CN103523768B - The apparatus and method that box sealing chemical gas phase reaction prepares continuous carbon nano-tube fibre - Google Patents
The apparatus and method that box sealing chemical gas phase reaction prepares continuous carbon nano-tube fibre Download PDFInfo
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- CN103523768B CN103523768B CN201310450490.0A CN201310450490A CN103523768B CN 103523768 B CN103523768 B CN 103523768B CN 201310450490 A CN201310450490 A CN 201310450490A CN 103523768 B CN103523768 B CN 103523768B
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Abstract
The present invention relates to the apparatus and method that box sealing chemical gas phase reaction prepares continuous carbon nano-tube fibre, described device includes high temperature chemical vapor reactor and to seal the casing of high temperature chemical vapor reactor.It is provided with the casing to move back and forth drawing screw mandrel and positioned at high temperature chemical vapor reactor and draw the spinning axle between screw mandrel to high temperature cvd reactor rear end.It the described method comprises the following steps：Reaction liquid enters catalytic pyrolysis reaction growth CNT in high temperature chemical vapor reactor, the CNT grown in gas phase stream assembles the backward high temperature chemical vapor reactor rear end movement to form aggregation in the gas phase, enter casing in the case where drawing screw mandrel draw after forming continuous carbon nano-tube aggregation, it is fine and close into being wound by spinning axle after fiber, continuous carbon nano-tube fibre is then made.Chemical gas phase reaction can be improved by, which being arranged such, prepares carbon nano-tube fibre stability of spinning process.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, more particularly to chemical gas phase reaction to prepare continuous carbon nano-tube fibre
The apparatus and method of dimension.
Background technology
CNT has unique one-dimensional nano structure and excellent electricity, calorifics and mechanical property, is made up of its assembling
The continuous fiber of macroscopic body have extensive potential application in fields such as technical fiber, function and service, bio-sensing and energy storages.
It is the committed step of realizing its numerous potential application that CNT is assembled into continuous carbon nano-tube fibre.
At present, preparing the method for carbon nano-tube fibre mainly has chemical gas phase reaction, array spinning and solution spinning processes.
It is that CNT directly is assembled into company in CNT building-up process that chemical gas phase reaction, which prepares continuous carbon nano-tube fibre,
Continuous aggregation, is one-step method, is expected to develop into continuous carbon nano-tube fibre prepare with scale, realizes the industry of carbon nano-tube fibre
Change.It is that continuous carbon nano-tube aggregation is first prepared in high-temperature reactor that chemical gas phase reaction, which prepares continuous carbon nano-tube fibre,
Carbon nanotube agglomerate is wound and handled in reactor back-end realization, its contraction is become carbon nano-tube fibre.Pyroreaction
Device rear end can pass through flange, gas or hydraulic seal chemical gas phase reaction system.
But flange seal chemical gas phase reaction difficulty realization prepares continuous carbon nano-tube fibre, spinning space and operability
It is all very poor.Air seal can provide big carbon nano-tube fibre spinning space, but carbon nanotube agglomerate prepared by gas phase reaction is non-
It is often light, it can be trembleed in the air-flow by being used to seal, cause CNT spinning unstable.Hydraulic seal and air seal class
Seemingly, it is possible to provide big carbon nano-tube fibre spinning space, but carbon nano-tube fibre from sealing liquid in pass through when and fluid friction,
Friction easily causes carbon nano-tube fibre and broken, and then make it that carbon nano-tube fibre spinning is unstable.
Therefore carbon nano-tube fibre spinning is prepared, it is necessary to be improved to prior art and carry out chemical gas phase reaction to be improved
Stability.
The content of the invention
It is an object of the invention to provide one kind carbon nano-tube fibre spinning stabilization is prepared to improve chemical gas phase reaction
The apparatus and method that the box sealing chemical gas phase reaction of property prepares continuous carbon nano-tube fibre.
For achieving the above object, the present invention provides a kind of box sealing chemical gas phase reaction and prepares continuous carbon nano-tube
The device of fiber, including with for reaction liquid, in the case where carrying airflow function, catalytic pyrolysis reaction grows the high temperature of carbon Micelle-like Nano-structure of Two
Cvd reactor and positioned at high temperature chemical vapor reactor rear end sealing the casing of high temperature chemical vapor reactor.
Further, it is provided with the casing and draws carbon nanometer to move back and forth to high temperature cvd reactor rear end
Aggregation draw screw mandrel and positioned at high temperature chemical vapor reactor and draw between screw mandrel winding carbon nano-tube fibre
Spin axle.
Further, the spinning axle is rotated or two-dimensional motion is wound to the carbon nano-tube fibre.
Further, it is provided with the casing to positioned at the carbon nanometer spun between axle and high temperature chemical vapor reactor
Pipe aggregation sprays the casing ultrasonic atomizer of organic liquid, and the organic liquid is ethanol, methanol, acetone, ethylene glycol or benzene
Organic liquid or several organic liquids mixing liquid.
Further, be additionally provided with liquid tank in the casing, be provided with the liquid tank to carbon nanotube agglomerate
The PVA aqueous solutions of contact, the xylene solution or ethanol liquid of Polycarbosilane.
Further, the present invention, which can also adopt the following technical scheme that, realizes the purpose of the present invention：
The present invention provides a kind of method that box sealing chemical gas phase reaction prepares continuous carbon nano-tube fibre, methods described
Comprise the following steps：Box sealing chemical gas phase reaction is provided and prepares continuous carbon nano-tube fibre device, described device includes height
Warm cvd reactor and positioned at high temperature chemical vapor reactor rear end sealing the case of high temperature chemical vapor reactor
Body, the casing is interior to draw screw mandrel and positioned at high temeperature chemistry gas provided with reciprocable to high temperature cvd reactor rear end
Phase reaction device and draw the spinning axle between screw mandrel, reaction liquid enters catalytic pyrolysis reaction growth carbon in high temperature chemical vapor reactor
Nanotube, the CNT are assembled to be formed after aggregation flows to high temperature chemical vapor reactor with carrier gas afterwards in the gas phase and moved
It is dynamic, form continuous carbon nano-tube aggregation, the carbon nanotube agglomerate enters casing in the case where drawing screw mandrel draw, densification into
Wound after fiber by spinning axle, continuous carbon nano-tube fibre is then made.
Further, high temperature chemical vapor reactor and spinning is provided with organic liquid to be atomized and to carbon nanometer between axle
The casing ultrasonic atomizer of pipe aggregation injection, carbon nanotube agglomerate run into the organic liquid of the atomization before spinning axle is reached
Densification is into fiber, and described ultrasonic atomizatio fluid flow is 1-500ml/min, and the load air flow rate of the ultrasonic atomizatio is 0-
10L/min。
Further, spin carbon nanotube agglomerate described in axle rotation process and pass through macromolecular liquid, CNT aggregation
Body is shrunk to fiber, becomes carbon nano tube composite fibre.
Further, spin axle and two-dimensional motion is rotated or carried out under motor driven, it is described to carbon nano-tube fibre spinning
Spinning speed is 2-100m/min.
The present invention provides the box sealing chemical gas phase reaction apparatus and method that prepare carbon nano-tube fibre, the casing with
High temperature chemical vapor reactor connects, there is provided and sufficiently large space provides the various processing of carbon nanotube agglomerate, containing drawing silk automatically,
Fine and close, compound and spinning etc. is handled.Casing causes carbon to receive in addition to sufficiently large space is provided for carbon nanotube agglomerate processing
Mitron aggregation, from external interference, and then realizes in processing procedure and stable prepares continuous carbon nano-tube fibre.
Brief description of the drawings
Fig. 1 is that the box sealing chemical gas phase reaction in the specific embodiment of the invention 1 prepares continuous carbon nano-tube fibre dress
The schematic diagram put；
Fig. 2 is that the box sealing chemical gas phase reaction in the specific embodiment of the invention 1 prepares continuous carbon nano-tube fibre dress
Put the scanning electron micrograph of obtained carbon nano-tube fibre；
Fig. 3 is that the box sealing chemical gas phase reaction of the specific embodiment of the invention 3 prepares continuous carbon nano-tube fibre device system
The sweep electron microscope photo of standby CNT/PVA composite fibres.
Embodiment
Below with reference to specific embodiment shown in the drawings, the present invention will be described in detail.What deserves to be explained is hereafter
Described embodiment is not intended to limit the present invention, structure that one of ordinary skill in the art is made according to these embodiments,
Method or conversion functionally are all contained in protection scope of the present invention.
The present invention provides a kind of casing 2 and seals the apparatus and method that chemical gas phase reaction prepares continuous carbon nano-tube fibre 6.
The device characteristic that the sealing of casing 2 chemical gas phase reaction prepares continuous carbon nano-tube fibre 6 is that high temperature chemical vapor reacts
The back-end sealing of device 1 is connected with the casing 2 being connected with high temperature chemical vapor reactor 1, and casing 2 provides enough large space realizations pair
The various processing of carbon nanotube agglomerate 5, and then obtain stabilization and prepare continuous carbon nano-tube fibre 6.
Described casing 2 can do the different shapes such as squarely, circle, ellipse, make chest material can be metal material,
The different materials such as fiberglass, plastics.The casing 2 provides enough large spaces, draws silk, densification, compound for carbon nanotube agglomerate 5
Operated with spinning etc..
It is described carbon nanotube agglomerate 5 is drawn in casing 2 silk be on casing 2 or rear end fix draw screw mandrel 21, draw silk
Bar 21 does front and rear reciprocating motion under conveyer belt 211 or motor power draw, can stretch into high temperature chemical vapor reactor 1
The lodgment of rear end carbon nanotube agglomerate 5, clings aggregation 5, back moves, and traction aggregation 5 enters in casing 2, reaches and turns
It is spun at dynamic spinning axle 22, realizes that it draws a function.The spinning axle 22 is connected with motor 221, and provides power by motor 221
Rotated or two-dimensional motion.
Described is to allow carbon nanotube agglomerate 5 to be punctured into carbon nanometer to 5 fine and close purpose of carbon nanotube agglomerate in casing 2
Pipe fiber 6.Fine and close continuous carbon nano-tube aggregation 5 has different methods, is included in going out for the rear end of high temperature chemical vapor reactor 1
Static housing ultrasonic atomizer 23 at mouthful, the casing ultrasonic atomizer 23 are included to the transfusion with providing organic liquid 235
Ultrasonic generator 231 that device is connected and the nozzle 232 of casing ultrasonic atomizer 23 being connected with casing 2, the infusion device
For the syringe 233 or other infusion devices being connected with infusion pump, in the present embodiment, the infusion device is syringe
233 and between syringe 233 and ultrasonic generator 231 conveying the infusion pipeline 234 of organic liquid 235.Institute
State ultrasonic generator 231 and be connected with carrier gas stream, organic liquid 235 forms fog or droplet by the atomization of casing ultrasonic atomizer 23
After enter in casing 2, fog or droplet run into the carbon nanotube agglomerate 5 drawn from high temperature chemical vapor reactor 1
So that carbon nanotube agglomerate 5 shrinks densification into carbon nano-tube fibre 6, wherein, the organic liquor of the casing ultrasonic atomizer 23
The flow of body 235 is 1-500ml/min, and the load air flow rate of the ultrasonic atomizatio is 0-10L/min；In addition, can also be from high temperature
The carbon nanotube agglomerate 5 drawn in cvd reactor 1 imposes sth. made by twisting processing, makes carbon nanotube agglomerate 5 in own rotation
It is lower fine and close into carbon nano-tube fibre 6；In addition, also carbon nanotube agglomerate 5 can be allowed to pass through and contact organic liquid 235, liquid hair
Thin power lures that it is fine and close into carbon nano-tube fibre 6 into, then realizes fine and close to carbon nanotube agglomerate 5.
It is compound to carbon nanotube agglomerate 5 in described casing 2 to refer to allow carbon nanotube agglomerate 5 to pass through and contact high score
Sub- liquid, realization prepare the composite of carbon nano-tube fibre 6 online.Lean on prepared by high temperature chemical vapor reactor 1 due to simple
The structure of carbon nanotube agglomerate 5 is very loose, so high polymer material easily enters between CNT, is arranged such, is easy to implement
The preparation of high-performance composite materials, solves the scattered problem of CNT.
Refer to the carbon nanotube agglomerate 5 to drawing the pull-out of screw mandrel 21 in described casing 2 to the spinning of carbon nanotube agglomerate 5
Carry out spinning winding, spinning speed 2-100m/min.
Various processing in described casing 2 to carbon nanotube agglomerate 5 can be combined with each other, for example, to CNT
Aggregation 5 draws silk and spinning；Silk, densification and spinning are drawn to carbon nanotube agglomerate 5；Draw silk, compound to carbon nanotube agglomerate 5
And spinning.
The method that the described sealing chemical gas phase reaction of casing 2 prepares continuous carbon nano-tube fibre 6 is that reaction liquid 4 is logical
Ejection of syringe pump is crossed into assisting ultrasonic atomizer 3 or is directly injected into high temperature chemical vapor reactor 1, reaction liquid 4 exists
Carry the reaction zone 13 for entering high temperature chemical vapor reactor 1 under airflow function, catalytic pyrolysis reaction growth CNT, gas phase stream
The CNT of middle growth assembles to form carbon nanotube agglomerate 5 in the gas phase, and carbon nanotube agglomerate 5 is with reaction gas flow to height
The movement of the warm rear end of cvd reactor 1, forms continuous carbon nano-tube aggregation 5, and carbon nanotube agglomerate 5 is led drawing screw mandrel 21
The effect of drawing is lower to enter casing 2, run into the fixation of the rear end of high temperature chemical vapor reactor 1 the atomization of casing ultrasonic atomizer 23 it is organic
The densification of body fluid body is wound into carbon nano-tube fibre 6, carbon nano-tube fibre 6 by the spinning axle 22 of axial rotation, and continuous carbon is then made
Nanotube fibers 6.
Specific embodiment 1
It refer to shown in Fig. 1, the device that the sealing of casing 2 chemical gas phase reaction prepares continuous carbon nano-tube fibre 6 contains
Two parts, first, pyroreaction prepares the equipment of carbon nanotube agglomerate 5, another part is casing 2 and carbon is received in casing 2
The equipment that mitron aggregation 5 is handled.In the present embodiment, high temperature chemical vapor consersion unit is prepared with ultrasonic atomizatio auxiliary
Continuous carbon nano-tube aggregation 5 it is similar, i.e. the high temperature chemical vapor reactor 1 is connected with assisting ultrasonic atomizer 3, institute
Stating high temperature chemical vapor reactor 1 includes reactor 11 and to heat the high-temperature heater 12 of the reactor 11, described
Assisting ultrasonic atomizer 3 includes the ultrasonic generator 31 and and high temperature to be connected with providing the infusion device of reaction liquid 4
The nozzle 311 of assisting ultrasonic atomizer 3 that cvd reactor 1 connects, the reactor 11 is in the nozzle of assisting ultrasonic atomizer 3
311 one end is additionally provided with to the gas-carrier pipeline 111 of the air-flow of 11 delivery of carrier gas of reactor 112.Described ultrasonic generator 31
There are two pipelines, be to convey the infusion pipeline 312 of reaction liquid 4, the infusion pipeline 312 into ultrasonic generator 31 all the way
It is connected with infusion device, reaction liquid 4 is inputted the mist of assisting ultrasonic atomizer 3 by infusion device by the infusion pipeline 312
It is melted into fog.Another way is to lead to the conveying air pipe 313 of conveying gas 32 into ultrasonic generator 31, in the work of conveying gas 32
The fog after atomization is dispelled with the lower nozzle 311 of assisting ultrasonic atomizer 3, high temeperature chemistry is input to after forming taper fog
In Gas-phase reactor 1.Described infusion device is the device being input to reaction liquid 4 in assisting ultrasonic atomizer 3, including defeated
Liquid pump and syringe 33, the syringe 33 be connected between infusion pump and ultrasonic generator 31 to ultrasonic generator
Input reaction liquid 4 in 31, the infusion device can be syringe pump etc. in other embodiments.Reaction liquid 4 is by auxiliary
Ultrasonic atomizer 3 is helped to enter formation carbon nanotube agglomerate 5 in high temperature chemical vapor reactor 1 after being atomized.High temeperature chemistry gas
The rear end of phase reaction device 1 is connected with casing 2 by flange, and the material for making casing 2 is metallic aluminium.The size of casing 2 is long 1600m,
High 400mm, wide 400mm.In order to handle carbon nanotube agglomerate 5, it is mounted with casing 2 to carbon nanotube agglomerate 5
Draw silk, densification and spinning components.Casing 2 away from be provided with the back outlet 600mm of high temperature chemical vapor reactor 1 draw screw mandrel 21 and
Conveyer belt, the screw mandrel 21 that draws are fixed on conveyer belt 211, and the conveyer belt 211, which moves to drive, to be drawn before and after screw mandrel 21 is done
Move back and forth, then realize and a function is drawn to carbon nanotube agglomerate 5.Carbon nanotube agglomerate 5 draw screw mandrel 21 act under from
The rear end of high temperature chemical vapor reactor 1 comes out, and is fixed in and exports casing ultrasound at 200mm away from high temperature chemical vapor reactor 1
The ethanol liquid densification of the nozzle 232 of atomizer 23 atomization is into carbon nano-tube fibre 6.Carbon nano-tube fibre 6 is drawn drawing screw mandrel 21
Under effect, reach at the spinning axle 22 away from the rear end 500mm of high temperature chemical vapor reactor 1, the spinning axle 22 being rotated is spun with 10m/min
Speed winding.As shown in Fig. 2 the scanning electron of the photo, i.e. carbon nano-tube fibre 6 of the carbon nano-tube fibre 6 is observed for SEM
Microphoto.The uniform diameter of carbon nano-tube fibre 6, it is 20um.Amplify SEM observation CNT macroscopic surfaces, between CNT
Tightly packed, CNT is distributed along fiber length direction, moreover it is possible to sees a small amount of particle.Transmission electron microscope observation carbon nanometer
Pipe fiber 6, is made up of double-walled carbon nano-tube, and double-walled carbon nano-tube diameter is mainly in 8-10nm, and double-walled carbon nano-tube is to restrain shape
Formula is present.
Specific embodiment 2
The device that the sealing of casing 2 chemical gas phase reaction prepares continuous carbon nano-tube fibre 6 is similar to Example 1, no
Be distance high-temperature cvd reactor 1 export 200mm ultrasonic atomizatios organic liquid 235 be methanol liquid, carbon is received
Mitron aggregation 5 runs into the densification of methanol fog and spins speed into carbon nano-tube fibre 6, carbon nano-tube fibre 6 with 50m/min and be wound into spinning
On axle 22, continuous carbon nano-tube fibre 6 is obtained.In other embodiments, the organic liquid 235 of the ultrasonic atomizatio can also be
One or more kinds of mixing liquids in ethanol, methanol, acetone, ethylene glycol, benzene or other small molecules.
Specific embodiment 3
The device that the sealing chemical gas phase reaction of casing 2 prepares continuous carbon nano-tube fibre 6 is similar to Example 1, different
It is to export fixed spinning axle 22 at 200mm in distance high-temperature cvd reactor 1, is additionally provided with casing 2 at spinning axle 22
Liquid tank, macromolecular liquid is filled in liquid tank, in the present embodiment, the macromolecular liquid is that 3wt.% PVA is water-based molten
Liquid, spin in the rotation process of axle 22 and pass through the PVA aqueous solution.Carbon nanotube agglomerate 5 enters in the case where drawing the draw of screw mandrel 21
In casing 2, by speckling with the spinning axle 22 of the PVA aqueous solution, carbon nanotube agglomerate 5 is shrunk to carbon nano-tube fibre 6, becomes carbon and receives
Mitron/PVA composite fibres, composite fibre spin fast spinning on axle 22 is spun with 15m/min.Received as shown in figure 3, observing carbon for SEM
The photo of mitron/PVA complex fiber materials, composite fibre uniform diameter, a diameter of 30um.Amplify SEM and observe micro- disconnection,
PVA macromolecules are penetrated into carbon nano-tube fibre 6, and carbon nano-tube bundle is separated.
Specific embodiment 4
The device that the sealing of casing 2 chemical gas phase reaction prepares continuous carbon nano-tube fibre 6 is similar to Example 1, no
Same is to export fixed spinning axle 22 at 200mm in distance high-temperature cvd reactor 1, is additionally provided with casing 2 positioned at spinning axle 22
The liquid tank at place, macromolecular liquid is filled in liquid tank, in the present embodiment, the macromolecular liquid is 50wt.% poly- carbon silicon
Alkane xylene solution, spin the xylene solution for passing through Polycarbosilane in the rotation process of axle 22.Carbon nanotube agglomerate 5 is drawing screw mandrel
Enter under 21 draws in casing 2, by being stained with the spinning axle 22 of the xylene solution for having Polycarbosilane, CNT aggregation
Body 5 is shrunk to fiber, becomes CNT/PCS composite fibres, and composite fibre spins fast spinning on axle 22 is spun with 5m/min.SEM
CNT/PCS complex fiber materials are observed, PCS macromolecules penetrate into carbon nano-tube fibre 6, carbon nano-tube bundle is separated.
Specific embodiment 5
The device that the sealing of casing 2 chemical gas phase reaction prepares continuous carbon nano-tube fibre 6 is similar to Example 3, no
Same is not provided with casing ultrasonic atomizer 23, but is filled in distance high-temperature cvd reactor 1 exports 200mm liquid tanks
The organic liquid, it is in the present embodiment ethanol liquid.Carbon nanotube agglomerate 5 is in the case where drawing screw mandrel 21 and acting on from high temperature
The spinning axle 22 away from the rear end 500mm of high temperature chemical vapor reactor 1 is directly reached after learning the rear end of Gas-phase reactor 1 out.Spin axle 22
Pass through ethanol liquid in rotation process.Carbon nanotube agglomerate 5 is entering in casing 2 under drawing the draw of screw mandrel 21, by being stained with
There is the spinning axle 22 of ethanol, carbon nanotube agglomerate 5 is shrunk to fiber, becomes carbon nano-tube fibre 6.SEM observation CNTs gather
The surface CNT distribution of collective 5, CNT are distributed along the length direction of aggregation 5, and the CNT of part is more than orientation carbon and received
Between mitron, CNT is connected into three-dimensional net structure.
Specific embodiment 6
The device that the sealing chemical gas phase reaction of casing 2 prepares continuous carbon nano-tube fibre 6 is similar to Example 1, different
It is to export 200mm without casing ultrasonic atomizer 23 in distance high-temperature cvd reactor 1, away from high temperature chemical vapor reactor 1
Have at the 500mm of rear end and spin axle 22, two-dimensional motion can be carried out simultaneously by spinning axle 22.That is, described spinning axle 22 can show CNT greatly and gather
Collective 5 is that axle center carries out rotation twisting.The two-dimensional motion twists carbon nanotube agglomerate 5, meanwhile, twisting densification is become
Fiber receive silk, then obtain carbon nano-tube fibre 6.
In summary, the case of the rear end connection sealing function of the equipment of carbon nanotube agglomerate 5 is prepared in high temperature chemical vapor
Body 2, the carbon nanotube agglomerate 5 prepared in casing 2 to high temperature chemical vapor reactor 1 carry out drawing silk, densification, compound and spinning
The different disposal of silk.The spinning process of casing 2 is completed in sealed environment, is not disturbed by extraneous environment, meanwhile,
Avoiding impurity particle in air influences carbon nano-tube fibre 6, in addition, with the fine and close mistake of carbon nanotube agglomerate 5 of organic liquid 235
It is to be carried out in casing 2 in journey, avoids and air contact, improves the stability of processing carbon nanotube agglomerate 5, therefore,
Methods described is adapted to development scale to prepare continuous carbon nano-tube fibre 6.
It should be appreciated that although the present specification is described in terms of embodiments, not each embodiment only includes one
Individual independent technical scheme, this narrating mode of specification is only that those skilled in the art will should say for clarity
For bright book as an entirety, the technical scheme in each embodiment may also be suitably combined to form those skilled in the art can
With the other embodiment of understanding.
Those listed above is a series of to be described in detail only for feasibility embodiment of the invention specifically
Bright, they simultaneously are not used to limit the scope of the invention, all equivalent implementations made without departing from skill spirit of the present invention
Or change should be included in the scope of the protection.
Claims (8)
1. a kind of box sealing chemical gas phase reaction prepares the device of continuous carbon nano-tube fibre, it is characterised in that：Including to
For reaction liquid in the case where carrying airflow function catalytic pyrolysis reaction growth carbon Micelle-like Nano-structure of Two high temperature chemical vapor reactor and
Be provided with positioned at high temperature chemical vapor reactor rear end to seal the casing of high temperature chemical vapor reactor, in the casing to
Move back and forth to high temperature cvd reactor rear end traction carbon Micelle-like Nano-structure of Two and draw screw mandrel and positioned at high temperature chemical vapor
Reactor and draw to wind the spinning axle of carbon nano-tube fibre between screw mandrel, the box sealing chemical gas phase reaction prepares continuous
The device of carbon nano-tube fibre also includes the assisting ultrasonic atomizer being connected with the high temperature chemical vapor reactor other end, described
High temperature chemical vapor reactor includes reactor and to heat the high-temperature heater of the reactor, the assisting ultrasonic mist
Change device to react including the ultrasonic generator with the infusion device of offer reaction liquid to be connected and with high temperature chemical vapor
The ultrasonic atomizer nozzle of device connection, reaction liquid enter high temperature chemical vapor reaction after the atomization of assisting ultrasonic atomizer
The carbon Micelle-like Nano-structure of Two is formed in device.
2. box sealing chemical gas phase reaction according to claim 1 prepares the device of continuous carbon nano-tube fibre, it is special
Sign is：The spinning axle is rotated or two-dimensional motion carries out spinning to the carbon nano-tube fibre.
3. box sealing chemical gas phase reaction according to claim 1 prepares the device of continuous carbon nano-tube fibre, it is special
Sign is：It is provided with the casing to be sprayed to positioned at the carbon nanotube agglomerate spun between axle and high temperature chemical vapor reactor
The casing ultrasonic atomizer of organic liquid is penetrated, the organic liquid is the organic liquid of ethanol, methanol, acetone, ethylene glycol or benzene
Or the mixing liquid of several organic liquids.
4. box sealing chemical gas phase reaction according to claim 1 prepares the device of continuous carbon nano-tube fibre, it is special
Sign is：Liquid tank is additionally provided with the casing, the PVA water to be contacted with carbon nanotube agglomerate is provided with the liquid tank
Property solution, the xylene solution of Polycarbosilane or ethanol liquid.
5. a kind of method that box sealing chemical gas phase reaction prepares continuous carbon nano-tube fibre, it is characterised in that：Methods described
Comprise the following steps：Box sealing chemical gas phase reaction is provided and prepares continuous carbon nano-tube fibre device, described device includes height
Warm cvd reactor and positioned at high temperature chemical vapor reactor rear end sealing the case of high temperature chemical vapor reactor
Body, the casing is interior to draw screw mandrel and positioned at high temeperature chemistry gas provided with reciprocable to high temperature cvd reactor rear end
Phase reaction device and draw the spinning axle between screw mandrel, reaction liquid enters catalytic pyrolysis reaction growth carbon in high temperature chemical vapor reactor
Nanotube, the CNT are assembled to be formed after aggregation flows to high temperature chemical vapor reactor with carrier gas afterwards in the gas phase and moved
It is dynamic, form continuous carbon nano-tube aggregation, the carbon nanotube agglomerate enter in the case where drawing screw mandrel draw casing densification into
Wound after fiber by spinning axle, continuous carbon nano-tube fibre is then made.
6. the method that box sealing chemical gas phase reaction according to claim 5 prepares continuous carbon nano-tube fibre, it is special
Sign is：It is provided between high temperature chemical vapor reactor and spinning axle to be atomized organic liquid and be sprayed to carbon nanotube agglomerate
The casing ultrasonic atomizer penetrated, carbon nanotube agglomerate reach spin axle before run into the organic liquid densification of the atomization into fibre
Dimension, described ultrasonic atomizatio fluid flow is 1-500ml/min, and the load air flow rate of the ultrasonic atomizatio is 0-10L/min.
7. the method that box sealing chemical gas phase reaction according to claim 5 prepares continuous carbon nano-tube fibre, it is special
Sign is：Spin carbon nanotube agglomerate described in axle rotation process and pass through macromolecular liquid, carbon nanotube agglomerate is shrunk to fibre
Dimension, becomes carbon nano tube composite fibre.
8. the method that box sealing chemical gas phase reaction according to claim 5 prepares continuous carbon nano-tube fibre, it is special
Sign is：Spinning axle rotates or carried out under motor driven two-dimensional motion and is to carbon nano-tube fibre spinning, described spinning speed
2-100m/min。
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| CN103922313B (en) * | 2014-04-24 | 2016-03-02 | 苏州捷迪纳米科技有限公司 | Sponge state carbon nanotube gas phase collection device and method |
| CN107057278B (en) * | 2016-11-25 | 2023-07-14 | 深圳前海量子翼纳米碳科技有限公司 | Preparation device and preparation method for preparing carbon nano tube film composite material in one step |
| CN107473203B (en) * | 2017-08-10 | 2020-03-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method and device for continuously preparing carbon nano tube composite film or fiber |
| KR101987337B1 (en) * | 2018-03-21 | 2019-06-10 | 주식회사 제이오 | Carbon nanotube fiber and apparatus for manufacturing the carbon nanotube fiber |
| CN110592726B (en) * | 2019-10-08 | 2022-02-15 | 常州大学 | Method and device for preparing continuous carbon nanotube fibers by CVD method |
| CN112289983B (en) * | 2020-09-18 | 2022-09-06 | 合肥国轩高科动力能源有限公司 | SiO (silicon dioxide) x -MWCNTs/C core-shell composite anode material and preparation method and application thereof |
| CN114572765B (en) * | 2022-02-23 | 2023-11-21 | 武汉市碳翁科技有限公司 | Carbon nano tube twisting and collecting device and using method |
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| KR100376202B1 (en) * | 2000-10-02 | 2003-03-15 | 일진나노텍 주식회사 | Apparatus of vapor phase-synthesis for carbon nanotubes or carbon nanofibers and synthesizing method of using the same |
| WO2006073017A1 (en) * | 2005-01-05 | 2006-07-13 | Dialight Japan Co., Ltd. | Apparatus for manufacturing carbon film by plasma cvd, method for manufacturing the same, and carbon film |
| CN100552105C (en) * | 2007-09-04 | 2009-10-21 | 天津大学 | Apparatus and method for preparing continuous carbon nanotube fibers by catalytic reaction of liquid-enclosed gas phase flow |
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