CN111463018A - Titanium tricarboxide/molybdenum disulfide composite film and preparation method and application thereof - Google Patents
Titanium tricarboxide/molybdenum disulfide composite film and preparation method and application thereof Download PDFInfo
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- CN111463018A CN111463018A CN202010267589.7A CN202010267589A CN111463018A CN 111463018 A CN111463018 A CN 111463018A CN 202010267589 A CN202010267589 A CN 202010267589A CN 111463018 A CN111463018 A CN 111463018A
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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
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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
- H01G11/44—Raw materials therefor, e.g. resins or coal
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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
Abstract
The present invention provides a Ti3C2/MoS2A composite film and a preparation method and application thereof relate to the technical field of electric energy storage. The preparation method provided by the invention comprises the following steps: MoS by using rosin amine aqueous solution2Performing electrostatic adsorption treatment on the powder to obtain rosin amine modified MoS2An aqueous solution of (a); modifying the rosin amine into MoS2Aqueous solution of (2) and Ti3C2Mixing the powders, performing electrostatic assembly, sequentially performing suction filtration and drying to obtain Ti3C2/MoS2Composite filmAnd (3) a membrane. The preparation method provided by the invention can effectively solve the problem of Ti in the prior art3C2The technical problem of aggregation and stacking existing between sheets, and increase of Ti3C2/MoS2Electrochemical and mechanical properties of the composite film.
Description
Technical Field
The invention relates to the technical field of electric energy storage, in particular to Ti3C2/MoS2Composite film and its productionPreparation method and application.
Background
Super capacitors are receiving much attention because of their ultra-high power density, long cycle life and wide operating temperature, and they are widely used in electric vehicles, portable electronic devices, memory backup devices, large industrial devices and renewable energy power plans, super capacitors can be classified into two types, an electric double layer capacitor (ED L C) and a pseudo capacitor, ED L C is composed of carbonaceous materials such as Activated Carbon (AC), Carbon Nanotubes (CNT) or graphene, and charge storage occurs at an electrode/electrolyte interface.
At present, the preparation methods of pseudocapacitive flexible electrodes are various, and the preparation of the filter membrane-based self-supporting carbon (carbon nano tube and graphene) flexible electrode by adopting a vacuum filtration method is one of effective methods. The flexible filter membrane not only can provide a supporting function for the active substances, but also can provide excellent mechanical properties for the super capacitor. However, binders and other additives are often added to the filtrate, which has a great influence on the electrode capacity. Therefore, it is important to prepare a binder-free electrode material.
In recent years, two-dimensional carbon materials have proven to be excellent flexible electrode materials for supercapacitors, among which two-dimensional layered Ti3C2The material has good hydrophilicity, high conductivity, adjustable structure, good chemical stability and excellent charge storage capacity, so that the material has very wide application prospect in the aspect of preparing binderless electrodes. However, it was found that Ti3C2The hydrogen bonds between the sheets are strong, which causes the aggregation and stacking between the sheets, thereby greatly reducing the transmission efficiency of the electrolyte and seriously limiting Ti3C2The electrochemical properties of the sheet play a role.
Disclosure of Invention
In view of the above, the present invention aims to provide a Ti3C2/MoS2The preparation method provided by the invention can effectively solve the problem of Ti in the prior art3C2The technical problem of aggregation and stacking between sheets.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a Ti3C2/MoS2The preparation method of the composite film comprises the following steps:
MoS by using rosin amine aqueous solution2Performing electrostatic adsorption treatment on the powder to obtain rosin amine modified MoS2An aqueous solution of (a);
modifying the rosin amine into MoS2Aqueous solution of (2) and Ti3C2Mixing the powders, performing electrostatic assembly, sequentially performing suction filtration and drying to obtain Ti3C2/MoS2And (3) compounding the film.
Preferably, the MoS2The mass ratio of the powder to the rosin amine in the rosin amine aqueous solution is 1-2: 1 to 5.
Preferably, the mass concentration of the rosin amine aqueous solution is 1%.
Preferably, the Ti3C2MoS modified with powder and rosin amine2The mass ratio of (1-10) to (10-1).
Preferably, the Ti3C2The particle size of the powder was 8000 mesh.
Preferably, the material of the filter membrane for suction filtration comprises nylon, polypropylene, polyvinylidene fluoride or polytetrafluoroethylene.
Preferably, the pore diameter of the filter membrane for suction filtration is 0.45 μm.
The invention also provides Ti prepared by the preparation method of the technical scheme3C2/MoS2Composite film of Ti3C2And rosin amine modified MoS2Said Ti3C2And rosin amine modified MoS2The mass ratio of (1-10) to (10-1), the Ti3C2/MoS2The thickness of the composite film was 10 μm.
The invention also provides the Ti in the technical scheme3C2/MoS2The application of the composite film in the preparation of the electrode of the super capacitor.
Preferably, the electrolyte of the supercapacitor electrode is L i2SO4Electrolyte with a molar concentration of 1 mol/L.
The invention provides a Ti3C2/MoS2The preparation method of the composite film comprises the following steps: MoS by using rosin amine aqueous solution2Performing electrostatic adsorption treatment on the powder to obtain rosin amine modified MoS2An aqueous solution of (a); modifying the rosin amine into MoS2Aqueous solution of (2) and Ti3C2Mixing the powders, performing electrostatic assembly, sequentially performing suction filtration and drying to obtain Ti3C2/MoS2And (3) compounding the film. In the present invention, the Zeta potential of the rosin amine aqueous solution is positive, MoS2The Zeta potential of the powder in the aqueous solution is negative, and the invention utilizes the aqueous solution of the rosin amine to MoS2The powder is subjected to electrostatic adsorption treatment, and the rosin amine is adsorbed on MoS2Surface of powder, to MoS2Modifying to obtain modified MoS2Zeta potential in aqueous solution is positive and MoS is increased2Electrostatic assembly capability. And Ti3C2Zeta potential of the powder in aqueous solution is negative, and the invention modifies the rosin amine into MoS2With Ti3C2Mixing the powders, performing electrostatic assembly, and assembling into Ti3C2Modified MoS with rosin amine inserted between layers2Destruction of Ti3C2Hydrogen bonding between the sheets to prevent Ti3C2Aggregation and stacking between sheets to form Ti3C2Can fully exert the function, and MoS2Also has good electrochemical performance and can effectively improve Ti3C2/MoS2Electrochemical performance of the composite film. The Ti is obtained by suction filtration3C2/MoS2Composite film capable of effectively increasing Ti3C2/MoS2Mechanical properties of the composite film. Therefore, the preparation method provided by the invention can effectively solve the problem of Ti in the prior art3C2The technical problem of aggregation and stacking between sheets.
The preparation method provided by the invention is simple, efficient and low in cost, does not add a binder or other additives, and is environment-friendly.
The invention is to mix Ti3C2/MoS2The composite film is used for preparing the electrode of the super capacitor, and can effectively improve the specific capacitance and tensile strength of the electrode.
Drawings
FIG. 1 is Ti3C2Scanning electron microscope photographs of (a);
FIG. 2 shows Ti obtained in example 13C2/MoS2Scanning electron microscope photographs of the composite films;
FIG. 3 is Ti3C2Modified MoS with rosin amine2Zeta potential in water, and Ti obtained in example 13C2/MoS2Zeta potential of the composite film;
FIG. 4 shows Ti obtained in example 23C2/MoS2A folded optical pattern of the composite film;
FIG. 5 is a CV diagram of the capacitor electrode prepared in example 2 under different scanning speed conditions;
FIG. 6 is a CV diagram of the capacitor electrode prepared in example 2 under different current density conditions;
FIG. 7 is a graph showing the area specific capacity of the capacitor electrodes obtained in examples 1 to 6 and comparative example.
Detailed Description
The invention provides a Ti3C2/MoS2The preparation method of the composite film comprises the following steps:
MoS by using rosin amine aqueous solution2Performing electrostatic adsorption treatment on the powder to obtain rosin amine modified MoS2An aqueous solution of (a);
modifying the rosin amine into MoS2Aqueous solution of (2) and Ti3C2Mixing the powders, performing electrostatic assembly, sequentially performing suction filtration and drying to obtain Ti3C2/MoS2And (3) compounding the film.
In the present invention, the raw materials used are all commercial products conventional in the art unless otherwise specified.
The invention utilizes the rosin amine aqueous solution to the MoS2Performing electrostatic adsorption treatment on the powder to obtain rosin amine modified MoS2An aqueous solution of (a).
In the invention, the mass concentration of the rosin amine in the rosin amine aqueous solution is preferably 1%; the source of rosin amine in the rosin amine aqueous solution is preferably rosin amine hydrochloride, and further preferably comprises rosin amine hydrochloride and/or rosin amine hydrobromide. In the present invention, the MoS2The mass ratio of the powder to the rosin amine in the rosin amine aqueous solution is preferably 1-2: 1 to 5, and more preferably 1.5 to 1.7: 2 to 3. In the present invention, the MoS2The particle size of the powder is preferably 8000 mesh.
In the invention, the electrostatic adsorption treatment is preferably carried out under an ultrasonic condition, and the power of the ultrasonic treatment is preferably 120-1000W. In the invention, the time of the electrostatic adsorption treatment is preferably 6-8 h. In the present invention, the Zeta potential of the rosin amine aqueous solution is positive, MoS2The Zeta potential of the powder in the aqueous solution is negative, and the invention utilizes the aqueous solution of the rosin amine to MoS2The powder is subjected to electrostatic adsorption treatment, and the rosin amine is adsorbed on MoS2Surface of powder, to MoS2Modifying to obtain modified MoS2Zeta potential in aqueous solution is positive and MoS is increased2Electrostatic assembly capability.
After the electrostatic adsorption treatment, the invention preferably performs solid-liquid separation on the obtained electrostatic adsorption treatment product to obtain the modified MoS of the rosin amine2Then, the rosin amine modified MoS2Mixing with water to obtain the modified MoS of rosin amine2An aqueous solution. In the present invention, the solid-liquid separation is preferably performed by centrifugation, and the specific operation of the centrifugation is not particularly limited in the present invention, and the centrifugation known to those skilled in the art may be usedExcess rosin amine was removed by centrifugation. In the present invention, the mixing method is not particularly limited, and MoS after modification of rosin amine can be used2And (4) uniformly dispersing. The invention has no special limitation on the using amount of the water, and can modify the rosin amine into MoS2And (4) uniformly dispersing.
Obtaining rosin amine modified MoS2After the aqueous solution is prepared, the invention modifies the rosin amine into MoS2Aqueous solution of (2) and Ti3C2Mixing the powders, performing electrostatic assembly, sequentially performing suction filtration and drying to obtain Ti3C2/MoS2And (3) compounding the film.
In the present invention, the Ti is3C2MoS modified with powder and rosin amine2The mass ratio of (A) to (B) is preferably (1-10): (10-1), more preferably (1-5): (5-1), and still more preferably 1: 2. When said Ti is3C2MoS modified with powder and rosin amine2When the mass ratio of (A) to (B is too large, Ti3C2Too high content of Ti may cause3C2The lamination is stacked, and the area specific capacitance performance cannot be fully exerted; when said Ti is3C2MoS modified with powder and rosin amine2When the mass ratio of (A) is too small, MoS2Too high a content of (b) may lower the conductivity, resulting in a severe decrease in area specific capacitance. In the present invention, the Ti is3C2The particle size of the powder is preferably 8000 mesh.
In the present invention, the mixing mode is preferably magnetic stirring, and the rotation speed of the magnetic stirring is preferably 3600 revolutions per minute; the magnetic stirring time is preferably 4-6 h. In the present invention, the Ti is3C2MoS modified with powder and rosin amine2Preferably, the electrostatic assembly is performed while mixing. The invention modifies the rosin amine into MoS2With Ti3C2Mixing the powders, performing electrostatic assembly, and assembling into Ti3C2Modified MoS with rosin amine inserted between layers2Destruction of Ti3C2Hydrogen bonding between the sheets to prevent Ti3C2Aggregation and stacking between sheets to form Ti3C2Electrochemical property ofCan fully exert the function, and MoS2Also has good electrochemical performance and can effectively improve Ti3C2/MoS2Electrochemical performance of the composite film. The Ti is obtained by suction filtration3C2/MoS2Composite film capable of effectively increasing Ti3C2/MoS2Mechanical properties of the composite film.
In the invention, the material of the filter membrane for suction filtration preferably comprises nylon, polypropylene, polyvinylidene fluoride or polytetrafluoroethylene; the pore diameter of the filtration membrane for suction filtration is preferably 0.45. mu.m. The Ti is obtained by suction filtration3C2/MoS2Composite film capable of effectively increasing Ti3C2/MoS2Mechanical properties of the composite film. The suction filtration method is not particularly limited in the present invention, and a suction filtration method known to those skilled in the art may be adopted.
In the present invention, the drying method is preferably natural drying.
The invention also provides Ti prepared by the preparation method of the technical scheme3C2/MoS2A composite film of the Ti3C2/MoS2Ti in composite film3C2Modified MoS with rosin amine2The mass ratio of (1-10) to (10-1) of Ti3C2/MoS2The thickness of the composite film was 10 μm.
The invention also provides the Ti in the technical scheme3C2/MoS2The application of the composite film in the preparation of the electrode of the super capacitor.
In the present invention, the Ti is3C2/MoS2Size of composite film is preferably 1cm × 2 cm. in the invention, electrolyte of the supercapacitor electrode is preferably L i2SO4The molar concentration of the electrolyte of the supercapacitor electrode is preferably 1 mol/L, the working system of the supercapacitor electrode is a three-electrode system, the composition of the three-electrode system is not particularly limited in the invention, and the composition known by the skilled person can be adoptedThe preparation method of the supercapacitor electrode is not particularly limited, and the preparation method of the supercapacitor electrode known to those skilled in the art can be adopted.
The following examples are given to provide Ti3C2/MoS2The composite films and the methods of preparation and use thereof are described in detail, but they should not be construed as limiting the scope of the invention.
Example 1
1gMoS2Adding powder (particle size of 8000 mesh) into 1% rosin amine aqueous solution 100m L, performing electrostatic adsorption treatment for 8h under the condition of ultrasonic power of 120W, and centrifuging to obtain modified MoS2Modifying the obtained rosin amine to obtain MoS2Dispersing in water to obtain the modified MoS of rosin amine2An aqueous solution;
mixing Ti3C2Adding powder (particle size of 8000 meshes) into modified MoS of rosin amine2In aqueous solution, Ti3C2Powder and rosin amine modified MoS2The mass ratio of Ti to the components is 5:1, the magnetic stirring is carried out for 6 hours, the rotating speed is 3600 r/min, the Ti is obtained by vacuum filtration and film forming on a nylon filter membrane (the aperture is 0.45 mu m) and natural drying after full electrostatic assembly3C2/MoS2And (3) compounding the film.
The obtained Ti3C2/MoS2The composite film is cut into 1cm × 2cm, and a three-electrode system is adopted at 1 mol/LL i2SO4The electrochemical performance and the tensile strength of the electrolyte are tested, the test results are shown in the table 1, and the test method of the tensile strength is a mechanical measurement method for measuring the thickness of GB6672 plastic films and sheets.
FIG. 1 is Ti3C2FIG. 2 is a photograph of Ti prepared in example 1 by scanning electron microscope3C2/MoS2Scanning electron microscope photograph of the composite film. As can be seen from FIGS. 1 and 2, the Ti produced by the present invention3C2/MoS2MoS inserted in composite film2Can destroy Ti3C2Hydrogen bonding between the sheets to prevent Ti3C2Aggregation and aggregation between sheetsAnd (4) stacking.
FIG. 3 is Ti3C2Modified MoS with rosin amine2Zeta potential in water, and Ti obtained in example 13C2/MoS2Zeta potential of the composite film. As can be seen from the figure, the present invention utilizes an aqueous rosin amine solution to MoS2The powder is subjected to electrostatic adsorption treatment to modify the rosin amine into MoS2Zeta potential in aqueous solution is positive with Ti3C2After the powder is mixed, electrostatic assembly can be carried out, so that the MoS is modified by rosin amine2Insertion of Ti3C2Between the layers.
Example 2
2gMoS2Adding powder (particle size of 8000 mesh) into 1% rosin amine aqueous solution with mass concentration of 500m L, performing electrostatic adsorption treatment for 8h under the condition of ultrasonic power of 120W, and centrifuging to obtain modified MoS2Modifying the obtained rosin amine to obtain MoS2Dispersing in water to obtain the modified MoS of rosin amine2An aqueous solution;
mixing Ti3C2Adding powder (particle size of 8000 meshes) into modified MoS of rosin amine2In aqueous solution, Ti3C2Powder and rosin amine modified MoS2The mass ratio of Ti to the components is 1:2, the magnetic stirring is carried out for 6 hours, the rotating speed is 3600 r/min, the Ti is obtained by vacuum filtration and film forming on a nylon filter membrane (the aperture is 0.45 mu m) and natural drying after full electrostatic assembly3C2/MoS2And (3) compounding the film.
The obtained Ti3C2/MoS2The composite film is cut into 1cm × 2cm, and a three-electrode system is adopted at 1 mol/LL i2SO4The electrochemical performance and the tensile strength of the electrolyte are tested, the test results are shown in the table 1, and the test method of the tensile strength is a mechanical measurement method for measuring the thickness of GB6672 plastic films and sheets.
FIG. 4 shows Ti obtained in example 23C2/MoS2The folded optical pattern of the composite film, as can be seen, has the ability to be easily folded.
Fig. 5 is a CV graph of the capacitor electrode prepared in example 2 under different scanning speed conditions, and it can be seen from the graph that the capacitor electrode has better electrochemical performance.
Fig. 6 is a CV graph of the capacitor electrode prepared in example 2 under different current density conditions, and it can be seen that the capacitor electrode has better area specific capacity.
Example 3
1.5g of MoS2Adding powder (particle size of 8000 mesh) into 200m L mass concentration 1% rosin amine aqueous solution, performing electrostatic adsorption treatment for 8h under the condition of ultrasonic power of 120W, and centrifuging to obtain rosin amine modified MoS2Modifying the obtained rosin amine to obtain MoS2Dispersing in water to obtain the modified MoS of rosin amine2An aqueous solution;
mixing Ti3C2Adding powder (particle size of 8000 meshes) into modified MoS of rosin amine2In aqueous solution, Ti3C2Powder and rosin amine modified MoS2The mass ratio of Ti to the components is 10:1, the magnetic stirring is carried out for 6 hours, the rotating speed is 3600 r/min, the Ti is obtained by vacuum filtration and film forming on a nylon filter membrane (the aperture is 0.45 mu m) and natural drying after full electrostatic assembly3C2/MoS2And (3) compounding the film.
The obtained Ti3C2/MoS2The composite film is cut into 1cm × 2cm, and a three-electrode system is adopted at 1 mol/LL i2SO4The electrochemical performance and the tensile strength of the electrolyte are tested, the test results are shown in the table 1, and the test method of the tensile strength is a mechanical measurement method for measuring the thickness of GB6672 plastic films and sheets.
Example 4
1.5g of MoS2Adding powder (particle size of 8000 mesh) into 200m L mass concentration 1% rosin amine aqueous solution, performing electrostatic adsorption treatment for 8h under the condition of ultrasonic power of 120W, and centrifuging to obtain rosin amine modified MoS2Modifying the obtained rosin amine to obtain MoS2Dispersing in water to obtain the modified MoS of rosin amine2An aqueous solution;
mixing Ti3C2Adding powder (particle size of 8000 meshes) into modified MoS of rosin amine2In aqueous solution, Ti3C2Powder and rosin amine modified MoS2The mass ratio of Ti to the components is 1:10, the magnetic stirring is carried out for 6 hours, the rotating speed is 3600 r/min, the Ti is obtained by vacuum filtration and film forming on a nylon filter membrane (the aperture is 0.45 mu m) and natural drying after full electrostatic assembly3C2/MoS2And (3) compounding the film.
The obtained Ti3C2/MoS2The composite film is cut into 1cm × 2cm, and a three-electrode system is adopted at 1 mol/LL i2SO4The electrochemical performance and the tensile strength of the electrolyte are tested, the test results are shown in the table 1, and the test method of the tensile strength is a mechanical measurement method for measuring the thickness of GB6672 plastic films and sheets.
Example 5
1.5g of MoS2Adding powder (particle size of 8000 mesh) into 200m L mass concentration 1% rosin amine aqueous solution, performing electrostatic adsorption treatment for 8h under the condition of ultrasonic power of 120W, and centrifuging to obtain rosin amine modified MoS2Modifying the obtained rosin amine to obtain MoS2Dispersing in water to obtain the modified MoS of rosin amine2An aqueous solution;
mixing Ti3C2Adding powder (particle size of 8000 meshes) into modified MoS of rosin amine2In aqueous solution, Ti3C2Powder and rosin amine modified MoS2The mass ratio of Ti to the component (A) is 4:3, the magnetic stirring is carried out for 6 hours, the rotating speed is 3600 r/min, the Ti is obtained by vacuum filtration membrane forming and natural drying after full electrostatic assembly on a nylon filter membrane (the aperture is 0.45 mu m)3C2/MoS2And (3) compounding the film.
The obtained Ti3C2/MoS2The composite film is cut into 1cm × 2cm, and a three-electrode system is adopted at 1 mol/LL i2SO4The electrochemical performance and the tensile strength of the electrolyte are tested, the test results are shown in the table 1, and the test method of the tensile strength is a mechanical measurement method for measuring the thickness of GB6672 plastic films and sheets.
Example 6
1.5g of MoS2Adding powder (particle size of 8000 mesh) into 200m L mass concentration 1% rosin amine water solution, and ultrasonic processingUnder the condition of 120W, after electrostatic adsorption treatment for 8h, centrifuging to obtain the modified MoS of rosin amine2Modifying the obtained rosin amine to obtain MoS2Dispersing in water to obtain the modified MoS of rosin amine2An aqueous solution;
mixing Ti3C2Adding powder (particle size of 8000 meshes) into modified MoS of rosin amine2In aqueous solution, Ti3C2Powder and rosin amine modified MoS2The mass ratio of Ti to the components is 1:15, the magnetic stirring is carried out for 6 hours, the rotating speed is 3600 r/min, the Ti is obtained by vacuum filtration and film forming on a nylon filter membrane (the aperture is 0.45 mu m) and natural drying after full electrostatic assembly3C2/MoS2And (3) compounding the film.
The obtained Ti3C2/MoS2The composite film is cut into 1cm × 2cm, and a three-electrode system is adopted at 1 mol/LL i2SO4The electrochemical performance and the tensile strength of the electrolyte are tested, the test results are shown in the table 1, and the test method of the tensile strength is a mechanical measurement method for measuring the thickness of GB6672 plastic films and sheets.
Comparative example
Will contain 5g Ti3C2Filtering the aqueous solution on a nylon filter membrane (the aperture is 0.45 mu m) to form a membrane and naturally drying to obtain Ti3C2A film.
The obtained Ti3C2/MoS2The composite film is cut into 1cm × 2cm, and a three-electrode system is adopted at 1 mol/LL i2SO4The electrochemical performance and the tensile strength of the electrolyte are tested, the test results are shown in the table 1, and the test method of the tensile strength is a mechanical measurement method for measuring the thickness of GB6672 plastic films and sheets.
Table 1 test results of area specific capacity and tensile strength of the capacitor electrodes prepared in examples 1 to 6 and comparative example.
FIG. 7 is a graph showing the area specific capacity of the capacitor electrodes obtained in examples 1 to 6 and comparative example, and is analyzed in conjunction with FIG. 7 and Table 1Known as Ti3C2/MoS2The composite film has a specific Ti3C2The area specific capacity and tensile strength of the film are more excellent.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. Ti3C2/MoS2The preparation method of the composite film is characterized by comprising the following steps:
MoS by using rosin amine aqueous solution2Performing electrostatic adsorption treatment on the powder to obtain rosin amine modified MoS2An aqueous solution of (a);
modifying the rosin amine into MoS2Aqueous solution of (2) and Ti3C2Mixing the powders, performing electrostatic assembly, sequentially performing suction filtration and drying to obtain Ti3C2/MoS2And (3) compounding the film.
2. The method of claim 1, wherein the MoS is prepared by a method comprising2The mass ratio of the powder to the rosin amine in the rosin amine aqueous solution is 1-2: 1 to 5.
3. The production method according to claim 1 or 2, wherein the concentration by mass of the rosin amine aqueous solution is 1%.
4. The method according to claim 1, wherein the Ti is3C2Powder and rosin amine modified MoS2The mass ratio of (1-10) to (10-1).
5. The production method according to claim 1 or 4, wherein the Ti is3C2The particle size of the powder was 8000 mesh.
6. The method according to claim 1, wherein the material of the filtration membrane for suction filtration comprises nylon, polypropylene, polyvinylidene fluoride, or polytetrafluoroethylene.
7. The production method according to claim 1 or 6, wherein the pore size of the filtration membrane for suction filtration is 0.45 μm.
8. Ti produced by the production method according to any one of claims 1 to 73C2/MoS2Composite film of Ti3C2And rosin amine modified MoS2Said Ti3C2And rosin amine modified MoS2The mass ratio of (1-10) to (10-1), the Ti3C2/MoS2The thickness of the composite film was 10 μm.
9. Ti according to claim 83C2/MoS2The application of the composite film in the preparation of the electrode of the super capacitor.
10. The use according to claim 9, wherein the electrolyte of the supercapacitor electrode is L i2SO4Electrolyte with a molar concentration of 1 mol/L.
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Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0466523A (en) * | 1990-07-04 | 1992-03-02 | Kanebo Ltd | Agent for suppressing proliferation of pathogen of periodontosis |
| CN103042208A (en) * | 2013-01-22 | 2013-04-17 | 广东新劲刚新材料科技股份有限公司 | Iron and titanium carbide mixture and method for manufacturing coating on surface of cold pressing mold |
| CN106057471A (en) * | 2016-05-27 | 2016-10-26 | 同济大学 | Preparation method and application of three-dimensional graphene aerogel load molybdenum disulfide nano-sheet hybridization material |
| US20170062143A1 (en) * | 2015-08-24 | 2017-03-02 | Aruna Zhamu | Production process for a supercapacitor having a high volumetric energy density |
| CN106532015A (en) * | 2016-12-27 | 2017-03-22 | 天津大学 | MoS2 inserted-layer Ti3C2 lithium ion battery negative electrode material and preparation method thereof |
| CN106833810A (en) * | 2016-12-27 | 2017-06-13 | 唐林元 | A kind of preparation method of stable type Composite nanometer antiwear agent |
| US20180130609A1 (en) * | 2011-04-15 | 2018-05-10 | Energ2 Technologies, Inc. | Flow ultracapacitor |
| CN108172903A (en) * | 2017-12-26 | 2018-06-15 | 深圳先进技术研究院 | Electrolyte, sodium ion secondary battery and preparation method thereof |
| CN108735984A (en) * | 2018-04-11 | 2018-11-02 | 燕山大学 | A kind of preparation method of molybdenum disulfide/carbonization titanium composite material |
| CN109036877A (en) * | 2018-07-10 | 2018-12-18 | 扬州大学 | Porous type graphene/transient metal chalcogenide compound film preparation method |
| CN109243843A (en) * | 2018-10-08 | 2019-01-18 | 西安交通大学 | A kind of ultra-fine sulfide/graphene Two-dimensional Composites and its preparation method and application |
| CN109608697A (en) * | 2018-12-20 | 2019-04-12 | 中国地质大学（武汉） | A kind of modified MoS of phosphorus-containing compound2The preparation method and applications of nanoscale twins |
| CN109830675A (en) * | 2019-04-04 | 2019-05-31 | 兰州理工大学 | MXene/MoS for negative electrode of lithium ion battery2Composite material and preparation method thereof |
| CN110229502A (en) * | 2018-03-06 | 2019-09-13 | 中国科学院化学研究所 | A kind of PA6 nanocomposite and preparation method thereof |
-
2020
- 2020-04-08 CN CN202010267589.7A patent/CN111463018B/en active Active
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0466523A (en) * | 1990-07-04 | 1992-03-02 | Kanebo Ltd | Agent for suppressing proliferation of pathogen of periodontosis |
| US20180130609A1 (en) * | 2011-04-15 | 2018-05-10 | Energ2 Technologies, Inc. | Flow ultracapacitor |
| CN103042208A (en) * | 2013-01-22 | 2013-04-17 | 广东新劲刚新材料科技股份有限公司 | Iron and titanium carbide mixture and method for manufacturing coating on surface of cold pressing mold |
| US20170062143A1 (en) * | 2015-08-24 | 2017-03-02 | Aruna Zhamu | Production process for a supercapacitor having a high volumetric energy density |
| CN106057471A (en) * | 2016-05-27 | 2016-10-26 | 同济大学 | Preparation method and application of three-dimensional graphene aerogel load molybdenum disulfide nano-sheet hybridization material |
| CN106532015A (en) * | 2016-12-27 | 2017-03-22 | 天津大学 | MoS2 inserted-layer Ti3C2 lithium ion battery negative electrode material and preparation method thereof |
| CN106833810A (en) * | 2016-12-27 | 2017-06-13 | 唐林元 | A kind of preparation method of stable type Composite nanometer antiwear agent |
| CN108172903A (en) * | 2017-12-26 | 2018-06-15 | 深圳先进技术研究院 | Electrolyte, sodium ion secondary battery and preparation method thereof |
| CN110229502A (en) * | 2018-03-06 | 2019-09-13 | 中国科学院化学研究所 | A kind of PA6 nanocomposite and preparation method thereof |
| CN108735984A (en) * | 2018-04-11 | 2018-11-02 | 燕山大学 | A kind of preparation method of molybdenum disulfide/carbonization titanium composite material |
| CN109036877A (en) * | 2018-07-10 | 2018-12-18 | 扬州大学 | Porous type graphene/transient metal chalcogenide compound film preparation method |
| CN109243843A (en) * | 2018-10-08 | 2019-01-18 | 西安交通大学 | A kind of ultra-fine sulfide/graphene Two-dimensional Composites and its preparation method and application |
| CN109608697A (en) * | 2018-12-20 | 2019-04-12 | 中国地质大学（武汉） | A kind of modified MoS of phosphorus-containing compound2The preparation method and applications of nanoscale twins |
| CN109830675A (en) * | 2019-04-04 | 2019-05-31 | 兰州理工大学 | MXene/MoS for negative electrode of lithium ion battery2Composite material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 王佳: "纳米MoS2在润滑脂中的分散稳定性研究", 《石油炼制与化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113675408A (en) * | 2020-09-02 | 2021-11-19 | 山东大学 | MoS for high-performance potassium ion battery2/Ti3C2Preparation method of MXene composite material |
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