CN114220670A - Preparation method of non-covalent hybrid MOF graphene aerogel/molybdenum capacitor electrode material - Google Patents
Preparation method of non-covalent hybrid MOF graphene aerogel/molybdenum capacitor electrode material Download PDFInfo
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- CN114220670A CN114220670A CN202111537152.1A CN202111537152A CN114220670A CN 114220670 A CN114220670 A CN 114220670A CN 202111537152 A CN202111537152 A CN 202111537152A CN 114220670 A CN114220670 A CN 114220670A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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 OR LIGHT-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 OR LIGHT-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 OR LIGHT-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
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention belongs to the field of preparation of electrode materials, and particularly relates to a preparation method of a non-covalent hybrid MOF graphene aerogel/molybdenum capacitor electrode material. To the graphene aerogel suspension, molybdenum pentachloride, 2-aminoterephthalic acid, 4-aminobenzoic acid, and HCl were added to a glass vial. The resulting mixture was sonicated. The resulting mixture was transferred to a 120 ℃ oven and then washed with methanol and dried under nitrogen. And then uniformly mixing the prepared non-covalent hybrid MOF graphene aerogel/molybdenum, acetylene black and polytetrafluoroethylene emulsion, blowing the mixture into a paste, coating the paste material on the foamed nickel by using the foamed nickel as a current collector, and performing vacuum drying for 24 hours to finally prepare the required electrode. The non-covalent hybrid MOF graphene aerogel/molybdenum electrode prepared by the invention has the advantages of greenness, no toxicity, low density, excellent electrochemical performance and wide application in portable and flexible electrode materials.
Description
Technical Field
The invention belongs to the field of preparation of electrode materials, and particularly relates to a preparation method of a non-covalent hybrid MOF graphene aerogel/molybdenum capacitor electrode material.
Background
Molybdenum is particularly attractive due to its high ionic conductivity and high alkali cation capacity, making it suitable for use in supercapacitors. The crystal layers are stacked by van der waals force. The weak interaction between the layers promotes the intercalation and de-intercalation of ions. In addition, the ion intercalation interlayer space is large, and the oxidation state range of Mo (Mo) in the oxidation-reduction reaction2+∼Mo6+) Is wider. Therefore, the electrode material has good prospect as an electrode material of the pseudocapacitor. However, Mo has the disadvantage of low conductivity and is prone to agglomeration during the manufacturing process, which may lead to low ion transfer rates and limit effective contact between the active material and the electrolyte. An effective way to overcome these drawbacks is to use a conductive material as a substrate to limit its growth and to increase its conductivity. Graphene is one of the competitive candidates due to its good electrical conductivity, large surface area and excellent chemical stability.
Disclosure of Invention
The invention aims to provide a preparation method of a non-covalent hybrid MOF graphene aerogel/molybdenum capacitor electrode material aiming at the defects of the prior art. The non-covalent hybrid MOF graphene aerogel/molybdenum capacitor electrode prepared by the invention has the advantages of large specific surface area, no toxicity, excellent electrochemical performance and extremely wide application in portable and flexible electrode materials.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a non-covalent hybrid MOF graphene aerogel/molybdenum capacitor electrode material specifically comprises the following steps:
(1) synthesis of graphene aerogel
The preparation method specifically comprises the following steps of: 400mg of graphene oxide was added to 100mL of DI water to obtain 4mg/mL of graphene oxide. After dispersing and sonicating for 2 hours, the suspension was sealed in an autoclave lined with polytetrafluoroethylene and heated to 180 ℃ for 16 hours; after cooling to room temperature, the sample was washed with deionized water; finally, the graphene aerogel was further frozen to-70 ℃ and dried for 48 hours.
(2) Preparation of non-covalent hybrid MOF graphene aerogel/molybdenum
Under ultrasonic treatment, 100 mg of graphene aerogel is dispersed in 10 mL of DMF solution for 30 minutes; adding molybdenum pentachloride, 2-aminoterephthalic acid, 4-aminobenzoic acid and 0.16ml of HCl into the graphene aerogel suspension; sonicating the resulting mixture for 30 minutes; placing the mixture in an oven at 120 ℃ for 2 days; washing the obtained black gel with methanol, and drying at 150 ℃ in a nitrogen atmosphere to obtain non-covalent hybrid MOF graphene aerogel/molybdenum;
(3) adding the non-covalent hybrid MOF graphene aerogel/molybdenum, acetylene black and polytetrafluoroethylene emulsion prepared in the step (2) into the same weighing bottle according to the mass ratio of 80:10:10, uniformly stirring and mixing, blowing the sample into paste by using a hair drier, coating the paste material on the foamed nickel by using the foamed nickel as a current collector, and performing vacuum drying at 80 ℃ for 24 hours to finally prepare the required electrode material.
Further, the molar ratio of molybdenum pentachloride, 2-aminoterephthalic acid and 4-aminobenzoic acid is 1:2: 1.
Further, the mass ratio of the graphene aerogel to the molybdenum pentachloride is 100: 233.
The invention has the beneficial effects that:
(1) the intercalation of Mo lamellar ions into interlayer space is large, and the oxidation state range of Mo in redox reaction (Mo)2+∼Mo6+) The width is wider, so that more electrons can be stored in the charging and discharging process, and the storage performance of the electrode is improved;
(2) the added graphene can provide growing points for the MOF, so that the specific surface area of the material is increased, and the electrochemical performance is improved;
(3) the conductivity of the MOF is poor, the conductivity of the whole system can be improved by adding the graphene, and carbon quantum dots exposed on the surface layer can provide more active sites;
(4) the non-covalent hybrid MOF graphene aerogel/molybdenum electrode prepared by the invention has the advantages of large specific surface area, no toxicity, excellent electrochemical performance and wide application in portable and flexible electrode materials.
Drawings
Figure 1 SEM picture of covalent hybrid MOF graphene aerogel/molybdenum.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples.
Example 1
(1) Synthesis of graphene aerogel
400mg of graphene oxide was added to 100mL of DI water to obtain 4mg/mL of graphene oxide. After dispersion and sonication for 2 hours, the suspension was sealed in an autoclave lined with polytetrafluoroethylene and heated to 180 ℃ for 16 hours. After cooling to room temperature, the samples were washed with deionized water. Finally, the graphene aerogel was further frozen to-70 ℃ and dried for 48 hours.
(2) Preparation of non-covalent hybrid MOF graphene aerogel/molybdenum
100 mg of graphene aerogel was dispersed in 10 mL of DMF solution for 30 minutes under sonication. To the graphene aerogel suspension, molybdenum pentachloride (233mg), 2-aminoterephthalic acid (280mg), 4-aminobenzoic acid (244mg), and 0.16ml HCl were added, mixed, and charged into a 25ml glass vial. The resulting mixture was sonicated for 30 minutes. The resulting mixture was transferred to a 50 ml glass vial and placed in an oven at 120 ℃ for 2 days. Washing the obtained black gel with methanol, and drying at 150 ℃ in a nitrogen atmosphere to obtain the non-covalent hybrid MOF graphene aerogel/molybdenum.
(3) Adding the non-covalent hybrid MOF graphene aerogel/molybdenum, acetylene black and polytetrafluoroethylene emulsion prepared in the step (2) into the same weighing bottle according to the mass ratio of 80:10:10, uniformly stirring and mixing, blowing the sample into paste by using a hair drier, coating the paste material on the foamed nickel by using the foamed nickel as a current collector, and performing vacuum drying at 80 ℃ for 24 hours to finally prepare the required electrode.
Example 2
(1) Synthesis of graphene aerogel
400mg of graphene oxide was added to 100mL of DI water to obtain 4mg/mL of graphene oxide. After dispersion and sonication for 2 hours, the suspension was sealed in an autoclave lined with polytetrafluoroethylene and heated to 180 ℃ for 16 hours. After cooling to room temperature, the samples were washed several times with deionized water. Finally, the graphene aerogel was further frozen to-70 ℃ and dried for 48 hours.
(2) Preparation of non-covalent hybrid MOF graphene aerogel/molybdenum
100 mg of graphene aerogel was dispersed in 10 mL of DMF solution for 30 minutes under sonication. To the graphene aerogel suspension, molybdenum pentachloride (233mg), 2-aminoterephthalic acid (332mg), 4-aminobenzoic acid (244mg), and 0.16ml HCl were added, mixed, and charged into a 25ml glass vial. The resulting mixture was sonicated for 30 minutes. The resulting mixture was transferred to a 50 ml glass vial and placed in an oven at 120 ℃ for 2 days. Washing the obtained black gel with methanol for several times, and drying at 150 ℃ in nitrogen atmosphere to obtain the non-covalent hybrid MOF graphene aerogel/molybdenum.
(3) Adding the non-covalent hybrid MOF graphene aerogel/molybdenum, acetylene black and polytetrafluoroethylene emulsion prepared in the step (2) into the same weighing bottle according to the mass ratio of 80:10:10, uniformly stirring and mixing, blowing the sample into paste by using a hair drier, coating the paste material on the foamed nickel by using the foamed nickel as a current collector, and performing vacuum drying at 80 ℃ for 24 hours to finally prepare the required electrode.
Example 3
(1) Synthesis of graphene aerogel
400mg of graphene oxide was added to 100mL of DI water to obtain 4mg/mL of graphene oxide. After dispersion and sonication for 2 hours, the suspension was sealed in an autoclave lined with polytetrafluoroethylene and heated to 180 ℃ for 16 hours. After cooling to room temperature, the samples were washed several times with deionized water. Finally, the graphene aerogel was further frozen to-70 ℃ and dried for 48 hours.
(2) Preparation of non-covalent hybrid MOF graphene aerogel/molybdenum
100 mg of graphene aerogel was dispersed in 10 mL of DMF solution for 30 minutes under sonication. To the graphene aerogel suspension, molybdenum pentachloride (233mg), 2-aminoterephthalic acid (200mg), 4-aminobenzoic acid (244mg), and 0.16ml HCl were added, mixed, and then charged into a 25ml glass vial. The resulting mixture was sonicated for 30 minutes. The resulting mixture was transferred to a 50 ml glass vial and placed in an oven at 120 ℃ for 2 days. Washing the obtained black gel with methanol, and drying at 150 ℃ in a nitrogen atmosphere to obtain the non-covalent hybrid MOF graphene aerogel/molybdenum.
(3) Adding the non-covalent hybrid MOF graphene aerogel/molybdenum, acetylene black and polytetrafluoroethylene emulsion prepared in the step (2) into the same weighing bottle according to the mass ratio of 80:10:10, uniformly stirring and mixing, blowing the sample into paste by using a hair drier, coating the paste material on the foamed nickel by using the foamed nickel as a current collector, and performing vacuum drying at 80 ℃ for 24 hours to finally prepare the required electrode.
The obtained electrode was subjected to density, specific surface area and electrochemical performance tests, and the results are shown in table 1.
Comparative example 1
A preparation method of a non-covalent hybrid MOF graphene aerogel/molybdenum for a capacitor electrode specifically comprises the following steps:
(1) synthesis of graphene aerogel
400mg of graphene oxide was added to 100mL of DI to obtain 4mg/mL of graphene oxide. After dispersion and sonication for 2 hours, the suspension was sealed in an autoclave lined with polytetrafluoroethylene and heated to 180 ℃ for 16 hours. After cooling to room temperature, the samples were washed with deionized water. Finally, the graphene aerogel was further freeze-dried for 48 hours.
(2) Preparation of non-covalent hybrid MOF graphene aerogel/molybdenum
Under sonication, 50 mg of graphene aerogel was dispersed in 10 mL of DMF solution for 30 minutes. To the graphene aerogel suspension, molybdenum pentachloride (233mg), 2-aminoterephthalic acid (166mg), 4-aminobenzoic acid (244mg), and 0.16ml HCl were added to a 25ml glass vial. The resulting mixture was sonicated for 30 minutes. The resulting mixture was transferred to a 50 ml glass vial and placed in an oven at 120 ℃ for 2 days. The resulting black gel was washed with methanol and dried under nitrogen at 150 ℃.
(3) Adding the non-covalent hybrid MOF graphene aerogel/molybdenum, acetylene black and polytetrafluoroethylene emulsion prepared in the step (2) into the same weighing bottle according to the mass ratio of 80:10:10, uniformly stirring and mixing, blowing the sample into paste by using a hair drier, coating the paste material on the foamed nickel by using the foamed nickel as a current collector, and performing vacuum drying at 80 ℃ for 24 hours to finally prepare the required electrode.
Table 1 various properties of non-covalent hybrid MOF graphene aerogel/molybdenum electrodes
Changes in the weight of terephthalic acid in the examples, changes in material surface area and properties were achieved. The weight of the graphene and the weight of the terephthalic acid of the comparative example are both below the range, and the performance is poor.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (10)
1. A preparation method of a non-covalent hybrid MOF graphene aerogel/molybdenum capacitor electrode material is characterized by comprising the following steps: the method specifically comprises the following steps:
(1) synthesis of graphene aerogel
The preparation method specifically comprises the following steps of: adding graphene oxide into DI water to obtain a graphene oxide solution; after dispersion and ultrasound, the suspension was sealed in an autoclave lined with polytetrafluoroethylene and heated to 180 ℃; after cooling to room temperature, the sample was washed with deionized water; finally, further freezing the graphene aerogel to-70 ℃ and drying for 48 hours;
(2) preparation of non-covalent hybrid MOF graphene aerogel/molybdenum
Dispersing the graphene aerogel obtained in the step (1) in a DMF solution under ultrasonic treatment; adding molybdenum pentachloride, 2-aminoterephthalic acid, 4-aminobenzoic acid and HCl into the graphene aerogel suspension; carrying out ultrasonic treatment on the obtained mixture; reacting the obtained mixture in an oven; washing the obtained black gel with methanol, and drying under nitrogen to obtain non-covalent hybrid MOF graphene aerogel/molybdenum;
(3) adding the non-covalent hybrid MOF graphene aerogel/molybdenum, acetylene black and polytetrafluoroethylene emulsion prepared in the step (2) into the same weighing bottle, stirring and mixing uniformly, blowing the sample into paste by using a hair drier, coating the paste material on foamed nickel by using the foamed nickel as a current collector, and performing vacuum drying to finally prepare the required electrode material.
2. The preparation method of the non-covalent hybrid MOF graphene aerogel/molybdenum capacitor electrode material according to claim 1, characterized in that: the heating in the step (1) is specifically carried out for 16 hours at 180 ℃.
3. The preparation method of the non-covalent hybrid MOF graphene aerogel/molybdenum capacitor electrode material according to claim 1, characterized in that: the mass ratio of the molybdenum pentachloride, the 2-amino terephthalic acid and the 4-aminobenzoic acid in the step (2) is 233: 200-400: 244; the volume ratio of DMF solution to HCl is 10: 0.16.
4. the preparation method of the non-covalent hybrid MOF graphene aerogel/molybdenum capacitor electrode material according to claim 1, characterized in that: and (3) the mass ratio of the graphene aerogel to the molybdenum pentachloride in the step (2) is 100: 233.
5. The preparation method of the non-covalent hybrid MOF graphene aerogel/molybdenum capacitor electrode material according to claim 1, characterized in that: step (3) the resulting mixture was sonicated for 30 minutes.
6. The preparation method of the non-covalent hybrid MOF graphene aerogel/molybdenum capacitor electrode material according to claim 1, characterized in that: and (3) placing the mixture in the oven of the step (2) for 2 days at the temperature of 120 ℃.
7. The preparation method of the non-covalent hybrid MOF graphene aerogel/molybdenum capacitor electrode material according to claim 1, characterized in that: the drying under nitrogen in the step (2) is specifically drying under nitrogen atmosphere at 150 ℃.
8. The preparation method of the non-covalent hybrid MOF graphene aerogel/molybdenum capacitor electrode material according to claim 1, characterized in that: and (3) the mass ratio of the non-covalent hybrid MOF graphene aerogel/molybdenum to the acetylene black to the polytetrafluoroethylene emulsion is 80:10: 10.
9. The preparation method of the non-covalent hybrid MOF graphene aerogel/molybdenum capacitor electrode material according to claim 1, characterized in that: and (3) vacuum drying at 80 ℃ for 24 h.
10. A non-covalent hybrid MOF graphene aerogel/molybdenum capacitor electrode material prepared by the method of any one of claims 1-9.
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