KR20160135382A - Apparatus and method for synthesizing carbon nanotube - Google Patents
Apparatus and method for synthesizing carbon nanotube Download PDFInfo
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- KR20160135382A KR20160135382A KR1020150068539A KR20150068539A KR20160135382A KR 20160135382 A KR20160135382 A KR 20160135382A KR 1020150068539 A KR1020150068539 A KR 1020150068539A KR 20150068539 A KR20150068539 A KR 20150068539A KR 20160135382 A KR20160135382 A KR 20160135382A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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- C—CHEMISTRY; METALLURGY
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- C01B2202/00—Structure or properties of carbon nanotubes
Abstract
Description
TECHNICAL FIELD The present invention relates to a carbon nanotube synthesizing apparatus and method for synthesizing carbon nanotubes that maintain excellent crystallinity and a long length in the synthesis of carbon nanotubes.
Conventional methods for synthesizing carbon nanotubes (CNTs) include methods such as an electric discharge method, a laser fusing method, a plasma chemical vapor deposition method, a thermochemical vapor deposition method, and a vapor phase growth method. The gas phase growth method, which is mainly used in the above-mentioned methods, can be generally an electric furnace heating method. In the method of using the electric furnace, catalytic reduction of ferrocene or the like and generation reaction of CNT are generated in a tubular reaction apparatus such as a quartz tube, so that it is possible to produce continuous CNTs. However, this method may be difficult to produce pure single-walled carbon nanotubes (SWCNTs) because it is difficult to maintain the small size and uniform distribution of the catalyst particles due to problems such as the temperature rise.
As another method, in the case of a synthesis method using thermal plasma, it is possible to form a uniform catalyst due to the high temperature of the plasma, but since the reaction time is relatively short and the reaction time is difficult to control, There is a limit to synthesize CNTs having long and excellent crystallinity.
In addition, when the CNT synthesis proceeds through the pretreatment process for the activation of the catalyst, the pretreatment process section and the synthesis and reaction process sections must be separated and managed separately, which is inefficient.
Therefore, the development of an improved device for CNT synthesis is required.
It is an object of the present invention to provide an apparatus for synthesizing carbon nanotubes (CNTs).
It is still another object of the present invention to provide a CNT synthesis method for efficient production by simplifying the CNT synthesis process with the apparatus.
The present invention
A vertical reactor body having a reaction zone;
A reaction material injection unit provided at an upper end of the reaction zone;
A plasma generating means provided at an upper end of the reaction material injecting unit; And
A carbon nanotube outlet provided at a lower end of the reaction zone;
The present invention also provides a carbon nanotube synthesizing apparatus.
According to one embodiment, the reaction material injected into the reaction material injecting unit is heated by the plasma generated from the plasma generating means to form an initial CNT, and the generated initial CNT is allowed to grow while moving downward along the reaction region Lt; / RTI >
According to one embodiment, the plasma torch may be a source of plasma, gas, electricity, electromagnetic waves, high frequency or a combination thereof.
According to one embodiment, it may further comprise heating means for heating the reaction zone.
According to one embodiment, the reaction material injecting part may be provided with a gas injection port, a carbon source, and a catalyst injection port.
According to one embodiment, the gas inlet, the carbon source, and the catalyst inlet may be arranged to face the center of the upper end of the reaction zone, but face each other.
According to another embodiment, the gas injection port, the carbon source, and the catalyst injection port may be arranged so as to face the center of the upper end of the reaction zone, but have different vertical heights.
According to one embodiment, the carbon source and the catalyst may be injected in the form of a catalyst or a catalyst precursor dispersed in a liquid carbon source.
According to another embodiment, the reaction material injecting unit may further include a transfer gas injecting unit.
According to one embodiment, a laminar flow forming unit may be further provided in the lower part of the reactor.
According to one embodiment, the gas may comprise a reducing gas, an inert gas or a combination thereof.
According to one embodiment, the catalyst may comprise iron, nickel, cobalt, copper, yttrium, platinum, ruthenium, molybdenum, vanadium, titanium, zirconium, palladium, silicon or combinations thereof.
According to one embodiment, the carbon source is selected from the group consisting of ethane, ethanol, ethylene, methane, methanol, propane, propene, propanol, acetone, xylene, carbon monoxide, chloroform, ethyl acetic acid, acetylene, diethyl ether, polyethylene glycol, , Mesitylene (1,3,5-trimethylbenzene), tetrahydrofuran, dimethylformamide, dichloromethane, hexane, benzene, carbon tetrachloride, pentane or combinations thereof.
The present invention also provides a CNT synthesis method using the CNT synthesizer, and a CNT fiber synthesis method.
Other details of the embodiments of the present invention are included in the following detailed description.
INDUSTRIAL APPLICABILITY According to the carbon nanotube (CNT) synthesizer and the CNT synthesis method of the present invention, it is possible to provide a CNT having excellent crystallinity and a long length, in particular, a pure single walled carbon nanotube (SWCNT) .
In addition, CNTs having improved physical properties can be produced as described above, so that they can be applied to the synthesis of CNT fibers.
1 is a schematic view of a carbon nanotube synthesizer according to an embodiment of the present invention.
2 is a projection electron microscope (TEM) photograph of a carbon nanotube according to Example 1. Fig.
3 is a graph showing the results of Raman analysis of carbon nanotubes prepared according to Example 1
FIG. 4 is a scanning electron microscope (SEM) photograph of carbon nanotubes according to the length of the reactor according to Example 2. FIG.
BRIEF DESCRIPTION OF THE DRAWINGS The present invention is capable of various modifications and various embodiments, and specific embodiments are illustrated in the drawings and described in detail in the detailed description. It is to be understood, however, that the invention is not to be limited to the specific embodiments, but includes all modifications, equivalents, and alternatives falling within the spirit and scope of the invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.
It is to be understood that when an element is referred to herein as being "connected" or "connected" to another element, it is to be understood that other elements may be directly connected or connected or intervening in the other element .
The singular expressions include plural expressions unless otherwise specified.
The terms "comprises", "having", or "having" mean that there is a feature, a value, a step, an operation, an element, a component or a combination thereof described in the specification, Does not exclude the possibility that a number, a step, an operation, an element, a component, or a combination thereof may be present or added.
The term "carbon nanotube fibers" in the present specification refers to both carbon nanotubes grown in a fiber form or formed by fusing a plurality of carbon nanotubes in a fiber form.
Hereinafter, a carbon nanotube (CNT) synthesizing apparatus and a carbon nanotube synthesizing method according to embodiments of the present invention will be described in detail.
Specifically, the apparatus according to the present invention
A vertical reactor body having a reaction zone (10);
A reaction
A plasma generating means (14) provided at an upper end of the reaction material injecting portion; And
A carbon nanotube outlet (not shown) provided at the lower end of the reaction zone;
The present invention also provides a carbon nanotube synthesizing apparatus.
According to a preferred embodiment of the present invention, heating means (12) for heating the reaction zone may further be provided.
According to a preferred embodiment of the present invention, in order to solve the problems of each CNT synthesizing apparatus using an electric furnace or plasma, a CNT synthesis having a plasma generating section on a reactor having a heating region (for example, an electric furnace) Device is provided.
By providing the plasma and the electric furnace in combination with one CNT synthesizer, CNTs can be continuously produced by the catalyst, and CNTs having excellent crystallinity can be obtained due to the generation of small and uniform catalyst particles. In addition, CNTs having a longer length can be synthesized by complementing the disadvantage that the reaction time of CNT is short in the conventional thermal plasma synthesis method.
More specifically, according to the present invention, the reaction material injected into the reaction
At the beginning of the CNT synthesis reaction, the carbon source is thermally decomposed into hydrogen and carbon components by the
The apparatus according to the present invention can form a catalyst of a smaller size as compared with a fluidized bed reactor in which a reaction material is supplied from the lower end of the reaction zone to the upper end thereof to progress the reaction and consequently carbon nanotubes having a smaller thickness can be manufactured .
As a result, the CNT by the CNT synthesizer according to the present invention may have a diameter of several nanometers to several tens of nanometers and a length of several micrometers to several centimeters. In particular, pure single walled carbon nanotubes (SWCNTs) with improved crystallinity can be synthesized by reaction and growth at high temperatures. This feature is difficult to implement due to the low reaction temperature in the process using a fluidized bed reactor.
On the other hand, the plasma can be divided into a high-temperature plasma and a low-temperature plasma depending on the temperature. The high-temperature plasma includes an arc plasma and a high-temperature glow plasma, and can be used for fusion, melting point, cutting, ion propulsion engine, Glow, corona, flat arc, dusty, gliding plasma, etc., and can be used for chemical process, material synthesis, surface modification, material reduction and decomposition, electronics industry, environmental industry and the like. The low-temperature plasma may be useful for preventing thermal deformation by thermal contact during the process, and may have a characteristic of having a large electron energy compared to heat energy. In addition, a type of plasma has a thermal plasma having a relatively low temperature but a high heat capacity, and a thermal plasma can be generated by the plasma torch.
According to an embodiment of the present invention, the plasma generating unit may be a plasma torch that supplies gas, electricity, electromagnetic waves, high frequency waves, or a combination thereof. Specifically, for example, the plasma torch may include a gas plasma torch, an electric plasma torch, a high frequency plasma torch, a direct current-high frequency hybrid plasma torch, etc., depending on the source.
The structure of the plasma torch may include an electrode, a nozzle, a cap, a cooling water inlet, a gas inlet, and the like. The internal structure of the plasma torch may vary depending on the type of the working gas and the electrode material. For example, the plasma torch may have a tungsten electrode rod, which may be argon, hydrogen, nitrogen, or a combination thereof, and the gas supply system may be an axial flow type. Also, the gas supply system may be a swirl type. Further, gas, cooling water or a combination thereof may be used as the auxiliary fluid, and for example, carbon dioxide gas may be used as the auxiliary gas. The plasma torch may be a water-cooled or air-cooled plasma torch. In the CNT synthesis process, the plasma torch can start the reaction of the carbon source and the catalyst by treating the catalyst with fine particles, and the temperature of the heat generated by the plasma torch may be several thousands to several tens of thousands of degrees centigrade.
According to one embodiment, a reaction
According to another embodiment, the
The reaction
According to one embodiment, the
According to another embodiment, the
According to another embodiment, the
The carbon source and the catalyst inlet may or may not be the same. For example, the carbon source and the catalyst may be mixed and injected through the same injection port, or the carbon source and the catalyst may be injected through different injection ports.
According to one embodiment, the catalyst or catalyst precursor may be injected into the liquid carbon source in a dispersed form.
According to an embodiment, it is possible to further include a transport gas inlet for smooth transport of the CNTs.
In addition, a solvent, a surfactant, etc. may be further injected through the
The
According to one embodiment, the method of injecting the gas, the catalyst, and the carbon source is not particularly limited, and bubbling, ultrasonic jet injection, vaporization injection, spraying spray, pulse introduction using a pump, Different injection methods can be applied to each injection port.
According to one embodiment, the gas may be an inert gas, a reducing gas, or a combination thereof. Examples of the inert gas include argon and nitrogen, and examples of the reducing gas include hydrogen and ammonia. The gas may comprise argon, nitrogen, hydrogen, helium, neon, krypton, chlorine or combinations thereof, and may include, for example, hydrocarbons, carbon monoxide, ammonia, hydrogen sulfide or combinations thereof. The gas reacts with the amorphous carbon or impurities that can be produced in the CNT synthesis process and is discharged together. Thus, the gas can improve the purity of synthesized CNTs and can serve as a carrier for moving the catalyst and CNTs. It can also play a role. For example, the gas may be injected at a linear velocity of 0.5 to 50 cm / min and may vary depending on the kind of the transport gas, the size of the reactor, the type of the catalyst, and the like.
According to one embodiment, the catalyst can be in liquid or gaseous form and can act as a synthesis initiator in CNT synthesis. The catalyst may include, for example, iron, nickel, cobalt, copper, yttrium, platinum, ruthenium, molybdenum, vanadium, titanium, zirconium, palladium, silicon, A sulfide, a sulfide, a nitrate, a mixture, an organic complex, or a combination thereof, and may be included as a catalyst precursor. For example, the catalyst may be a compound such as metallocene collectively referred to as bis (cyclopentadienyl) metal, which is a new organometallic compound in which cyclopentadiene and a transition metal are bonded in a sandwich structure, and the cyclopentadiene is a compound It is possible to perform electrophilic reaction, acylation and alkylation reaction. Examples of the metallocene include ferrocene, cobaltocene, osmosene, and ruthenocene. Among them, ferrocene, which is a compound of iron, is relatively thermally stable compared to most metallocenes and is not decomposed to 470 ° C .
Specific examples ferrocene of the catalyst, of molybdenum hexa-carbonyl, cyclopentadienyl cobalt -dicarbonyl ((C 5 H 5) Co (CO) 2), nickel-dimethyl glyoxime, ferric chloride (FeCl 3), ferrous acetate hydroxide , Iron acetylacetonate or iron pentacarbonyl. When the amount of the catalyst is larger than that of the carbon source, the catalyst may act as an impurity, which may be difficult to obtain CNT of high purity, and may be a factor that hinders the thermal, electrical, and physical properties of the CNT. Can be selected and adjusted. In addition, the catalyst may be supplied in a dissolved state in an organic solvent containing at least one compound such as water, ethanol, methanol, benzene, xylene, toluene and the like.
The catalyst may be, for example, a sulfur-containing compound as an auxiliary catalyst, and specific examples thereof include sulfur-containing aliphatic compounds such as methylthiol, methylethylsulfide, dimethylthioketone and the like; Sulfur-containing aromatic compounds such as phenylthiol, diphenylsulfide and the like; Sulfur-containing heterocyclic compounds such as pyridine, quinoline, benzothiophene, thiophene and the like, preferably thiophene. 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 nanotubes. For example, when 1 to 5% by weight of thiophene is mixed with ethanol, multi-walled carbon nanotube fibers can be obtained. Ethanol A single cobalt carbon nanotube can be obtained by mixing thiophene in an amount of 0.5 wt% or less.
According to one embodiment, the synthesis rate, length, diameter, surface state, etc. of the CNT can be controlled by adjusting the concentration of the catalyst or the catalyst precursor. For example, if the concentration of the injected catalyst is increased, since the number of catalyst particles in the reactor increases, the number of synthesized CNTs can be increased, and thus the diameter of the CNTs can be reduced. On the other hand, when the concentration of the catalyst is decreased, the CNT diameter can be increased because the number of generated CNTs is decreased.
According to one embodiment, the carbon source may be gaseous or liquid and may be, for example, ethane, ethylene, ethanol, methane, methanol, propane, propene, propanol, acetone, xylene, carbon monoxide, chloroform, acetylene, , Diethyl ether, polyethylene glycol, ethyl formate, mesitylene (1,3,5-trimethylbenzene), tetrahydrofuran, dimethylformamide, carbon tetrachloride, naphthalene, anthracene, dichloromethane, ketone, ether, Heptane, octane, pentane, pentene, hexene, benzene, carbon tetrachloride, toluene, or combinations thereof.
According to one embodiment, the carbon source may be overlapped with a gas supply source containing carbon. For example, when the carbon compound contained in the raw material supply source is benzene, examples of the carbon source included in the source gas include benzene, Ethylene, methane, or the like, may be selected by those skilled in the art according to the process conditions.
According to one embodiment, the heating means 12 for heating the
According to one embodiment, the heating means 12 may be provided in a form of wholly or partially enclosing the outside of the reactor body, and the reactor may have heat resistance and pressure resistance. The size of the reactor is not particularly limited and may be appropriately set according to the amount of the introduced source. Specifically, the reactor having the heat resistance and the pressure resistance may be formed of a material including quartz, graphite, stainless steel, aluminum steel, silicon carbide, ceramics, glass, or the like, During the synthesis process, all or part of the reactor may be heated to 1,000 to 3,000 DEG C to sustain the growth of CNTs. The temperature in the reactor can affect the diffusion rate of carbon. The CNT growth rate can be controlled by adjusting the temperature in the reactor. In general, the higher the temperature, the faster the CNT growth rate and the crystallinity and the strength can be increased.
According to an embodiment, the carbon nanotube synthesizing apparatus may further include a gas and a CNT outlet. The outlet may be provided at a lower portion of the CNT synthesizer in a state of being connected to the reactor. CNTs initiated to react and synthesize by the plasma torch are introduced into the reactor, CNTs starting to be synthesized move from the upper part of the reactor to the lower part, and the CNTs can be continuously grown and discharged together with the gas and discharged to the discharge port.
According to one embodiment, the CNT synthesizing apparatus may further include a laminar flow forming unit, and the laminar flow may serve to improve reaction time and CNT characteristics by dispersing the source particles in the reactor. Specifically, the laminar flow forming part that can be formed in the lower part of the reactor can increase the reaction time of the CNT by increasing the time of the catalyst and the CNT staying in the reactor. As a result, CNT fiber production may be possible.
According to the CNT synthesizing apparatus, the pre-processing step of the catalyst, the synthesizing step of the CNT, and the CNT recovering step can be continuously performed in one apparatus. By coupling the CNT synthesizing apparatus to an apparatus other than the above- And can be applied to simplify and apply the CNT synthesis process. For example, in addition to the CNT synthesis apparatus constituent unit, a further process may be performed by combining a transfer device, a post-processing device, a cleaning device, and the like. For example, the CNT synthesizing apparatus may further include a winding means and the like in addition to the constituent elements to easily obtain CNT fibers.
As described above, according to the CNT synthesizing apparatus of the present invention, the synthesis of single-walled carbon nanotubes (SWCNTs) or multi-wall CNTs can be controlled according to the injection rate of gas, carbon source and the rate of injection of catalyst. In addition, the SWCNT can be greatly influenced by the electronic properties due to slight changes in the structure of the diameter or the atomic lattice arrangement. Therefore, the CNT synthesizer can satisfy a reliable method of fabricating structurally uniform SWCNTs.
Hereinafter, embodiments of the present invention will be described in detail so that those skilled in the art can easily carry out the present invention. The present invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Example 1: Manufacture of carbon nanotubes by thermal plasma apparatus
Carbon nanotubes were prepared under the following conditions using a thermal plasma apparatus having a reactor length of 10 cm. The thermal plasma apparatus used a DC thermal plasma torch, and the experiment was conducted under conditions of 25V and 200A at a torch output of 10 kW level. Argon gas is injected through the reaction
Specifically, FIG. 2 shows a photograph of a carbon nanotube synthesized under the conditions of an ethylene flow rate of 500 ml / min and a ferrosin feed rate of 0.002 g / min by a projection type transmission microscope (TEM). As shown in FIG. 2, it can be confirmed that the synthesized carbon nanotubes are synthesized mainly as single-walled carbon nanotubes although the double wall and the triple wall are partially included.
The results of Raman analysis of the synthesized carbon nanotubes are shown in FIG. In general, carbon nanotubes according to the present invention are superior to carbon nanotubes because the D-band peak size is very small compared to the G band size.
Example 2: Synthesis of carbon nanotubes according to change in length of thermal plasma apparatus
Carbon nanotubes were synthesized in the same manner as in Example 1 except that the length of the reactor was changed to 5, 10 and 15 cm. FIG. 4 shows a photograph of the synthesized carbon nanotube observed with a scanning electron microscope. The longer the length of the reactor, the longer the carbon nanotubes are produced.
It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the invention. something to do. It is therefore intended that the scope of the invention be defined by the claims appended hereto and their equivalents.
Claims (15)
A reaction material injection unit provided at an upper end of the reaction zone;
A plasma generating means provided at an upper end of the reaction material injecting unit; And
A carbon nanotube outlet provided at a lower end of the reaction zone;
And the carbon nanotube composite device.
Wherein the reaction raw material injected into the reaction material injecting unit is heated by the plasma generated from the plasma generating means to form an initial CNT and the generated initial CNT is allowed to grow while moving down along the reaction region, Device.
Wherein the plasma generating means comprises a plasma source as a gas, electricity, electromagnetic wave, high frequency or a combination thereof.
And a heating means for heating the reaction region.
Wherein the reaction material injecting part is provided with a gas injection port, a carbon source and a catalyst injection port.
Wherein the gas inlet, the carbon source, and the catalyst inlet are arranged to face the center of the upper end of the reaction zone, facing each other.
Wherein the gas injection port, the carbon source, and the catalyst injection port are disposed so as to face the center of the upper end of the reaction zone and have different vertical heights.
Wherein the carbon source and the catalyst are injected in a form in which a catalyst or a catalyst precursor is dispersed in a liquid carbon source.
Wherein the reaction material injecting unit further comprises a transfer gas injecting unit.
And a laminar flow forming unit disposed under the reactor.
Wherein the gas comprises a reducing gas, an inert gas or a combination thereof.
Wherein the catalyst comprises iron, nickel, cobalt, copper, yttrium, platinum, ruthenium, molybdenum, vanadium, titanium, zirconium, palladium, silicon or a combination thereof.
Wherein the carbon source is selected from the group consisting of ethane, ethanol, ethylene, methane, methanol, propane, propene, propanol, acetone, xylene, carbon monoxide, chloroform, ethyl acetic acid, acetylene, diethyl ether, polyethylene glycol, ethyl formate, Carbon tetrachloride, pentane, or a combination thereof. 2. A carbon nanotube synthesizer as claimed in claim 1, wherein the carbon nanotube composite is a mixture of carbon nanotubes and carbon nanotubes.
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