CN111463018B - A kind of titanium dicarbide/molybdenum disulfide composite film and its preparation method and application - Google Patents
A kind of titanium dicarbide/molybdenum disulfide composite film and its preparation method and application Download PDFInfo
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- CN111463018B CN111463018B CN202010267589.7A CN202010267589A CN111463018B CN 111463018 B CN111463018 B CN 111463018B CN 202010267589 A CN202010267589 A CN 202010267589A CN 111463018 B CN111463018 B CN 111463018B
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- 239000002131 composite material Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 229910052719 titanium Inorganic materials 0.000 title claims description 3
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title description 101
- 239000010936 titanium Substances 0.000 title description 37
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims abstract description 100
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims abstract description 100
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims abstract description 100
- 150000001412 amines Chemical class 0.000 claims abstract description 67
- 239000007864 aqueous solution Substances 0.000 claims abstract description 54
- 239000000843 powder Substances 0.000 claims abstract description 54
- 238000000967 suction filtration Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000010408 film Substances 0.000 claims abstract 6
- 239000010409 thin film Substances 0.000 claims abstract 2
- 239000012528 membrane Substances 0.000 claims description 17
- 239000003792 electrolyte Substances 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 16
- 239000004677 Nylon Substances 0.000 claims description 10
- 229920001778 nylon Polymers 0.000 claims description 10
- -1 polypropylene Polymers 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 5
- 239000002033 PVDF binder Substances 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 18
- 238000004220 aggregation Methods 0.000 abstract description 7
- 230000002776 aggregation Effects 0.000 abstract description 4
- 238000004146 energy storage Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract description 2
- 229910052961 molybdenite Inorganic materials 0.000 description 99
- 229910009819 Ti3C2 Inorganic materials 0.000 description 73
- 238000002156 mixing Methods 0.000 description 16
- 239000003990 capacitor Substances 0.000 description 14
- 239000002985 plastic film Substances 0.000 description 14
- 238000000034 method Methods 0.000 description 13
- 238000013329 compounding Methods 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 238000003760 magnetic stirring Methods 0.000 description 8
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- 238000012360 testing method Methods 0.000 description 7
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- 229910052739 hydrogen Inorganic materials 0.000 description 4
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- 239000007772 electrode material Substances 0.000 description 3
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- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
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- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—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
- 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, 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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Abstract
本发明提供一种Ti3C2/MoS2复合薄膜及其制备方法和应用，涉及电能储能技术领域。本发明提供的制备方法，包括以下步骤：利用松香胺水溶液对MoS2粉末进行静电吸附处理，得到松香胺改性MoS2的水溶液；将所述松香胺改性MoS2的水溶液和Ti3C2粉末混合，进行静电组装后，依次进行抽滤和干燥，得到Ti3C2/MoS2复合薄膜。本发明提供的制备方法能够有效解决现有技术中Ti3C2片层间存在的聚集和堆叠的技术问题，并提高Ti3C2/MoS2复合薄膜的电化学性能和机械性能。
The invention provides a Ti 3 C 2 /MoS 2 composite film, a preparation method and application thereof, and relates to the technical field of electric energy storage. The preparation method provided by the present invention comprises the following steps: performing electrostatic adsorption treatment on MoS 2 powder with an aqueous rosin amine solution to obtain an aqueous solution of rosin amine - modified MoS 2 ; The powders are mixed and electrostatically assembled, followed by suction filtration and drying to obtain a Ti 3 C 2 /MoS 2 composite film. The preparation method provided by the invention can effectively solve the technical problems of aggregation and stacking between Ti 3 C 2 sheets in the prior art, and improve the electrochemical properties and mechanical properties of the Ti 3 C 2 /MoS 2 composite thin film.
Description
Technical Field
The invention relates to the technical field of electric energy storage, in particular to Ti3C2/MoS2A composite film and a preparation method and application thereof.
Background
Supercapacitors are of interest because of their ultra-high power density, long cycle life and wide operating temperature. They are widely used in electric vehicles, portable electronic devices, memory backup devices, large industrial devices, and renewable energy power plans. Supercapacitors can be divided into two categories, Electric Double Layer Capacitors (EDLCs) and pseudocapacitors, depending on the nature of the charge storage mechanism. EDLCs consist of carbonaceous materials, such as Activated Carbon (AC), Carbon Nanotubes (CNTs), or graphene, and charge storage occurs at the electrode/electrolyte interface. The pseudocapacitive electrode is a flexible electrode, and the charge storage of the pseudocapacitive electrode depends on the intercalation process or the reversible redox reaction of an active material. It is reported that pseudocapacitive electrodes have a stronger specific capacitance and a higher energy density than EDLCs. Therefore, the development of pseudo-capacitive flexible electrode materials is needed.
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, electrostatic assembling, vacuum filtering, and dryingTo 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 Li2SO4And the molar concentration of the electrolyte is 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 inventionIn the aqueous solution of rosin amine, the Zeta potential 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 preferably8000 meshes.
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 used, and the excess rosin amine is removed by centrifugation in the present invention. 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 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.
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/MoS2The size of the composite film is preferably 1cm × 2 cm. In the present invention, the electrolyte of the supercapacitor electrode is preferably Li2SO4An electrolyte; the molar concentration of the electrolyte of the supercapacitor electrode is preferably 1 mol/L. In the invention, 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 present invention, and the composition known to those skilled in the art may be used. The preparation method of the supercapacitor electrode is not particularly limited, and the preparation method of the supercapacitor electrode, which is well 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 the powder (with the particle size of 8000 meshes) into 100mL of 1% rosin amine aqueous solution, performing electrostatic adsorption treatment for 8h under the condition that the ultrasonic power is 120W, and 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 Ti3C2Powder (particle size 8000 mesh) is added toMoS modified by 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 a size of 1cm multiplied by 2cm, and a three-electrode system is adopted to be 1mol/LLI2SO4The 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 stacking occurs between sheets.
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 the powder (with the particle size of 8000 meshes) into 500mL of 1% rosin amine aqueous solution, performing electrostatic adsorption treatment for 8h under the condition that the ultrasonic power is 120W, and 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 1:2, 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 a size of 1cm multiplied by 2cm, and a three-electrode system is adopted to be 1mol/LLI2SO4The 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 the powder (with the particle size of 8000 meshes) into 200mL of 1% rosin amine aqueous solution, performing electrostatic adsorption treatment for 8h under the condition that the ultrasonic power is 120W, and 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 MoS2Mass ratio ofStirring for 6h at 3600 rpm under magnetic force of 10:1, performing electrostatic assembly, vacuum filtering on nylon filter membrane (aperture of 0.45 μm) to obtain film, and naturally drying to obtain Ti3C2/MoS2And (3) compounding the film.
The obtained Ti3C2/MoS2The composite film is cut into a size of 1cm multiplied by 2cm, and a three-electrode system is adopted to be 1mol/LLI2SO4The 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 the powder (with the particle size of 8000 meshes) into 200mL of 1% rosin amine aqueous solution, performing electrostatic adsorption treatment for 8h under the condition that the ultrasonic power is 120W, and 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 1:10, 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 a size of 1cm multiplied by 2cm, and a three-electrode system is adopted to be 1mol/LLI2SO4The 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 200mL of 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 productPost sexual 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 a size of 1cm multiplied by 2cm, and a three-electrode system is adopted to be 1mol/LLI2SO4The 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 the powder (with the particle size of 8000 meshes) into 200mL of 1% rosin amine aqueous solution, performing electrostatic adsorption treatment for 8h under the condition that the ultrasonic power is 120W, and 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 a size of 1cm multiplied by 2cm, and a three-electrode system is adopted to be 1mol/LLI2SO4The electrochemical properties and tensile strength were measured in the electrolyte and the results are shown in Table 1The tensile strength is measured mechanically by measuring the thickness of the plastic film and sheet of GB 6672.
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 a size of 1cm multiplied by 2cm, and a three-electrode system is adopted to be 1mol/LLI2SO4The 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 analysis of Ti is shown in combination with FIG. 7 and Table 13C2/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.
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