing the two materials into an autoclave together, and keeping the two materials in the autoclave at the temperature of 150 ℃ and 180 ℃ for 10-15 h;
4) taking out the foamed nickel, cleaning and drying;
5) annealing the dried foam nickel at the temperature of 250-350 ℃ for 1-3 hours;
6) taking the foamed nickel prepared in the step 5) as an anode, and performing electrochemical deposition in electrolyte by adopting a balanced voltage method, wherein the weight concentration of EDOT in the electrolyte is 0.1-5 wt%; the solvent is aminobenzenesulfonic acid solution; the voltage of the electrochemical deposition is 1.2V, and the time is 150-200S;
7) drying the foamed nickel after the step 6) at the temperature of 60-100 ℃ to obtain the product with the attached CoFe2O4Foamed nickel electrode of/PEDOT active material.
5. The method for preparing an electrode with good cycle performance according to claim 4, wherein the method comprises the following steps: in the step 1), the foamed nickel is cleaned and dried and then soaked in ethanol for 20 minutes to 1 hour.
6. A supercapacitor, characterized by: an electrode having good cycling performance according to any one of claims 1-3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110928739.9A CN113675007A (en) | 2021-08-13 | 2021-08-13 | Electrode with good cycle performance, preparation method thereof and super capacitor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110928739.9A CN113675007A (en) | 2021-08-13 | 2021-08-13 | Electrode with good cycle performance, preparation method thereof and super capacitor |
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| CN202110928739.9A Pending CN113675007A (en) | 2021-08-13 | 2021-08-13 | Electrode with good cycle performance, preparation method thereof and super capacitor |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104852042A (en) * | 2014-12-20 | 2015-08-19 | 青岛科技大学 | Preparation method and application of cobalt-iron composite oxide nanorods for lithium ion battery anode material |
| CN108190963A (en) * | 2017-12-15 | 2018-06-22 | 郑州大学 | A kind of hollow CoFe of multistage2O4Material, CoFe2O4The preparation method and application of/C composite |
| CN110415989A (en) * | 2019-08-07 | 2019-11-05 | 哈尔滨师范大学 | A kind of method that electrodeposition process prepares the super capacitor material of cobaltous selenide |
-
2021
- 2021-08-13 CN CN202110928739.9A patent/CN113675007A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104852042A (en) * | 2014-12-20 | 2015-08-19 | 青岛科技大学 | Preparation method and application of cobalt-iron composite oxide nanorods for lithium ion battery anode material |
| CN108190963A (en) * | 2017-12-15 | 2018-06-22 | 郑州大学 | A kind of hollow CoFe of multistage2O4Material, CoFe2O4The preparation method and application of/C composite |
| CN110415989A (en) * | 2019-08-07 | 2019-11-05 | 哈尔滨师范大学 | A kind of method that electrodeposition process prepares the super capacitor material of cobaltous selenide |
Non-Patent Citations (1)
| Title |
|---|
| KUNSONG等: "（"The structures of CoFe2O4/PEDOT electrodes effect on the stability and specific capacity for electrochemical energy storage"", 《APPLIED SURFACE SCIENCE》 * |
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