CN110217777B - Carbon nano tube preparation device and method - Google Patents

Carbon nano tube preparation device and method Download PDF

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CN110217777B
CN110217777B CN201910533219.0A CN201910533219A CN110217777B CN 110217777 B CN110217777 B CN 110217777B CN 201910533219 A CN201910533219 A CN 201910533219A CN 110217777 B CN110217777 B CN 110217777B
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CN110217777A (en
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陈名海
袁鑫鑫
阮超
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Jiangxi Copper Technology Research Institute Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/158Carbon nanotubes
    • C01B32/16Preparation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/158Carbon nanotubes
    • C01B32/16Preparation
    • C01B32/162Preparation characterised by catalysts

Abstract

The invention belongs to the technical field of new materials, and relates to a nano carbon material, in particular to a carbon nano tube preparation device and a method. Simultaneously, carrier gas and carbon source gas are respectively introduced from a catalyst evaporation cavity and a chemical vapor deposition cavity, and the catalyst reacts with the high-temperature cracked organic carbon source to generate carbon nano tubes, and then the carbon nano tubes are separated and collected by a gas-solid separation device. The method can keep the catalyst generated by arc high temperature evaporation to enter a chemical vapor phase growth zone in an ultrafine scale or even an atomic state, has high activity and small scale, and is an effective way for preparing the high crystallinity single-walled carbon nanotube. And the device is simple, can realize continuous preparation, and has great industrialization value.

Description

Carbon nano tube preparation device and method
Technical Field
The invention belongs to the technical field of new materials, relates to a nano carbon material, and in particular relates to a device and a method for preparing a carbon nano tube.
Background
The carbon nano tube is formed by sp 2 The tubular nanomaterial formed by the hybridized carbon-carbon covalent bonds has a series of advantages of light weight, high strength, high heat conductivity, large surface area, stable structure and the like, has been widely paid attention to since the birth of the tubular nanomaterial, leads to hot spots of nanomaterial technology, and has wide application prospects in the fields of structural composite materials, energy sources, catalysis and functional devices.
At present, the preparation method of the carbon nano tube mainly comprises the following steps: chemical vapor deposition, arc ablation, laser, plasma, etc., which are relatively well established process routes, have found industrial application. However, the chemical vapor deposition method has the defect of low crystallization degree of the carbon nano tube due to the inherent low reaction temperature, so that the defect content of the carbon nano tube prepared by the chemical vapor deposition method is high. In particular, when preparing carbon nanotubes with a small diameter and single-walled carbon nanotubes, the surface defects are high, so that the conductivity of the carbon nanotubes is greatly limited and cannot be compared with the carbon nanotubes prepared by a high-temperature method. The traditional chemical vapor deposition method has the defects that the internal defects of the carbon nano tube are caused because the reaction temperature is low and carbon-carbon cannot well cross the bond barrier in the reconstruction process, so that the electron transmission is seriously hindered and the conductivity of the carbon nano tube is reduced. Therefore, increasing the catalyst activity or increasing the reaction temperature is a key element for preparing the fine-diameter carbon nanotubes.
Chinese patent No. CN200710098478.2 discloses a method and apparatus for continuously producing carbon nanotubes, which uses a multistage countercurrent reactor and uses a fluidized bed chemical vapor deposition process to continuously produce carbon nanotubes. Chinese patent 201010234322.4 discloses a method for preparing a diameter-controllable single-walled carbon nanotube, wherein carbon powder and a metal catalyst are filled into a carbon electrode by high-temperature arc ablation, and the carbon nanotube is prepared by arc direct ablation. Chinese patent 201110315452.5 discloses a preparation method of carbon nanotubes, which comprises loading a metal salt solution on a molybdenum or zirconium substrate, placing on a deposition table in a cavity of a direct current plasma jet chemical vapor deposition device, forming high-temperature plasma by a direct current arc, decomposing and reducing the metal salt to generate Ni/MgO catalyst, and then introducing hydrocarbon gas for high-temperature pyrolysis to form the carbon nanotubes. But realizing the controllable preparation of the catalyst particle size and activity, thereby preparing the fine-caliber carbon nano tube and even the single-walled carbon nano tube, which is still a challenging work.
Disclosure of Invention
The invention mainly aims to provide a device and a method for preparing carbon nanotubes, which are used for overcoming the defects in the prior art.
In order to achieve the aim of the invention, the invention adopts the following technical scheme: the device is used for realizing the combination of high-temperature physical evaporation and chemical vapor deposition by connecting the catalyst evaporation cavity with the chemical vapor deposition cavity in a sealing way through a pipeline, so that the catalyst directly enters the chemical vapor deposition cavity through a connecting channel, and meanwhile, a gas circuit system is used for leading carrier gas and carbon source gas in from the catalyst evaporation cavity and the chemical vapor deposition cavity respectively, so that the catalyst reacts with a high-temperature cracked organic carbon source to generate carbon nanotubes, and then the carbon nanotubes are separated and collected through the gas-solid separation cavity.
Further, the carbon nanotube preparation device has the structure that: the catalyst evaporation cavity, the chemical vapor deposition cavity and the gas-solid separation cavity are sequentially connected in a sealing manner from left to right;
an organic carbon source mixed gas inlet is arranged at the joint of the catalyst evaporation cavity and the chemical vapor deposition cavity; the other end of the catalyst evaporation cavity is provided with a carrier gas inlet and a high-temperature evaporation spray gun;
the vacuum system is connected with the gas-solid separation cavity; the gas path system is respectively connected with the organic carbon source mixed gas inlet and the carrier gas inlet; the cooling system is arranged on the side wall of the chemical vapor deposition cavity, and the power supply system provides power.
Further: the catalyst evaporation cavity adopts a high-temperature physical evaporation mode; the high-temperature physical evaporation mode is high-temperature arc, high-temperature radio frequency plasma or high-temperature microwave plasma; the catalyst evaporation cavity is a double-layer water-cooled stainless steel shell lined with a high-temperature heat insulation layer, and the lining high-temperature heat insulation layer is porous ceramic, ceramic fiber felt, graphite or graphite felt.
Further: the chemical vapor deposition cavity is a quartz tube furnace.
Further: the separation mode that gas-solid separation chamber adopted is: any one of centrifugal separation, cyclone separation and filtration separation modes.
Another object of the present invention is to provide a method for preparing carbon nanotubes using the above-mentioned apparatus for preparing carbon nanotubes, which specifically includes the following steps:
s1) placing a catalyst in a catalyst evaporation cavity, starting a vacuum system to discharge air in the catalyst evaporation cavity, and starting a gas circuit system to switch and introduce inert gas carrier gas;
s2) starting a chemical vapor deposition cavity to heat and raise the temperature, and raising the temperature to a specified temperature;
s3) then starting a high-temperature evaporation spray gun to evaporate the catalyst in the catalyst evaporation cavity, and enabling the catalyst to enter the chemical vapor deposition cavity along with the carrier gas through pipeline connection;
s4) introducing an organic carbon source gas mixture into the chemical vapor deposition cavity, and enabling the generated product to enter the gas-solid separation cavity along with carrier gas through a connecting pipeline, so as to obtain a final product after separation.
Further: the catalyst in the S1) is a metal catalyst, and the metal catalyst comprises one or more of iron, cobalt and nickel; the carrier gas is any one of nitrogen, argon and helium.
Further: the temperature in S2) is 500-1500 ℃.
Further: the highest temperature of the high-temperature evaporation spray gun in the S3) is higher than 2000 ℃, and the power is higher than 10 kW.
Further: the organic carbon source gas mixture in the S4) comprises an organic carbon source gas, an inert carrier gas and hydrogen; wherein the volume of the organic carbon source gas is 5-80%; the hydrogen volume is 0.1-10%, and the rest is inert carrier gas.
Further: the organic carbon source gas is one or more of methane, ethane, ethylene, ethanol and methanol.
Compared with the prior art, the invention has the advantages that:
(1) The device combining the high-temperature physical evaporation process and the chemical vapor deposition is adopted, so that the catalyst preparation and the carbon nano tube growth are continuously carried out, the activity of the catalyst is effectively ensured, the catalyst failure caused by the oxidation and aggregation of the intermittent preparation catalyst is avoided, and the subsequent chemical vapor deposition catalytic efficiency is improved;
(2) The catalyst is prepared by adopting a high-temperature physical evaporation process, so that metal is directly evaporated in a gaseous state, superfine catalyst particles can be obtained, and the efficient preparation of superfine-diameter carbon nanotubes and even single-wall carbon nanotubes is facilitated;
(3) The whole device integrates the functions of catalyst preparation, carbon nano tube preparation, separation and collection, can realize continuous preparation, and has the characteristics of high production efficiency, simple and convenient process and the like.
Drawings
Fig. 1 is a schematic structural diagram of a carbon nanotube manufacturing apparatus according to the present invention.
FIG. 2 is a schematic diagram of a scanning electron microscope of a carbon nanotube product prepared in example 1 of the method of the present invention.
FIG. 3 is a schematic diagram of a scanning electron microscope of a carbon nanotube product prepared in example 2 of the method of the present invention.
In the figure:
1. a catalyst evaporation chamber; 2. a carrier gas inlet; 3. a high temperature evaporation spray gun; 4. a catalyst; 5. an organic carbon source mixed gas inlet; 6. a chemical vapor deposition chamber; 7. a gas-solid separation cavity.
Detailed Description
The technical scheme of the invention is further described below with reference to the accompanying drawings and specific embodiments.
As shown in FIG. 1, the carbon nanotube preparation device comprises a catalyst evaporation cavity, a chemical vapor deposition cavity and a gas-solid separation cavity, wherein the catalyst evaporation cavity is connected with the chemical vapor deposition cavity in a sealing way through a pipeline to realize the combination of high-temperature physical evaporation and chemical vapor deposition, so that a catalyst directly enters the chemical vapor deposition cavity through a connecting channel, and meanwhile, a gas circuit system respectively introduces carrier gas and carbon source gas from the catalyst evaporation cavity and the chemical vapor deposition cavity to enable the catalyst to react with a high-temperature cracked organic carbon source to generate carbon nanotubes, and the carbon nanotubes are separated and collected through the gas-solid separation cavity.
Further, the carbon nanotube preparation device has the structure that: the catalyst evaporation cavity, the chemical vapor deposition cavity and the gas-solid separation cavity are sequentially connected in a sealing manner from left to right;
an organic carbon source mixed gas inlet is arranged at the joint of the catalyst evaporation cavity and the chemical vapor deposition cavity; the other end of the catalyst evaporation cavity is provided with a carrier gas inlet and a high-temperature evaporation spray gun;
the vacuum system is connected with the gas-solid separation cavity; the gas path system is respectively connected with the organic carbon source mixed gas inlet and the carrier gas inlet; the cooling system is arranged on the side wall of the chemical vapor deposition cavity, and the power supply system provides power.
Further: the catalyst evaporation cavity adopts a high-temperature physical evaporation mode; the high-temperature physical evaporation mode is high-temperature arc, high-temperature radio frequency plasma or high-temperature microwave plasma; the catalyst evaporation cavity is a double-layer water-cooled stainless steel shell lined with a high-temperature heat insulation layer, and the lining high-temperature heat insulation layer is porous ceramic, ceramic fiber felt, graphite or graphite felt.
Further: the chemical vapor deposition cavity is a quartz tube furnace.
Further: the separation mode that gas-solid separation chamber adopted is: any one of centrifugal separation, cyclone separation and filtration separation modes.
Another object of the present invention is to provide a process for preparing carbon nanotubes using the above-mentioned apparatus for preparing carbon nanotubes, which specifically includes the following steps:
s1) placing a catalyst in a catalyst evaporation cavity, starting a vacuum system to discharge air in the catalyst evaporation cavity, and starting a gas circuit system to switch and introduce inert gas carrier gas;
s2) starting a chemical vapor deposition cavity to heat and raise the temperature, and raising the temperature to a specified temperature;
s3) then starting a high-temperature evaporation spray gun to evaporate the catalyst in the catalyst evaporation cavity, and enabling the catalyst to enter the chemical vapor deposition cavity along with the carrier gas through pipeline connection;
s4) introducing an organic carbon source gas mixture into the chemical vapor deposition cavity, and enabling the generated product to enter the gas-solid separation cavity along with carrier gas through a connecting pipeline, so as to obtain a final product after separation.
Further: the catalyst in the S1) is a metal catalyst, and the metal catalyst comprises one or more of iron, cobalt and nickel; the carrier gas is any one of nitrogen, argon and helium.
Further: the temperature in S2) is 500-1500 ℃.
Further: the highest temperature of the high-temperature evaporation spray gun in the S3) is higher than 2000 ℃, and the power is higher than 10 kW.
Further: the organic carbon source gas mixture in the S4) comprises an organic carbon source gas, an inert carrier gas and hydrogen; wherein the volume of the organic carbon source gas is 5-80%; the hydrogen volume is 0.1-10%, and the rest is inert carrier gas.
Further: the organic carbon source gas is one or more of methane, ethane, ethylene, ethanol and methanol.
Example 1
The carbon nanotube preparation device is formed by connecting a catalyst evaporation cavity, a chemical vapor deposition cavity and a gas-solid separation cavity in series, wherein the catalyst evaporation cavity is a high-temperature electric arc device with the power of 20kW, and the outer layer consists of a double-layer water-cooled stainless steel shell lined with a graphite high-temperature heat insulation layer; the chemical vapor deposition cavity consists of a quartz tube furnace; the gas-solid separation cavity is a cyclone separation device. Iron is used as a metal catalyst, the catalyst is firstly placed in a catalyst evaporation cavity, and after vacuumizing and air removal, helium gas is switched and fed into inert gas carrier gas. Meanwhile, the chemical vapor deposition cavity is heated to 1200 ℃, then a high-temperature arc generated by an arc device is started, and after the iron atoms are gasified, carrier gas helium is led into the chemical vapor deposition cavity through a pipeline. The temperature of the chemical vapor deposition cavity is controlled at 1200 ℃, and the organic carbon source mixed gas is methane (45%), helium (50%) and hydrogen (5%), and is injected into the chemical vapor deposition cavity through an organic carbon source mixed gas inlet. The carbon source is catalyzed and cracked by the catalyst to grow the carbon nano tube at high temperature, and the rear end is connected with a cyclone separation device to carry out gas-solid separation to realize continuous preparation and collection, so as to obtain the morphology of the carbon nano tube product scanned by an electron microscope (shown in figure 2).
Example 2
The carbon nanotube preparation device is formed by connecting a catalyst evaporation cavity, a chemical vapor deposition cavity and a gas-solid separation cavity in series, wherein the catalyst evaporation cavity is high-temperature radio-frequency plasma with power of 25kW, and the outer layer consists of a double-layer water-cooled stainless steel shell lined with a porous ceramic high-temperature heat insulation layer; the chemical vapor deposition cavity consists of a quartz tube furnace; the gas-solid separation cavity is a cyclone separation device. Iron is used as a metal catalyst, the catalyst is firstly placed in a catalyst evaporation cavity, and after vacuumizing and air removal, inert gas carrier gas argon is switched to be introduced. Meanwhile, the chemical vapor deposition cavity is heated to 1300 ℃, then a high-temperature arc generated by an arc device is started, and after the iron atoms are gasified, carrier gas argon is led into the chemical vapor deposition cavity through a pipeline. The temperature of the chemical vapor deposition cavity is controlled at 1300 ℃, and the organic carbon source mixed gas is ethylene (5%), argon (85%) and hydrogen (10%), and is injected into the chemical vapor deposition cavity through an organic carbon source mixed gas inlet. The carbon source is catalyzed and cracked by the catalyst to grow the carbon nano tube at high temperature, the rear end is connected with a cyclone separation device to realize continuous preparation and collection by gas-solid separation, and the morphology of the carbon nano tube product scanned by an electron microscope is obtained (as shown in figure 3)
Example 3
The carbon nanotube preparation device is formed by connecting a catalyst evaporation cavity, a chemical vapor deposition cavity and a gas-solid separation cavity in series, wherein the catalyst evaporation cavity is high-temperature microwave plasma with power of 25kW, and the outer layer consists of a double-layer water-cooled stainless steel shell lined with a ceramic fiber felt high-temperature heat insulation layer; the chemical vapor deposition cavity consists of a quartz tube furnace; the gas-solid separation cavity is a cyclone separation device. Iron is used as a metal catalyst, the catalyst is firstly placed in a catalyst evaporation cavity, and after vacuumizing and air removal, helium gas is switched and fed into inert gas carrier gas. Meanwhile, the chemical vapor deposition cavity is heated to 500 ℃, then a high-temperature arc generated by an arc device is started, and after the iron atoms are gasified, the iron atoms are introduced into the chemical vapor deposition cavity through a carrier gas helium gas pipeline. The temperature of the chemical vapor deposition cavity is controlled at 500 ℃, and the organic carbon source mixed gas is methanol (80%), nitrogen (15%) and hydrogen (5%), and is injected into the chemical vapor deposition cavity through an organic carbon source mixed gas inlet. The carbon source is catalytically cracked and grown into carbon nano tube at high temperature, and the back end is connected with a cyclone separator for gas-solid separation to realize continuous preparation and collection.
Example 4
The carbon nanotube preparation device is formed by connecting a catalyst evaporation cavity, a chemical vapor deposition cavity and a gas-solid separation cavity in series, wherein the catalyst evaporation cavity is a high-temperature electric arc device with the power of 20kW, and the outer layer consists of a double-layer water-cooled stainless steel shell lined with a graphite high-temperature heat insulation layer; the chemical vapor deposition cavity consists of a quartz tube furnace; the gas-solid separation cavity is a cyclone separation device. Iron is used as a metal catalyst, the catalyst is firstly placed in a catalyst evaporation cavity, and after vacuumizing and air removal, helium gas is switched and fed into inert gas carrier gas. Meanwhile, the chemical vapor deposition cavity is heated to 1500 ℃, then a high-temperature arc generated by an arc device is started, and after the iron atoms are gasified, the iron atoms are introduced into the chemical vapor deposition cavity through a carrier gas helium gas pipeline. The temperature of the chemical vapor deposition cavity is controlled at 1500 ℃, and the organic carbon source mixed gas is ethanol (45%), helium (54.9%) and hydrogen (0.1%), and is injected into the chemical vapor deposition cavity through an organic carbon source mixed gas inlet. The carbon source is catalytically cracked and grown into carbon nano tube at high temperature, and the back end is connected with a cyclone separator for gas-solid separation to realize continuous preparation and collection.
Example 5
The carbon nanotube preparation device is formed by connecting a catalyst evaporation cavity, a chemical vapor deposition cavity and a gas-solid separation cavity in series, wherein the catalyst evaporation cavity is a high-temperature electric arc device with the power of 20kW, and the outer layer consists of a double-layer water-cooled stainless steel shell lined with a graphite high-temperature heat insulation layer; the chemical vapor deposition cavity consists of a quartz tube furnace; the gas-solid separation cavity is a cyclone separation device. Cobalt is used as a metal catalyst, the catalyst is firstly placed in a catalyst evaporation cavity, and after vacuumizing and air removal, helium gas is switched and fed into inert gas carrier gas. Meanwhile, the chemical vapor deposition cavity is heated to 1200 ℃, then a high-temperature arc generated by an arc device is started, and after the iron atoms are gasified, carrier gas helium is led into the chemical vapor deposition cavity through a pipeline. The temperature of the chemical vapor deposition cavity is controlled at 1200 ℃, and the organic carbon source mixed gas is ethane (45%), helium (45%) and hydrogen (5%), and is injected into the chemical vapor deposition cavity through an organic carbon source mixed gas inlet. The carbon source is catalytically cracked and grown into carbon nano tube at high temperature, and the back end is connected with a filtering device for gas-solid separation to realize continuous preparation and collection.
Example 6
The carbon nanotube preparation device is formed by connecting a catalyst evaporation cavity, a chemical vapor deposition cavity and a gas-solid separation cavity in series, wherein the catalyst evaporation cavity is a high-temperature arc device with the power of 50kW, and the outer layer consists of a double-layer water-cooled stainless steel shell lined with a graphite high-temperature heat insulation layer; the chemical vapor deposition cavity consists of a quartz tube furnace; the gas-solid separation cavity is a cyclone separation device. Nickel is used as a metal catalyst, the catalyst is firstly placed in a catalyst evaporation cavity, and after vacuumizing and air removal, helium gas is switched and fed into inert gas carrier gas. Meanwhile, the chemical vapor deposition cavity is heated to 1200 ℃, then a high-temperature arc generated by an arc device is started, and after the iron atoms are gasified, carrier gas helium is led into the chemical vapor deposition cavity through a pipeline. The temperature of the chemical vapor deposition cavity is controlled at 1200 ℃, and the organic carbon source mixed gas is methane (45%), helium (45%) and hydrogen (5%), and is injected into the chemical vapor deposition cavity through an organic carbon source mixed gas inlet. The carbon source is catalytically cracked and grown into carbon nano tube at high temperature, and the back end is connected with a cyclone separator for gas-solid separation to realize continuous preparation and collection.
Example 7
The carbon nanotube preparation device is formed by connecting a catalyst evaporation cavity, a chemical vapor deposition cavity and a gas-solid separation cavity in series, wherein the catalyst evaporation cavity is a high-temperature arc device with the power of 50kW, and the outer layer consists of a double-layer water-cooled stainless steel shell lined with a graphite high-temperature heat insulation layer; the chemical vapor deposition cavity consists of a quartz tube furnace; the gas-solid separation cavity is a cyclone separation device. Iron and cobalt are used as metal catalysts, firstly, the catalysts are placed in a catalyst evaporation cavity, and after vacuumizing and air exhausting, helium gas is switched and fed into inert gas carrier gas. Meanwhile, the chemical vapor deposition cavity is heated to 1200 ℃, then a high-temperature arc generated by an arc device is started, and after the iron atoms are gasified, carrier gas helium is led into the chemical vapor deposition cavity through a pipeline. The temperature of the chemical vapor deposition cavity is controlled at 1200 ℃, and the organic carbon source mixed gas is methane (45%), helium (45%) and hydrogen (5%), and is injected into the chemical vapor deposition cavity through an organic carbon source mixed gas inlet. The carbon source is catalytically cracked and grown into carbon nano tube at high temperature, and the back end is connected with a cyclone separator for gas-solid separation to realize continuous preparation and collection.
In view of the shortcomings in the prior art, the inventor of the present invention has long studied and put forward a technical solution of the present invention, and the technical solution, the implementation process and principle thereof will be further explained as follows.

Claims (6)

1. The preparation method is characterized in that a preparation device adopted by the method comprises a catalyst evaporation cavity, a chemical vapor deposition cavity and a gas-solid separation cavity, wherein the catalyst evaporation cavity is connected with the chemical vapor deposition cavity in a sealing way through a pipeline, so that the combination of high-temperature physical evaporation and chemical vapor deposition is realized, and meanwhile, a gas circuit system is used for leading the chemical vapor deposition cavity in, so that the catalyst reacts with a high-temperature cracked organic carbon source to generate carbon nanotubes, and the carbon nanotubes are separated and collected through the gas-solid separation cavity; the carbon nanotube preparation device has the structure that: the catalyst evaporation cavity, the chemical vapor deposition cavity and the gas-solid separation cavity are sequentially connected in a sealing manner from left to right; an organic carbon source mixed gas inlet is arranged at the joint of the catalyst evaporation cavity and the chemical vapor deposition cavity; the other end of the catalyst evaporation cavity is provided with a carrier gas inlet and a high-temperature evaporation spray gun; the vacuum system is connected with the gas-solid separation cavity; the gas path system is respectively connected with the organic carbon source mixed gas inlet and the carrier gas inlet; the cooling system is arranged on the side wall of the chemical vapor deposition cavity, and the power supply system provides power; the highest temperature of the high-temperature evaporation spray gun is more than 2000 ℃, and the power is more than 10kW; the preparation method specifically comprises the following steps:
s1) placing a catalyst in a catalyst evaporation cavity, starting a vacuum system to discharge air in the catalyst evaporation cavity, and starting a gas circuit system to switch and introduce inert gas carrier gas;
s2) starting a chemical vapor deposition cavity to heat and raise the temperature, and raising the temperature to a specified temperature;
s3) then starting a high-temperature evaporation spray gun to evaporate the catalyst in the catalyst evaporation cavity, and enabling the catalyst to enter the chemical vapor deposition cavity along with the carrier gas through pipeline connection;
s4) introducing an organic carbon source gas mixture into the chemical vapor deposition cavity, and enabling the generated product to enter a gas-solid separation cavity along with carrier gas through a connecting pipeline, so as to obtain a final product after separation;
the organic carbon source gas mixture comprises an organic carbon source gas, an inert carrier gas and hydrogen; wherein the volume of the organic carbon source gas is 5-80%; the volume of the hydrogen is 0.1-10%, and the rest is inert carrier gas; the catalyst is iron.
2. The method according to claim 1, characterized in that: the high-temperature physical evaporation mode is high-temperature arc, high-temperature radio frequency plasma or high-temperature microwave plasma; the catalyst evaporation cavity is a double-layer water-cooled stainless steel shell lined with a high-temperature heat insulation layer, and the lining high-temperature heat insulation layer is porous ceramic, ceramic fiber felt, graphite or graphite felt.
3. The method according to claim 1, characterized in that: the chemical vapor deposition cavity is a quartz tube furnace; the separation mode that gas-solid separation chamber adopted is: any one of centrifugal separation, cyclone separation and filtration separation modes.
4. The method according to claim 1, characterized in that: the carrier gas is any one of nitrogen, argon and helium.
5. The method according to claim 1, characterized in that: the temperature in S2) is 500-1500 ℃.
6. The method according to claim 1, characterized in that: the organic carbon source gas is one or more of methane, ethane, ethylene, ethanol and methanol.
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JP2021529513A JP7178494B2 (en) 2019-06-19 2019-11-26 Method for producing carbon nanotubes
PCT/CN2019/120827 WO2020253104A1 (en) 2019-06-19 2019-11-26 Carbon nano tube preparation device and method
KR1020217000292A KR102535679B1 (en) 2019-06-19 2019-11-26 Apparatus and method for manufacturing carbon nanotubes

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