CN113675010A - A method for preparing Ce-Ni-MOF-based supercapacitor electrode material by electrodeposition - Google Patents
A method for preparing Ce-Ni-MOF-based supercapacitor electrode material by electrodeposition Download PDFInfo
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- 239000007772 electrode material Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000013099 nickel-based metal-organic framework Substances 0.000 title claims abstract description 21
- 238000004070 electrodeposition Methods 0.000 title claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 28
- 239000004744 fabric Substances 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims description 13
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 claims description 4
- 229940075397 calomel Drugs 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000008151 electrolyte solution Substances 0.000 claims description 2
- QMKYBPDZANOJGF-UHFFFAOYSA-N trimesic acid Natural products OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 claims 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims 1
- 238000012546 transfer Methods 0.000 abstract description 6
- 239000000758 substrate Substances 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 239000012917 MOF crystal Substances 0.000 abstract description 2
- 239000011230 binding agent Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 230000006911 nucleation Effects 0.000 abstract description 2
- 238000010899 nucleation Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000006258 conductive agent Substances 0.000 abstract 1
- 239000012621 metal-organic framework Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 239000012923 MOF film Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000013246 bimetallic metal–organic framework Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001453 impedance spectrum Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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- 238000013268 sustained release Methods 0.000 description 1
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- 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
- H01G11/84—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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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
-
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- 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
本发明公开了一种电沉积法制备Ce‑Ni‑MOFs基超级电容器电极材料的方法。首先将前处理好的碳布置于配置好的Ce和Ni的电沉积溶液中，在一定的电压下通过电沉积法在碳布表面沉积生成Ce‑Ni‑MOFs电极材料。该方法所述的电极材料不需使用导电剂和粘结剂，而是直接利用电沉积一步合成Ce‑Ni‑MOFs并沉积附着在柔性导电基底碳布的表面。本发明方法操作容易，温和的反应条件和短时间合成过程中的快速电荷转移导致衬底上的MOF晶体的快速成核和生长。该方法制备的产物Ce‑Ni‑MOFs在碳布上分布均匀、密集，结构紧凑，充放电性能好，且生长迅速，风险极低，容易工业化应用。
The invention discloses a method for preparing a Ce-Ni-MOFs-based supercapacitor electrode material by an electrodeposition method. Firstly, the pretreated carbon was arranged in the electrodeposition solution of Ce and Ni, and the electrode material of Ce-Ni-MOFs was deposited on the surface of the carbon cloth by electrodeposition method under a certain voltage. The electrode material described in the method does not need to use conductive agents and binders, but directly uses electrodeposition to synthesize Ce-Ni-MOFs in one step and deposit and attach to the surface of the flexible conductive substrate carbon cloth. The method of the present invention is easy to operate, and the mild reaction conditions and the rapid charge transfer during the short-time synthesis lead to the rapid nucleation and growth of MOF crystals on the substrate. The product Ce-Ni-MOFs prepared by this method has uniform and dense distribution on carbon cloth, compact structure, good charge-discharge performance, rapid growth, extremely low risk, and easy industrial application.
Description
Technical Field
The invention belongs to the technical field of preparation of electrode materials of supercapacitors, and particularly relates to a method for preparing a Ce-Ni-MOF-based electrode material of a supercapacitor by an electrodeposition method.
Background
Supercapacitors (SCS), a type of electrochemical energy storage device, have power density and cycling stability that are superior to batteries and conventional capacitors. In the last decade, the new power type energy storage element which is continuously appeared along with the breakthrough of material science realizes the transformation from the research level to the marketization of the commodity in a short time. Since the world, the global demand is huge, and the method becomes a new highlight in the chemical power industry field. The super capacitor has huge application value and market potential in the fields of electric automobiles, mixed fuel automobiles, special trucks, electric power, railways, communication, national defense and the like, and is widely concerned by countries all over the world. Under the social big background of overall pursuit of sustainable development, the development of efficient, clean and sustainable energy and energy storage and conversion technology is a problem to be solved urgently at present. Although supercapacitors have made significant progress in theoretical research and also in practical applications, the lower energy density and higher production costs still limit the way to commercialization for civilian use. Whether the electrode material has good energy storage characteristics or not directly influences the performance of the supercapacitor. Therefore, parameters such as conductivity, power density and energy density, and cost performance are important factors in the development of electrode materials and the production process of supercapacitors.
Metal-organic frameworks (MOFs) have the characteristics of both inorganic materials and organic materials, and have the unique advantages of high specific surface area, high porosity, adjustable structure, high exposure and uniformly dispersed active sites, and the like, so that the metal-organic frameworks have wide application prospects in many fields, such as gas absorption and storage, catalysis of fine chemical engineering, drug sustained release and the like. The technology for preparing the nano material by using the MOFs material as the template is rapidly developed, and the MOFs material is subjected to heat treatment under a proper condition, so that a carbon material with high conductivity and a metal oxide with rapid oxidation-reduction reaction can be obtained, and the nano material is a porous composite structure with rich pore channels. These characteristics make it extremely potential as an electrode material. Preliminary research on the preparation of morphology-controllable composite structure materials serving as electrode materials by taking single-metal MOFs as templates has been carried out, but the bimetallic MOFs-based electrode materials prepared by utilizing the synergistic effect of bimetal still need to be researched. Therefore, the Ce-Ni bimetal frame structure material is prepared on the carbon cloth by using an electrodeposition method, and the structure and the performance of the Ce-Ni bimetal frame structure material are tested by a series of methods. The product obtained by the electrode material prepared by the method has the advantages of uniform growth, higher purity, excellent charge transfer property, simple operation, reduced use of binder and easy realization of industrial application.
Disclosure of Invention
The invention aims to provide a method for preparing an electrode material of a Ce-Ni-MOF-based supercapacitor by an electrodeposition method.
The method comprises the following specific steps:
(1) selecting 1X 1cm2Carbon Cloth (CC) is used as a substrate material, and the carbon cloth is sequentially subjected to ultrasonic treatment for 30-50 min by using 0.5-1M sulfuric acid, absolute ethyl alcohol and deionized water to obtain a clean surface. And then drying the mixture for 8 to 12 hours at the temperature of between 50 and 100 ℃ for later use.
(2) 1-10 mmol of 1, 3, 5-trimesic acid, 0.5-1.5 mmol of cerium nitrate hexahydrate, 1-5 mmol of nickel nitrate hexahydrate and 30-60 ml of N, N-dimethylformamide are ultrasonically stirred and dissolved for 1-2 hours to obtain a uniformly mixed solution.
(3) Clamping the carbon cloth obtained in the step (1) by using a stainless steel working electrode, placing the carbon cloth in a three-electrode system with a platinum electrode as a counter electrode and a calomel electrode as a reference electrode and a solution obtained in the step (2) as an electrolyte, placing the carbon cloth and the counter electrode in parallel, depositing for 10-60 min at a constant voltage of-1.0-1.5V, taking out the carbon cloth, cleaning the carbon cloth, and drying for 8-12 h at the temperature of 60-100 ℃ to obtain the Ce-Ni-MOF/CC electrode material.
The method of the invention is easy to operate, mild reaction conditions and rapid charge transfer during short-time synthesis lead to rapid nucleation and growth of MOF crystals on the substrate. Directly obtaining the MOF film with the crystallite dimension on the carbon cloth by an electrodeposition method. The obtained product has uniform and compact growth, rapid reaction, extremely low risk and easy industrial application.
Drawings
FIG. 1 is an SEM image of pure carbon cloth and an SEM image of a Ce-Ni-MOF/CC electrode material prepared by an embodiment of the invention
FIG. 2 shows CV tests of Ce-Ni-MOF/CC electrode materials prepared by the embodiment of the invention under different scanning rates.
FIG. 3 shows the GCD test of the Ce-Ni-MOF/CC electrode material prepared by the embodiment of the invention under different current densities.
FIG. 4 is a resistance test of the Ce-Ni-MOF/CC electrode material prepared by the embodiment of the invention.
Detailed Description
Example (b):
(1) selecting 1X 1cm2And (3) taking the carbon cloth as a substrate material, and sequentially performing ultrasonic treatment on the carbon cloth for 30min by using sulfuric acid, absolute ethyl alcohol and deionized water to obtain a clean surface. Then dried at 50 ℃ for 12h to be ready for use.
(2) Dissolving 5mmol of 1, 3, 5-trimesic acid, 1.25mmol of cerium nitrate hexahydrate, 3.75mmol of nickel nitrate hexahydrate and 50ml of N, N-dimethylformamide for 1 hour by ultrasonic stirring to obtain a uniformly mixed solution.
(3) Clamping the carbon cloth obtained in the step (1) by using a stainless steel working electrode, placing the carbon cloth in a three-electrode system with a platinum electrode as a counter electrode, a calomel electrode as a counter electrode and the solution obtained in the step (2) as electrolyte, ensuring that the carbon cloth is parallel to the counter electrode, and depositing for 30min at constant voltage of-1.2V. And then, taking out the carbon cloth, placing the carbon cloth in a vacuum drying oven, and drying for 12 hours at the temperature of 80 ℃ to obtain the Ce-Ni-MOF/CC electrode material.
As can be seen from the comparison between the carbon cloth and the Ce-Ni-MOF/CC electrode material in the SEM representation in FIG. 1, the Ce-Ni MOF is uniformly and densely distributed on the carbon cloth, two metals are grown in a staggered mode, the structure is compact, and more active sites and surface areas can be provided for electrochemical reactions. FIG. 2 is a CV test of the Ce-Ni-MOF/CC electrode material prepared in the embodiment under different sweep rates, and it can be seen from the graph that the response current is linearly increased along with the increase of the sweep rate, and a distinct peak is shown at 0.15V, which indicates that the material undergoes redox reaction during anode and cathode potential scanning, while the shape of the curve is not significantly changed along with the increase of the sweep rate, which indicates that the electrode material has good capacitance and electrochemical reversibility. Fig. 3 shows the GCD test of the Ce-Ni-MOF/CC electrode material prepared in this example under different current densities, and from the figure, two obvious platforms can be seen, which belong to the GCD curve of the battery type, and the effect is consistent with the CV curve in fig. 2. The GCD curves at different current densities in the figure are asymmetric and plateaus appear, indicating good pseudocapacitive properties of this material. Fig. 4 is an electrochemical ac impedance curve of the Ce-Ni-MOF/CC electrode material prepared in this example, the electrochemical ac impedance curve mainly consists of two frequency regions: high frequency region (arc), low frequency region (straight line). The radius of the arc in the high frequency region represents the charge transfer resistance, and the slope of the line in the low frequency region represents the diffusion resistance of electrons in the electrolyte solution. As can be seen from fig. 4, a small radius of the arc is shown in the high frequency region of the ac impedance spectrum, which indicates that the material has a low resistance in charge transfer. The slope is larger in the low-frequency region of the alternating-current impedance spectrogram, which shows that the molecular diffusion seed resistance of the material is smaller and the proton transfer rate is faster.
Claims (2)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114045525A (en) * | 2021-12-03 | 2022-02-15 | 张黎丽 | Nickel-based self-supporting water electrolysis catalyst and preparation method thereof |
| CN114105486A (en) * | 2021-12-24 | 2022-03-01 | 广西大学 | Preparation method of bimetallic center metal organic framework electrochromic film |
| CN114388828A (en) * | 2021-12-29 | 2022-04-22 | 天津大学 | Alloy nanocrystal, carbon cloth loaded with alloy nanocrystal, preparation method and application |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114045525A (en) * | 2021-12-03 | 2022-02-15 | 张黎丽 | Nickel-based self-supporting water electrolysis catalyst and preparation method thereof |
| CN114105486A (en) * | 2021-12-24 | 2022-03-01 | 广西大学 | Preparation method of bimetallic center metal organic framework electrochromic film |
| CN114105486B (en) * | 2021-12-24 | 2024-02-20 | 广西大学 | Preparation method of bimetallic center metal organic framework electrochromic film |
| CN114388828A (en) * | 2021-12-29 | 2022-04-22 | 天津大学 | Alloy nanocrystal, carbon cloth loaded with alloy nanocrystal, preparation method and application |
| CN114388828B (en) * | 2021-12-29 | 2023-08-22 | 天津大学 | Alloy nanocrystalline, carbon cloth loaded with alloy nanocrystalline, preparation method and application |
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Application publication date: 20211119 |