CN110182787B - Device and method for continuously growing carbon nano tube - Google Patents
Device and method for continuously growing carbon nano tube Download PDFInfo
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- CN110182787B CN110182787B CN201910533877.XA CN201910533877A CN110182787B CN 110182787 B CN110182787 B CN 110182787B CN 201910533877 A CN201910533877 A CN 201910533877A CN 110182787 B CN110182787 B CN 110182787B
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- C01B32/00—Carbon; Compounds thereof
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- C01B32/158—Carbon nanotubes
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Abstract
The invention relates to the technical field of arc discharge thermal plasma methods, in particular to an arc device for continuously growing carbon nanotubes and a method thereof. The device mainly comprises an arc chamber, a thermostatic chamber and a deposition chamber which are connected in series in sequence through pipelines. The arc chamber contains metal anode and graphite arc groove cathode with bend angle, the gas to be ignited is injected into the arc chamber from the graphite groove, and the stable arc is formed after voltage is applied between the two electrodes. The outside of the arc chamber is provided with a heat insulation shell, the deposition chamber is provided with a double-layer water-cooling stainless steel chamber wall, and a cage type collecting device is arranged in the deposition chamber. After the carbon source substance is catalytically decomposed in the arc chamber, the carbon source substance enters the constant temperature chamber to start growing and finally is condensed in the deposition chamber, and the incompletely reacted gas can be further collected and injected into the combined device to carry out the circulating catalytic reaction.
Description
Technical Field
The invention relates to the technical field of arc discharge thermal plasma methods, in particular to an arc device for continuously growing carbon nanotubes and a method thereof.
Background
Arc discharge is a self-sustaining discharge mode which is the strongest of gas discharge: when a power supply provides electric energy with larger power, the voltage between electrodes only needs dozens of volts, and gas between the two electrodes can be ionized to form plasma through stronger current (5 to 600A), so that strong brilliance is emitted while high temperature (2000 to 10000 ℃) is generated. Under the dual actions of high-temperature electric arc and ion bombardment, even high-melting-point substances such as graphite, titanium, tungsten, molybdenum and the like can be evaporated and recrystallized to prepare high-purity metals, alloys and the like; the arc discharge can also be used for reactions such as halogenation of metal oxides, thermal cracking of low-boiling hydrocarbons and the like, so the arc discharge has extremely high engineering application value.
The arc discharge method is a traditional method for preparing high-crystallinity carbon nano materials, chinese patents such as CN 1823006A, CN 2475983Y, CN 1765735A, CN 102009974A and the like all introduce an arc device or a method for growing carbon nano materials by using graphite ablation electrodes by adopting the traditional arc discharge method, so that the graphite electrodes are forced to be evaporated and ablated at extremely high temperature (the melting point is 3850 +/-50 ℃, and the boiling point is 4250 ℃), and the overall energy consumption of an arc system is further increased; on the other hand, the ablated graphite anode is easy to be exhausted due to the influence of the size of the graphite anode, at the moment, the graphite anode is emptied, the electric arc furnace is opened to replace the graphite anode and then vacuumized after the electric arc furnace is completely cooled, ionized gas is introduced to preheat and repeat the electric arc reaction, the preparation efficiency is greatly reduced, and the method is difficult to be used for industrial batch production.
The invention achieves the aim of continuously growing the high-crystallinity carbon nano tube by continuously introducing hydrocarbon raw materials into the arc reaction chamber. On one hand, the catalytic decomposition temperature (600 to 1000 ℃) of most of hydrocarbons is lower than that of graphite, the energy consumption of an electric arc system can be greatly reduced, the concentration of evaporated carbon atoms can be efficiently controlled by adopting the hydrocarbons, and amorphous carbon impurities cannot be easily generated by adopting solid electrodes with high carbon content such as graphite and the like; meanwhile, the traditional ablation graphite anode is changed into a metal powder anode, and in the arc discharge process, the metal anode is gradually heated and does not cause large-area ablation phenomenon, but is melted and slowly evaporated to be used as an atomic-scale catalyst for catalyzing hydrocarbon, so that the carbon nano tube with high crystallinity can be efficiently grown. On the other hand, because a large amount of metal can be charged into the bottom of the arc chamber, the arc reaction can be continued for a long time; if the reaction time needs to be further prolonged to enlarge the production capacity, a feeding port for supplementing metal powder can be additionally arranged at the top of the arc chamber.
Disclosure of Invention
It is a primary object of the present invention to provide a method of continuously growing an apparatus for carbon nanotubes, which solves any of the above and other potential problems of the prior art.
In order to achieve the purpose, the technical scheme of the embodiment of the disclosure is as follows: a device for continuously growing carbon nano tubes comprises an arc chamber, a thermostatic chamber and a deposition chamber which are sequentially connected in a sealing way through pipelines,
the arc chamber comprises a heat-insulating outer wall and a hollow reaction chamber, wherein a cathode is arranged in the hollow reaction chamber, a hollow air inlet path is arranged in the cathode, one end of the hollow air inlet path is connected with a reaction gas bottle arranged on the outer side of the arc chamber, an anode is arranged at the bottom of the hollow reaction chamber, and an arc welding device for initiating an electric arc is arranged between the cathode and the anode.
According to the embodiment of the disclosure, the cathode is a graphite arc groove, one end of the graphite arc groove is an air inlet end, the other end of the graphite arc groove is an air outlet end, a certain included angle is formed between the air inlet end and the air outlet end, and the included angle ranges from 90 degrees to 150 degrees, so that cathode loss caused by permeation of electric arc to the inside of the cathode after arc starting is effectively prevented.
According to an embodiment of the present disclosure, the metal anode is a transition metal with catalytic properties, the purity of which is greater than 99.9%.
According to the embodiment of the disclosure, the thermostatic chamber is protected by adopting an insulating outer wall or is arranged in a bedroom tube furnace to keep constant temperature.
According to this disclosed embodiment, the deposit room includes double-deck water-cooling stainless steel chamber wall and inside cavity, inside cavity is equipped with the collection device who comprises a plurality of rotatable stainless steel filter screens.
Another object of the embodiments of the present disclosure is to provide a method for preparing carbon nanotubes using the above-mentioned apparatus, which specifically includes the following method,
s1) firstly, the arc chamber is pumped to the vacuum degree P0，0<P0<100Pa, and then introducing arc striking gas and carbon source substances into the arc chamber;
s2) turning on the power supply of the electric arc welding device, and applying a voltage U between the cathode and the anode0，5V≤U0Arc forming is carried out when the voltage is less than or equal to 50V, the vacuum pump is started, the vacuum degree is adjusted to be opened again to ensure that the vacuum degree of the arc chamber is maintained at 60000Pa,
the metal anode is gradually melted and evaporated to start catalytic cracking of carbon source substances, and the formed precursor enters a thermostatic chamber to grow into C with relatively low electronic state2Or an aromatic ring, or a mixture of two or more aromatic rings,
and S3) entering the deposition chamber again to be rapidly cooled to form the carbon nano material with high crystallinity.
According to the embodiment of the disclosure, the method further comprises S4) collecting tail gas exhausted from the deposition chamber, and introducing the tail gas into the electric arc system again for re-reaction or combusting the tail gas to supply heat to the thermostatic chamber so as to reduce energy consumption and pollution.
According to the embodiment of the disclosure, the arc striking gas in S1) is one or two of hydrogen, helium and argon.
According to the embodiment of the disclosure, the carbon source substance in S1 is one or more of methane, coal bed methane, biogas, acetylene, ethylene, propane, propylene, benzene, toluene, xylene, methanol, ethanol, butanol, acetone, and butanone, and when the added carbon source substance is in a liquid state under normal conditions, the carbon source substance needs to be gasified by a preheating device and then enters the gas path.
According to the embodiment of the disclosure, the flow ratio of the arc striking gas to the carbon source substance in the gas path is 1-10.
The operation of the combination of the invention is as follows: firstly introducing arc striking gas and carbon source substances into an arc chamber, then applying voltage between a cathode and an anode to form an arc, gradually melting and evaporating a metal anode to start catalytic cracking of the carbon source substances, and allowing formed precursors such as carbonium ions and the like to enter a thermostatic chamber to grow into C with relatively low electronic state2Or an aromatic ring, and then enters the deposition chamber to be rapidly cooled to form the carbon nano material with high crystallinity. The collected and discharged tail gas can be introduced into an electric arc system again for re-reaction or be combusted in a heat supply thermostatic chamber so as to reduce energy consumption and pollute the environment.
The invention is characterized in that: the metal anode is slowly evaporated to be used as an atomic catalyst to crack carbon source substances, and the electric arc process can be maintained for a long time, so that the aim of continuously growing the carbon nano tube is fulfilled. In addition, a transition constant temperature chamber is adopted to ensure that the temperature of the precursor cracked by the electric arc is uniform, and the carbon in the precursor is rapidly cooled and crystallized into the carbon nano tube after the atomic states of the carbon in the precursor are controlled to be similar. The system discharges a small amount of inert gases such as helium or argon for maintaining the stability of the electric arc, and has no other pollutant gases.
Drawings
Fig. 1 is a schematic structural diagram of an apparatus for continuously growing carbon nanotubes according to the present invention.
FIG. 2 is a scanning topography of the carbon nanotubes prepared in example 2 of the present invention.
FIG. 3 is a graph showing the effect of the arc discharge method and the reaction time for preparing carbon nanotubes according to the present invention.
In the figure:
1. the device comprises an arc chamber, 11 heat-insulating and insulating outer walls, 12 hollow reaction chambers, 13 cathodes, 131 air inlet ends, 132 air outlet ends, 14 hollow air inlet gas circuits, 15 reaction gas cylinders, 16 anodes, 17 arc welding devices, 18 arcs, 19 anode melts, 2 thermostatic chambers, 3 deposition chambers, 31 collecting devices, 32 exhaust ports.
Detailed Description
The present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
As shown in fig. 1, the apparatus for continuously growing carbon nanotubes of the present invention comprises an arc chamber, a thermostatic chamber and a deposition chamber which are hermetically connected in sequence by a pipe,
the arc chamber comprises an insulating outer wall and a hollow reaction chamber,
the arc welding device comprises a hollow reaction chamber, a cathode, a hollow air inlet circuit, a reaction gas bottle, an anode and an arc welding device, wherein the cathode is arranged in the hollow reaction chamber, the hollow air inlet circuit is arranged in the cathode, one end of the hollow air inlet circuit is connected with the reaction gas bottle arranged on the outer side of the arc chamber, the anode is arranged at the bottom of the hollow reaction chamber, and the arc welding device for initiating electric arc is arranged between the cathode and the anode.
According to the embodiment of the disclosure, the cathode is a graphite arc groove, one end of the graphite arc groove is an air inlet end, the other end of the graphite arc groove is an air outlet end, a certain included angle is formed between the air inlet end and the air outlet end, and the included angle ranges from 90 degrees to 150 degrees so as to effectively prevent anode loss caused by penetration of electric arc to the inside of the cathode after arc starting.
According to the embodiment of the disclosure, the metal anode is a transition metal with catalytic performance, the form of the metal anode comprises metal sheets, metal chips, metal blocks or metal powder, and the purity of the metal anode is more than 99.9%.
According to the embodiment of the disclosure, the thermostatic chamber is protected by adopting an insulating outer wall or is arranged in a bedroom tube furnace to keep constant temperature.
According to this disclosed embodiment, the deposit room includes double-deck water-cooling stainless steel chamber wall and inside cavity, inside cavity is equipped with the collection device who comprises a plurality of rotatable stainless steel filter screens.
Another object of the disclosed embodiments is to provide a method for preparing carbon nanotubes using the above-mentioned apparatus, which specifically includes the following method,
s1) firstly, the arc chamber is pumped to the vacuum degree P0，0<P0<100Pa, thenIntroducing arc striking gas and carbon source substances into the arc chamber;
s2) turning on the power supply of the electric arc welding device, and applying a voltage U between the cathode and the anode0，5V≤U0Arcing is carried out at the voltage of less than or equal to 50V, a vacuum pump is started, the vacuum degree is adjusted until the vacuum pump is started again to ensure that the vacuum degree of an arc chamber is maintained at 60000Pa,
the metal anode is gradually melted and evaporated to start catalytic cracking of carbon source substances, and the formed precursors such as carbon ions enter a thermostatic chamber to initially grow into C with relatively low electronic state2Or an aromatic ring, or a mixture of aromatic rings,
and S3) entering the deposition chamber again to be rapidly cooled to form the carbon nano material with high crystallinity.
According to the embodiment of the disclosure, the method further comprises S4) collecting the tail gas exhausted from the deposition chamber, and introducing the tail gas into the electric arc system again for re-reaction or burning the tail gas to a heat supply thermostatic chamber so as to reduce energy consumption and pollute the environment.
According to the embodiment of the disclosure, the arc striking gas in S1) is one or two of hydrogen, helium and argon.
According to the embodiment of the disclosure, the carbon source substance in S1 is one or more of methane, coal bed gas, methane, acetylene, ethylene, propane, propylene, benzene, toluene, xylene, methanol, ethanol, butanol, acetone, butanone, and natural gas, and when the added carbon source substance is in a liquid state in a normal condition, the carbon source substance needs to be gasified by a preheating device and then enters the gas path.
According to the embodiment of the disclosure, the flow ratio of the arc striking gas to the carbon source substance in the gas path is 1-10.
The device in the technical scheme of the invention adopts the following embodiments to verify the parameters of the method for growing the carbon nano tube:
example 1
Pumping the vacuum degree of the whole device to 5 Pa, closing a vacuum pump, then filling 300 Torr argon into a hollow air inlet gas circuit, opening a power supply of an electric arc welding device, adjusting the current to 200A to initiate electric arc, opening the vacuum pump again, adding argon and methane (the flow rate is 2.
Example 2
Pumping the vacuum degree of the whole device to 5 Pa, closing a vacuum pump, then filling 300 Torr argon into a hollow air inlet gas circuit, opening a power supply of an electric arc welding device, adjusting the current to 200A to initiate electric arc, opening the vacuum pump again, adding argon and methane (the flow rate is 2.
Example 3
Pumping the vacuum degree of the whole device to 5 Pa, closing a vacuum pump, then filling 300 Torr argon into a hollow air inlet gas circuit, opening a power supply of an arc welding device, adjusting the current to 200A to initiate electric arc, opening the vacuum pump again, adding argon and methane (the flow rate is 2.
In examples 1 to 3, the arc discharge method in the arc discharge vacuum furnace may be dc arc discharge, ac arc discharge, or ac/dc hybrid arc discharge, and the graph of the carbon nanotubes versus the reaction time is shown in fig. 3.
The reaction time is sequentially prolonged from the examples 1 to 3, and the yield of the carbon nanotubes is linearly increased, which shows that the device can continuously grow the carbon nanotubes for a long time, and has a mass production and commercialization prospect.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (7)
1. A method for continuously growing carbon nanotubes is characterized in that the method adopts the following devices: the electric arc chamber comprises a heat insulation outer wall and a hollow reaction chamber, wherein a cathode is arranged in the hollow reaction chamber, a hollow air inlet path is arranged in the cathode, one end of the hollow air inlet path is connected with a reaction gas bottle arranged outside the electric arc chamber, an anode is arranged at the bottom of the hollow reaction chamber, and an electric arc welding device for initiating electric arc is arranged between the cathode and the anode,
s1) firstly pumping the arc chamber to a certain vacuum degree P0，0< P0<100Pa, and then introducing arc striking gas and carbon source substances into the arc chamber;
s2) turning on the power supply of the electric arc welding device, and applying a voltage U between the cathode and the anode0，5V≤U0Arc forming is carried out at the voltage of less than or equal to 50V, the vacuum pump is started again, the vacuum pump is regulated to be started again to ensure that the vacuum degree of the arc chamber is maintained at 60000Pa, the metal anode is gradually melted and evaporated to start catalytic cracking of carbon source substances, the arc welding power supply is closed and stopped after the reaction lasts for 4-40h, and the precursor formed by the reaction enters a thermostatic chamber to be primarily grown into C with relatively low electronic state2Or an aromatic ring;
s3) the product of the thermostatic chamber enters a deposition chamber to be rapidly cooled to form a carbon nano material with high crystallinity; the cathode is a graphite arc groove, one end of the graphite arc groove is an air inlet end, the other end of the graphite arc groove is an air outlet end, a certain included angle is formed between the air inlet end and the air outlet end, and the included angle ranges from 90 degrees to 150 degrees; the flow ratio of the arc striking gas to the carbon source substance in the gas path is 1-10.
2. The method of claim 1, wherein the metal anode is a transition metal having catalytic properties and a purity greater than 99.9%.
3. The method according to claim 1, wherein the thermostatic chamber is protected by an insulating outer wall or is placed in a horizontal tube furnace to be kept at a constant temperature.
4. The method of claim 1, wherein the deposition chamber comprises a double-layer water-cooled stainless steel chamber wall and an internal chamber, and a collection device consisting of a plurality of rotatable stainless steel screens is arranged in the internal chamber.
5. The method according to claim 1, further comprising S4) collecting the exhaust gas from the deposition chamber and feeding the exhaust gas into an electric arc system for re-reaction or a combustion heating thermostatic chamber to reduce energy consumption and pollution.
6. The method of claim 1, wherein the arc ignition gas in S1) is one or two of hydrogen, helium and argon.
7. The method as claimed in claim 1, wherein the carbon source material in S1) is one or more of methane, coal bed methane, biogas, acetylene, ethylene, propane, propylene, benzene, toluene, xylene, methanol, ethanol, butanol, acetone, and butanone.
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| CN112174113A (en) * | 2020-10-14 | 2021-01-05 | 宁波中乌新材料产业技术研究院有限公司 | Preparation method of bamboo-joint-type carbon nano tube |
| CN112796896B (en) * | 2021-02-04 | 2022-09-16 | 江苏大学 | Device and method for preparing carbon nano tube by adopting ignition type dual-fuel engine |
| CN113247881B (en) * | 2021-05-17 | 2023-06-20 | 常州大学 | Device and method for preparing nano carbon by methane plasma pyrolysis |
| CN114160801B (en) * | 2021-11-01 | 2024-03-19 | 沈阳工业大学 | Equipment and method for preparing alloy nano particles by arc method |
| CN115403030B (en) * | 2022-09-22 | 2023-09-19 | 江西铜业技术研究院有限公司 | Device and method for preparing single-walled carbon nanotubes by using flowing catalyst |
| CN116553527B (en) * | 2023-06-20 | 2023-12-15 | 烯格沃(上海)纳米技术有限公司 | Industrial synthesis device for single-walled carbon nanotubes |
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| CN102009974B (en) * | 2010-11-28 | 2012-08-29 | 上海大学 | Combined device for preparing single-wall carbon nano tube |
| US8137653B1 (en) * | 2011-01-30 | 2012-03-20 | Mcd Technologies S.A R.L. | System and method for producing carbon nanotubes |
| US20160207770A1 (en) * | 2013-01-22 | 2016-07-21 | Mikhail Rudolfovich Predtechenskiy | Method and apparatus for producing carbon nanostructures |
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