CN110670345B - Preparation method of textured carbon fiber cloth/carbon nanotube composite material - Google Patents
Preparation method of textured carbon fiber cloth/carbon nanotube composite material Download PDFInfo
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- CN110670345B CN110670345B CN201911045225.8A CN201911045225A CN110670345B CN 110670345 B CN110670345 B CN 110670345B CN 201911045225 A CN201911045225 A CN 201911045225A CN 110670345 B CN110670345 B CN 110670345B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/16—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
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Abstract
The invention discloses a preparation method of a textured carbon fiber cloth/carbon nanotube composite material, which takes cotton cloth impregnated with nickel nitrate as a substrate, nickel nitrate as a nickel source and acetonitrile as a carbon source, and controls the morphology of a carbon nanotube by regulating the amount of the nickel nitrate, the chemical vapor deposition time and the flow velocity of nitrogen after carbonization in a nitrogen atmosphere and chemical vapor deposition. The growth of the carbon nano tube not only improves the conductivity and the mechanical property of the textured carbon fiber cloth, but also leaves rich pore channels on the textured carbon fiber cloth in the reduction process of the nickel nitrate, and increases the specific surface area of the electrode, so that the nickel nitrate serving as the electrode of the super capacitor has excellent capacitance characteristics. The mutual interweaving of the carbon nano tubes is beneficial to the transmission of ions, and the wide application of the material in the field of energy storage is widened; in addition, the invention has the advantages of easily available raw materials, low cost and simple process, and can realize large-scale production.
Description
Technical Field
The invention belongs to the technical field of supercapacitors, and particularly relates to a preparation method of a textured carbon fiber cloth/carbon nanotube composite material.
Background
The textured carbon fiber cloth has a hollow structure and can be used as a growth substrate of an electrode material. Or directly applied to the supercapacitor in the form of an electrode. Lei topic group (Journal of Colloid and Interface science.553(2019)705-712) carbonizes cotton cloth as raw material to obtain textured carbon fiber cloth (TC), and then obtains a textured carbon fiber cloth (aTC) electrode with large specific surface area by activating potassium hydroxide to be applied to a super capacitor. Although the textured carbon fiber cloth has good application prospect as a supercapacitor electrode, the conductivity and the lower specific capacity limit the application of the textured carbon fiber cloth.
Carbon Nanotubes (CNTs), also known as buckytubes, are a quantum material with a particular structure (radial dimension is of the order of nanometers, axial dimension is of the order of micrometers, both ends of the tube are substantially sealed). Has excellent electrical conductivity, mechanical property and thermal conductivity. The flexible material is loaded on the flexible material, so that the conductivity, the mechanical property and the electrode loading capacity of the flexible material can be improved, and the performances of the electrode and a device are improved, which is paid attention to people. The Liu subject group (Energy Storage Mater.11(2018)75-82) loads the material on flexible commercial carbon cloth, and an asymmetric super capacitor is assembled by taking the flexible commercial carbon cloth as an electrode. However, the commercial carbon cloth has high cost, complex process and tedious process, and thus the load of the carbon nanotubes on the flexible material and the application of the carbon nanotubes are limited.
Disclosure of Invention
The invention aims to overcome the defects of the two prior arts and provide a method for preparing a textured carbon fiber cloth/carbon nanotube composite material by growing helical carbon nanotubes on the textured carbon fiber cloth.
Aiming at the purposes, the technical scheme adopted by the invention comprises the following steps:
1. ultrasonic cleaning waste cotton fiber fabrics in acetone, ethanol and deionized water in sequence, removing dust, impurities and organic pollutants on the surfaces of the fibers, and drying; the cotton fiber fabric after being cleaned and dried is soaked in nickel nitrate water solution, and then is dried to a wet state without flowing water on the surface, and then is frozen and dried.
2. And heating the freeze-dried cotton fiber fabric to 700-900 ℃ under the protection of nitrogen, and carbonizing at the constant temperature for 60-90 minutes to obtain the porous carbon fiber cloth loaded with nickel particles.
3. And continuously keeping the temperature of 700-900 ℃ for 10-20 min under the nitrogen atmosphere, and introducing acetonitrile through nitrogen in the constant temperature process to grow the carbon nano tubes on the porous carbon fiber cloth in situ to obtain the textured carbon fiber cloth/carbon nano tube composite material.
In the step 1, the concentration of the nickel nitrate in the nickel nitrate aqueous solution is 0.02-0.1 mol/L, and preferably the concentration of the nickel nitrate is 0.05-0.06 mol/L.
In the step 1, preferably, the cotton fiber fabric after being cleaned and dried is soaked in nickel nitrate water solution for 18-24 h, and then dried at 50-80 ℃ until the surface is in a wet state without flowing water.
In the step 2, preferably, the temperature of the cotton fiber fabric after freeze drying is raised to 780-820 ℃ under the protection of nitrogen with the gas flow rate of 20-35 sccm, and the cotton fiber fabric is carbonized at the constant temperature for 60-90 min to obtain the porous carbon fiber fabric loaded with nickel particles.
In the step 2, the temperature rise rate is 5-10 ℃/min.
In the step 3, preferably, the temperature is kept constant at 780-820 ℃ for 12-15 min under the nitrogen atmosphere with the gas flow rate of 10-16 sccm, and acetonitrile is brought in through nitrogen in the constant temperature process, so that the carbon nano tubes grow on the porous carbon fiber cloth in situ.
The invention has the following beneficial effects:
1. the invention takes the waste cotton fiber fabric which is common in nature as the initial raw material, and obtains the textured carbon fiber fabric/carbon nanotube composite material by methods such as carbonization, chemical vapor deposition and the like. The raw material source is rich and cheap; the waste cotton fiber fabric belongs to waste articles, effectively recovers the waste articles, reduces the production cost of the spiral carbon nano tube, and realizes macro preparation.
2. Compared with the prior art, the method for preparing the carbon nano tube has the advantages of low production condition, simple process, short production period, easy control and capability of massively preparing the carbon nano tube with uniform appearance and height. The method realizes carbonization of the cotton fiber cloth in one step based on the cotton fiber cloth and realizes the load of the carbon nano tube on the textured carbon fiber cloth by using a CVD method; and the formation of the catalyst nickel leaves abundant holes on the textured carbon fiber cloth and replaces the high cost of the flexible substrate in the past process.
3. The textured carbon fiber cloth/carbon nanotube composite material prepared by the invention is used as a supercapacitor electrode material, the composite material not only can provide sufficient space for introducing other nano materials, but also the elastic interweaving network of the carbon nanotubes is beneficial to the transmission of electrolyte ions, and the application of the composite material in the field of energy storage is widened.
Drawings
Fig. 1 is a scanning electron micrograph of the textured carbon fiber cloth/carbon nanotube composite obtained in example 1.
Fig. 2 is an X-ray diffraction pattern of the textured carbon fiber cloth/carbon nanotube composite obtained in example 1.
FIG. 3 shows N of the textured carbon fiber cloth/carbon nanotube composite obtained in example 12Adsorption and desorption curves.
Fig. 4 is a cyclic voltammetry curve of the textured carbon fiber cloth/carbon nanotube composite material obtained in example 1 as a supercapacitor electrode at a high scanning speed in a 6.0M KOH aqueous solution.
Fig. 5 is a graph of rate capability of the textured carbon fiber cloth/carbon nanotube composite obtained in example 1.
Fig. 6 is a resistance curve of the textured carbon fiber cloth/carbon nanotube composite material obtained in example 1 under different bending angles.
Fig. 7 is a resistance curve of the textured carbon fiber cloth/carbon nanotube composite material obtained in example 1 during 1000 times of bending.
Fig. 8 is a scanning electron micrograph of the textured carbon fiber cloth/carbon nanotube composite obtained in example 2.
Fig. 9 is a scanning electron micrograph of the textured carbon fiber cloth/carbon nanotube composite obtained in example 3.
Fig. 10 is a scanning electron micrograph of the textured carbon fiber cloth/carbon nanotube composite obtained in example 4.
Detailed Description
The invention will be further explained in more detail below with reference to the drawings and examples, but the scope of protection of the invention is not limited to these examples.
Example 1
1. Ultrasonic cleaning waste cotton fiber fabrics in acetone, ethanol and deionized water in sequence, removing dust, impurities and organic pollutants on the surfaces of the fibers, and drying; the cotton fiber fabric after being washed and dried is soaked in 0.05mol/L nickel nitrate hexahydrate aqueous solution for 24 hours, dried at 60 ℃ after being soaked to be in a wet state with no flowing water on the surface, and then is subjected to freeze drying.
2. And (3) placing the freeze-dried cotton fiber fabric in a tubular furnace, heating to 800 ℃ at the speed of 8 ℃/min under the protection of nitrogen with the gas flow rate of 30sccm, and carbonizing at constant temperature for 60 minutes to obtain the nickel particle-loaded porous carbon fiber cloth.
3. And adjusting the nitrogen flow rate to be 12sccm, continuously keeping the temperature at 800 ℃ for 15min, connecting a flask filled with 150mL of acetonitrile with the air inlet of the tube furnace in the constant temperature process, and introducing the acetonitrile into the tube furnace through flowing nitrogen to grow the carbon nano tube on the porous carbon fiber cloth in situ to obtain the textured carbon fiber cloth/carbon nano tube composite material.
The inventor adopts an X-ray diffractometer, a scanning electron microscope, a physical adsorption instrument and an electrochemical workstation to characterize the textured carbon fiber cloth/carbon nanotube composite material, and the results are shown in the figures 1-3. As can be seen from FIG. 1, the textured carbon fiber has a hollow structure, and the prepared spiral carbon nanotube with uniform morphology and height has a diameter less than 100nm and a high spiral degree. The comparison between the textured carbon fiber cloth/carbon nanotube composite material (TC/CNTs) and the textured carbon fiber cloth (TC) by the X-ray diffraction of fig. 2 shows that the graphitization degree of the textured carbon fiber cloth substrate is significantly increased by the combination with the carbon nanotubes. As can be seen from FIG. 3, the specific surface area of the obtained textured carbon fiber cloth/carbon nanotube composite material is 295m by the BET physical adsorption test2In terms of/g, total pore volume of 0.28cm3/g。
The inventor further tests the electrochemical performance and mechanics of the textured carbon fiber cloth/carbon nanotube composite material, and the results are shown in fig. 4-7. As can be seen from fig. 4 and 5, the cyclic voltammetry curve of the textured carbon fiber cloth/carbon nanotube composite material still shows a good rectangular shape even at a high scanning speed, and the increase of the scanning speed and the current has a linear relationship, which indicates that the composite material has higher conductivity and good capacitance retention rate. As can be seen from fig. 6 and 7, the electrical conductivity of the composite material remained intact regardless of the bending angle or the bending times, indicating that the composite material has good flexibility.
Example 2
1. Ultrasonic cleaning waste cotton fiber fabrics in acetone, ethanol and deionized water in sequence, removing dust, impurities and organic pollutants on the surfaces of the fibers, and drying; the washed and dried cotton fiber fabric was dipped in 0.1mol/L nickel nitrate hexahydrate aqueous solution for 24 hours, dried at 60 ℃ after dipping to a wet state with just no running moisture on the surface, and freeze-dried.
2. And (3) placing the freeze-dried cotton fiber fabric in a tubular furnace, heating to 800 ℃ at the speed of 8 ℃/min under the protection of nitrogen with the gas flow rate of 30sccm, and carbonizing for 90 minutes at constant temperature to obtain the porous carbon fiber cloth loaded with nickel particles.
3. Adjusting the nitrogen flow rate to 15sccm, continuously keeping the temperature at 800 ℃ for 15min, connecting a flask containing 150mL of acetonitrile with an air inlet of a tube furnace in the constant temperature process, and introducing the acetonitrile into the tube furnace through flowing nitrogen to grow the carbon nanotube on the porous carbon fiber cloth in situ to obtain the textured carbon fiber cloth/carbon nanotube composite material (see fig. 8).
Example 3
1. Ultrasonic cleaning waste cotton fiber fabrics in acetone, ethanol and deionized water in sequence, removing dust, impurities and organic pollutants on the surfaces of the fibers, and drying; the washed and dried cotton fiber fabric was dipped in 0.02mol/L nickel nitrate hexahydrate aqueous solution for 24 hours, dried at 60 ℃ after dipping to a wet state with just no running moisture on the surface, and freeze-dried.
2. And (3) placing the freeze-dried cotton fiber fabric in a tubular furnace, heating to 800 ℃ at the speed of 8 ℃/min under the protection of nitrogen with the gas flow rate of 30sccm, and carbonizing at constant temperature for 60 minutes to obtain the nickel particle-loaded porous carbon fiber cloth.
3. Adjusting the nitrogen flow rate to be 12sccm, continuously keeping the temperature at 800 ℃ for 10min, connecting a flask filled with 150mL of acetonitrile with an air inlet of a tube furnace in the constant temperature process, and bringing the acetonitrile into the tube furnace through flowing nitrogen to grow the carbon nano tube on the porous carbon fiber cloth in situ to obtain the textured carbon fiber cloth/carbon nano tube composite material (see figure 9).
Example 4
1. Ultrasonic cleaning waste cotton fiber fabrics in acetone, ethanol and deionized water in sequence, removing dust, impurities and organic pollutants on the surfaces of the fibers, and drying; the cotton fiber fabric after being washed and dried is soaked in 0.05mol/L nickel nitrate hexahydrate aqueous solution for 24 hours, dried at 60 ℃ after being soaked to be in a wet state with no flowing water on the surface, and then is subjected to freeze drying.
2. And (3) placing the freeze-dried cotton fiber fabric in a tubular furnace, heating to 800 ℃ at the speed of 8 ℃/min under the protection of nitrogen with the gas flow rate of 30sccm, and carbonizing at constant temperature for 75 minutes to obtain the nickel particle-loaded porous carbon fiber cloth.
3. Adjusting the nitrogen flow rate to 16sccm, continuously keeping the temperature at 800 ℃ for 20min, connecting a flask containing 150mL of acetonitrile with an air inlet of a tube furnace in the constant temperature process, and introducing the acetonitrile into the tube furnace through flowing nitrogen to grow the carbon nanotube on the porous carbon fiber cloth in situ to obtain the textured carbon fiber cloth/carbon nanotube composite material (see fig. 10).
Claims (8)
1. A preparation method of a textured carbon fiber cloth/carbon nanotube composite material is characterized by comprising the following steps:
(1) ultrasonic cleaning waste cotton fiber fabrics in acetone, ethanol and deionized water in sequence, removing dust, impurities and organic pollutants on the surfaces of the fibers, and drying; soaking the cleaned and dried cotton fiber fabric in nickel nitrate water solution, drying the soaked cotton fiber fabric until the surface of the cotton fiber fabric is in a wet state without flowing water, and freeze-drying the cotton fiber fabric;
(2) heating the freeze-dried cotton fiber fabric to 700-900 ℃ under the protection of nitrogen, and carbonizing at the constant temperature for 60-90 minutes to obtain porous carbon fiber cloth loaded with nickel particles;
(3) and continuously keeping the temperature of 700-900 ℃ for 10-20 min under the nitrogen atmosphere, and introducing acetonitrile through nitrogen in the constant temperature process to grow the carbon nano tubes on the porous carbon fiber cloth in situ to obtain the textured carbon fiber cloth/carbon nano tube composite material.
2. The method for preparing the textured carbon fiber cloth/carbon nanotube composite material according to claim 1, wherein the method comprises the following steps: in the step (1), the concentration of the nickel nitrate in the nickel nitrate aqueous solution is 0.02-0.1 mol/L.
3. The method for preparing the textured carbon fiber cloth/carbon nanotube composite material according to claim 2, wherein the method comprises the following steps: in the step (1), the concentration of the nickel nitrate in the nickel nitrate aqueous solution is 0.05-0.06 mol/L.
4. The method for preparing the textured carbon fiber cloth/carbon nanotube composite material according to claim 2 or 3, wherein: in the step (1), the cleaned and dried cotton fiber fabric is soaked in a nickel nitrate water solution for 18-24 hours.
5. The method for preparing the textured carbon fiber cloth/carbon nanotube composite material according to claim 1, wherein the method comprises the following steps: in the step (1), drying at 50-80 ℃ after impregnation until the surface is in a wet state without flowing water.
6. The method for preparing the textured carbon fiber cloth/carbon nanotube composite material according to claim 1, wherein the method comprises the following steps: in the step (2), the temperature of the cotton fiber fabric after freeze drying is raised to 780-820 ℃ under the protection of nitrogen with the air flow rate of 20-35 sccm, and the cotton fiber fabric is carbonized at the constant temperature for 60-90 min to obtain the porous carbon fiber fabric loaded with nickel particles.
7. The method for preparing the textured carbon fiber cloth/carbon nanotube composite material according to claim 1 or 6, wherein: in the step (2), the temperature rise rate is 5-10 ℃/min.
8. The method for preparing the textured carbon fiber cloth/carbon nanotube composite material according to claim 6, wherein: and (3) continuously keeping the temperature of 780-820 ℃ for 12-15 min in a nitrogen atmosphere with the gas speed of 10-16 sccm, and introducing nitrogen into acetonitrile in the constant temperature process to grow the carbon nano tubes on the porous carbon fiber cloth in situ.
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| CN108091497A (en) * | 2017-12-06 | 2018-05-29 | 中国科学院上海技术物理研究所 | A kind of preparation method of multidimensional structure carbon fiber flexible electrode |
| CN108264034A (en) * | 2018-02-06 | 2018-07-10 | 陕西师范大学 | The method of growth spiral shape carbon nanotube on the porous carbon of timber |
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| CN108091497A (en) * | 2017-12-06 | 2018-05-29 | 中国科学院上海技术物理研究所 | A kind of preparation method of multidimensional structure carbon fiber flexible electrode |
| CN108264034A (en) * | 2018-02-06 | 2018-07-10 | 陕西师范大学 | The method of growth spiral shape carbon nanotube on the porous carbon of timber |
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Effective date of registration: 20230330 Address after: 710062 No. 199 South Changan Road, Shaanxi, Xi'an Patentee after: Shaanxi Normal University Patentee after: SHAANXI COAL AND CHEMICAL TECHNOLOGY INSTITUTE Co.,Ltd. Address before: 710062 No. 199 South Changan Road, Shaanxi, Xi'an Patentee before: Shaanxi Normal University |