CN109830381B - MXene/MoS for supercapacitor electrodes2Method for preparing composite material - Google Patents
MXene/MoS for supercapacitor electrodes2Method for preparing composite material Download PDFInfo
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- CN109830381B CN109830381B CN201910268631.4A CN201910268631A CN109830381B CN 109830381 B CN109830381 B CN 109830381B CN 201910268631 A CN201910268631 A CN 201910268631A CN 109830381 B CN109830381 B CN 109830381B
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/13—Energy storage using capacitors
Abstract
The preparation method of the MXene/MoS2 composite material for the supercapacitor electrode comprises the following steps: ultrasonically dispersing the monolayer MXene powder in water to obtain MXene dispersion liquid, and adding polyethyleneimine, namely PEI solution to obtain positive-charge MXene dispersion liquid; the single layer MoS2Dispersing the powder in deionized water and performing ultrasonic treatment to obtain single-layer MoS2A dispersion liquid; mixing positively charged MXene and negatively charged MoS2The dispersion liquid is sequentially sprayed on a polyethylene terephthalate (PET) substrate, and MXene/MoS for the electrode material of the super capacitor is obtained after drying2A layered composite material.
Description
Technical Field
The invention relates to MXene/MoS for super capacitor electrode2A preparation technology of the composite material.
Background
The super capacitor is used as an energy storage device between a secondary battery and a traditional capacitor, and has the advantages of high power density, high charging and discharging speed, good cycle stability and the like. The electrode material is the primary factor that directly affects the performance of the supercapacitor. MXene and MoS2Due to the unique two-dimensional layered structure, the electrode material can provide a rapid diffusion channel for electrolyte ions, and becomes a super capacitor electrode material with great development prospect. However, MXene is subject to self-stacking during use, making its surface underutilized and hindering rapid transport of electrolyte ions, resulting in a relatively low theoretical capacity. MoS2Although high specific capacity, the conductivity is lower than MXene, so that the rate capability is limited. MXene/MoS thus prepared by electrostatic self-assembly method2The layered composite material can have MXene and MoS2The electrode material has the advantages of being an ideal pseudocapacitance electrode material. However, the self-assembly method reported at present is mainly to combine MoS with opposite charges2Mixing with MXene dispersion to obtain MoS2And MXene through electrostatic interaction to form MXene/MoS2A layered composite material. The self-assembly method has poor controllability, and MXene/MoS is difficult to accurately control2The number of layers and the thickness of the layered composite material. Therefore, the invention provides a method for preparing MXene/MoS by using a spraying self-assembly method2Layered composite material prepared by mixing oppositely charged MoS with spray gun2And MXene dispersion were sequentially sprayed onto the substrate.
Disclosure of Invention
The invention aims to provide MXene/MoS for a supercapacitor electrode2A method for preparing a composite material.
The invention relates to MXene/MoS for super capacitor electrode2The preparation method of the composite material comprises the following steps: ultrasonically dispersing the monolayer MXene powder in water to obtain MXene dispersion liquid, and adding polyethyleneimine, namely PEI solution to obtain MXene dispersion liquid with positive charges; the single layer MoS2Dispersing the powder in deionized water and performing ultrasonic treatment to obtain single-layer MoS2A dispersion liquid; mixing positively charged MXene and negatively charged MoS2The dispersion liquid is sequentially sprayed on a polyethylene terephthalate (PET) substrate, and MXene/MoS for the electrode material of the super capacitor is obtained after drying2A layered composite material.
The invention has the advantages that: compared with the traditional liquid-phase electrostatic self-assembly, the method effectively avoids disorder during self-assembly, has good controllability, can not only enable two layered materials to be alternately intercalated and distributed, but also accurately control the layer number and the thickness of the composite material, and is an important innovation and supplement for the existing self-assembly technology.
Detailed Description
The invention relates to MXene/MoS for super capacitor electrode2The preparation method of the composite material comprises the following steps: ultrasonically dispersing the monolayer MXene powder in deionized water to obtain MXene dispersion liquid, and adding polyethyleneimine, namely PEI solution, to obtain MXene dispersion liquid with positive charges; the single layer MoS2Dispersing the powder in deionized water and performing ultrasonic treatment to obtain single-layer MoS2A dispersion liquid; mixing positively charged MXene and negatively charged MoS2The dispersion liquid is sequentially sprayed on a polyethylene terephthalate (PET) substrate, and after drying, the PET substrate is peeled off to obtain MXene/MoS for the electrode material of the super capacitor2A layered composite material.
MXene/MoS for supercapacitor electrodes as described above2The preparation method of the composite material comprises the following specific steps:
(1) adding 30 mg of MXene powder into 120 mL of deionized water, and carrying out ultrasonic treatment for 1 h to obtain MXene dispersion liquid;
(2) taking 120 mL of PEI aqueous solution with the concentration of 8 mg/mL, adding the PEI aqueous solution into the MXene dispersion liquid obtained in the step (1) under stirring, and carrying out water bath at 60 ℃ for 12 h;
(3) centrifuging and washing the dispersion liquid obtained in the step (2) at 4000 rad/min for 5 min each time until the pH of a supernatant is =7 to obtain an MXene dispersion liquid with positive charges;
(4) 100 mg of single-layer MoS is taken2Dispersing the powder in 50 mL deionized water, and performing ultrasonic treatment for 1 h to obtain MoS2A dispersion liquid;
(5) MXene and MoS obtained in the step (3) and the step (4) are sprayed by a spray gun2Sequentially spraying the dispersion liquid on a PET substrate, drying for 24 h at 60 ℃, and stripping the PET substrate to obtain MXene/MoS for the electrode material of the supercapacitor2A layered composite material.
MXene/MoS for supercapacitor electrodes as described above2The MXene is Ti3C2Tx，Or Ti2CTxOr V2CTxOr Mo or3C2Tx。
MXene/MoS for supercapacitor electrodes as described above2The preparation method of the composite material uses a German schutze KA-2 automatic spray gun, and the caliber of a nozzle of the spray gun is 0.2 mm and 0.3 mm.
MXene/MoS for supercapacitor electrodes as described above2The composite material is prepared by spraying at 4 bar, 4.5 bar, 5 bar, 5.5 bar, or 6 bar.
Example 1:
(1) adding 30 mg of MXene powder into 120 mL of deionized water, and carrying out ultrasonic treatment for 1 h to obtain MXene dispersion liquid;
(2) taking 120 mL of PEI aqueous solution with the concentration of 8 mg/mL, adding the PEI aqueous solution into the MXene dispersion liquid obtained in the step (1) under stirring, and carrying out water bath at 60 ℃ for 12 h;
(3) centrifuging and washing the dispersion liquid obtained in the step (2) at 4000 rad/min for 5 min each time until the pH of a supernatant is =7 to obtain an MXene dispersion liquid with positive charges;
(4) 100 mg of single-layer MoS is taken2Dispersing the powder in 50 mL deionized water, and performing ultrasonic treatment for 1 h to obtain MoS2A dispersion liquid;
(5) MXene and MoS obtained in the steps (3) and (4) are treated by using a German schutze KA-2 automatic spray gun with the caliber of a nozzle of 0.2 mm and the atomization pressure of 4 bar2Sequentially spraying the dispersion liquid on a PET substrate, drying for 24 h at 60 ℃, and stripping the PET substrate to obtain MXene/MoS for the electrode material of the supercapacitor2A layered composite material.
Example 2:
(1) adding 30 mg of MXene powder into 120 mL of deionized water, and carrying out ultrasonic treatment for 1 h to obtain MXene dispersion liquid;
(2) taking 120 mL of PEI aqueous solution with the concentration of 8 mg/mL, adding the PEI aqueous solution into the MXene dispersion liquid obtained in the step (1) under stirring, and carrying out water bath at 60 ℃ for 12 h;
(3) centrifuging and washing the dispersion liquid obtained in the step (2) at 4000 rad/min for 5 min each time until the pH of a supernatant is =7 to obtain an MXene dispersion liquid with positive charges;
(4) 100 mg of single-layer MoS is taken2Dispersing the powder in 50 mL deionized water, and performing ultrasonic treatment for 1 h to obtain MoS2A dispersion liquid;
(5) MXene and MoS obtained in the steps (3) and (4) are treated by using a German schutze KA-2 automatic spray gun with the caliber of a nozzle of 0.2 mm and the atomization pressure of 4.5 bar2Sequentially spraying the dispersion liquid on a PET substrate, drying for 24 h at 60 ℃, and stripping the PET substrate to obtain MXene/MoS for the electrode material of the supercapacitor2A layered composite material.
Example 3:
(1) adding 30 mg of MXene powder into 120 mL of deionized water, and carrying out ultrasonic treatment for 1 h to obtain MXene dispersion liquid;
(2) taking 120 mL of PEI aqueous solution with the concentration of 8 mg/mL, adding the PEI aqueous solution into the MXene dispersion liquid obtained in the step (1) under stirring, and carrying out water bath at 60 ℃ for 12 h;
(3) centrifuging and washing the dispersion liquid obtained in the step (2) at 4000 rad/min for 5 min each time until the pH of a supernatant is =7 to obtain an MXene dispersion liquid with positive charges;
(4) 100 mg of single-layer MoS is taken2Dispersing the powder in 50 mL deionized water, and performing ultrasonic treatment for 1 h to obtain MoS2A dispersion liquid;
(5) MXene and MoS obtained in the steps (3) and (4) are treated by using a German schutze KA-2 automatic spray gun with the caliber of a nozzle of 0.2 mm and the atomization pressure of 5 bar2Sequentially spraying the dispersion liquid on a PET substrate, drying for 24 h at 60 ℃, and stripping the PET substrate to obtain MXene/MoS for the electrode material of the supercapacitor2A layered composite material.
Example 4:
(1) adding 30 mg of MXene powder into 120 mL of deionized water, and carrying out ultrasonic treatment for 1 h to obtain MXene dispersion liquid;
(2) taking 120 mL of PEI aqueous solution with the concentration of 8 mg/mL, adding the PEI aqueous solution into the MXene dispersion liquid obtained in the step (1) under stirring, and carrying out water bath at 60 ℃ for 12 h;
(3) centrifuging and washing the dispersion liquid obtained in the step (2) at 4000 rad/min for 5 min each time until the pH of a supernatant is =7 to obtain an MXene dispersion liquid with positive charges;
(4) 100 mg of single-layer MoS is taken2Dispersing the powder in 50 mL deionized water, and performing ultrasonic treatment for 1 h to obtain MoS2A dispersion liquid;
(5) MXene and MoS obtained in the steps (3) and (4) are treated by using a German schutze KA-2 automatic spray gun with the caliber of a nozzle of 0.3 mm and the atomization pressure of 5.5 bar2Sequentially spraying the dispersion liquid on a PET substrate, drying for 24 h at 60 ℃, and stripping the PET substrate to obtain MXene/MoS for the electrode material of the supercapacitor2A layered composite material.
Example 5:
(1) adding 30 mg of MXene powder into 120 mL of deionized water, and carrying out ultrasonic treatment for 1 h to obtain MXene dispersion liquid;
(2) taking 120 mL of PEI aqueous solution with the concentration of 8 mg/mL, adding the PEI aqueous solution into the MXene dispersion liquid obtained in the step (1) under stirring, and carrying out water bath at 60 ℃ for 12 h;
(3) centrifuging and washing the dispersion liquid obtained in the step (2) at 4000 rad/min for 5 min each time until the pH of a supernatant is =7 to obtain an MXene dispersion liquid with positive charges;
(4) 100 mg of single-layer MoS is taken2Dispersing the powder in 50 mL deionized water, and performing ultrasonic treatment for 1 h to obtain MoS2A dispersion liquid;
(5) MXene and MoS obtained in the steps (3) and (4) are treated by using a German schutze KA-2 automatic spray gun with the caliber of a nozzle of 0.3 mm and the atomization pressure of 6 bar2Sequentially spraying the dispersion liquid on a PET substrate, drying for 24 h at 60 ℃, and stripping the PET substrate to obtain MXene/MoS for the electrode material of the supercapacitor2A layered composite material.
The above description is an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications that can be made by using the equivalent structures or equivalent processes of the present invention as described in the specification of the present invention or applied to other related fields directly or indirectly are intended to be encompassed by the present invention.
Claims (4)
1. MXene/MoS for supercapacitor electrodes2The preparation method of the composite material is characterized by comprising the following steps: ultrasonically dispersing the monolayer MXene powder into deionized water to obtain MXene dispersion liquid, and adding polyethyleneimine, namely PEI solution to obtain MXene dispersion liquid with positive charges; the single layer MoS2Dispersing the powder in deionized water and performing ultrasonic treatment to obtain single-layer MoS2A dispersion liquid; mixing positively charged MXene and negatively charged MoS2The dispersion liquid is sequentially sprayed on a polyethylene terephthalate (PET) substrate, and after drying, the PET substrate is peeled off to obtain MXene/MoS for the electrode material of the super capacitor2A layered composite material;
the method comprises the following specific steps:
(1) adding 30 mg of MXene powder into 120 mL of deionized water, and carrying out ultrasonic treatment for 1 h to obtain MXene dispersion liquid;
(2) taking 120 mL of PEI aqueous solution with the concentration of 8 mg/mL, adding the PEI aqueous solution into the MXene dispersion liquid obtained in the step (1) under stirring, and carrying out water bath at 60 ℃ for 12 h;
(3) centrifuging and washing the dispersion liquid obtained in the step (2) at 4000 rad/min for 5 min each time until the pH of a supernatant is =7 to obtain an MXene dispersion liquid with positive charges;
(4) 100 mg of single-layer MoS is taken2Dispersing the powder in 50 mL deionized water, and performing ultrasonic treatment for 1 h to obtain MoS2A dispersion liquid;
(5) MXene and MoS obtained in the step (3) and the step (4) are sprayed by a spray gun2Sequentially spraying the dispersion liquid on a PET substrate, drying for 24 h at 60 ℃, and stripping the PET substrate to obtain MXene/MoS for the electrode material of the supercapacitor2A layered composite material.
2. MXene/MoS for supercapacitor electrode according to claim 12The preparation method of the composite material is characterized by comprising the following steps: the MXene is Ti3C2TxOr Ti2CTxOr V2CTxOr Mo or3C2Tx。
3. MXene/MoS for supercapacitor electrode according to claim 12The preparation method of the composite material is characterized by comprising the following steps: the nozzle bore of the spray gun used was 0.2 mm or 0.3 mm.
4. MXene/MoS for supercapacitor electrode according to claim 12The preparation method of the composite material is characterized by comprising the following steps: the atomization pressure of the spray gun is 4 bar, or 4.5 bar, or 5 bar, or 5.5 bar, or 6 bar.
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| CN105609319A (en) * | 2016-01-29 | 2016-05-25 | 西北师范大学 | Flaky titanium carbide-loaded manganese dioxide composite material for super capacitor electrode material and preparation of flaky titanium carbide-loaded manganese dioxide composite material |
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| KR101400593B1 (en) * | 2012-12-06 | 2014-05-27 | 삼성정밀화학 주식회사 | Cathode active material, method for preparing the same, and lithium secondary batteries comprising the same |
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