CN106276846B - A kind of system and method for preparing CNT - Google Patents
A kind of system and method for preparing CNT Download PDFInfo
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- CN106276846B CN106276846B CN201610561905.5A CN201610561905A CN106276846B CN 106276846 B CN106276846 B CN 106276846B CN 201610561905 A CN201610561905 A CN 201610561905A CN 106276846 B CN106276846 B CN 106276846B
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Abstract
The invention belongs to carbon nanotube preparation technology field, and in particular to a kind of system and method for preparing CNT.The system is nine grids flame reactor, and the agent structure of reactor is symmetrical, and shape of cross section is nine grids；What it is positioned at centre grid is flame of centre passage, and on four angles is four external flame passages that are identical and being centrosymmetric；Between every two adjacent external flame passages, it is disposed with that four identical and what is be centrosymmetric prepares reaction channel.Flame reactor provided by the invention can be with continuous producing carbon nano-tube, and has the advantages of cost is low, yield is high, equipment and operating method are simple.
Description
Technical field
The invention belongs to carbon nanotube preparation technology field, and in particular to a kind of system and method for preparing CNT.
Background technology
CNT is described as " king of nanometer ", many surprising characteristics is shown, such as its strength modulus and diamond
It is almost identical, have fabulous flexibility；Electric current can be conveyed at room temperature non-resistance；Nano electron device etc. can be constructed.Therefore, more
It is begun one's study come more scholars, CNT is into one of most popular research topic at present in the world.CNT has
There is typical cannulated structure, tube wall is the hexagon carbocyclic ring structure for being combined and being formed by the carbon atom of class graphite crystal
Into.The radial dimension of CNT is smaller, and caliber is typically in several nanometers to several tens of nanometers or so, but the length of pipe can reach
Micron dimension, there is very big draw ratio, therefore, CNT is considered as a kind of typical monodimension nanometer material.
For many years, the technology of preparing of CNT is constantly subjected to the concern of domestic and international scientist.At present, the system of CNT
Preparation Method mainly has four kinds：Arc discharge method, laser evaporization method, chemical vapour deposition technique and flame method.Wherein, first three methods
Research work carry out more, comparative maturity so far, but this several method cost, equipment, operation etc. by compared with
Big restriction.And although the existing flame method for preparing CNT realizes the target that cost is relatively low, easy to operate, but
Most of yield are not high, and the utilization rate of carbon source is relatively low, and equipment is also not simple enough, does not possess a large amount of quantity-produced conditions.
Therefore, it is necessary to seek more effective preparation method of carbon nano-tube so that the preparation process of CNT is continuous, criticizes
Amount, controllable, cost is low, equipment is simple and convenient to operate.
The content of the invention
The invention provides a kind of system and method for preparing CNT, concrete technical scheme are as follows：
A kind of system for preparing CNT, the system are nine grids flame reactor, the agent structure pair of reactor
Claim, shape of cross section is nine grids；What it is positioned at centre grid is flame of centre passage, and on four angles is four complete
External flame passage that is identical and being centrosymmetric；Between every two adjacent external flame passages, four complete phases are disposed with
Together and what is be centrosymmetric prepares reaction channel.
Preferably, flame of centre passage prepares reaction channel height with being respectively positioned at the upper end outlet of external flame passage
5%~50% part, and passage of flame and the relative altitude for preparing between reaction channel can be adjusted as needed.
Preferably, a piece of fin is respectively installed on four angles of reactor top.
The method that CNT is prepared using system as described above：Fuel gas and air are from flame of centre passage and four
The lower end input of bar external flame passage, is ignited at upper end outlet, forms flame of centre and external flame straight up,
So as to provide required heat energy to prepare CNT；Reacting gas inputs from four lower ends for preparing reaction channel, not completely
The remaining carbon-source gas of reaction and other flammable reacting gas are ignited at upper end outlet；In flame of centre and external flame
Dual-heated effect under, carbon-source gas in reacting gas chemically react preparing in reaction channel, decomposite before this
Substantial amounts of carbon atom, after then carbon atom undergoes a succession of complicated process, simultaneously stone is separated out on the surface of active catalyst particles
Mo Hua, and then nucleating growth is CNT；The process that carbon-source gas decomposite substantial amounts of carbon atom is preparing reaction channel
Lower half is carried out, and the process that carbon atom is combined into CNT is carried out in the first half for preparing reaction channel.
Preferably, the fuel gas is the acetylene that flame is concentrated, caloric value is high.
Preferably, the reacting gas is CO, H2And He, wherein CO are described carbon-source gas, H2For flammable reaction gas
Body.
Preferably, reaction zone is prepared with CNT to measure carbon atom dissociation reaction area using contactless thermometer
Temperature.
Preferably, the contactless thermometer is thermocouple.
Preferably, the mass flow of gas is measured and controlled using gas mass flow controller, and by with
The read out instrument of set is come the mass flow observing and record gas.
Preferably for the CNT prepared, sampling mode is：By sampling substrate from the upper end for preparing reaction channel
Near exit is sampled, or sample probe is stretched into the inside sampling for preparing reaction channel.
Be respectively positioned at the upper end outlet of flame of centre passage and external flame passage prepare reaction channel height 5%~
50% part, and passage of flame and the relative altitude for preparing between reaction channel can be adjusted as needed.This construction
Mode naturally enough separates the dissociation process of carbon atom and the generating process of CNT, is advantageous to the control of preparation condition
System, sampling mode also become simple and flexible.
Each prepares reaction channel and is all acted on simultaneously by the dual and Bidirectional heating of flame of centre and external flame, makes
Flame heating effect it is more obvious, prepare being uniformly heated for gas in reaction channel, be advantageous to improve heating-up temperature,
Eliminate temperature deviation.
Four identical and be centrosymmetric, each bars just the same with heating condition by hot mode that prepare reaction channel
The composition of gas does not have difference with flow yet in passage, i.e. this four physical and chemical condition prepared in reaction channel complete one
Cause, ensure that the CNT being prepared all does not have bigger difference in terms of form, quality.So, only need to be in this four systems
Standby reaction channel samples simultaneously, by the form, the quality that contrast four groups of samples, it is possible to eliminates the contingency of experimental result, increases
The confidence level and convincingness tested by force；The position to be gone wrong in reactor can also be rapidly found out when breaking down；In addition
The sampling stand-by period of repeated experiment is also a saving, drastically increases efficiency.
Because external flame passage is in atmospheric environment, therefore when desired flame temperature is not especially high, without to
Wherein input air, the flow of fuel gas that need to only fix or change input can maintain the burning of external flame or regulation outer
Enclose the temperature of flame.Although the surrounding of flame of centre passage is produced reaction channel and surrounded, its top is still complete
Unlimited, there is the burning that enough air can maintain flame of centre, the temperature to adjust flame of centre can be to central flame
Flame passage inputs appropriate air.
External flame passage is not fixed together with preparing reaction channel, and the relative altitude between them can be random
Change, is so advantageous to control and adjust the dissociation temperature of carbon atom and the generation temperature of CNT.By the dissociation of carbon atom
React the reaction of formation with CNT to be controlled by respectively, can more preferably, quickly control the generating process of CNT, together
When be advantageous to analyze experimental result and discussed.
Meanwhile flame of centre passage prepares reaction channel height with being respectively positioned at the upper end outlet of external flame passage
5%~50% part, and the relative altitude between them can be adjusted as needed, be advantageous to control carbon atom solution respectively
From reaction zone and the temperature in CNT reaction of formation area.
In the present invention, it is CO, H to prepare the reacting gas in reaction channel2And He.CO provides carbon source, and it can be by competing
Striving active site prevents catalyst surface from being covered by amorphous carbon, and crushes the iron of bulky grain, produces more active surfaces.H2
CO hydrogenations is separated out carbon, and promote the carbon of dissociation to be adsorbed by iron particle, be advantageous to carbon nano tube growth, moreover it is possible to keep catalyst
Activity.He primarily serves the effect of partial dilution and cooling, and the helium for carrying vaporific catalyst into reactor is also affected and urged
The supply rate of agent.In addition, H2Also have the function that to purge carbon nano tube surface and purify with He, while also can be effectively
Maintain the activity of catalyst.
In a particular embodiment, CO can be substituted with other carbon sources.
A piece of fin is respectively installed on four angles of nine grids type reactor top, on the one hand they can cause periphery
Caused CO after flame combustion2Gas streams, so as to caused CO after being burnt with flame of centre2Gas converges, and makes a large amount of
CO2Gas encirclement prepares reaction channel top, hinders the entrance of oxygen, so as to form the environment of relatively hypoxia, reduces and prepares instead
The flame temperature on passage top is answered, the CNT for preventing from preparing is burned off, and is favorably improved the yield of CNT；The opposing party
Face promotes external flame backflow, with overheavy firing, improves the utilization rate of fuel gas, saves fuel.
In the present invention, the temperature that carbon atom dissociation reaction area is prepared with CNT needed for reaction zone is higher, can not make
Measured with general thermometer.Simultaneously, it is contemplated that the factor of accuracy of measurement, therefore select high-precision thermocouple with it is other non-
Contact tehermometer carrys out measurement temperature.
Flame reactor provided by the invention can with continuous producing carbon nano-tube, and with cost is low, yield is high, equipment with
The advantages of operating method is simple.
Brief description of the drawings
Fig. 1 is the top view of nine grids type reactor；
Fig. 2 is the 3D schematic diagrames (lateral to overlook) of nine grids type reactor；
Fig. 3 is the 3D schematic diagrames (laterally looking up) of nine grids type reactor；
Label in figure：1- external flame passages, 2- flame of centre passages, 3- prepare reaction channel, 4- fins, 5- nine grids
Flame reactor, the input of 6- reacting gas, the input of 7- flame fuels.
Embodiment
The present invention is described further with specific embodiment below in conjunction with the accompanying drawings.
Fig. 1 show a kind of nine grids flame reactor for preparing CNT, and the agent structure of reactor is symmetrical, transversal
Face is shaped as nine grids；What it is positioned at centre grid is flame of centre passage, on four angles be four it is identical and
The external flame passage being centrosymmetric；Between every two adjacent external flame passages, be disposed with four it is identical and be in
It is centrosymmetric to prepare reaction channel.
From Fig. 2, Fig. 3, flame of centre passage is logical with being respectively positioned on preparation reaction at the upper end outlet of external flame passage
5%~50% part of road height, and passage of flame and the relative altitude for preparing between reaction channel can be carried out as needed
Adjustment.And a piece of fin is respectively installed on four angles of reactor top.
The method that CNT is prepared using system as described above：Acetylene is outer from flame of centre passage and four with air
The lower end input of passage of flame is enclosed, is ignited at upper end outlet, forms flame of centre and external flame straight up；CO、
H2Inputted with He from four lower ends for preparing reaction channel, H2And the remaining CO not reacted completely is ignited at upper end outlet；
Under the effect of the dual-heated of flame of centre and external flame, CO chemically reacts preparing in reaction channel, decomposes before this
Go out substantial amounts of carbon atom, after then carbon atom undergoes a succession of complicated process, separated out simultaneously on the surface of active catalyst particles
Graphitization, and then nucleating growth is CNT；The process that carbon-source gas decomposite substantial amounts of carbon atom is preparing reaction channel
Lower half carry out, carbon atom is combined into the process of CNT and carried out in the first half for preparing reaction channel.
The temperature of reaction zone is prepared with CNT to measure carbon atom dissociation reaction area using contactless thermometer.Adopt
The mass flow of gas is measured and controlled with gas mass flow controller, and by supporting read out instrument come
Observation and the mass flow of record gas.For the CNT prepared, sampling mode is：Reacted by sampling substrate from preparation
The upper end outlet of passage is nearby sampled, or sample probe is stretched into the inside sampling for preparing reaction channel.
Claims (9)
1. a kind of system for preparing CNT, it is characterised in that the system is nine grids flame reactor (5), reactor
Agent structure it is symmetrical, shape of cross section is nine grids；What it is positioned at centre grid is flame of centre passage (2), positioned at four
On angle is four external flame passages (1) that are identical and being centrosymmetric；Every two adjacent external flame passages (1)
Between, it is disposed with that four are identical and what is be centrosymmetric prepares reaction channel (3)；Flame of centre passage (2) and periphery fire
Be respectively positioned at the upper end outlet of flame passage (1) prepare reaction channel (3) height 5%~50% part, and passage of flame with
The relative altitude prepared between reaction channel (3) can be adjusted as needed.
2. a kind of system for preparing CNT according to claim 1, it is characterised in that at four of reactor top
A piece of fin (4) is respectively installed on angle.
3. the method for preparing CNT using the system described in claim any one of 1-2, it is characterised in that fuel gas with
Air is ignited at upper end outlet, formed from the lower end input of flame of centre passage (2) and four external flame passages (1)
Flame of centre and external flame straight up；
Reacting gas prepares the lower end input of reaction channel (3) from four, the remaining carbon-source gas that do not react completely and it is other can
The reacting gas of combustion is ignited at upper end outlet；Under the effect of the dual-heated of flame of centre and external flame, reacting gas
In carbon-source gas chemically react in reaction channel (3) preparing, decomposite substantial amounts of carbon atom before this, then carbon atom
After undergoing a succession of complicated process, simultaneously graphitization, and then nucleating growth is received for carbon is separated out on the surface of active catalyst particles
Mitron；
The process that carbon-source gas decomposite substantial amounts of carbon atom is carried out in the lower half for preparing reaction channel (3), and carbon atom combines
Carried out for the process of CNT in the first half for preparing reaction channel (3).
4. according to the method for claim 3, it is characterised in that the fuel gas is acetylene.
5. according to the method for claim 3, it is characterised in that the reacting gas is CO, H2And He, wherein CO are described
Carbon-source gas, H2For flammable reacting gas.
6. according to the method for claim 3, it is characterised in that it is anti-that carbon atom dissociation is measured using contactless thermometer
Area is answered to prepare the temperature of reaction zone with CNT.
7. according to the method for claim 6, it is characterised in that the contactless thermometer is thermocouple.
8. according to the method for claim 3, it is characterised in that the quality stream using gas mass flow controller to gas
Amount is measured and controlled, and by supporting read out instrument come the mass flow observing and record gas.
9. according to the method for claim 3, it is characterised in that for the CNT prepared, sampling mode is：By taking
Sample substrate is nearby sampled from the upper end outlet for preparing reaction channel (3), or sample probe is stretched into and prepares the interior of reaction channel (3)
Portion samples.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610561905.5A CN106276846B (en) | 2016-07-15 | 2016-07-15 | A kind of system and method for preparing CNT |
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| CN201610561905.5A CN106276846B (en) | 2016-07-15 | 2016-07-15 | A kind of system and method for preparing CNT |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP1102298A1 (en) * | 1999-11-05 | 2001-05-23 | Iljin Nanotech Co., Ltd. | Field emission display device using vertically-aligned carbon nanotubes and manufacturing method thereof |
| CN1093507C (en) * | 2001-07-22 | 2002-10-30 | 太原理工大学 | Preparation of carbon nanometer pipe material and its equipment |
| CN1284726C (en) * | 2002-04-29 | 2006-11-15 | 中国科学院成都有机化学研究所 | Reaction unit and process of continuous preparation of carbon nano-tube |
| CN2632063Y (en) * | 2003-07-04 | 2004-08-11 | 上海扬泽纳米新材料有限公司 | Electrode device for producing carbon nanometer tube by arc process |
| CN2666887Y (en) * | 2003-10-28 | 2004-12-29 | 黄德欢 | Apparatus for continuous producing carbon nano-tube |
| KR100682863B1 (en) * | 2005-02-19 | 2007-02-15 | 삼성에스디아이 주식회사 | Carbon nanotube structure and fabricating method thereof, and field emission device using the carbon nanotube structure and fabricating method thereof |
| CN100344532C (en) * | 2005-03-25 | 2007-10-24 | 清华大学 | Carbon nanotube array growing device |
| CN100376478C (en) * | 2005-04-22 | 2008-03-26 | 清华大学 | Apparatus for preparing carbon nano tube array structure |
| CN100418876C (en) * | 2005-08-19 | 2008-09-17 | 清华大学 | Device and method for preparing array of Nano carbon tube |
| CN100482584C (en) * | 2005-10-21 | 2009-04-29 | 鸿富锦精密工业（深圳）有限公司 | Carbon nanotube preparation apparatus |
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