CN110428976B - Preparation method and application of Cu-Co-S-MOF nanosheet - Google Patents
Preparation method and application of Cu-Co-S-MOF nanosheet Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000000243 solution Substances 0.000 claims abstract description 25
- 239000012621 metal-organic framework Substances 0.000 claims abstract description 24
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 24
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000011259 mixed solution Substances 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000012921 cobalt-based metal-organic framework Substances 0.000 claims abstract description 14
- 239000007772 electrode material Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 10
- FTXJFNVGIDRLEM-UHFFFAOYSA-N copper;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O FTXJFNVGIDRLEM-UHFFFAOYSA-N 0.000 claims abstract description 9
- UKODFQOELJFMII-UHFFFAOYSA-N pentamethyldiethylenetriamine Chemical compound CN(C)CCN(C)CCN(C)C UKODFQOELJFMII-UHFFFAOYSA-N 0.000 claims abstract description 9
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- 229910016507 CuCo Inorganic materials 0.000 claims description 10
- 239000006260 foam Substances 0.000 claims description 9
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000013384 organic framework Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000002086 nanomaterial Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000002484 cyclic voltammetry Methods 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 4
- NHPHQYDQKATMFU-UHFFFAOYSA-N [Cu]=S.[Co] Chemical compound [Cu]=S.[Co] NHPHQYDQKATMFU-UHFFFAOYSA-N 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- -1 transition metal sulfide Chemical class 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 229910002090 carbon oxide Inorganic materials 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 238000010277 constant-current charging Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 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
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- INPLXZPZQSLHBR-UHFFFAOYSA-N cobalt(2+);sulfide Chemical compound [S-2].[Co+2] INPLXZPZQSLHBR-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007581 slurry coating method Methods 0.000 description 1
- 210000000130 stem cell Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- H01G11/30—Electrodes characterised by their material
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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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention relates to a preparation method of a Cu-Co-S-MOF nanosheet, which comprises the following steps: s1: dissolving cobalt nitrate hexahydrate in deionized water to obtain a solution A, dissolving 2-methylimidazole in deionized water to obtain a solution B, mixing the solution A and the solution B, and then adding clean foamed nickel for reaction to obtain foamed nickel with Co-MOF; s2: dissolving copper nitrate hexahydrate and cobalt nitrate hexahydrate in isopropanol to obtain a mixed solution C, and adding carbon disulfide and pentamethyldiethylenetriamine into the mixed solution C to obtain a mixed solution D; s3: adding foamed nickel with Co-MOF into the mixed solution D, transferring the mixed solution D into a reaction kettle for hydrothermal reaction, and obtaining the Cu-Co-S-MOF nanosheet after the reaction is finished. Compared with the prior art, the preparation method is environment-friendly, simple in process and convenient for large-scale production, and the obtained Cu-Co-S-MOF nanosheet can obtain excellent electrochemical performance when applied to an electrode material.
Description
Technical Field
The invention relates to the technical field of electrochemistry and nano materials, in particular to a preparation method and application of a Cu-Co-S-MOF nanosheet.
Background
The increasing consumption of fossil fuels and the emission of greenhouse gases have a great impact on the environment, resulting in a growing global demand for sustainable energy supplies. But only sustainable energy is insufficient, and the world needs to explore an efficient, stable and environment-friendly energy storage device to improve the energy storage efficiency. Super Capacitors (SC) have received a great deal of attention as an energy storage device with high power density, long cycle life, low cost, and fast charge and discharge time, and therefore, development and utilization of renewable clean energy sources are becoming more and more important.
Electrodes prepared by conventional slurry coating techniques have two disadvantages: on one hand, the surface area is small, so that the capacity performance is limited; another aspect is that the binder used can reduce the conductivity.
The metal organic framework has a unique crystal structure and chemical diversity, and is widely applied to the fields of water splitting, fuel cells, solar cells, lithium ion batteries, stem cells, sensors, biosensors and the like. Recently, much research has focused on the design and fabrication of MOFs with tunable morphologies. However, the design and fabrication of MOFs is not a practical, or cost-effective, method, which hinders their practical application in the commercial field. To achieve greater cost effectiveness, there is a need to simplify the design and fabrication of MOFs with high electrochemical performance. In recent years, a small amount of MOFs have been reported as the SCs electrode material, but their specific capacity and rate performance are relatively low, and the preparation method is only suitable for laboratory model, so that the industrial application cannot be implemented.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method and application of a Cu-Co-S-MOF nanosheet.
A preparation method of a Cu-Co-S-MOF nanosheet comprises the following steps:
s1: dissolving cobalt nitrate hexahydrate in deionized water to obtain a solution A, dissolving 2-methylimidazole in deionized water to obtain a solution B, mixing the solution A and the solution B, stirring, adding clean foamed nickel for reaction, and drying a reaction product after the reaction is finished to obtain foamed nickel with Co-MOF;
s2: dissolving copper nitrate hexahydrate and cobalt nitrate hexahydrate in isopropanol to obtain a mixed solution C, and adding carbon disulfide and pentamethyldiethylenetriamine into the mixed solution C to obtain a mixed solution D;
s3: adding foamed nickel with Co-MOF into the mixed solution D, transferring the mixed solution D into a reaction kettle for hydrothermal reaction, and obtaining the Cu-Co-S-MOF nanosheet after the reaction is finished.
Further, the Cu-Co-S-MOF nanosheet is CuCo-bearing2S4Foam nickel of @ Co-MOF.
Further, an organic framework in the Cu-Co-S-MOF nanosheet is a cobalt-based metal organic framework.
Further, in the step S1, the molar ratio of cobalt nitrate hexahydrate to 2-methylimidazole is 1: 8.
further, the molar ratio of the copper nitrate hexahydrate to the cobalt nitrate hexahydrate in the mixed solution C is 1: 2.
Further, in step S3, the volume ratio of carbon disulfide to pentamethyldiethylenetriamine is 1: 8.3.
further, in step S3, the mixed solution D is obtained and then immediately placed in a reaction kettle for hydrothermal reaction at 150 ℃ for 8 hours.
The Cu-Co-S-MOF nanosheet prepared by the method can be widely applied to electrode materials.
The transition metal sulfide has higher conductivity and better redox performance than the transition metal oxide, CuCo2S4The method has high theoretical specific capacity and low cost, and cobalt and copper ions have strong oxidation-reduction performance, namely ternary copper cobalt sulfide (CuCo)2S4) The electrochemical performance of the copper sulfide or cobalt sulfide is better than that of binary metal. In addition, CuCo is low in electronegativity2S4Compared with Cu and Co oxides, the copper-based conductive material has excellent conductivity, higher electrocatalytic activity and higher theoretical capacity. According to the invention, MOFs is used as a template to prepare porous carbon/metal oxide, and the porous carbon/metal oxide is applied to an energy storage device.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention directly synthesizes CuCo on the foam nickel2S4The @ Co-MOF electrode material greatly simplifies reaction steps, improves preparation efficiency, ensures that the solution generated in the preparation process is pollution-free, has high atom utilization rate in the whole preparation process and low preparation material cost, and can be used for large-scale industrial production.
2. CuCo prepared by the invention2S4One of the most important characteristics of @ Co-MOF is that the nanomaterial is in a three-dimensional stereo spherical floral cluster structure (see FIG. 1).
3. Prepared by the inventionCuCo2S4The @ Co-MOF nanosheet has high specific capacitance which can reach 950F/g.
Drawings
FIG. 1 is a CuCo solution obtained in example 12S4SEM image of @ Co-MOF nanomaterial at 1 μm;
FIG. 2 is a CuCo solution obtained in example 12S4SEM image of @ Co-MOF nanomaterial at 10 μm;
FIG. 3 is a CuCo solution obtained in example 12S4CV diagram of @ Co-MOF nanomaterials;
FIG. 4 is a CuCo solution obtained in example 12S4The GCD plot of the @ Co-MOF nanomaterials.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
Firstly, growing a cobalt-based metal organic framework (Co-MOF) on foamed nickel (1cm multiplied by 1cm) by adopting a solution method: 0.05M cobalt nitrate hexahydrate was dissolved in 40ml of deionized water and designated solution A. 0.4M 2-methylimidazole was dissolved in 40ml of deionized water and designated solution B. The solution A and the solution B are quickly mixed and stirred, and then the mixture is put into clean foamed nickel to react for 4 hours at room temperature. After the reaction is finished, washing the foamed nickel with the Co-MOF by using ethanol and deionized water, and drying the foamed nickel in a drying oven at 60 ℃.
And secondly, dissolving 0.5mmol of copper nitrate hexahydrate and 1mmol of cobalt nitrate hexahydrate in 5ml of isopropanol to obtain a mixed solution C after the copper nitrate hexahydrate and the cobalt nitrate hexahydrate are completely dissolved, adding 120 mu l of carbon disulfide and 1ml of Pentamethyldiethylenetriamine (PMDTA) to obtain a mixed solution D, immersing the foamed nickel with the Co-MOF in the mixed solution D, and then quickly transferring the foamed nickel with the Co-MOF to a polytetrafluoroethylene hydrothermal kettle to perform solvothermal reaction for 150 ℃ and 8 hours. Cooling to room temperature after the reaction is finished, adding CuCo2S4The foamed nickel of the @ Co-MOF is taken out, washed for 3 times by deionized water and ethanol in turn, and then put into a vacuum drying oven at 60 ℃ for 12 hours.
The Chenghua CHI760e electrochemical workstation detects the material by cyclic voltammetry and constant current charging and dischargingThe specific capacitance and the cyclic stability, and cyclic voltammetry tests show that the material has excellent redox capability. The high specific surface area of the metamaterial is provided with a foundation by using an electron scanning microscope (for representing the surface microstructure of the electrode material). The specific capacitance of the electrode material of the invention reached 950F/g in 2M KOH solution and at a current density of 1A/g. As shown in FIG. 1 and FIG. 2, the electrode material is in a cluster sphere shape, the specific surface area of a three-dimensional structure is increased, the electrode material can be fully contacted with electrolyte, and ion exchange is quicker. According to the GCD curve of FIG. 4, the specific capacitance of 1Ag can be calculated-1The specific capacitance of the capacitor (2) can reach 950F/g at the current density of (3).
Example 2
Clean foam nickel was prepared for use in the following experiments (clean foam nickel was selected as the substrate and example 1 required foam nickel with Co-MOF as the substrate). Dissolving 0.5mmol of copper nitrate hexahydrate and 1mmol of cobalt nitrate hexahydrate in 5ml of isopropanol, adding 120 mu l of carbon disulfide and 1ml of Pentamethyldiethylenetriamine (PMDTA) after the copper nitrate hexahydrate and the cobalt nitrate hexahydrate are completely dissolved, immersing clean foamed nickel in the solution, and then quickly transferring the foamed nickel into a polytetrafluoroethylene hydrothermal kettle to perform solvothermal reaction for 150 ℃ for 8 hours. Cooling to room temperature after the reaction is finished, adding CuCo2S4The foamed nickel is taken out, washed for 3 times by deionized water and ethanol in sequence, and then put into a vacuum drying oven at 60 ℃ for 12 hours.
The Chenhua CHI760e electrochemical workstation adopts cyclic voltammetry and constant-current charging and discharging methods to detect the specific capacitance and cyclic stability of the material, and cyclic voltammetry tests show that the material has excellent redox capability. The high specific surface area of the metamaterial is provided with a foundation by using an electron scanning microscope (for representing the surface microstructure of the electrode material). The specific capacitance of the electrode material of the invention reaches 520F/g in 2M KOH solution and at a current density of 0.5A/g.
Comparative example 1
The morphology, the synthetic material and the specific capacitance of the copper cobalt sulfide electrode material with other morphologies synthesized in the present example are shown in table 1, and it can be seen from the results that the structure synthesized in example 1 has a higher specific capacitance value under the same test environment.
TABLE 1 morphology of copper cobalt sulfide electrode materials, composite materials and specific capacitance
Reference in table 1:
[1]Guo S H,Chen W Q,Li M,et al.Effect of reaction temperature on the amorphous-crystalline transition of copper cobalt sulfide for supercapacitors[J]. Electrochimica Acta,2018,271,498-506.
[2]Lee Y H,Kang B K,Kim M S,et al.Synthesis and Characterization of Highly Uniform CuCo2S4Ball-in-Ball Hollow Nanospheres as High Performance Electrode for Supercapacitors[J].physica status solidi(a),2018,215(20):1700936.
[3]Wang T,Liu M,Ma H.Facile synthesis of flower-like copper-cobalt sulfide as binder-free faradaic electrodes for supercapacitors with improved electrochemical properties[J].Nanomaterials,2017,7(6):140.
[4]Jin C,Cui Y,Zhang G,et al.Synthesis of copper-cobalt hybrid oxide microflowers as electrode material for supercapacitors[J].Chemical Engineering Journal,2018,343: 331-339.
the embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
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| CN112103092B (en) * | 2020-07-27 | 2022-02-11 | 浙江工业大学 | Metal cation doped cobalt polysulfide/cobalt hydroxide composite material and preparation method and application thereof |
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| CN113363080B (en) * | 2021-05-28 | 2023-02-10 | 上海应用技术大学 | A kind of NF@Co-MOF@NiMoO4 composite material and its preparation method and application |
| CN114524465A (en) * | 2022-01-12 | 2022-05-24 | 河北大学 | Preparation method and application of MOF (Metal organic framework) -derived copper-cobalt bimetallic sulfide |
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