CN108385450B - Carbon nanotube paper and preparation method thereof - Google Patents
Carbon nanotube paper and preparation method thereof Download PDFInfo
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- CN108385450B CN108385450B CN201810062419.8A CN201810062419A CN108385450B CN 108385450 B CN108385450 B CN 108385450B CN 201810062419 A CN201810062419 A CN 201810062419A CN 108385450 B CN108385450 B CN 108385450B
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21J—FIBREBOARD; MANUFACTURE OF ARTICLES FROM CELLULOSIC FIBROUS SUSPENSIONS OR FROM PAPIER-MACHE
- D21J7/00—Manufacture of hollow articles from fibre suspensions or papier-mâché by deposition of fibres in or on a wire-net mould
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
- D21H13/02—Synthetic cellulose fibres
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
Abstract
The invention belongs to the technical field of carbon nano materials, and particularly relates to carbon nano tube paper which comprises carbon nano tubes and chemical fibers. The invention also relates to a preparation method of the carbon nanotube paper, which comprises the following steps: placing a carbon nano tube in an alcohol solvent for ultrasonic dispersion; placing chemical fibers in an alcohol solvent for high-speed dispersion; step two, mixing the chemical fiber dispersion liquid and the carbon nano tube dispersion liquid to obtain a uniform mixed liquid; step three, the uniform mixed solution is placed in a corresponding filtering device for filtering, and carbon nano tube wet paper with uniform thickness is formed on a filter membrane; putting the carbon nano tube wet paper and the filter membrane into an oven for baking; and step five, stripping the dried carbon nanotube paper from the filter membrane, and rolling by adopting a rolling machine. The carbon nanotube paper and the preparation method thereof have the advantages of low cost, few working procedures, high purity and convenient transfer, and are suitable for large-scale production.
Description
Technical Field
The invention belongs to the technical field of carbon nano materials, and particularly relates to carbon nano tube paper and a preparation method thereof.
Background
The carbon nanotube, also known as Baseband tube, is a one-dimensional quantum material with special structure (radial dimension is nanometer magnitude, axial dimension is micrometer magnitude, both ends of the tube are basically sealed), and mainly comprises carbon atoms arranged in hexagon to form coaxial circular tubes with several to tens of layers. The carbon nano tube has an extremely high length-diameter ratio structure, good conductivity, excellent mechanical property and large specific surface area. Carbon nanotubes can be regarded as being formed by winding graphene sheets, and thus can be classified into single-walled carbon nanotubes and multi-walled carbon nanotubes according to the number of graphene sheets. The commonly used methods for preparing carbon nanotubes mainly include arc discharge, laser ablation, chemical vapor deposition (pyrolysis of hydrocarbon gas), solid phase pyrolysis, glow discharge, gas combustion, and polymerization synthesis.
The carbon nanotube paper (bucky paper) is composed of disordered carbon nanotubes with a certain length, has the specific surface area far larger than that of carbon fiber paper, the strength close to that of a heat-conducting graphite sheet, good electric and thermal conductivity and chemical stability, and has great application value in the fields of fuel cell gas diffusion layers, electrochemical super capacitors, lithium ion battery cathodes, heat dissipation pads of high-power electronic devices, high-performance polymer composite materials and the like.
Due to the nanometer size and the special long-diameter structure of the carbon nano tube, the dispersion is very difficult. And the traditional carbon nanotube paper has fluffy structure and poor mechanical property. According to the above disadvantages, many carbon paper manufacturing methods are made, for example, as described in chinese patent publication No. 106396680a, carbon tubes and a dispersant are mixed in a solvent, subjected to ultrasonic dispersion treatment, added with paper pulp, subjected to high-speed shear dispersion and mixing, formed by a common paper making process, subjected to high-temperature modification treatment, subjected to carbonization treatment, and finally subjected to roll forming; also like chinese patent publication No. 102877367a, the carbon tube is first mixed with a dispersant, stirred and dispersed, then short fibers are added, high-speed shear dispersion is performed, then a tape-casting papermaking process is used for molding, and finally the dispersant is taken out after post-treatment to obtain a target product; such a large number of steps increases the cost, and the dispersant easily affects the conductivity of the carbon nanotubes, thereby reducing the performance of the carbon nanotube paper.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the carbon nanotube paper and the preparation method thereof, which have the advantages of low cost, less working procedures, high purity, convenient transfer and suitability for large-scale production.
The invention is realized by the following steps:
the invention provides carbon nanotube paper, which comprises carbon nanotubes and chemical fibers.
Further, the mass ratio of the carbon nanotubes to the chemical fibers in the carbon nanotube paper is (90-99.9): (0.1-10).
The invention also provides a preparation method of the carbon nanotube paper, which comprises the following steps:
step one, dispersing: placing the carbon nano tube in an alcohol solvent for ultrasonic dispersion to obtain a carbon nano tube dispersion liquid; placing chemical fibers in an alcohol solvent for high-speed dispersion to obtain a chemical fiber dispersion liquid;
step two, mixing: mixing the chemical fiber dispersion liquid with the carbon nano tube dispersion liquid, and stirring at a high speed to obtain a uniform mixed liquid;
step three, filtering: filtering the mixed solution prepared in the step two in a corresponding filtering device to form carbon nano tube wet paper with uniform thickness on a filter membrane;
step four, baking: putting the carbon nano tube wet paper and the filter membrane into an oven for baking, and removing the solvent;
step five, tabletting: and stripping the dried carbon nanotube paper from the filter membrane, and rolling the dried carbon nanotube paper by using a rolling machine to obtain a target product.
Further, the ratio of the mass (mg) of the carbon nano-tubes to the volume (mL) of the alcohol solvent in the first step is 0.01mg/mL-0.5 mg/mL; the power of ultrasonic dispersion is 30W-600W, and the time of ultrasonic dispersion is 0.1h-5 h.
Further, the ratio of the mass (mg) of the chemical fiber to the volume (mL) of the alcohol solvent in the first step is 0.1mg/mL-1 mg/mL; the rotating speed of the high-speed dispersion is 1000-.
Further, the rotation speed of the high-speed stirring in the second step is 500-10000 rpm; in the mixed solution, the mass ratio of the carbon nano tubes to the chemical fibers is (90-99.9): (0.1-10).
Further, the filtering mode in the third step can be vacuum filtration or filter pressing; the pumping speed of the vacuum pump for vacuum filtration is 0.1L/s-20.0L/s; the pressure of the filter pressing is 0.3-3 MPa.
Further, the filter membrane in the third step is any one of a polyethylene filter membrane, a polypropylene filter membrane, a polytetrafluoroethylene filter membrane and a nylon filter membrane, and the aperture of the filter membrane is 0.05-50 μm.
Furthermore, the baking temperature in the fourth step is 25-150 ℃, the baking time is 0.1-5 h, and the baking mode is blast baking or vacuum baking.
Further, the compacted density of the carbon nano tube pressed sheet in the fifth step is 0.5-2g/cm3。
The principle of the invention is as follows: the carbon nano tube has better compatibility in an alcohol solvent, and the molecules of the carbon nano tube are integrally dispersed in the solvent under the action of ultrasonic dispersion; high-speed stirring is carried out in advance, chemical fibers are dispersed, and chemical fiber dispersion liquid and carbon nano tube dispersion liquid are mixed and dispersed at high speed, so that the mixed liquid is more uniform; then, in the filtering process, self-assembly effects are formed among the carbon nano-tube molecules and among the chemical fibers, and the binding force is mainly expressed as the cross-linking action between the van der Waals force of the molecules and the long-diameter molecules; in the carbon nanotube paper, the carbon nanotube molecules are mutually entangled through van der Waals force and the crosslinking action between long-diameter molecules, and meanwhile, chemical fibers are staggered together to form a three-dimensional network structure, so that the carbon nanotube paper provides support for the carbon nanotube and improves the flexibility and the bending performance of the carbon nanotube paper.
Compared with the prior art, the invention has the following beneficial effects:
(1) the carbon nanotube paper prepared by the invention comprises carbon nanotubes and chemical fibers; the chemical fiber is made from natural fiber or protein fiber or natural inorganic substance or carbon-containing polymer as raw material by chemical treatment and mechanical processing, and can be classified into artificial fiber (regenerated fiber), synthetic fiber and inorganic fiber. The chemical fiber has strong mechanical property and stable structure, does not damage the structure of the carbon nano tube, and can select the chemical fiber with proper diameter, length and molecular weight according to the requirement; a small amount of chemical fibers can bind the carbon nano tubes, reduce the loss of the carbon nano tubes and enhance the mechanical property of the carbon nano tube paper; meanwhile, the chemical fiber content is low, so that the overall conductivity of the carbon nanotube paper is not influenced; therefore, a small amount of chemical fibers not only ensure good conductivity of the carbon nanotube paper, but also ensure good bending performance of the carbon nanotube paper;
(2) the carbon nanotube paper provided by the invention has few working procedures and simple process in the preparation process; in the preparation process, no additional functional group is introduced, the cleanliness is high, the carbon nanotube paper after filtration can be free from loss, and the solvent can be recycled, so that the production cost is reduced, and powerful conditions are provided for large-scale production;
(3) the carbon nanotube molecules in the carbon nanotube paper provided by the invention are mutually entangled through the van der Waals force and the crosslinking action between long-diameter molecules; meanwhile, the chemical fibers are staggered together to form a three-dimensional net structure, so that the carbon nano tubes are supported, and the flexibility and the bending performance of the carbon nano tube paper are improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a photograph of a carbon nanotube paper provided in accordance with the present invention;
FIG. 2 is an SEM photograph of carbon nanotube paper provided in the present invention;
fig. 3 is a flexible display diagram of the carbon nanotube paper provided in the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention provides carbon nanotube paper, which comprises carbon nanotubes and chemical fibers. The chemical fiber is made from natural fiber or protein fiber or natural inorganic substance or carbon-containing polymer as raw material by chemical treatment and mechanical processing, as shown in fig. 1-2.
Further, the mass ratio of the carbon nanotubes to the chemical fibers in the carbon nanotube paper is (90-99.9): (0.1-10).
The chemical fiber in the embodiment has strong mechanical property and stable structure, the structure of the carbon nano tube cannot be damaged, a small amount of chemical fiber can bind the carbon nano tube, the loss of the carbon nano tube is reduced, and the mechanical property of the carbon nano tube paper is enhanced; meanwhile, the chemical fiber content is low, so that the overall conductivity of the carbon nanotube paper is not influenced; therefore, a small amount of chemical fibers ensures good conductivity of the carbon nanotube paper and also provides good bending properties, as shown in fig. 3.
The invention also provides a preparation method of the carbon nanotube paper, which comprises the following steps:
step one, dispersing: placing the carbon nano tube in an alcohol solvent for ultrasonic dispersion to obtain a carbon nano tube dispersion liquid; placing chemical fibers in an alcohol solvent for high-speed dispersion to obtain a chemical fiber dispersion liquid;
step two, mixing: mixing the chemical fiber dispersion liquid with the carbon nano tube dispersion liquid, and stirring at a high speed to obtain a uniform mixed liquid;
step three, filtering: filtering the mixed solution prepared in the step two in a corresponding filtering device to form carbon nano tube wet paper with uniform thickness on a filter membrane;
step four, baking: putting the carbon nano tube wet paper and the filter membrane into an oven for baking, and removing the solvent;
step five, tabletting: and stripping the dried carbon nanotube paper from the filter membrane, and rolling the dried carbon nanotube paper by using a rolling machine, so that the bulk density of the carbon nanotube paper is improved, the mechanical property of the carbon nanotube paper is enhanced, and the target product is obtained.
In the preparation process of the carbon nanotube paper in the embodiment, the working procedures are few, and the process is simple; in the preparation process, no additional functional group is introduced, the cleanliness is high, the carbon nanotube paper after filtration can be free from loss, and the solvent can be recycled, so that the production cost is reduced, and powerful conditions are provided for large-scale production; in addition, the carbon nano tube molecules are mutually entangled through van der Waals force and the crosslinking action between long-diameter molecules; meanwhile, the chemical fibers are staggered together to form a three-dimensional net structure, so that the carbon nano tubes are supported, and the flexibility and the bending performance of the carbon nano tube paper are improved.
Further, the ratio of the mass (mg) of the carbon nano-tubes to the volume (mL) of the alcohol solvent in the first step is 0.01mg/mL-0.5 mg/mL; the power of ultrasonic dispersion is 30W-600W, and the time of ultrasonic dispersion is 0.1h-5 h.
Further, the ratio of the mass (mg) of the chemical fiber to the volume (mL) of the alcohol solvent in the first step is 0.1mg/mL-1 mg/mL; the rotating speed of the high-speed dispersion is 1000-.
Further, the alcohol solvent is at least one of ethanol, ethylene glycol, isopropanol, and n-butanol.
Further, the chemical fiber is any one of polyethylene fiber, polypropylene fiber and polymethyl methacrylate fiber.
Further, the rotation speed of the high-speed stirring in the step two is 500-10000 rpm; in the mixed solution, the mass ratio of the carbon nano tube to the chemical fiber is (90-99.9): (0.1-10).
Further, the filtering mode in the third step can be vacuum filtration or filter pressing; the pumping speed of the vacuum pump for vacuum filtration is 0.1L/s-20.0L/s; the pressure of filter pressing is 0.3-3 MPa.
Further, the filter membrane in the third step is any one of a polyethylene filter membrane, a polypropylene filter membrane, a polytetrafluoroethylene filter membrane and a nylon filter membrane, and the aperture of the filter membrane is 0.05-50 μm.
Furthermore, the baking temperature in the fourth step is 25-150 ℃, the baking time is 0.1-5 h, and the baking mode is blast baking or vacuum baking.
Further, the compaction density of the carbon nano tube pressed sheet in the fifth step is not more than 0.5-2g/cm3。
Example one
Placing the carbon nanotubes in an isopropanol solvent, wherein the ratio of the mass (mg) of the carbon nanotubes to the volume (mL) of the isopropanol solvent is 0.01mg/mL, dispersing the carbon nanotubes in the isopropanol solvent by using an ultrasonic method, wherein the ultrasonic power is 60W, and the ultrasonic time is 0.5 h; dissolving polyethylene fiber in isopropanol solvent, dispersing at 5000rpm for 1 hr, and making the ratio of chemical fiber mass (mg) to isopropanol solvent volume (mL) be 0.1 mg/mL; wherein the polyethylene fibers have a molecular weight3×104Diameter of 70 nm and length of 350 μm; after the dispersion is finished, mixing the two dispersions, and stirring at a high speed of 5000rpm for 1h to obtain a uniform mixed solution; in the mixed solution, the mass ratio of the carbon nano tubes to the polyethylene fibers is 98: 2; transferring the uniform mixed solution into a filtering device, and carrying out vacuum filtration, wherein the air suction rate of a vacuum pump is 1L/s, and the filter membrane is a polyethylene filter membrane; after the filtration, putting the filter membrane and the carbon nano tube wet paper into a forced air drying oven for baking at the baking temperature of 100 ℃ for 1 h; finally transferring the dried carbon nanotube paper from the polyethylene filter membrane, and selectively tabletting to obtain the target carbon nanotube paper, wherein the compacted density of the carbon nanotube paper is 0.5g/cm3。
Example two
Placing the carbon nano tube in an ethanol and ethylene glycol solvent, wherein the volume ratio (mL) of the ethanol to the ethylene glycol is 1:2, the ratio of the mass (mg) of the carbon nano tube to the volume (mL) of the alcohol mixed solvent is 0.5mg/mL, dispersing the carbon nano tube in the alcohol mixed solvent by using an ultrasonic method, wherein the ultrasonic power is 100W, and the ultrasonic time is 0.5 h; dissolving polypropylene fiber in ethanol solvent, dispersing at 6000rpm for 1.5 hr, wherein the ratio of chemical fiber mass (mg) to ethanol solvent volume (mL) is 1mg/mL, and the molecular weight of polypropylene fiber is 20 × 104Diameter of 50nm and length of 300 μm; after the dispersion is finished, mixing the two dispersions, and stirring at 8000rpm for 0.5h to obtain a uniform mixed solution; in the mixed solution, the mass ratio of the carbon nano tube to the polypropylene fiber is 99.5: 0.5; transferring the uniform mixed solution into a filtering device, and performing filter pressing under the pressure of 2MPa, wherein the filter membrane is a polytetrafluoroethylene filter membrane; after filter pressing is finished, putting the filter membrane and the carbon nano tube wet paper into a forced air drying oven for baking, wherein the baking temperature is 80 ℃, and the baking time is 0.5 h; finally transferring the dried carbon nanotube paper from the polytetrafluoroethylene filter membrane, and selectively tabletting to obtain the target carbon nanotube paper, wherein the compacted density of the carbon nanotube paper is 2g/cm3。
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A preparation method of carbon nanotube paper is characterized by comprising the following steps: the carbon nanotube paper comprises carbon nanotubes and polypropylene fibers; the mass ratio of the carbon nanotubes to the polypropylene fibers in the carbon nanotube paper is 99.5: 0.5; the polypropylene fiber has a molecular weight of 20 x 104Diameter of 50nm and length of 300 μm; the preparation method of the carbon nanotube paper comprises the following steps:
step one, dispersing: placing the carbon nano tube in an alcohol solvent for ultrasonic dispersion to obtain a carbon nano tube dispersion liquid; placing polypropylene fibers in an alcohol solvent for high-speed dispersion to obtain polypropylene fiber dispersion liquid;
step two, mixing: mixing the polypropylene fiber dispersion liquid with the carbon nano tube dispersion liquid, and stirring at a high speed to obtain a uniform mixed liquid;
step three, filtering: filtering the mixed solution prepared in the step two in a corresponding filtering device to form carbon nano tube wet paper with uniform thickness on a filter membrane;
step four, baking: putting the carbon nano tube wet paper and the filter membrane into an oven for baking, and removing the solvent;
step five, tabletting: stripping the dried carbon nanotube paper from the filter membrane, and rolling the dried carbon nanotube paper by using a rolling machine to obtain a target product;
the filter membrane in the third step is any one of a polyethylene filter membrane, a polypropylene filter membrane, a polytetrafluoroethylene filter membrane and a nylon filter membrane, and the aperture of the filter membrane is 0.05-50 mu m.
2. The method for producing a carbon nanotube paper according to claim 1, characterized in that: the ratio of the mass of the carbon nano tube to the volume of the alcohol solvent in the first step is 0.01mg/mL-0.5 mg/mL; the power of ultrasonic dispersion is 30W-600W, and the time of ultrasonic dispersion is 0.1h-5 h.
3. The method for producing a carbon nanotube paper according to claim 1, characterized in that: the ratio of the mass of the polypropylene fiber to the volume of the alcohol solvent in the first step is 0.1mg/mL-1 mg/mL; the rotating speed of the high-speed dispersion is 1000-.
4. The method for producing a carbon nanotube paper according to claim 1, characterized in that: the rotation speed of the high-speed stirring in the step two is 500-10000 rpm.
5. The method for producing a carbon nanotube paper according to claim 1, characterized in that: the filtering mode in the third step is vacuum filtration or filter pressing; the pumping speed of the vacuum pump for vacuum filtration is 0.1L/s-20.0L/s; the pressure of the filter pressing is 0.3-3 MPa.
6. The method for producing a carbon nanotube paper according to claim 1, characterized in that: the baking temperature in the fourth step is 25-150 ℃, the baking time is 0.1-5 h, and the baking mode is blast baking or vacuum baking.
7. The method for producing a carbon nanotube paper according to claim 1, characterized in that: the compacted density of the carbon nano tube paper in the step five is 0.5-2g/cm3。
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| CN108749194A (en) * | 2018-08-30 | 2018-11-06 | 天津工业大学 | A kind of electromagnetic shielding sandwich laminated film and preparation method thereof |
| CN109167093A (en) * | 2018-09-03 | 2019-01-08 | 江西克莱威纳米碳材料有限公司 | A kind of hydroxylating whisker carbon nanotube paper and preparation method thereof and a kind of lithium-sulfur cell |
| CN109371742B (en) * | 2018-11-02 | 2021-05-14 | 杭州特种纸业有限公司 | Cup packing paper and preparation method thereof |
| CN109834960A (en) * | 2019-02-15 | 2019-06-04 | 柔电（武汉）科技有限公司 | A kind of carbon nano-tube film and preparation method thereof |
| CN111778779A (en) * | 2020-07-06 | 2020-10-16 | 上海安崎智能科技有限公司 | Whisker carbon nanotube far infrared paper and preparation method thereof |
| CN113073496B (en) * | 2020-09-17 | 2022-07-29 | 江汉大学 | Method for preparing conductive fiber paper with hydrophilic-hydrophobic lithium gradient structure and conductive fiber paper |
| CN112176772A (en) * | 2020-09-25 | 2021-01-05 | 柔电（武汉）科技有限公司 | Preparation method of lithium-philic carbon nanotube paper and preparation method of composite metal lithium cathode |
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