KR102024892B1 - Carbon nanotube fiber composite and the producing thereof - Google Patents
Carbon nanotube fiber composite and the producing thereof Download PDFInfo
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- KR102024892B1 KR102024892B1 KR1020150174097A KR20150174097A KR102024892B1 KR 102024892 B1 KR102024892 B1 KR 102024892B1 KR 1020150174097 A KR1020150174097 A KR 1020150174097A KR 20150174097 A KR20150174097 A KR 20150174097A KR 102024892 B1 KR102024892 B1 KR 102024892B1
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- D—TEXTILES; PAPER
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- 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
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- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
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- 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
- D06M17/00—Producing multi-layer textile fabrics
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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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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/06—Load-responsive characteristics
- D10B2401/063—Load-responsive characteristics high strength
Abstract
The present invention relates to a carbon nanotube fiber composite and a method for manufacturing the same, and more particularly, in order to produce a high-density carbon nanotube fiber without using a strong acid and an oxidizing agent, two polymers are multi-layered on the carbon nanotube fiber The present invention relates to a carbon nanotube fiber composite and a method for manufacturing the same, which form a laminated coating layer, and allow the coating layer to penetrate into the fiber and achieve chemical bonding between the coating layers to achieve high density and high strength of the carbon nanotubes.
Description
The present invention relates to a carbon nanotube fiber composite material and a method for manufacturing the same, in which two kinds of polymers are laminated on carbon nanotube fibers to realize high density and high strength of carbon nanotubes.
Carbon nanotubes are tiny molecules that are 1 nm in diameter, with long, long carbons connected by hexagonal rings. Specifically, a honeycomb carbon plane in which three carbon atoms are bonded to each other is rolled to form a tube-shaped carbon crystal having a diameter of 0.5 to 10 nm, and has high tensile strength and electrical conductivity, and is drawing attention as a next-generation advanced material.
Carbon nanotubes can be utilized in various types of materials. Particularly, when agglomerated carbon nanotubes are processed into a fiber form, super-strength fibers that are not broken, highly durable fibers that resist heat and friction, and nanofibers having excellent electrical conductivity and thermal conductivity can be manufactured. It is thought to be endless. Even today, carbon nanotube fibers are used in high-tech precision industries, including semiconductors and displays, in the form of antistatic fibers and low-hardness high-capacitance fibers, which significantly increase their productivity.
These carbon nanotube fibers are subjected to further processing to have appropriate strength and physical properties before commercialization. In particular, in the case of using the direct spinning (direct spinning method), which is one of the conventional manufacturing methods in the production of carbon nanotube fibers, there is an advantage that a large amount of carbon nanotube fibers can be produced compared to other methods, but long and stable It is common to be used after modification through manufacture, such as to form a coating layer, because it is difficult to produce the fiber in the form.
There have been steady studies and attempts on the production of modified carbon nanotube fibers, and one of the conventionally used methods is to introduce a functional group on the surface of carbon nanotube fibers using a strong acid, and then Try chemical bonds. However, the above method can improve the strength of the carbon nanotube fibers, but by using a strong acid or oxidizing agent to form defects on the surface of the fiber during the treatment process from which the characteristics of the carbon nanotube fibers inherent There is a disadvantage to reduce. In addition, the reaction time is long, and high temperature conditions for reflux of the strong acid are indispensable, and after the reaction, there is an inconvenience such as having a problem of treating the used strong acid.
Therefore, there is a need for an improved proposal for a manufacturing method capable of imparting excellent strength to carbon nanotube fibers without the use of strong acids and oxidants.
The inventors of the present invention, in order to solve the above-mentioned conventional problems, as a result of stacking the meta (acrylic acid) polymer and polyvinyl alcohol layers sequentially from the surface of the carbon nanotube fibers, but chemically bonding them The prepared carbon nanotube fiber composite, and from this it was confirmed that the production of carbon nanotube fibers of high density and high strength without using a strong acid and an oxidizing agent was completed the present invention.
It is therefore an object of the present invention to provide a stable, high density and high strength carbon nanotube fiber composite.
It is still another object of the present invention to provide a method for producing a carbon nanotube fiber composite having improved process efficiency and convenience without using strong acid and oxidizing agent.
The present invention to achieve the above object,
Carbon nanotube fibers;
(Meth) acrylic acid polymer layer formed on the fiber; And
And a polyvinyl alcohol layer formed on the (meth) acrylic acid polymer layer.
The (meth) acrylic acid-based polymer layer and the polyvinyl alcohol layer provides an ester-bonded carbon nanotube fiber composite.
In addition, the present invention,
(a) forming a (meth) acrylic acid polymer layer on the surface of the carbon nanotube fibers;
(b) forming a polyvinyl alcohol layer on the (meth) acrylic acid polymer layer; And
(c) performing the two layer esterification reactions;
Provided is a method for producing a carbon nanotube fiber composite.
Through the above problem solving means, the carbon nanotube fiber composite of the present invention is integrated at a high density to have a stable and high strength.
In addition, according to the manufacturing method of the carbon nanotube fiber composite of the present invention, it is possible to modify without the problem of causing defects on the surface of the carbon nanotube fibers without using a strong acid and an oxidizing agent, high temperature conditions for reflux during the process This is not necessary, and the reaction time is also significantly reduced, and the cumbersome treatment of the used strong acid treatment is not accompanied, thereby improving the efficiency and convenience of the overall process.
1 is a cross-sectional view of the carbon nanotube fiber composite of the present invention.
Figure 2 is a photograph of a microscope (Scanning Electron Microscopem, 20um standard) of the surface of the carbon nanotube fiber bundle having no coating layer.
Figure 3 is a microscope (Scanning Electron Microscopem, 20um standard) observation photo of the surface of the carbon nanotube fiber bundle having a coating layer according to the present invention.
4 is a photograph of a microscope (Scanning Electron Microscopem, based on 500nm) observation of the surface of the carbon nanotube fiber bundle having no coating layer.
5 is a photograph of a microscope (Scanning Electron Microscopem, based on 500nm) observation of the surface of the carbon nanotube fiber bundle having a coating layer according to the present invention.
The present invention proposes a carbon nanotube fiber composite having excellent strength and a manufacturing method capable of producing the same without using a strong acid and an oxidizing agent. Specifically, in the carbon nanotube fiber composite of the present invention, two kinds of polymers are sequentially stacked on individual strand surfaces of carbon nanotube fibers densely packed in bundles, and chemical bonds are formed between the polymer layers to form a coating layer. . From this, the fiber bundle made of carbon nanotube fibers in the form of a composite including a coating layer realizes high density and high strength.
To clearly define the terminology used herein, the term 'carbon nanotube composite' refers to carbon nanotube fibers having a coating layer.
In addition, the term 'bundle of carbon nanotube fibers (or carbon nanotube fiber composites)' as used herein is a term that is distinguished from the carbon nanotube composite material. Several strands of carbon nanotube fibers are concentrated to form a single fiber unit. It means doing. Typically, when the carbon nanotube fibers are utilized, several strands of fibers are concentrated in bundles and used as one fiber unit having a specific diameter.
Hereinafter, the content of the present invention will be described in more detail. However, the following contents are described only for the most representative embodiments in order to help the understanding of the present invention, and the scope of the present invention is not limited thereto, and the present invention should be understood to cover all ranges equivalent to the following contents.
Carbon Nanotube Fiber Composites
Carbon nanotube fiber composite of the present invention will be described in detail with reference to FIG.
1 is a cross-sectional view in the longitudinal direction showing the structure of a carbon nanotube fiber composite according to the present invention.
1, the carbon nanotube fiber
Referring to the configuration of the carbon nanotube fiber
The
The (meth) acrylic acid polymer constituting the (meth) acrylic
It is preferable that the thickness of the said (meth) acrylic-
The polyvinyl alcohol layer (5) is a compound containing a hydroxyl group (-OH) for the esterification reaction, it is easily dissolved in water and easy to use.
The
The (meth) acrylic
Specifically, the ester bond is formed from esterification of the carboxy group in the (meth) acrylic acid polymer and the hydroxyl group in the polyvinyl alcohol.
For the sake of understanding, as an example of the esterification reaction, the structure of the copolymer produced by the polymerization of polymethacrylic acid and polyvinyl alcohol is represented by the following Chemical Formula 1 (indicated by an ester bond).
Carbon nanotube
<Method for producing carbon nanotube fiber composite material>
Meanwhile, the carbon nanotube composite described above
(a) forming a (meth) acrylic acid polymer layer on the surface of the carbon nanotube fibers;
(b) forming a polyvinyl alcohol layer on the (meth) acrylic acid polymer layer; And
(c) performing the two layer esterification reactions;
It can be prepared through a method for producing a carbon nanotube fiber composite.
At this time, as the carbon nanotube fiber of the step (a) of the manufacturing method of the present invention, it is most preferable to use the one prepared by direct spinning (direct spinning, direct spinning method). Direct spinning is one of the dry methods for producing carbon nanotube fibers, in which carbon nanotubes are synthesized in a heating furnace by injecting a liquid carbon source and a catalyst together with a carrier gas into the upper inlet of a vertical heating furnace. And it refers to a method that can be obtained by winding the carbon nanotube aggregate that is lowered to the bottom of the furnace with a carrier gas (wind-up) inside or outside the furnace.
Hereinafter, the above manufacturing method will be described in detail for each step.
The step (a) is to form a (meth) acrylic
The monomer may be at least one selected from the group consisting of acrylic acid and methacrylic acid.
The coating solution including the monomer may further include a co-monomer for copolymerization with the monomer.
On the other hand, since the monomer included in the coating solution is polymerized in the form of polymer, such as poly (meth) acrylic acid to participate in the next esterification reaction, the monomer is used together with the initiator for polymerization.
The initiator may use thermal initiator and / or photoinitiator depending on the polymerization method, preferably potassium persulfate (KPS), benzoyl peroxide (BPO), benzoin (Benzoin, BN), benzoin methyl ether (BME), 2,2-dimethoxy-2-phenylacetone (2,2-dimethoxy-2-phenylacetophenone) at least one selected from the group consisting of Can be used.
The monomer or polymer described above may form a coating solution in a form diluted in a conventional organic solvent or the like as necessary.
The method of providing the coating solution in this step may be both spraying or dipping, but preferably by dipping. Since the impregnation time may vary depending on the specific process conditions when the immersion process is performed, the impregnation time is not necessarily limited to any specific range, but may be preferably 30 minutes to 12 hours. This is because a sufficient impregnation effect is less likely to be seen below the time range, and a difference in impregnation effects is not so large that it is uneconomical. In consideration of both the efficiency of the process and the impregnation rate, the impregnation may be preferably performed within about 1 hour.
After the
It is preferable to make the said heating into the temperature range of 20-100 degreeC. Below the above temperature range, the even coating effect of the (meth) acrylic acid-based polymer on the carbon nanotube fibers and the polymerization reaction in the case of containing the monomer are less likely to occur, and above the above range, the thermal decomposition or vaporization of the (meth) acrylic acid-based polymer Or other side reactions may occur. Most preferably, this step can be carried out at a temperature of about 50 ℃.
The heating time may vary depending on the specific process conditions, but is not particularly limited. However, when the heating time is too short, the penetration and coating effect of the (meth) acrylic acid polymer into the carbon nanotube fiber bundle and the polymerization rate of the monomer may be It can be degraded and, if too long, a nonsensical process with no difference in effect can be continued and uneconomical. Therefore, preferably 30 minutes to 12 hours, more preferably within about 1 hour as a time for sufficient effect expression and efficient process performance of the present invention.
Next, in the step (b), the
The method of providing the coating solution may be both spraying or dipping, but preferably by dipping.
In the immersion step, the impregnation time may vary depending on the specific process conditions, but is not necessarily limited to any specific range, but may be preferably within about 1 hour. This is because a sufficient impregnation effect is less likely to be seen below the time range, and a difference in impregnation effects is not so large that it is uneconomical.
Next, step (c) includes the (meth) acrylic
Specifically, if the carbon nanotube fiber (1) is impregnated with the polyvinyl alcohol coating solution in step (b) before the heat treatment, it is preferable to remove the excess solvent by removing the carbon nanotube fiber (1) from the coating solution and then heat it. In addition, the excess solvent may be further removed during the heating process. At this time, a vacuum oven or the like can be used as necessary.
The heating temperature for the heat treatment of this step is preferably set to 150 ~ 250 ℃. It is because esterification is less than sufficient in the said temperature range, and when it exceeds, the problem of pyrolysis, vaporization, side reaction, etc. of a (meth) acrylic-acid polymer and / or polyvinyl alcohol may arise. Most preferably, this step can be carried out at a temperature of about 200 ℃.
The heating time may vary depending on the specific process conditions, but is not limited to any particular range. However, if the heating time is too short, the esterification efficiency may be lowered. If the heating time is too long, the meaningless process may be continued and uneconomical. In order to exhibit sufficient effects of the present invention and to perform an efficient process, the heating may be performed in a range of preferably 30 minutes to 12 hours, more preferably 6 hours.
The method for producing the carbon nanotube
The carbon nanotube fiber composite prepared as described above may have high density and high strength, and may be applied to various fields of clothing, semiconductors, displays, and sensors in the form of super strong fibers, high durability fibers, conductive fibers, and the like.
Hereinafter, the preparation examples, examples and experimental examples are presented to help the understanding of the present invention. However, the following contents are only examples of configurations and effects of the present invention, and the scope and effects of the present invention are not limited thereto.
< Production Example >- direct Spinning Preparation of Carbon Nanotube Fibers Using
A spinning solution in which 4.0% by weight of thiophene was mixed with 96.0% by weight of acetone and hydrogen as a carrier gas were prepared. 10 ml / hr of the spinning solution, 2 L / min of carrier gas, and ferrocene, a catalyst precursor, were sublimed at 80 ° C. and heated together with a carrier gas to a temperature of 1,200 ° C. at a rate of 0.015 L / min. Flowed to the top. Thereafter, the carbon nanotube fibers discharged to the outlet of the reactor bottom were recovered by winding with a winding means composed of bobbins.
< Example >-Two layers Polymer Introduction
1.Polymethacrylic Acid Impregnation and Polymer Polymerization
2.5 g of polymethacrylic acid was mixed with 7.5 g of distilled water to prepare a coating solution, and the carbon nanotube fibers prepared above were impregnated for 1 hour.
After sufficient impregnation, the carbon nanotube fibers were removed from the coating solution to remove excess coating solution, and then heated at 75 ° C. for 2 hours to form a polymethacrylic acid coating layer.
2. Polyvinyl Alcohol Impregnation and Esterification Reaction
The carbon nanotube fibers having the polymethacrylic acid coating layer prepared above were impregnated into an aqueous solution in which polyvinyl alcohol was dissolved at 5% as a coating solution.
After impregnating for 1 hour, the excess polyvinyl alcohol coating solution was removed, and then heated at 200 ° C. for 1 hour to perform an esterification reaction to prepare a carbon nanotube fiber composite.
< Experimental Example 1>-Surface Observation of Carbon Nanotube Fiber Bundles
The surface of the carbon nanotube fiber bundles prepared according to Preparation Example and Example 1 was compared by using a scanning electron microscope (SEM). Two observations were performed, the first observation was performed at 20unm and the second observation was performed at 50 nm.
Based on 20 μm, the observation results of the carbon nanotube fibers prepared according to the preparation example are shown in FIG. 2, and the observation results of the carbon nanotube fiber composites prepared according to Example 1 are shown in FIG. 3. .
As a result of the observation, as shown in FIG. 2, bundles of carbon nanotube fibers having no coating layer had a large and distinctly observed gap between fiber strands in the bundle, whereas as shown in FIG. It was confirmed that the bundles of carbon nanotube fiber composites having densities are densely composed of little gaps between the fibers in the bundles.
On the other hand, based on 50nm for a more detailed observation, the observation result for the carbon nanotube fiber prepared according to the preparation example to Figure 4, the observation of the carbon nanotube fiber composite prepared according to Example 1 The results are shown in FIG.
As a result of the above observation, as shown in FIG. 4, the bundle of carbon nanotube fibers having no coating layer was sparsely arranged, and the fiber strands constituting it were sparsely arranged, and there was clearly a slip in the bundle. On the other hand, as shown in Figure 5 it can be seen that the carbon nanotube fiber of the composite form having a coating layer according to the present invention constitutes a dense bundle with a thick thickness and little gap between the fiber strands.
< Experimental Example 2>- Carbon Nano Tube IR analysis for composites
In Experimental Example 2, the final structure was confirmed by performing IR analysis on the carbon nanotube fiber composite according to the present invention. IR data is shown in FIG. 6.
Referring to the IR data of FIG. 6, it can be seen that the coating layer formed by ester bonding of the polymethacrylic acid layer and the polyvinyl alcohol layer to the carbon nanotube fiber composite of the present invention is present.
< Experimental Example 3>- Carbon Nano Tube Breaking strength measurement of composite
In Experimental Example 3, the Favimat + Fiber Test device manufactured by Textechno was used to measure the breaking strength of the carbon nanotube fiber composite according to the present invention. The grip distance of the specimen was 20 mm and the grip was held at a speed of 2 mm / min in the tensile direction. The breaking strength was measured until the fracture occurred.
The measurement results of the breaking strength are shown in Table 1 below.
Referring to Table 1, it can be seen that the carbon nanotube fiber composite having the coating layer of the present invention prepared according to the embodiment has an improved strength at about twice the break compared to the case of the preparation example without the coating layer.
10: carbon nanotube fiber composite
1: carbon nanotube fiber
3: (meth) acrylic acid polymer layer
5: polyvinyl alcohol layer
Claims (14)
(b) forming a polyvinyl alcohol layer on the (meth) acrylic acid polymer layer; And
(c) performing the two interlayer esterification reactions;
The (meth) acrylic acid-based polymer layer is formed by coating a coating solution containing a monomer and an initiator or a coating solution containing a poly (meth) acrylic acid on the surface of the carbon nanotube fiber and then performing heat treatment.
The heat treatment is a method of producing a carbon nanotube fiber composite, characterized in that carried out at 20 ~ 80 ℃.
The monomer is a method for producing a carbon nanotube fiber composite, characterized in that it comprises one selected from the group consisting of acrylic acid, methacrylic acid and combinations thereof.
The coating solution comprising the monomer further comprises a co-monomer (co-monomer) for copolymerization with the monomer.
The polyvinyl alcohol layer is a method for producing a carbon nanotube fiber composite, characterized in that formed by coating a coating solution containing polyvinyl alcohol on the (meth) acrylic acid polymer layer.
The esterification reaction is a method of producing a carbon nanotube fiber composite, characterized in that carried out by heat treatment at 150 ~ 250 ℃.
The coating is a method of producing a carbon nanotube fiber composite, characterized in that carried out by a spraying or dipping process.
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JP2004506530A (en) * | 2000-08-24 | 2004-03-04 | ウィリアム・マーシュ・ライス・ユニバーシティ | Polymer wrapped single-walled carbon nanotubes |
JP2008044820A (en) * | 2006-08-17 | 2008-02-28 | Fuji Xerox Co Ltd | Carbon nanotube film, its production method and capacitor using the same |
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