CN110589804B - Method for preparing in-line carbon nanotube film - Google Patents
Method for preparing in-line carbon nanotube film Download PDFInfo
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- CN110589804B CN110589804B CN201910831548.3A CN201910831548A CN110589804B CN 110589804 B CN110589804 B CN 110589804B CN 201910831548 A CN201910831548 A CN 201910831548A CN 110589804 B CN110589804 B CN 110589804B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/18—Processes for applying liquids or other fluent materials performed by dipping
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
Abstract
The invention discloses a method for preparing a carbon nano tube film by a pulling method, which comprises the following steps: injecting the carbon nanotube solution into a container; immersing the substrate in the carbon nanotube solution; injecting a first solution incompatible with the carbon nanotube solution along the substrate or the sidewall of the container; and lifting the substrate to form the carbon nanotube film parallel to the interface of the two liquid layers on the substrate. The method has the advantages that the liquid level is easy to control, the solution can be repeatedly utilized, and the problem of volatilization pollution is avoided.
Description
Technical Field
The invention relates to the field of carbon nanotubes, in particular to a method for preparing an in-line carbon nanotube film.
Background
Carbon nanotubes are a novel carbon material discovered by Iijima of NEC corporation of japan in 1991 and can be classified into single-walled carbon nanotubes and multi-walled carbon nanotubes. The special structure of the carbon nanotube determines the special properties of the carbon nanotube, such as high tensile strength and high thermal stability; the carbon nanotubes may exhibit metallic or semiconducting properties, etc., according to the change in the helical form of the carbon nanotubes. Because the carbon nano tube has an ideal one-dimensional structure and excellent properties in the fields of mechanics, electricity, thermal engineering and the like, the carbon nano tube has a wide application prospect in the fields of interdisciplines such as material science, chemistry, physics and the like, and is more and more concerned in scientific research and industrial application, but the carbon nano tube prepared under the general condition is granular or powdery, which causes great inconvenience to the application of people.
At present, Caoqing et al in the prior art use an LS method to prepare a carbon nanotube membrane, which is extruded back and forth at a certain speed by a push-pull plate; then, the carbon tube array on the solution is transferred to the substrate in parallel by the Langmuir-Schaefer method. Hongsik Park et al use trenching to allow carbon tubes to enter the trenches. Arnold et al, university of wisconsin, usa, uses the principle of evaporation to prepare a strip-shaped carbon tube. However, the preparation method in the prior art still has various defects, the carbon nanotube film prepared by the method of Caoqing et al has large-area nonuniformity, and the carbon nanotube film is multi-layer and has bad influence on the electrical performance (transistor).
The method of Hongsik Park or Arnold et al is disadvantageous in that the carbon nanotube obtained by the method is not a continuous film but a strip shape, and is not suitable for industrial large-area processing; and the minimum size of the groove in the method of Arnold et al can only be made to 70nm, which has great limitation. Therefore, there is a need for an apparatus and method suitable for large-area production of carbon nanotube thin films.
Disclosure of Invention
The invention aims to provide a device and a method for preparing an in-line carbon nanotube film, which have the advantages of simple structure, low cost, suitability for large-area preparation and capability of effectively avoiding the problem of non-uniform thickness of the carbon nanotube film.
The invention provides a method for preparing a carbon nano tube film by adopting a pulling method, which mainly comprises the following steps:
s1, injecting the carbon nanotube solution into a container;
s2, clamping a substrate on a drawing machine, and vertically immersing the substrate in the carbon nano tube solution;
s3, injecting sealing liquid which is not dissolved with the carbon nano tube solution along the side wall of the substrate or the container;
and S4, pulling the substrate, and forming the carbon nano tube film parallel to the interface of the two liquid layers on the substrate.
Preferably, the carbon nanotube solution is formed by dissolving carbon nanotubes in one or more halogenated hydrocarbons, and organic solvents such as chloroform, dichloroethane, trichloroethane, chlorobenzene, dichlorobenzene, bromobenzene and the like are preferred.
Preferably, the carbon nanotubes are selected from one or more of single-walled carbon nanotubes, double-walled carbon nanotubes or multi-walled carbon nanotubes.
Preferably, the speed of said pulling or said inserting is between 0.1 and 20 microns/second.
Preferably, the sealing liquid is one or more of polyalcohol, amine solution or water.
Preferably, the substrate is glass, metal or plastic.
Preferably, the method comprises the step of cleaning the film, wherein the cleaning solution is ethanol, isopropanol, acetone, toluene, xylene and tetrahydrofuran.
In another aspect of the present invention, the carbon nanotube solution and a filling medium may be injected into the container in the step S1, wherein the filling medium includes a liquid or a solid substance, and the liquid is selected from solvents having a relatively high density and immiscible with the carbon nanotube solution, such as dichloroacetic acid, tetrafluoropropanol, heavy liquid, and the like, or a mixture thereof. The solid substance is selected from molecular sieve, polytetrafluoroethylene ball and glass ball filler. The filling medium is mixed into the carbon nanotube solution, so that the using amount of the carbon nanotube solution is greatly reduced, the great cost advantage is achieved, and meanwhile, the change caused by the fact that the substrate is soaked in the solution for a long time can be avoided.
In addition, another aspect of the present invention provides a method for preparing a carbon nanotube film by using a specific solution formulation in combination with a pulling method, in step S1, injecting a carbon nanotube solution into a container, and adding a substance that interacts with carbon nanotubes; then dispersing for 5min by adopting a water area ultrasonic or probe ultrasonic mode; the substance forming interaction with the carbon nano tube is polyalcohol or mercaptan, and preferably 1-70% of 3-methyl-propylene glycol.
The carbon nanotube film prepared by the technical scheme of the invention has the advantages that the film forming speed can be realized by controlling the moving speed of the substrate, and the control is very easy; in addition, the carbon nanotube solution does not need to be discharged or evaporated, so that the carbon nanotube solution does not have loss and pollution, can be recycled, and can greatly reduce the cost.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent by describing embodiments thereof with reference to the accompanying drawings in which:
FIG. 1 shows a flow chart of a process for preparing a carbon nanotube film according to the present invention;
FIG. 2 is a schematic diagram showing the structure of an apparatus for manufacturing a carbon nanotube film according to embodiment 1 of the present invention;
FIG. 3 is a schematic diagram showing a carbon nanotube film formation apparatus according to embodiment 3 of the present invention;
FIG. 4 is a diagram showing the structure of an apparatus for manufacturing a carbon nanotube film according to example 4 of the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings and examples.
Example 1
Fig. 1 is a flow chart showing a process for manufacturing a carbon nanotube film according to a first embodiment of the present invention. The following describes an embodiment of the present invention in detail according to the flow chart shown in fig. 1 and the structure diagram of the apparatus for manufacturing the carbon nanotube film shown in fig. 2.
As shown in fig. 1 and 2, according to step S1, a carbon nanotube solution 13 is first prepared, and carbon nanotubes are dissolved in one or more halogenated hydrocarbons, preferably organic solvents such as chloroform, dichloroethane, trichloroethane, chlorobenzene, dichlorobenzene, bromobenzene, etc. Wherein the carbon nanotubes are selected from single-walled carbon nanotubes, double-walled carbon nanotubes or multi-walled carbon nanotubes, and of course, two or more of them can be selected without affecting the quality of the film layer. Therefore, the method is convenient to select the carbon nano tube, does not need special treatment and is convenient for industrialized production. The halogenated hydrocarbon is preferably chloroform, dichloroethane, trichloroethane, chlorobenzene, dichlorobenzene or bromobenzene. The above halogenated hydrocarbon is used, and the carbon nanotube has better solubility. The prepared carbon nanotube solution 13 is then injected into the container 11.
A substrate 12 is then clamped to the drawing machine and vertically immersed in the carbon nanotube solution 13 according to step S2. The substrate 12 may be glass, metal, or plastic. It may be flexible or rigid in shape, which is selected primarily based on the shape and properties of the film. The substrate is a base for forming the carbon nanotube thin film, and the shape thereof may be set according to a desired film shape, and may be a rectangle, a square, a circle, or other patterns or shapes, which is not limited herein.
The substrate 12 may be placed after the carbon nanotube solution is injected into the container, or before the carbon nanotube solution is injected into the container, and the placing order has no influence on the carbon nanotube film formation. When the substrate 12 enters the carbon nanotube solution 13, it is not necessary to enter the substrate completely, and the substrate may be selected according to the size of the film. In the light of cost saving, it is preferable that the substrate is immersed in the carbon nanotube solution 13 as much as possible, but since the upper end of the substrate needs to hold the substrate moving mechanism, it is further preferable that this portion is exposed to the outside of the carbon nanotube solution.
According to step S3, a sealing liquid 14 immiscible with the carbon nanotube solution 13 is injected along the substrate 12 or the sidewall of the container 11. The sealing liquid 14 may be one or more of a polyol, an amine solution, or water, which are all immiscible with the carbon nanotube solution 13. By such an option, an immiscible double liquid surface interface can be formed in the container 11. Because the carbon nanotube solution 13 and the sealing liquid 14 are immiscible with each other, and intermolecular forces including hydrogen bonds/van der waals forces/other non-covalent bonds and covalent bonds or ionic bond forces are provided between the two, a double liquid layer is formed on a contact surface, the carbon nanotubes in the solution are firstly adsorbed on the interface of the double liquid layer, the position of the interface of the double liquid layer on the substrate is changed along with the change of the position of the substrate, and the carbon nanotubes on the interface are arranged on the substrate in a row, so that the carbon nanotube film is formed. In addition, the temperature of the carbon nanotube film during the preparation process is from the freezing point of the liquid to the boiling point of the carbon nanotube solution, and the freezing point refers to the freezing point temperature with the higher freezing point in both the sealing liquid 14 and the carbon nanotube solution 13.
Then, according to step S4, the substrate 12 is pulled up by a puller, and a carbon nanotube film parallel to the interface of the two liquid layers is formed on the substrate 12. In order to ensure the quality of the film layer, the pulling speed is kept at a constant speed, and the phenomenon that the film layer quality is poor due to the change of the thickness and the uniformity of the film layer caused by sudden speed change is avoided. In addition, the pulling speed is too high, and the coating quality is poor; if the pulling speed is too slow, the production efficiency is low, the cost is high, and the industrial popularization is not met. The pull rate is preferably between 0.1 and 20 microns/second.
After the pulling is finished, a cleaning step can be further included. The film can be directly cleaned without additional operations such as stripping, wherein the cleaning solution can be selected from organic solvents such as ethanol, isopropanol, toluene, xylene, tetrahydrofuran, N-dimethylformamide and the like.
Example 2
In the present embodiment, the preparation of the carbon nanotube solution 13 is completed first, and the carbon nanotube solution 13 is injected into the container 11, wherein the formula of the carbon nanotube solution is the same as that in embodiment 1. Then, according to step S2, a sealing liquid 14 immiscible with the carbon nanotube solution 13 is injected onto the carbon nanotube solution 13 along the sidewall of the container 11, wherein the sealing liquid 14 may be one or more of a polyol, an amine solution or water.
Then, a substrate 12 is inserted into the container at a certain speed and immersed into the carbon nanotube solution, a carbon nanotube film perpendicular to the interface of the two liquid layers is formed on the substrate 12, and the carbon nanotubes in the lower liquid are adsorbed to the interface of the upper liquid and the lower liquid and then are adsorbed to the substrate in a transverse direction.
When the method is used for preparing the carbon nanotube film, the carbon nanotube solution 13 and the sealing liquid 14 are firstly added into the container and then inserted into the substrate 12. And changing the height change of the contact part of the substrate and the interface of the two liquid layers by utilizing downward movement to realize the formation of the carbon nanotube film layer, wherein the insertion speed is preferably between 0.1 and 20 microns/second.
After the substrate is inserted into the substrate to complete the preparation of the carbon nanotube film, the substrate is integrally pulled out, and the subsequent cleaning step is carried out, wherein the cleaning solution can also be selected from organic solvents such as ethanol, isopropanol, toluene, xylene, tetrahydrofuran or N, N-dimethylformamide and the like.
Example 3
As shown in fig. 3, in this embodiment, a carbon nanotube solution 13 is first prepared, and then the carbon nanotube solution 13 and a filling medium 15 are injected into a container 11 together, wherein the formulation of the carbon nanotube solution is the same as that in embodiment 1, the filling medium 15 comprises a liquid or a solid substance, the liquid may be selected from solvents having a relatively high density and being immiscible with the carbon nanotube solution 13, such as dichloroacetic acid, tetrafluoropropanol, heavy liquid, or a mixture thereof, and the solid substance may be selected from molecular sieves, polytetrafluoroethylene spheres, glass sphere fillers, and the like.
Then, a substrate 12 is clamped on a drawing machine and vertically immersed in the carbon nanotube solution 3 according to step S2, and then a sealing liquid 14 immiscible with the carbon nanotube solution is injected along the substrate or the sidewall of the container according to step S3. The kind of the sealing liquid 14 is the same as that in example 1. The substrate 12 is pulled by a pulling machine, and a carbon nanotube film parallel to the interface of the two liquid layers is formed on the substrate 12. Wherein the pulling rate is preferably between 0.1 and 20 μm/sec.
After the pulling is finished, a cleaning step can be further included. The film can be directly cleaned without additional operations such as stripping. Specifically, the cleaning solution may be selected from organic solvents such as ethanol, isopropanol, toluene, xylene, tetrahydrofuran, or N, N-dimethylformamide.
In the embodiment, the filling medium is added into the carbon nanotube solution, so that the using amount of the carbon nanotube solution is greatly reduced, the great cost advantage is achieved, and meanwhile, the change caused by the fact that the substrate is soaked in the solution for a long time can be avoided.
Example 4
As shown in fig. 4, in this embodiment, the carbon nanotube solution 13 is first prepared, the components are selected as in embodiment 1, and then a substance that interacts with the carbon nanotube-dispersant complex is added to the carbon nanotube solution, wherein the substance that interacts with the carbon nanotube-dispersant complex is a polyol or a thiol, preferably 1% -70% 3-methyl-propanediol. Then dispersing for 5min by adopting a water area ultrasonic or probe ultrasonic mode to form a carbon nano tube solution 16 with a dispersing agent.
A substrate 12 is then clamped to a drawing machine and vertically immersed in the carbon nanotube solution with dispersant 16, and a sealing liquid 14 incompatible with the carbon nanotube solution is injected along the substrate or the sidewall of the container. The kind of the sealing liquid 14 is the same as that in example 1. The substrate 12 is pulled by a puller, wherein the pulling rate is preferably between 0.1 and 20 microns/second.
After the pulling is finished, a cleaning step can be further included. The film can be directly cleaned without additional operations such as stripping. Specifically, the cleaning solution may be selected from organic solvents such as ethanol, isopropanol, toluene, xylene, tetrahydrofuran, or N, N-dimethylformamide.
The carbon nanotube film prepared by the method can realize the control of the film coating speed by controlling the movement speed of the substrate, can prepare the carbon nanotube array film fully paved on the whole substrate, and has the advantages of repeated utilization of the solution, no volatile pollution problem and the like.
Although the invention has been described in detail hereinabove with respect to specific embodiments thereof, it will be apparent to those skilled in the art that modifications and improvements can be made thereto without departing from the scope of the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (12)
1. A method of making an in-line carbon nanotube film, comprising:
s1, injecting the carbon nano tube solution with the dispersant into a container, adding polyalcohol or mercaptan which forms interaction with the carbon nano tube-dispersant compound, and then dispersing the carbon nano tube solution with the dispersant by adopting a water area ultrasonic or probe ultrasonic mode;
s2, clamping a substrate on a drawing machine, and vertically immersing the substrate in the carbon nano tube solution;
s3, injecting one or more of polyalcohol, amine solution or water which are not soluble with the carbon nano tube solution along the substrate or the side wall of the container;
and S4, pulling the substrate at a speed of 0.1-20 microns/second to form an in-line carbon nanotube film parallel to the interface of the two liquid layers on the substrate.
2. The method of claim 1, wherein the carbon nanotube solution is formed by dissolving carbon nanotubes in one or more halogenated hydrocarbons.
3. The method of claim 2, wherein the halogenated hydrocarbon is selected from chloroform, dichloroethane, trichloroethane, chlorobenzene, dichlorobenzene, bromobenzene.
4. The method of claim 2, wherein the carbon nanotubes are selected from one or more of single-walled carbon nanotubes, double-walled carbon nanotubes, or multi-walled carbon nanotubes.
5. The method of making an aligned carbon nanotube film according to claim 1, further comprising the step of washing said film.
6. The method of claim 5, wherein the cleaning solution is one of ethanol, isopropanol, acetone, toluene, xylene, or tetrahydrofuran.
7. The method for preparing an in-line carbon nanotube film according to any one of claims 1 to 6, wherein the step S1 is performed by injecting a carbon nanotube solution and a filling medium into the container.
8. The method of claim 7, wherein the fill medium comprises a liquid or solid substance.
9. The method of making an in-line carbon nanotube film of claim 8, wherein said liquid is selected from dichloroacetic acid or tetrafluoropropanol.
10. The method of claim 8, wherein the solid material is selected from one of molecular sieve, polytetrafluoroethylene spheres, or glass sphere packing.
11. The method of claim 1, wherein the carbon nanotube solution with the dispersant is dispersed for 5min by water ultrasound or probe ultrasound.
12. The method of claim 1, wherein the polyol is 1% to 70% 3-methyl-propylene glycol.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910831548.3A CN110589804B (en) | 2019-09-04 | 2019-09-04 | Method for preparing in-line carbon nanotube film |
| PCT/CN2020/113382 WO2021043236A1 (en) | 2019-09-04 | 2020-09-04 | Apparatus and method for manufacturing high-density in-line carbon nanotube thin film |
| PCT/CN2020/113380 WO2021043235A1 (en) | 2019-09-04 | 2020-09-04 | Method for manufacturing high-density in-line carbon nanotube thin film |
| US17/640,224 US20220314265A1 (en) | 2019-09-04 | 2020-09-04 | Apparatus and method for manufacturing high-density in-line carbon nanotube thin film |
| US17/640,219 US20220332584A1 (en) | 2019-09-04 | 2020-09-04 | Method for manufacturing high-density in-line carbon nanotube thin film |
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| CN201910831548.3A CN110589804B (en) | 2019-09-04 | 2019-09-04 | Method for preparing in-line carbon nanotube film |
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| US20220332584A1 (en) * | 2019-09-04 | 2022-10-20 | Beijing Hua Tan Yuan Xin Electronics Technology Co., Ltd | Method for manufacturing high-density in-line carbon nanotube thin film |
| CN111056526B (en) * | 2019-12-30 | 2024-05-03 | 中国科学院空间应用工程与技术中心 | Method for preparing semiconductor carbon nano tube array film |
| CN112201754B (en) * | 2020-02-18 | 2022-08-19 | 天津大学 | Ultrathin crystalline continuous organic semiconductor film and preparation method and application thereof |
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| CN1922106A (en) * | 2004-02-16 | 2007-02-28 | 独立行政法人科学技术振兴机构 | Carbon nanotube structure-selective separation and surface fixation |
| CN104334494A (en) * | 2012-04-26 | 2015-02-04 | 布鲁尔科技公司 | Multifunctional alcohol dispersions of carbon nanotubes |
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| CN100591412C (en) * | 2006-12-27 | 2010-02-24 | 清华大学 | Method for preparing nano film |
| CN106477548A (en) * | 2016-09-18 | 2017-03-08 | 北京华碳元芯电子科技有限责任公司 | A kind of preparation method of carbon nano-tube film |
| CN109534317B (en) * | 2017-09-21 | 2021-11-23 | 中国科学院物理研究所 | Preparation method of carbon nanotube film |
| CN109081329B (en) * | 2018-09-29 | 2020-03-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method and system for separating carbon nano tube from polymer |
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| CN1922106A (en) * | 2004-02-16 | 2007-02-28 | 独立行政法人科学技术振兴机构 | Carbon nanotube structure-selective separation and surface fixation |
| CN104334494A (en) * | 2012-04-26 | 2015-02-04 | 布鲁尔科技公司 | Multifunctional alcohol dispersions of carbon nanotubes |
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| Title |
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| Assembly of aligned semiconducting carbon nanotubes in organic solvents via introducing inter-tube electrostatic repulsion;Bing Gao et al.;《Carbon》;20190130;第146卷;第173-174页"2.实验" * |
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