KR101990610B1 - Appratus for yarning carbon nanotubes - Google Patents
Appratus for yarning carbon nanotubes Download PDFInfo
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- KR101990610B1 KR101990610B1 KR1020150171172A KR20150171172A KR101990610B1 KR 101990610 B1 KR101990610 B1 KR 101990610B1 KR 1020150171172 A KR1020150171172 A KR 1020150171172A KR 20150171172 A KR20150171172 A KR 20150171172A KR 101990610 B1 KR101990610 B1 KR 101990610B1
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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
- D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
- D01F9/133—Apparatus therefor
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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
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
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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 present invention relates to a carbon nanotube fiberizing apparatus for producing carbon nanotube fibers, which comprises a reaction chamber for synthesizing carbon nanotubes, a heater for applying heat to the reaction chamber, and an outlet for discharging the synthesized carbon nanotube, And a fibrous nozzle whose diameter gradually decreases from the reaction chamber to the outlet. The carbon nanotube fiberizing apparatus of the present invention produces a high-density carbon nanotube fiber having high strength.
Description
BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a carbon nanotube fiberizing device, and more particularly, to a carbon nanotube fiberizing device for producing carbon nanotube fibers having high strength by passing a synthesized carbon nanotube through a fiberizing device whose diameter gradually decreases .
Carbon nanotubes (carbon nanotubes) is a kind of carbon isotopes, carbon atoms are combined into a hexagonal honeycomb shape. Carbon nanotubes have excellent electrical conductivity and thermal conductivity, and have high mechanical strength and high mechanical properties based on the graphite crystal structure. The excellent electrical, thermal and mechanical properties of carbon nanotubes are attributed to the SP 2 bond of carbon, stronger than iron, lighter than aluminum, and have electrical conductivity similar to that of metals.
However, carbon nanotubes remain chemically very stable due to strong covalent bonding between carbon atoms. However, the use of pure carbon nanotubes is short in length and difficult to be dispersed in an organic solvent due to van der Waals force, Is very limited. Therefore, studies have been made to overcome the inherent problems of pure carbon nanotubes by preparing carbon nanotubes in a fiber form.
The method of manufacturing carbon nanotube fibers can be roughly divided into a dry method and a wet method. Coagulation spinning, in which carbon nanotubes are fiberized by injecting a dispersion solution containing carbon nanotubes and a dispersant into a polymer solution, And liquid-crystalline spinning in which a carbon nanotube solution forms a liquid crystal under specific conditions. The physical properties of carbon nanotubes are inferior to the coagulation spinning method, and the liquid crystal spinning method is evaluated as being very slow in spinning speed and in a liquid crystal forming condition.
Meanwhile, Direct Spinning proposed by Professor Winle of the University of Cambridge is a method for producing carbon nanotube fiberization, which can continuously produce carbon nanotube fibers. However, carbon nanotube fibers, which are aggregates of thousands to tens of thousands of carbon nanotubes, are not much different from the theoretical properties of carbon nanotubes. This is because weak shear characteristics and interfacial bonding between carbon nanotubes composed of fibrous aggregates are not good.
To address this problem, recent research trends for carbon nanotube fiberization focus on improving strength through post-treatment of fibers. The post-treatment method of carbon nanotube fibers can be largely a physical or chemical method. The physical method is to enhance the physical properties by increasing the density by bundling carbon nanotubes in a bundle shape. The chemical method is a method in which functional properties Thereby improving the interfacial bonding force. The physical method is problematic because a slip is generated between the carbon nanotube fibers. In the case of the above-mentioned chemical method, the carbon nanotube fibers are concentrated only on the outer surface of the carbon nanotube fibers produced after spinning, and the inner portion of the carbon nanotube fibers is not highly concentrated, so that it is difficult to expect high strength.
The following Non-Patent Document 1 discloses that the synthesized carbon nanotube fibers are squeezed by using a roller under a constant pressure. However, as in Non-Patent Document 1, when a roller is used to press the carbon nanotube fibers, the gap between the carbon nanotube fibers may be reduced and the carbon nanotube fibers may be highly dense. However, And there are many restrictions on application to various fields.
The present inventors have conducted various studies to solve the above problems. As a result, they have found that a cone-shaped fibrous nozzle whose diameter gradually decreases from a reaction chamber for synthesizing carbon nanotubes to an outlet through which carbon nanotubes are discharged is called carbon It has been confirmed that carbon nanotube fibers with high strength can be manufactured by mounting the nanotube fibers in a nanotube fiberizing apparatus.
Accordingly, it is an object of the present invention to provide a carbon nanotube fiberizing device for producing carbon nanotube fibers of high strength by highly compacting carbon nanotube fibers so that no gap is formed between carbon nanotube fibers.
In order to achieve the above object,
A reaction chamber for synthesizing carbon nanotubes;
A heater for applying heat to the reaction chamber; And
And a fibrous nozzle having a discharge port through which the synthesized carbon nanotube is discharged and whose diameter gradually decreases from the reaction chamber to the discharge port.
Wherein the fibrous nozzle is connected to the reaction chamber,
The fibrous nozzle has a conical shape, and the curved surface of the fibrous nozzle extending from the reaction chamber to the discharge port may have a straight or curved shape.
The carbon nanotube fibrillation apparatus according to the present invention is equipped with a cone-shaped fibrous nozzle whose diameter gradually decreases from the reaction chamber to the discharge port through which the carbon nanotubes are discharged to produce high-density carbon nanotube fibers with high strength. In addition, fibrosis nozzle is the ratio of the diameter (D 1) to the diameter (D 2) of the discharge opening of the associated boundary, and reaction chamber 7: 1 to 14: By constituting in the range of 1, to minimize the back pressure that may occur in the discharge opening .
1 is an internal schematic diagram of a carbon nanotube fiberizing apparatus according to a first embodiment of the present invention.
2 is an enlarged view of an enlarged view of the fibrous nozzle of the carbon nanotube fiberizing apparatus shown in Fig.
3 is an internal schematic diagram of a carbon nanotube fiberizing apparatus according to a second embodiment of the present invention.
4 is an enlarged view of an enlarged view of the fibrous nozzle of the carbon nanotube fibrousizing apparatus shown in Fig.
5 is an image showing a pressure distribution of a fibrous nozzle (Example 2) having a discharge port diameter of 1 cm.
6 is an image showing the instantaneous speed at which a carbon nanotube moves through a fibrous nozzle (Example 2) having a discharge port diameter of 1 cm.
The present invention is capable of various modifications and various forms, and specific embodiments are illustrated in the drawings and described in detail in the text. It should be understood, however, that the invention is not intended to be limited to the particular forms disclosed, but includes all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
The terms first, second, etc. may be used to describe various components, but the components should not be limited by the terms. The terms are used only for the purpose of distinguishing one component from another. For example, without departing from the scope of the present invention, the first component may be referred to as a second component, and similarly, the second component may also be referred to as a first component.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The singular expressions include plural expressions unless the context clearly dictates otherwise.
Hereinafter, preferred embodiments of the present invention will be described in more detail with reference to the accompanying drawings.
1 is an internal schematic diagram of a carbon nanotube fiberizing apparatus according to a first embodiment of the present invention. Referring to FIG. 1, a carbon nanotube fiberizing
The
The reactant inlet (Y 1 ) contains the reactant from the outside, which comprises a liquid or gaseous carbon compound which is a carbon source. The liquid reactant may be selected from the group consisting of ethanol, methanol, propanol, acetone, xylene, chloroform, ethyl acetic acid, diethyl ether, polyethylene glycol, ethyl formate, mesitylene, tetrahydrofuran (THF), dimethylformamide , Hexane, benzene, carbon tetrachloride, pentane, and mixtures thereof. (C 2 H 5 OH), xylene (C 8 H 10 ), diethyl ether [(C 2 H 5 ) 2 O], polyethylene glycol [(CH 2 -CH 2 -O) 9 ] , 1-propanol (CH 3 CH 2 CH 2 OH ), acetone (CH 3 OCH 3), ethyl formate (CH 3 CH 2 COOH), benzene (C 6 H 6), hexane (C 6 H 14), mesh Tylene [C 6 H 3 (CH 3 ) 3 ], and mixtures thereof. The gaseous reactant includes, but is not limited to, carbon compounds such as ethylene, methane, ethane, propane, butane, acetylene, propylene, butylene, ethyl formate and the like.
The reactive material may further comprise a catalyst. The catalyst includes iron, nickel, cobalt, platinum, ruthenium, molybdenum, vanadium and oxides thereof. Preferably iron, nickel, cobalt or the like, and may be in the form of a metallocene such as ferrocene. The catalyst may have a particle shape, and preferably a nano-sized particle shape. The catalyst may be mixed in an amount of from 0.3 to 15% by weight, or from 1 to 5% by weight, based on the total weight of the reactants. When the catalyst is used in an amount exceeding 15% by weight based on the total weight of the reactants, it is difficult to obtain high-purity carbon nanotubes because the catalyst acts as an impurity. Rather, the thermal, electrical and physical properties of the carbon nanotubes can be impaired. If the catalyst is used in an amount of less than 0.3% by weight based on the total weight of the reactants, the reaction rate may be lowered.
The reactant may further comprise a catalytic activator. Carbon nanotubes are synthesized by diffusion of carbon into the catalyst in the molten state and then precipitating. The catalytic activator is used as a promoter in the synthesis of carbon nanotubes to increase the carbon diffusion rate, . Examples of the catalyst activator is thiophene (Thiophene, C 4 H 4 S ), hydrogen sulfide (H 2 S), sulfur dioxide (SO 2), sulfur trioxide (SO 3), sulfuric acid (H 2 SO 4), dibasic sulfur (S 2 Cl 2), sulfur hexafluoride (SF 6), thionyl chloride (SOCl 2), chloride, sulfuryl (SO 2 Cl 2), sulfurous acid (H 2 SO 3), sodium sulfite (Na 2 SO 3) includes a sulfur compound, such as But is not limited thereto. Thiophene reduces the melting point of the catalyst and removes the amorphous carbon, allowing synthesis of high purity carbon nanotubes at low temperatures. The content of the catalytic activator may also affect the structure of the carbon nanotube. The catalytic activator may be mixed in an amount of 0.5 to 5% by weight based on the total weight of the reactant.
In order to supply the reaction material to the
The transfer gas inlet (Y 2 ) can regulate the amount of reactant introduced into the
The injection rate of the transfer gas injected into the
The
The
The
For example, the
2 is an enlarged view of an enlarged view of the fibrous nozzle of the carbon nanotube fiberizing apparatus shown in Fig. 1 and 2, the
Accordingly, when the
If out of the range be the diameter of D 2 relatively small, it becomes the amount discharged from the
From the center point of the boundary, depending on the correlation of the discharge opening (Y 3) D 1 and D 2 (L) line length to the center point, the relationship, there is the strength of the carbon nanotube to be produced crystals, the L, D 1, and D 2 can be determined by the following equation (1), and the diameter (D 2 ) of the outlet (Y 3 ) may be 0.1 to 1 cm.
[Equation 1]
L = {10 (D 2 ) + D 1 } ± 5
The carbon
The
The heating means (150) increases the temperature of the fibrous nozzle (130). This is to prevent the carbon nanotubes clinging to the
The winding means 160 collects the carbon nanotube fibers discharged from the discharge port Y 3 . The winding means 160 includes, but is not limited to, a bobbin, a drum, a reel, a spindle, and a conveyor.
The
FIG. 3 is an internal schematic view of a carbon nanotube fiberizing device according to a second embodiment of the present invention, and FIG. 4 is an enlarged view of a fibrousizing nozzle of the carbon nanotube fiberizing device shown in FIG.
3 and 4, a carbon
The carbon
The
The
As shown in FIGS. 3 and 4, when the
≪ Fabrication of fibrous nozzle &
But the linear length (L) of the boundary between the diameter (D 1) of the fiberization nozzle connected to the reaction chamber to 7cm, the outlet from the boundary between the center point of fiberization nozzle center point equally made of 20cm, diameter of the discharge opening (D 2) is 100μm, 500 mm, 1 mm, 5 mm, and 1 cm were fabricated, respectively, and mounted on a carbon nanotube fiberizing apparatus.
When a certain pressure in (a flow rate of the feed gas is 1L / min) of carbon nanotubes to be discharged from the discharge port of the fiberization nozzle, the diameter of the discharge port (D 2) in and out of the outlet pressure according to a change difference (△ P) and carbon The nanotube discharge rate (V) was measured using Comsol Multiphysics ® as shown in Table 1 below.
(Examples 1 and 2), the pressure difference (ΔP) between the inside and the outside of the discharge port was set to 5 mm or 1 cm when the diameter of the discharge port was made 5 mm or 1 cm considering the border diameter D 1 of the fibrous nozzle connected to the reaction chamber was 7 cm. It was confirmed that the back pressure was not generated at the outlet when the carbon nanotube fiber was discharged. On the other hand, in the case where the diameter of the discharge port was 100 μm, 500 μm, and 1 mm (Comparative Examples 1 to 3), it was confirmed that the pressure difference ΔP between the inside and the outside of the discharge port was generated and back pressure was generated.
5 is an image showing a pressure distribution of a fibrous nozzle (Example 2) having a discharge port diameter of 1 cm. Referring to FIG. 5, it was confirmed that the pressure at the outlet position of the fibrous nozzle remained the same as the pressure of the entire fibrous nozzle, and no back pressure was generated.
6 is an image showing the instantaneous speed at which the carbon nanotubes move to a fibrous nozzle (Example 2) having a discharge port diameter of 1 cm. Referring to FIG. 6, it can be seen that as the diameter of the fibrous nozzle narrows, the speed at which the carbon nanotubes move increases at the portion where the discharge port is located.
As described above, the carbon nanotube fiberizing apparatus according to the present invention is equipped with a cone-shaped fibrous nozzle whose diameter gradually decreases from the reaction chamber to the discharge port through which the carbon nanotubes are discharged, .
In addition, fibrosis is the ratio of the nozzle diameter (D 1) to the diameter (D 2) of the discharge opening of the associated boundary, and reaction chamber 7: 1 to 14: constituted by one to minimize the back pressure that may occur at the outlet.
100, 200: Carbon nanotube fiberizing device
110, 210:
130, 230:
150, 250: heating means 160, 260: winding means
170, 270: pump
Y1: Reactant inlet
Y2: Transfer gas inlet
Y3: Outlet
Claims (7)
A heater for applying heat to the reaction chamber; And
And a fibrous nozzle having a discharge port through which the synthesized carbon nanotube is discharged and whose diameter gradually decreases from the reaction chamber to the discharge port,
Wherein the fibrous nozzle has a ratio of a diameter D 1 of a boundary portion connected to the reaction chamber to a diameter D 2 of a discharge port of 7: 1 to 14: 1,
When the straight line length from the center point of the boundary where the fibrous nozzle and the reaction chamber are connected to the center point of the outlet is L,
Wherein L, D 1 , and D 2 satisfy the following formula (1).
[Equation 1]
L = {10 (D 2 ) + D 1 } ± 5
Wherein the fibrous nozzle is connected to the reaction chamber,
Wherein the fibrous nozzle has a conical shape and a curved surface of the fibrous nozzle extending from the reaction chamber to the discharge port has a straight or curved cross section.
Wherein the outlet has a diameter of 0.1 to 1 cm.
The carbon nanotube fiberizing apparatus
A fibrous chamber connected to the reaction chamber and containing the fibrous nozzle;
Winding means disposed inside the fibrous chamber for collecting the carbon nanotube fibers; And
And a pump for adjusting an amount of the carbon nanotube fibers discharged to the discharge port.
The carbon nanotube fiberizing apparatus
And a second heating means for applying heat to the fibrous nozzle.
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JP7455805B2 (en) * | 2019-02-22 | 2024-03-26 | 住友電気工業株式会社 | Carbon nanotube production method, carbon nanotube assembly wire production method, carbon nanotube assembly wire bundle production method, carbon nanotube production apparatus, carbon nanotube assembly wire production apparatus, and carbon nanotube assembly wire bundle production apparatus |
CN114540987B (en) * | 2022-03-30 | 2023-04-18 | 江西省纳米技术研究院 | Thin-diameter carbon nanotube fiber, reaction furnace tube thereof, preparation equipment and preparation method |
Citations (3)
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US20040213727A1 (en) * | 2002-12-11 | 2004-10-28 | Schiavon Mauro | Device and method for production of carbon nanotubes, fullerene and their derivatives |
JP2010065339A (en) * | 2008-09-10 | 2010-03-25 | Toray Ind Inc | Method and apparatus for producing carbon nanotube continuous fiber |
JP2013011039A (en) | 2011-06-30 | 2013-01-17 | Toray Ind Inc | Device for producing carbon nanotube continuous fiber and producing method thereof |
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Publication number | Priority date | Publication date | Assignee | Title |
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US20040213727A1 (en) * | 2002-12-11 | 2004-10-28 | Schiavon Mauro | Device and method for production of carbon nanotubes, fullerene and their derivatives |
JP2010065339A (en) * | 2008-09-10 | 2010-03-25 | Toray Ind Inc | Method and apparatus for producing carbon nanotube continuous fiber |
JP2013011039A (en) | 2011-06-30 | 2013-01-17 | Toray Ind Inc | Device for producing carbon nanotube continuous fiber and producing method thereof |
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