CN109830381B - Preparation method of MXene/MoS2 composites for supercapacitor electrodes - Google Patents
Preparation method of MXene/MoS2 composites for supercapacitor electrodes 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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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical class S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract 8
- 238000002360 preparation method Methods 0.000 title claims description 8
- 239000006185 dispersion Substances 0.000 claims abstract description 60
- 239000002131 composite material Substances 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 24
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 24
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 24
- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 22
- 229920002873 Polyethylenimine Polymers 0.000 claims abstract description 21
- 239000000758 substrate Substances 0.000 claims abstract description 21
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- 239000002356 single layer Substances 0.000 claims abstract description 19
- 239000007772 electrode material Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- -1 polyethylene terephthalate Polymers 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 239000007921 spray Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- 238000000889 atomisation Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 description 44
- 238000009210 therapy by ultrasound Methods 0.000 description 14
- 239000003990 capacitor Substances 0.000 description 8
- 238000005507 spraying Methods 0.000 description 8
- 238000005406 washing Methods 0.000 description 6
- 238000001338 self-assembly Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000000707 layer-by-layer assembly Methods 0.000 description 2
- 229910009819 Ti3C2 Inorganic materials 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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
Landscapes
- Electric Double-Layer Capacitors Or The Like (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
用于超级电容器电极的MXene/MoS2复合材料制备方法，其步骤为：将单层MXene粉末超声分散于水中得到MXene分散液，加入聚乙烯亚氨，即PEI溶液得到带正电荷的MXene分散液；将单层MoS2粉末分散在去离子水中并超声，得到单层MoS2分散液；将带正电荷的MXene和带负电荷的MoS2分散液依次喷涂于聚对苯二甲酸乙二酯，即PET基底上，干燥后得到用于超级电容器电极材料的MXene/MoS2层状复合材料。A method for preparing an MXene/MoS2 composite material for supercapacitor electrodes, comprising the steps of: ultrasonically dispersing a single-layer MXene powder in water to obtain an MXene dispersion, and adding polyethyleneimine, that is, a PEI solution, to obtain a positively charged MXene dispersion; The monolayer MoS2 powder was dispersed in deionized water and sonicated to obtain a monolayer MoS2 dispersion; the positively charged MXene and the negatively charged MoS2 dispersion were sequentially sprayed on polyethylene terephthalate, i.e. On the PET substrate, the MXene/MoS 2 layered composite material for supercapacitor electrode material was obtained after drying.
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)
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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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Effective date of registration: 20210719 Address after: 310018 room 1201, 12th floor, Yifu science and technology building, East District, China University of metrology, No. 258 Xueyuan street, economic and Technological Development Zone, Hangzhou, Zhejiang Province Patentee after: Hangzhou Realistic New Materials Technology Co.,Ltd. Address before: 730050, No. 287 Lan Ping Road, Qilihe District, Gansu, Lanzhou Patentee before: LANZHOU University OF TECHNOLOGY |