CN112331486A - Preparation method of plasma modified carbon cloth and MXene flexible electrode material - Google Patents
Preparation method of plasma modified carbon cloth and MXene flexible electrode material Download PDFInfo
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- CN112331486A CN112331486A CN202010719873.3A CN202010719873A CN112331486A CN 112331486 A CN112331486 A CN 112331486A CN 202010719873 A CN202010719873 A CN 202010719873A CN 112331486 A CN112331486 A CN 112331486A
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- carbon cloth
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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
- H01G11/30—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
- H01G11/84—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 invention discloses a preparation method of a plasma modified carbon cloth and MXene flexible electrode material, which comprises the following steps: 1) adding MAX powder into a mixed solution of hydrochloric acid and lithium fluoride, and continuously stirring to remove an element A in MAX; 2) continuously carrying out centrifugal cleaning on the mixed solution, and carrying out ultrasonic treatment on a product after centrifugal cleaning to obtain MXene suspension; 3) soaking the carbon cloth in an acetone solution, putting the carbon cloth into an oven for drying after soaking, and cleaning dust and impurities on the surface of the carbon cloth after drying; 4) placing the cleaned carbon cloth in a plasma vapor deposition box, and etching the surface of the carbon cloth by using argon and oxygen as etching gases; 5) and (3) dipping the carbon cloth subjected to plasma treatment in MXene suspension for 1 hour to ensure that the surface of the carbon cloth is fully contacted with the MXene suspension, and then placing the carbon cloth in a vacuum oven to dry for 24 hours at 40 ℃ to obtain the carbon cloth and MXene flexible electrode material.
Description
Technical Field
The invention relates to the field of electrode material preparation, in particular to a preparation method of a plasma modified carbon cloth and MXene flexible electrode material.
Background
Supercapacitors, also known as electrochemical capacitors, are considered the most important energy storage and transportation devices of the 21 st century. The super capacitor has the characteristics of high power performance, long cycle life, long storage time, fast charge and discharge and wide working temperature range. Due to its safety and reliability, as well as high power density and cycling stability, it is widely used in many areas, such as portable electronic products and energy storage devices, backup power supplies, etc.
In recent years, two-dimensional transition metal carbides or nitrides (MXene) have attracted much attention. MXene has abundant physical properties such as conductivity, magnetism, light, thermal stability, mechanical properties and the like, has larger specific surface area and good conductivity, and has very good application prospect in flexible supercapacitors due to good tensile strength and flexibility.
However, pure MXene sheet materials are easily stacked together to affect their electrochemical performance. Another effective method of reducing the stacking of MXene plies, in addition to delamination, is to compound with other materials. Carbon fibers have excellent properties such as high strength, high modulus and fatigue resistance. As a reinforcing material for composite materials, carbon fibers have been widely used in aerospace, automobile manufacturing, and many other fields. However, the mechanical properties of the composite material may be affected to some extent due to disadvantages such as poor adhesion between the carbon fibers and the substrate. In order to improve the interfacial bonding strength of the composite material, the carbon fiber needs to be surface-treated to improve the interfacial structure.
Disclosure of Invention
The invention aims to provide a preparation method of a plasma modified carbon cloth and an MXene flexible electrode material aiming at the defects in the prior art so as to solve the problems in the prior art.
The technical problem solved by the invention can be realized by adopting the following technical scheme:
a preparation method of plasma modified carbon cloth and MXene flexible electrode materials comprises the following steps:
1) adding MAX powder into a mixed solution of hydrochloric acid and lithium fluoride, continuously stirring, and removing an element A in MAX through an etching reaction;
2) after the etching reaction is finished, continuing to centrifugally clean the mixed solution, and carrying out ultrasonic treatment on a product after centrifugal cleaning to obtain a required MXene suspension;
3) soaking the carbon cloth in an acetone solution, putting the carbon cloth into an oven for drying after soaking, and cleaning dust and impurities on the surface of the carbon cloth after drying;
4) placing the cleaned carbon cloth in a plasma vapor deposition box, etching the surface of the carbon cloth by using argon and oxygen as etching gases, and controlling the roughness and wettability of the surface of the carbon cloth by adjusting the volume parameter and the power parameter of the plasma vapor deposition gas;
5) and (3) dipping the carbon cloth subjected to plasma treatment in MXene suspension for 1 hour to ensure that the surface of the carbon cloth is fully contacted with the MXene suspension, and then placing the carbon cloth in a vacuum oven to dry for 24 hours at 40 ℃ to obtain the carbon cloth and MXene flexible electrode material.
Further, the MAX powder in the step 1) is Ti3AlC2And the element A is Al element.
Further, the etching reaction time in the step 1) is 24 hours, and the temperature is 35 ℃.
Further, the rotation speed of centrifugal cleaning in the step 2) is 8000r/min, and the ultrasonic time is 6 hours.
Further, the soaking time of the acetone solution in the step 3) is 2 hours.
Further, the volume ratio of argon to oxygen in the step 4) is 12: 0,11: 1,10: 2 and 9: and 3, the power parameters are 110W, 175W and 230W.
Further, the loading amount of MXene on the carbon cloth in the step 5) is 2 wt.%, 4 wt.% and 6 wt.%, respectively.
Compared with the prior art, the invention has the beneficial effects that:
the plasma modified carbon cloth/MXene flexible electrode material provided by the invention is prepared by a simple dipping method, the method is mild in condition and simple to operate, and the appearance of the product is controlled.
The plasma modified carbon cloth/MXene flexible electrode material provided by the invention takes the carbon cloth as a flexible substrate, has excellent mechanical properties such as stretchability and bendability, does not significantly influence the properties of the carbon cloth after plasma treatment, and can be used as a good candidate substrate of a wearable flexible electronic device.
The wettability of the surface of the carbon cloth after plasma treatment is greatly increased, the interface bonding strength of the carbon cloth and MXene can be improved, and the loading capacity of the MXene is effectively improved.
The preparation method of the electrode provided by the invention is simple and convenient and is easy to operate.
Drawings
Fig. 1 is a schematic flow chart of a preparation method of the plasma modified carbon cloth and the MXene flexible electrode material according to the present invention.
Fig. 2 is a schematic surface contact angle diagram of the preparation method of the plasma modified carbon cloth and the MXene flexible electrode material.
Fig. 3 is a scanning electron microscope microscopic morphology image of the plasma modified carbon cloth/MXene flexible electrode.
Fig. 4 is an electrode cyclic voltammetry curve diagram of different MXene concentrations of the plasma modified carbon cloth/MXene flexible electrode of the present invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Referring to fig. 1 to 4, the preparation method of the plasma modified carbon cloth and MXene flexible electrode material of the present invention includes the following steps:
1) adding MAX powder into a mixed solution of hydrochloric acid and lithium fluoride, continuously stirring, and removing an element A in MAX through an etching reaction;
2) after the etching reaction is finished, continuing to centrifugally clean the mixed solution, and carrying out ultrasonic treatment on a product after centrifugal cleaning to obtain a required MXene suspension;
3) soaking the carbon cloth in an acetone solution, putting the carbon cloth into an oven for drying after soaking, and cleaning dust and impurities on the surface of the carbon cloth after drying;
4) placing the cleaned carbon cloth in a plasma vapor deposition box, etching the surface of the carbon cloth by using argon and oxygen as etching gases, and controlling the roughness and wettability of the surface of the carbon cloth by adjusting the volume parameter and the power parameter of the plasma vapor deposition gas;
5) and (3) dipping the carbon cloth subjected to plasma treatment in MXene suspension for 1 hour to ensure that the surface of the carbon cloth is fully contacted with the MXene suspension, and then placing the carbon cloth in a vacuum oven to dry for 24 hours at 40 ℃ to obtain the carbon cloth and MXene flexible electrode material.
Example 1
In this example, the MXene suspension was prepared by the following steps: 1gMAX (Ti)3AlC2) Was slowly added to a mixed solution containing 20 ml of 6M hydrochloric acid and 1g of lithium fluoride and then stirred at 40 ℃ for 45 hours. Then, the obtained acidic solution is washed 5-8 times with deionized water (DI) under the condition of a centrifuge (8000rpm) until the pH value is 6. This was followed by sonication in water (under argon) for about 6 hours and post-centrifugation (3500 rpm) for 30 minutes to give a stable dark green supernatant of MXene. MXene suspensions of different concentrations were prepared by controlling the amount of water added during sonication. The preparation of the plasma modified carbon cloth comprises the following steps: after cleaning surface impurities of a commercially available carbon cloth with acetone, putting the carbon cloth into a cavity of plasma vapor deposition, wherein the volume of oxygen is 9, the volume of argon is 3, the power is 175W, the time is 15 minutes, and the front side and the back side of the carbon cloth are treated under the same conditions. The preparation method of the plasma modified carbon cloth/MXene flexible electrode comprises the following steps: the carbon cloth after plasma treatment is placed in MXene suspension, and MXene can be attached due to good moisture absorption performance of the modified carbon clothA sandwich structure is formed on the surface of the carbon cloth.
Example 2
In this example, the MXene suspension was prepared by the following steps: 1g of MAX (Ti3AlC2) was slowly added to a mixed solution containing 20 ml of 6M hydrochloric acid and 1g of lithium fluoride and then stirred at 40 ℃ for 45 hours. Then, the obtained acidic solution is washed 5-8 times with deionized water (DI) under the condition of a centrifuge (8000rpm) until the pH value is 6. This was followed by sonication in water (under argon) for about 6 hours and post-centrifugation (3500 rpm) for 30 minutes to give a stable dark green supernatant of MXene. MXene suspensions of different concentrations were prepared by controlling the amount of water added during sonication. The preparation of the plasma modified carbon cloth comprises the following steps: after cleaning surface impurities of a commercially available carbon cloth with acetone, putting the carbon cloth into a cavity of plasma vapor deposition, wherein the volume of oxygen is even 10, the volume of argon is 2, the power is 175W, the time is 15 minutes, and the front side and the back side of the carbon cloth are treated under the same conditions. The preparation method of the plasma modified carbon cloth/MXene flexible electrode comprises the following steps: the carbon cloth after plasma treatment is placed in MXene suspension, and MXene can be attached to the surface of the carbon cloth to form a sandwich structure due to the good moisture absorption performance of the modified carbon cloth.
Example 3
In this example, the MXene suspension was prepared by the following steps: 1g of MAX (Ti3AlC2) was slowly added to a mixed solution containing 20 ml of 6M hydrochloric acid and 1g of lithium fluoride and then stirred at 40 ℃ for 45 hours. Then, the obtained acidic solution is washed 5-8 times with deionized water (DI) under the condition of a centrifuge (8000rpm) until the pH value is 6. This was followed by sonication in water (under argon) for about 6 hours and post-centrifugation (3500 rpm) for 30 minutes to give a stable dark green supernatant of MXene. MXene suspensions of different concentrations were prepared by controlling the amount of water added during sonication. The preparation of the plasma modified carbon cloth comprises the following steps: after cleaning surface impurities of a commercially available carbon cloth with acetone, putting the carbon cloth into a cavity of plasma vapor deposition, wherein the volume of oxygen is even 11, the volume of argon is 1, the power is 175W, the time is 15 minutes, and the front side and the back side of the carbon cloth are treated under the same conditions. The preparation method of the plasma modified carbon cloth/MXene flexible electrode comprises the following steps: the carbon cloth after plasma treatment is placed in MXene suspension, and MXene can be attached to the surface of the carbon cloth to form a sandwich structure due to the good moisture absorption performance of the modified carbon cloth.
Example 4
In this embodiment, the preparation of the MXene suspension includes the following steps: 1g of MAX (Ti3AlC2) was slowly added to a mixed solution containing 20 ml of 6M hydrochloric acid and 1g of lithium fluoride and then stirred at 40 ℃ for 45 hours. Then, the obtained acidic solution is washed 5-8 times with deionized water (DI) under the condition of a centrifuge (8000rpm) until the pH value is 6. This was followed by sonication in water (under argon) for about 6 hours and post-centrifugation (3500 rpm) for 30 minutes to give a stable dark green supernatant of MXene. MXene suspensions of different concentrations were prepared by controlling the amount of water added during sonication. The preparation of the plasma modified carbon cloth comprises the following steps: after cleaning surface impurities of a commercially available carbon cloth with acetone, putting the carbon cloth into a cavity of plasma vapor deposition, wherein the volume of oxygen is even 12, the volume of argon is 0, the power is 175W, the time is 15 minutes, and the front side and the back side of the carbon cloth are treated under the same conditions. The preparation method of the plasma modified carbon cloth/MXene flexible electrode comprises the following steps: the carbon cloth after plasma treatment is placed in MXene suspension, and MXene can be attached to the surface of the carbon cloth to form a sandwich structure due to the good moisture absorption performance of the modified carbon cloth.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. A preparation method of plasma modified carbon cloth and MXene flexible electrode materials is characterized by comprising the following steps:
1) adding MAX powder into a mixed solution of hydrochloric acid and lithium fluoride, continuously stirring, and removing an element A in MAX through an etching reaction;
2) after the etching reaction is finished, continuing to centrifugally clean the mixed solution, and carrying out ultrasonic treatment on a product after centrifugal cleaning to obtain a required MXene suspension;
3) soaking the carbon cloth in an acetone solution, putting the carbon cloth into an oven for drying after soaking, and cleaning dust and impurities on the surface of the carbon cloth after drying;
4) placing the cleaned carbon cloth in a plasma vapor deposition box, etching the surface of the carbon cloth by using argon and oxygen as etching gases, and controlling the roughness and wettability of the surface of the carbon cloth by adjusting the volume parameter and the power parameter of the plasma vapor deposition gas;
5) and (3) dipping the carbon cloth subjected to plasma treatment in MXene suspension for 1 hour to ensure that the surface of the carbon cloth is fully contacted with the MXene suspension, and then placing the carbon cloth in a vacuum oven to dry for 24 hours at 40 ℃ to obtain the carbon cloth and MXene flexible electrode material.
2. The method for preparing the plasma modified carbon cloth and MXene flexible electrode material as claimed in claim 1, wherein the MAX powder in step 1) is Ti3AlC2And the element A is Al element.
3. The method for preparing the plasma modified carbon cloth and MXene flexible electrode material as claimed in claim 1, wherein the etching reaction time in step 1) is 24 hours and the temperature is 35 ℃.
4. The method for preparing the plasma modified carbon cloth and MXene flexible electrode material as claimed in claim 1, wherein the centrifugal cleaning rotation speed in step 2) is 8000r/min, and the ultrasonic time is 6 hours.
5. The method for preparing the plasma modified carbon cloth and MXene flexible electrode material as claimed in claim 1, wherein the acetone solution soaking time in step 3) is 2 hours.
6. The method for preparing the plasma modified carbon cloth and MXene flexible electrode material as claimed in claim 1, wherein the volume ratio of argon to oxygen in step 4) is 12: 0,11: 1,10: 2 and 9: and 3, power parameters are 150W, 175W and 200W.
7. The method for preparing the plasma modified carbon cloth and the MXene flexible electrode material as claimed in claim 1, wherein the loading amount of MXene on the carbon cloth in the step 5) is 2 wt.%, 4 wt.% and 6 wt.%, respectively.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114160176A (en) * | 2021-12-27 | 2022-03-11 | 浙江工业大学 | MXene-ACF composite material for catalyzing hydrochlorination of acetylene and preparation method and application thereof |
| CN114551888A (en) * | 2022-04-26 | 2022-05-27 | 北京三川烯能科技有限公司 | Method for inhibiting lithium precipitation of lithium ion battery negative electrode, slurry, negative electrode, battery and vehicle |
| CN114843700A (en) * | 2022-04-18 | 2022-08-02 | 西南交通大学 | Highly ordered terminated MXene and preparation method and application thereof |
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| CN108172417A (en) * | 2017-12-28 | 2018-06-15 | 南昌航空大学 | A kind of carbon cloth surfaces method of modifying for flexible super capacitor electrode |
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| CN108172417A (en) * | 2017-12-28 | 2018-06-15 | 南昌航空大学 | A kind of carbon cloth surfaces method of modifying for flexible super capacitor electrode |
| CN110648864A (en) * | 2019-09-30 | 2020-01-03 | 常州大学 | Manufacturing method of flexible low-temperature-resistant water system supercapacitor |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114160176A (en) * | 2021-12-27 | 2022-03-11 | 浙江工业大学 | MXene-ACF composite material for catalyzing hydrochlorination of acetylene and preparation method and application thereof |
| CN114160176B (en) * | 2021-12-27 | 2024-03-26 | 浙江工业大学 | MXene-ACF composite material for catalyzing hydrochlorination of acetylene as well as preparation method and application thereof |
| CN114843700A (en) * | 2022-04-18 | 2022-08-02 | 西南交通大学 | Highly ordered terminated MXene and preparation method and application thereof |
| CN114843700B (en) * | 2022-04-18 | 2023-07-07 | 西南交通大学 | Highly ordered end-group MXene and preparation method and application thereof |
| CN114551888A (en) * | 2022-04-26 | 2022-05-27 | 北京三川烯能科技有限公司 | Method for inhibiting lithium precipitation of lithium ion battery negative electrode, slurry, negative electrode, battery and vehicle |
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