CN107934955B - Method for activating commercial carbon fiber cloth - Google Patents
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- CN107934955B CN107934955B CN201711146631.4A CN201711146631A CN107934955B CN 107934955 B CN107934955 B CN 107934955B CN 201711146631 A CN201711146631 A CN 201711146631A CN 107934955 B CN107934955 B CN 107934955B
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
The invention discloses a method for activating commercial carbon fiber cloth, which comprises the following steps: the method comprises the steps of taking commercial carbon cloth as a raw material, placing the carbon cloth with a clean surface in a muffle furnace, and carrying out activation treatment for a certain time in an air atmosphere at 400-500 ℃ to obtain the activated commercial carbon cloth. The method directly activates the carbon cloth by utilizing the atmospheric environment for the first time without any inert gas protection and atmosphere and solution treatment, has the advantages of environment-friendly and controllable activation process, extremely simple and convenient operation and low production cost, and is suitable for large-scale industrial production. The activated flexible commercial carbon cloth material can be directly used as an electrode or a current collector of a wearable novel battery or a flexible super capacitor, is expected to be used as a carrier of a catalyst or an adsorbent, an oxidative degradation material, a desulfurization or air purification material and the like, and is applied to the fields of electronic devices, energy sources and environments.
Description
Technical Field
The invention relates to the field of commercial carbon cloth activation, in particular to a process method for activating commercial carbon fiber cloth (commercial carbon cloth for short), and particularly relates to a method for activating the commercial carbon cloth, which can be applied to industrial production in a large scale.
Background
With the development of science and technology, the demand of people on wearable electronic devices is ever increasing, and the development of flexible energy storage devices capable of supplying energy to the electronic devices is particularly important. As a novel energy storage device, the super capacitor has the advantages of the traditional capacitor and the secondary battery, and has wide and profound application prospect in various fields. The flexible super capacitor has higher energy density, faster charge and discharge speed and longer cycle stability, is concerned by many scholars, and becomes one of the hot spots of the current research. The preparation of the super capacitor which meets the actual requirements and is simple, convenient, controllable and low in cost faces huge challenges. The three electrode materials of the super capacitor are carbon-based materials, metal oxides and conductive polymers. On the one hand, among the three main types of materials, metal oxides and conductive polymers have high specific capacitance and high power density, but are generally expensive, have poor cycle performance and stability, and are prone to environmental pollution. The carbon-based material has the advantages of rich source, large specific surface area, good conductivity, high power density, low cost and the like, and is a main electrode material of a commercial super capacitor. On the other hand, in order to manufacture a flexible supercapacitor, many workers combine an active material, an electrolyte, a binder, a conductive agent, a separator, a current collector, an encapsulation body, and the like to constitute one device, and the proportion of the active material therein is small for the entire device. Resulting in a small capacitance based on the entire device and failing to meet practical requirements. For example, patent CN104795251A discloses a method for preparing a supercapacitor, which can obtain a high specific surface area alginate silicate based porous carbon powder. Since the material is in the form of powder, it cannot be directly used for flexible devices. And many thin films directly grown on the substrate to form the flexible device also have small capacitance of the whole device due to the small specific surface area of the used substrate and the small mass of active substances. Therefore, the development of the high-cost-performance flexible electrode material, the moving of the flexible electrode material out of a laboratory and the realization of industrial production are the most critical problems to be solved by researchers at present.
The commercial carbon fiber cloth is a carbon material textile fabric with carbon content of more than 95 percent and prepared by a traditional method. The commercial carbon cloth not only has the intrinsic property of the carbon material, but also has excellent properties of textile flexibility, processability, high specific strength, good creep resistance, low density, good thermal stability and chemical stability, lower thermal expansion coefficient, higher electrical conductivity and the like, and is widely used as a substrate material or a current collector of a flexible electrode in research. In many studies, different inorganic materials have been able to successfully grow nanostructures on commercial carbon fiber cloth, thereby improving the electrochemical performance of the composite material, and showing great commercial potential. For example, patent ZL01010610593.5 discloses a method for growing carbon nanoparticles on a carbon cloth, which can produce uniform carbon nanoparticles on the carbon cloth for preparing flexible field electron emission cold cathode devices. Also, as disclosed in CN102087921A, manganese oxide directly grows on carbon nanofibers to form a self-supporting flexible electrode composite material. However, since the commercial carbon fiber cloth has a smooth surface, a small specific surface area, and is chemically inert itself, the specific capacitance (1-2F &) of the commercial carbon cloth-1,～10mF﹒cm-2) Much lower than some other carbon materials, for example: graphene (100-200F. g)-1) And single-walled carbon nanotube (100-200F &. g)-1) And the like. Due to the series of reasons, commercial carbon cloth is rarely directly used as an electrode material in industrial production and laboratory research, which obviously greatly limits the application of the commercial carbon cloth. Therefore, it is necessary to activate the commercial carbon cloth by a proper method to improve the roughness thereof, so that the activated commercial carbon cloth has a large specific surface area and proper functional groups, thereby enabling the commercial carbon cloth to be directly used as a flexible electrode material with good electrochemical performance. At present, a plurality of carbon cloth activating treatment methods exist, for example, in patent CN104562631A, a surface treatment method of electrochemical anodic oxidation is adopted to activate the carbon cloth, and CN05869923A adopts a solution dipping recrystallization method to realize activating and opening, so as to improve the activity and roughness of the carbon fiber surface. Others are gas phase oxidation, liquid phase oxidation, plasma treatment, vapor deposition, electrochemical deposition, and the like. However, almost all methods need to adjust the ratio of reagents or atmosphere and protect with inert gas, and the treatment process is complicated, high in cost and easy to damage the fiber body, so that the comprehensive performance of the material is reduced.
Disclosure of Invention
The invention aims to provide a method for activating and treating commercial carbon fiber cloth, which has the advantages of extremely simple and convenient treatment method, strong industrial applicability, low cost, low energy consumption, excellent performance and obvious activation effect.
The invention aims to activate commercial carbon cloth and greatly improve the specific capacitance of the commercial carbon cloth, and specifically comprises the following steps:
(1) cleaning the commercial carbon cloth to obtain carbon cloth with a clean surface;
(2) placing the clean commercial carbon cloth obtained in the step (1) in a muffle furnace, and carrying out activation treatment in an ambient air atmosphere, wherein the treatment temperature is 400-500 ℃, and the time is 1-3 h;
(3) and after the reaction is finished, obtaining the activated commercial carbon cloth.
In the technical scheme, the carbon cloth is hydrophilic or hydrophobic commercial carbon cloth.
Preferably, the treatment temperature is 450 ℃ and the reaction time is 2 h.
After the above activation treatment, the activated carbon cloth had a mass per unit area of about 12 mg/cm-2The area-specific capacitance can reach 1350.2 mF--2Mass-to-capacitance can reach 112.5F &-1。
Compared with the prior art, the invention has the following main advantages:
the activation treatment method has the advantages of simple process, short time consumption and low cost, and can be realized in industrial production in a large scale. The activated commercial carbon cloth obtained by the method has high specific capacitance and good flexibility, and the surface roughness of the carbon cloth fiber can be improved in the high-temperature treatment process, so that the activated carbon cloth has a larger specific surface area, and the electrochemical performance of the material is improved. The preparation method is simple and convenient, the reaction system is an open system, the conditions are mild, the environment is protected, the controllability, the applicability and the transportability are strong, the cost is low, the energy consumption is low, the method is suitable for industrial production, and the prepared activated commercial carbon cloth material is expected to be widely applied to the fields of electronics, energy and environment, such as flexible energy storage device electrodes, carriers of catalysts or adsorbents, desulfurization or air purification materials and the like.
Drawings
FIG. 1 is a SEM photograph of the surface of a commercial carbon fiber cloth material without activation treatment in example 1.
Fig. 2 is a field emission scanning electron microscope photograph of the surface of the activated commercial carbon fiber cloth material prepared in example 1.
FIG. 3 shows the commercial carbon cloth of example 1 without activation and the commercial carbon cloth of examples 1-5 after activation with 100 mV--1Cyclic voltammogram at the scan rate.
FIG. 4 shows specific capacitance values of activated commercial carbon cloths of examples 1 to 5 at different discharge current densities.
FIG. 5 shows specific capacitance values of the activated commercial carbon cloths of examples 1-5 at different voltage scan rates.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
(1) Selecting the size of 2.5 multiplied by 2.5cm2And a commercial carbon cloth with the thickness of 0.35mm is used as a raw material, and the surface of the carbon cloth is cleaned by absolute ethyl alcohol, ultrasonically washed by deionized water and dried.
(2) Placing the clean carbon cloth obtained in the step (1) in a muffle furnace, and performing activation treatment for 1 hour at the temperature of 400 ℃ in the ambient air atmosphere;
(3) and after the reaction is finished, obtaining the activated carbon cloth.
The front and back field emission scanning electron microscope photographs of the obtained product are respectively shown in figures 1 and 2, and the observation result of the surface morphology shows that the commercial carbon cloth fiber without activation treatment has a smooth surface, and the surface of the carbon cloth fiber after activation treatment has a flat bubble-shaped rough structure. Electrochemical tests were performed on the activated commercial carbon cloth prepared, and the results are shown in fig. 4 and 5. The product was subjected to charge and discharge tests at different discharge current densities, with a value of 1 mA--2With discharge Current Density, specific capacitance of 27.7 mF. cm-2，50mA﹒cm-2With discharge current density, the area vs. capacitance still has an expiration of 8mF cm-2(ii) a Mush at 2mV in different Scan Rate Cyclic voltammetry tests-1With the scanning rate of (5), the area-to-capacitance was 62.61 mF. m.cm-2，100mV﹒s-1Has an area specific capacitance of 26.51 mF. cm-2。
Example 2
(1) Selecting the size of 2.5 multiplied by 2.5cm2And a commercial carbon cloth with the thickness of 0.35mm is used as a raw material, and the surface of the carbon cloth is cleaned by absolute ethyl alcohol, ultrasonically washed by deionized water and dried.
(2) Placing the clean carbon cloth obtained in the step (1) in a muffle furnace, and performing activation treatment for 1 hour in an ambient air atmosphere at the temperature of 450 ℃;
(3) and after the reaction is finished, obtaining the activated carbon cloth.
Electrochemical tests were carried out on the activated commercial carbon cloth thus prepared, and the results are shown in FIGS. 4 and 5. The product was subjected to charge and discharge tests at different discharge current densities, with a value of 1 mA--2At discharging current density, specific capacitance of 642.2 mF--2，50mA﹒cm-2With discharge current density, the area to capacitance still had 538 mF--2(ii) a Mush at 2mV in different Scan Rate Cyclic voltammetry tests-1With the scanning rate of (5), the area-to-capacitance was 643.54 mF. m.cm-2，100mV﹒s-1Has an area-to-capacitance value of 506.56 mF! cm-2。
Example 3
(1) Selecting the size of 2.5 multiplied by 2.5cm2And a commercial carbon cloth with the thickness of 0.35mm is used as a raw material, and the surface of the carbon cloth is cleaned by absolute ethyl alcohol, ultrasonically washed by deionized water and dried.
(2) Placing the clean carbon cloth obtained in the step (1) in a muffle furnace, and performing activation treatment for 2 hours at the temperature of 450 ℃ in the ambient air atmosphere;
(3) and after the reaction is finished, obtaining the activated carbon cloth.
Electrochemical tests were performed on the activated commercial carbon cloth prepared, and the results are shown in fig. 4 and 5. The product was subjected to charge and discharge tests at different discharge current densities, with a value of 1 mA--2At discharging current density, specific capacitance of 1100.6 mF--2，50mA﹒cm-2780mF & lt/EN & gt cm & lt/EN & gt in discharge current density-2(ii) a Mush at 2mV in different Scan Rate Cyclic voltammetry tests-1With the scanning rate of (5), the area-to-capacitance was 1136.72 mF. m.cm-2，100mV﹒s-1The area specific capacitance still remains 664.32mF cm-2。
Example 4
(1) Selecting the size of 2.5 multiplied by 2.5cm2And a commercial carbon cloth with the thickness of 0.35mm is used as a raw material, and the surface of the carbon cloth is cleaned by absolute ethyl alcohol, ultrasonically washed by deionized water and dried.
(2) Placing the clean carbon cloth obtained in the step (1) in a muffle furnace, and performing activation treatment for 3 hours at the temperature of 450 ℃ in the ambient air atmosphere;
(3) and after the reaction is finished, obtaining the activated carbon cloth.
Electrochemical tests were performed on the activated commercial carbon cloth prepared, and the results are shown in fig. 4 and 5. The product was subjected to charge and discharge tests at different discharge current densities, with a value of 1 mA--2At discharging current density, specific capacitance of 1350.2 mF--2，50mA﹒cm-2With the discharge current density, the area ratio of the capacitor still has a value of 672mF cm-2(ii) a Mush at 2mV in different Scan Rate Cyclic voltammetry tests-1With the scanning rate of (5), the area-to-capacitance was 1342.78 mF. m.cm-2，100mV﹒s-1The area specific capacitance still remains 442.29mF cm-2。
Example 5
(1) Selecting the size of 2.5 multiplied by 2.5cm2And a commercial carbon cloth with the thickness of 0.35mm is used as a raw material, and the surface of the carbon cloth is cleaned by absolute ethyl alcohol, ultrasonically washed by deionized water and dried.
(2) Placing the clean carbon cloth obtained in the step (1) in a muffle furnace, and performing activation treatment for 1 hour in an ambient air atmosphere at the temperature of 500 ℃;
(3) and after the reaction is finished, obtaining the activated carbon cloth.
Electrochemical tests were performed on the activated commercial carbon cloth prepared, and the results are shown in fig. 4 and 5. The product was subjected to charge and discharge tests at different discharge current densities, with a value of 1 mA--2Beverage with specific capacitance of 1205.2 mF--2，50mA﹒cm-2With discharge current density, area to capacitance still has a value of 482mF cm-2(ii) a Mush at 2mV in different Scan Rate Cyclic voltammetry tests-1With the scanning rate of (5), the area-to-capacitance was 1233.95 mF. m.cm-2，100mV﹒s-1The area specific capacitance still remains 426.65mF cm-2。
Claims (1)
1. A method for activating and treating commercial carbon fiber cloth, which is characterized in that the commercial carbon fiber cloth is hydrophilic or hydrophobic, and the method comprises the following steps:
(1) cleaning the commercial carbon fiber cloth to obtain commercial carbon cloth with a clean surface;
(2) placing the clean commercial carbon cloth obtained in the step (1) in a muffle furnace, and carrying out activation treatment in an ambient air atmosphere, wherein the treatment temperature is 450 ℃ and the time is 3 h;
(3) after the reaction is finished, obtaining activated commercial carbon cloth;
the commercial carbon fiber cloth treated by the method can be directly used as a flexible electrode material.
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| CN108767302A (en) * | 2018-06-19 | 2018-11-06 | 杭州电子科技大学 | The method for discarding rice husk is handled using MFC |
| CN109686595B (en) * | 2019-01-18 | 2020-11-10 | 三峡大学 | Activation method of conductive carbon cloth and application of supercapacitor of conductive carbon cloth |
| CN109817934A (en) * | 2019-01-30 | 2019-05-28 | 陕西科技大学 | A kind of hydro-thermal calcination method preparation carbon coating Sn/SnO2The method of/carbon cloth negative electrode material |
| CN109786717A (en) * | 2019-01-30 | 2019-05-21 | 陕西科技大学 | A kind of sodium-ion battery cathode SnO2The preparation method of/carbon cloth composite material |
| CN109972160A (en) * | 2019-04-23 | 2019-07-05 | 重庆文理学院 | A kind of preparation method of novel double-function catalyzing electrolysis water electrode |
| CN110302794A (en) * | 2019-06-19 | 2019-10-08 | 西安交通大学 | A kind of NiAlV ternary metal hydroxide nano chip arrays composite material and preparation method based on flexible carbon substrate |
| CN111128562A (en) * | 2020-01-07 | 2020-05-08 | 广东电网有限责任公司电力科学研究院 | Activated carbon fiber paper and preparation method and application thereof |
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