CN104843666B - A kind of device for growing carbon nanotube aerogel - Google Patents
A kind of device for growing carbon nanotube aerogel Download PDFInfo
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- CN104843666B CN104843666B CN201510150150.5A CN201510150150A CN104843666B CN 104843666 B CN104843666 B CN 104843666B CN 201510150150 A CN201510150150 A CN 201510150150A CN 104843666 B CN104843666 B CN 104843666B
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Abstract
Present invention is disclosed a kind of device for growing carbon nanotube aerogel, comprising: primary response chamber, it has an air inlet and the gas outlet being oppositely arranged with described air inlet；Collecting box, is connected with the gas outlet in primary response chamber；Wherein, at least one secondary response chamber connected with described primary response chamber also it is arranged with at described primary response intracavity, the described secondary response chamber air inlet near described primary response chamber is arranged, and the length in described secondary response chamber is less than the length in described primary response chamber in the axial direction in described primary response chamber.Compared with prior art, the present invention by solving the single reaction chamber drawback as reative cell growth CNT in primary response intracavity sheathed secondary response chamber, continuous print, uniform carbon nanotube aerogel can not only be grown, but also the productivity of carbon nanotube aerogel can be greatly improved by increasing reative cell caliber, save production cost, shorten the production time, make the industrialized production of carbon nanotube aerogel be possibly realized.
Description
Technical field
The present invention relates to nano material and manufacture field, particularly relate to a kind of device for growing carbon nanotube aerogel.
Background technology
CNT is the new construction form of the another kind of carbon found the beginning of the nineties after C60, nested for monolayer or Multi-layer graphite pipe, interior sky, a diameter of a few nanometer or the one-dimensional carbon structure form of tens nanometers, used after finding under high resolution electron microscopy from 1991, great research boom has just been caused in the whole world, as a kind of novel nano material, owing to the geometry of its uniqueness brings excellent mechanical performance with electronic band structure, electric property, thermal property and electromagnetic performance etc., the performance of these excellences makes CNT there is the most potential application advantage.As a kind of tridimensional network being made up of CNT, carbon nanotube aerogel can prepare carbon nano-tube macroscopic structure very easily by it, such as the macroscopical form of the relatively variforms such as thin film, thick film, block, macroscopic fibres, thus research carbon nanotube aerogel will have highly important promotion meaning to the application of CNT.The method preparing CNT at present mainly has: arc process, laser evaporization method, chemical vapour deposition technique.These three method the most all comparative maturities, can prepare single wall and multi-walled carbon nano-tubes.Chemical vapour deposition technique is because equipment is simple, most probable realizes industrialized production and becomes and study to obtain widest synthetic method at present.The method using chemical vapour deposition technique growth carbon nanotube aerogel at present mainly uses an independent quartz ampoule or alundum tube as reative cell, then with noble gas or reducing gas, also or both mixed gas, the high temperature reaction zone high-temperature catalytic cracking growth that reactant liquor is brought into reative cell obtains.
Growth carbon nanotube aerogel all uses single alundum tube or quartz ampoule growth at present, and production capacity is low with seriality, in terms of improving production capacity and seriality, use increase caliber and the method for tube length at present, also or the method using more expensive catalyst instead, complex process and relatively costly.
Summary of the invention
It is an object of the invention to provide a kind of device for growing carbon nanotube aerogel that can solve above-mentioned technical problem.
Wherein, the device being used for growing carbon nanotube aerogel includes:
Primary response chamber, it has an air inlet and the gas outlet being oppositely arranged with described air inlet；
Collecting box, is connected with the gas outlet in described primary response chamber；
Described primary response chamber is used for being catalyzed generation carbon nanotube aerogel, be provided with the collection device spinning axle and spinning on axle described in being arranged in described collecting box, described in spin axle and can drivingly be rotated so that the carbon nanotube aerogel that the catalysis of described primary response intracavity generates is wound on described collection device；
Wherein, at least one secondary response chamber connected with described primary response chamber also it is arranged with at described primary response intracavity, the described secondary response chamber air inlet near described primary response chamber is arranged, and the length in described secondary response chamber is less than the length in described primary response chamber in the axial direction in described primary response chamber.
As a further improvement on the present invention, the described device for growing carbon nanotube aerogel is included in the most sheathed multiple secondary response chambeies in described primary response chamber, and be arranged in multiple secondary response chambeies the most from inside to outside in described primary response chamber, described primary response chamber axially on length and be gradually increased at primary response chamber sectional area radially.
As a further improvement on the present invention, arbitrary secondary response chamber is coated with fully up at described primary response chamber axle and arranges in the inner and adjacent secondary response chamber.
As a further improvement on the present invention, described primary response chamber and described secondary response chamber are tubulose, described primary response chamber and described secondary response chamber and are coaxially disposed.
As a further improvement on the present invention, the concordant setting of air inlet in the one end in described secondary response chamber and described primary response chamber.
As a further improvement on the present invention, there is space between described primary response chamber and described secondary response chamber, described space uses heat-preservation cotton to fill.
As a further improvement on the present invention, described primary response chamber overcoat horizontal electric resistance furnace.
As a further improvement on the present invention, the material in described primary response chamber and described secondary response chamber is corundum or quartzy or mullite.
As a further improvement on the present invention, the described device for growing carbon nanotube aerogel also includes injection device, described injection device one in syringe pump, liquid ejector, ultrasonic atomizatio injection device.
As a further improvement on the present invention, between described injection device and described primary response chamber, carbon source inlet and carrier gas inlet it are additionally provided with.
Compared with prior art, the present invention by solving the single reaction chamber drawback as reative cell growth CNT in primary response intracavity sheathed secondary response chamber, continuous print, uniform carbon nanotube aerogel can not only be grown, but also the productivity of carbon nanotube aerogel can be greatly improved by increasing reative cell caliber, save production cost, shorten the production time, make the industrialized production of carbon nanotube aerogel be possibly realized.
Accompanying drawing explanation
Fig. 1 is for growing the structural representation of the device of carbon nanotube aerogel in an embodiment of the present invention.
Fig. 2 is for growing the stereoscan photograph of carbon nanotube aerogel macroscopic view continuum prepared by the device of carbon nanotube aerogel in an embodiment of the present invention.
Detailed description of the invention
Describe the present invention below with reference to detailed description of the invention shown in the drawings.But these embodiments are not limiting as the present invention, structure, method or conversion functionally that those of ordinary skill in the art is made according to these embodiments are all contained in protection scope of the present invention.
It should be understood that used herein such as " on ", " top ", D score, the representation space such as " lower section " be in order at relative to the term of position be easy to descriptive purpose describe as shown in the drawings a unit or feature relative to another unit or the relation of feature.The term of relative space position can be intended to the different azimuth including equipment in using or working in addition to orientation shown in figure.
Although also, it should be understood that term primary and secondary etc. can be used for describing various element or structure in this article, but these are described object and should not be limited by these terms.These terms are only used for these description object is distinguished from each other out.Such as, primary response chamber can be referred to as secondary response chamber, and secondary response chamber can also be referred to as primary response chamber similarly, and this is without departing from the protection domain of the application.
Ginseng Fig. 1, introduces a detailed description of the invention of the device 100 for growing carbon nanotube aerogel of the present invention.For growing collecting box 20 and the injection device 50 that the device 100 of carbon nanotube aerogel includes that a primary response chamber 11 connects with primary response chamber 11, wherein, primary response chamber 11 includes an air inlet 111 and the gas outlet 112 being oppositely arranged with air inlet 111, and collecting box 20 is connected with the gas outlet 112 in primary response chamber 11.
At the air inlet 111 in primary response chamber 11, at least one secondary response chamber 12 connected with primary response chamber 11 also it is arranged with in primary response chamber 11, and primary response chamber 11 axial last time reaction chamber 12 length less than the length in primary response chamber 11, primary response chamber 11 constitutes telescopic composite reaction chamber 10 together with secondary response chamber 12.
In the present invention, the most sheathed multiple secondary response chambeies 12 in primary response chamber 11, and be arranged in multiple secondary response chambeies the most from inside to outside in primary response chamber 11, primary response chamber 11 axially on length and be gradually increased at primary response chamber 11 sectional area radially.It should be noted that the word expressing position and direction described in the present invention, being all using the axis in primary response chamber 11 as reference, be interior near one end of the axis in primary response chamber 11, the one end away from the axis in primary response chamber 11 is outward.Arbitrary secondary response chamber is coated with fully up at primary response chamber 11 axle and arranges in the inner and adjacent secondary response chamber.Multiple secondary response chambeies 12 are close to the air inlet 111 in primary response chamber 11 and arrange, on from air inlet 111 to the direction of gas outlet 112, each reaction chamber in telescopic composite reaction chamber 10 length in the axial direction in primary response chamber 11 is gradually increased, and in primary response chamber 11, area of section radially is gradually increased each reaction chamber.I.e., the length in multiple secondary response chambeies and its area of section diametrically are different from, big secondary response chamber can be set in outside little secondary response chamber, multiple little secondary response chambeies in the way of sleeve in be enclosed within primary response chamber 11, it is structure in layer from inside to outside, the telescopic composite reaction chamber 10 combined is put into the burner hearth of horizontal electric resistance furnace 30.So design is advantageous in that, solve single employing pipe with small pipe diameter or the Large Diameter Pipeline drawback as reative cell, the alundum tube of pipe with small pipe diameter at the leading portion inner sleeve certain length of the alundum tube of Large Diameter Pipeline solves gas problem of air turbulence when entering reaction chamber, ensure that the carbon source reactant liquor after vaporization can be continuously, it is carried along into high temperature reaction zone equably by carrier gas, simultaneously because reacting gas can be relatively uniform after being stablized by the alundum tube of this section of pipe with small pipe diameter, mild enters into high temperature reaction zone, reacting gas is enable to be evenly distributed in whole high temperature reaction zone, metallic catalyst is easier to be reduced, it is thus possible to grow the higher CNT of degree of crystallinity, therefore, reative cell front end inner sleeve pipe with small pipe diameter alundum tube can not only play the effect of steady air flow, and the quality of grown CNT can also be improved.Reactant liquor high temperature reaction zone of entrance Large Diameter Pipeline under the carrying of carrier gas after vaporization, reactant liquor cracks in this region, simultaneously because caliber increases, the area not only making catalytic pyrolysis carbon source increases, growth efficiency improves, and owing to the air-flow in course of reaction is unobstructed, enables carbon nanotube aerogel to be moved out of reaction chamber smoothly, it is not easily blocked reaction chamber so that the seriality that growth is collected is greatly enhanced.
Preferably, primary response chamber 11 and secondary response chamber 12 are tubulose, and both materials are corundum or quartz or mullite, and primary response chamber 11 and each secondary response chamber 12 are all coaxially disposed to ensure that carbon source reactant liquor and carrier gas stream pass through.Especially, the concordant setting of air inlet 111 in the one end in secondary response chamber 12 and primary response chamber 11.
In the present embodiment, the alundum tube of a piece 60 × 350mm can be enclosed within 120 × 1400mm alundum tube, wherein 120 × 1400mm alundum tube is decided reaction chamber, the alundum tube of 60 × 350mm does secondary response chamber, space heat-preservation cotton between two pipes is filled, ensure that the center of circle of two pipe cross sections overlaps, then, the telescopic composite reaction chamber 10 combined is put into the burner hearth of horizontal electric resistance furnace 30, one end flange 60 of primary response chamber 11 air inlet 111 seals, gas outlet 112 connects with collecting box 20, completes to grow the installation of carbon nanotube aerogel device 100.Certainly, in other embodiments of the present invention, each reaction chamber can also be other suitable shape.The size Selection of the alundum tube in primary response chamber 11 and secondary response chamber 12 can also be varied, it is nested together in can be selected for two alundum tubes of 40 × 350mm and 100 × 1400mm, also may select 40 × 350mm, 100 × 700mm, tri-alundum tubes of 150 × 1400mm are nested together in carrying out, to improve the productivity of carbon nanotube aerogel.
Injection device 50, is used for carbon source reactant liquor is injected telescopic composite reaction chamber 10, it is preferable that injection device 50 can use the one in syringe pump, liquid ejector or ultrasonic atomizatio injection device, and injection mode can use single tube or multitube series connection or side-by-side configuration.
Carbon source inlet 41 and carrier gas inlet 42 it is additionally provided with, it is preferable that carbon source inlet 41 and carrier gas inlet 42 use stainless-steel pipe to make between injection device 50 and telescopic composite reaction chamber 10.Carbon source reactant liquor is injected in telescopic composite reaction chamber 10 by injection device 50 by carbon source inlet 41.Especially, at carrier gas inlet 42, it is additionally provided with mass-flow gas meter (not shown), is used for controlling to be passed through to telescopic composite reaction chamber 10 flow of carrier gas.
Collecting box 20, including a casing and be arranged in casing spin axle 21, the gas outlet 112 in primary response chamber 11 connects with a sidewall of the casing of collecting box 20.Preferably, casing is provided with air seal set (not shown), gas outlet (not shown) and observation window (not shown).After carbon nanotube aerogel growth collection completes, open air seal set, be passed through protective gas, the gases such as the carbon-source gas in casing and carrier gas are carried out certain dilution, carbon nanotube aerogel is taken out from casing.Observation window person convenient to operate observes the collection situation of box house carbon nanotube aerogel.
Spinning axle 21 is to hang in collecting box 20 by a mechanical arm (not shown), specifically, mechanical arm one end is fixing with the inner roof wall of collecting box 20 casing to be connected, the other end with spin that axle 21 is fixing to be connected, spin axle 21 be by a motor (not shown) drive and around himself axis rotate, the outside of casing 21 is located at by this motor.
As preferred embodiment, spinning and be additionally provided with collection device (not shown) on axle 21, this collection device is to be wrapped in the magnetic roller or magnetic track spun on axle 21, is used for being adsorbed onto on collection device carbon nanotube aerogel.It should be noted that magnetic roller here or magnetic track only need to can meet the collection needs of carbon nanotube aerogel with micromagnetism, and above-mentioned magnetic roller or magnetic track preferably employ and have resistance to chemical attack and resistant to elevated temperatures roller or crawler belt.
At this it is noted that collection device be arranged to can be controlled along spinning moving axially of axle 21, to realize the collection of the carbon nanotube aerogel to different in width.
The device utilizing above-mentioned growth carbon nanotube aerogel presented below prepares a specific embodiment of carbon nanotube aerogel.
S1, the preparation of carbon source reactant liquor
Choosing dehydrated alcohol as carbon source, add acetylferrocene as catalyst simultaneously in dehydrated alcohol, thiophene, as accelerator, is filtrated to get homogeneous, stable carbon source reactant liquor after ultrasonic one hour.Selected carbon source can also is that the one in methanol, ethanol, ethylene glycol, acetone, normal hexane, dimethylbenzene, it is also possible to being two kinds in above-mentioned substance or several mixture, at this, preferred dehydrated alcohol is as carbon source.Catalyst also can also is that 1,1-diethyl ferrocene, acetylferrocene, ferrocene, 1-(2-ethoxy) ferrocene, dicyclopentadienyl nickel, at this, preferred acetylferrocene is as catalyst, catalyst ratio shared by carbon source reactant liquor is in terms of the quality of ferrum element in catalyst, ferrum element accounts for the mass fraction of reactant liquor between 0.5%-1.0%, and the mass fraction of the carbon source reactant liquor that thiophene accounts for is between 1.0%-5.0%.
S2, the installation in telescopic composite reaction chamber
The present embodiment uses two alundum tube inner sleeves, forms telescopic composite reaction chamber in selecting the alundum tube of 60 × 350mm is enclosed within the alundum tube of 120 × 1400mm, and the alundum tube of 60 × 350mm does secondary response chamber, and the alundum tube of 120 × 1400mm is decided reaction chamber.
S3, the growth of carbon nanotube aerogel and collection
During carbon nanotube aerogel growth, if using pipe with small pipe diameter pipe to grow as reaction chamber, being primarily present the defect of following three aspects, one is due to catalysis limited area, and carbon source lysis efficiency is low, and the growth efficiency causing carbon nanotube aerogel is low.Two is owing to the space of reative cell is the least, and air-flow is not smooth, causes the carbon nanotube aerogel of generation quickly can not be moved out of reative cell, and the angle chemically balanced is said, also counteracts that the generating rate of carbon nanotube aerogel.Three be horizontal reacting chamber be horizontal positioned, cause the product horizontally entering into and generating can not arrive the mutually level other end in time and block, reaction is caused to interrupt, as needed restoration ecosystem, then require a great deal of time and growth parameter(s) be adjusted, the most not only need to take a significant amount of time, but also can because technique before and after discontinuous, the product grown has the difference of aspect of performance, and in follow-up utilization, product can be produced impact.
nullIf but using the pipe of Large Diameter Pipeline to grow as reaction chamber，The problem that the carbon source lysis efficiency that causes is low due to catalysis limited area can be solved，Thus improve carbon nanotube aerogel growth efficiency，Can also be that the product generated can be carried out reative cell by carrier gas rapidly，But，Carbon nanotube aerogel is passed through hydrogen in necessary for growth and carrys out reducing catalyst，It is passed through the noble gases such as argon to provide inert atmosphere，Above-mentioned gas also needs as carrier gas simultaneously，By uniform for the reactant liquor after vaporization、Stable carries to high temperature reaction zone，If using the pipe of Large Diameter Pipeline as reative cell，Then carrier gas can occur strong air turbulence in the moment entering reative cell，Not only can not smoothly the reactive component after vaporization be brought into the high temperature reaction zone reaction of reative cell，But also the gas phase stream of high temperature reaction zone can be caused also to get muddled，Cause the carbon nanotube aerogel cannot be continuous、Efficient growth，Thus，The carbon nanotube aerogel of continuous uniform cannot be collected at the port of export of reative cell.
In the present embodiment, using telescopic composite reaction chamber 10 to put into the burner hearth of horizontal electric resistance furnace 30, horizontal electric resistance furnace 30 uses resistance heating rod 31 to heat, and the temperature set point of horizontal electric resistance furnace is between 800 DEG C ~ 1600 DEG C.In the present embodiment, preferably by horizontal electric resistance furnace 30 temperature programming to 1300 DEG C.One end flange 60 of primary response chamber 11 air inlet 111 seals.First pass through carrier gas inlet 42 to be passed through a certain amount of argon and emptied with the air in collecting box 20 in telescopic composite reaction chamber 10, then, in telescopic composite reaction chamber 10, it is passed through hydrogen and argon by the control of mass-flow gas meter, after 20 minutes, in telescopic composite reaction chamber 10, carbon source reactant liquor is injected with 2ml/min by precise injection pump, after low-temperature space (the pipe with small pipe diameter alundum tube region) vaporization in front end, telescopic composite reaction chamber 10 of the carbon source reactant liquor, the high-temperature region catalytic cracking growth entering into primary response chamber 11 under the hydrogen the carrying with argon becomes carbon nanotube aerogel, and then the carbon nanotube aerogel generated can remove primary response chamber 11 under the carrying of air-flow together at gas outlet 112, spinning in collecting box 20 is collected on axle.In the reaction, reaction temperature can set according to CNT caliber, wall number or otherwise performance and requirement are done other, the set point of temperature is between 800 DEG C-1600 DEG C, and the injection rate of reactant liquor is injected between 0.2-7ml/min also dependent on being actually needed setting.
Driving is spun axle 21 and is rotated, in order to make the carbon nanotube aerogel of generation be wound on collection device.Owing to also remaining metallic catalyst on carbon nanotube aerogel, roller or the magnetic track absorption spinning magnetic on axle 21 can be wrapped in, spin axle 21 to be rotated by motor (not shown) driving, along with the rotation spinning axle 21, collection of being broken by carbon nanotube aerogel spins, defining carbon nanotube aerogel, its microscopic appearance is joined shown in Fig. 2.
After single collection completes, open air seal set, be passed through protective gas, preferably nitrogen, the carbon source raw material gas in collecting box 20 and carrier gas etc. are carried out certain dilution, carbon nanotube aerogel is taken out.Pass through said method, solve the single pipe drawback as reative cell growth CNT, the production productivity (collecting the quality of the carbon nanotube aerogel obtained in the unit interval) that can also make carbon nanotube aerogel brings up to more than 20 times of single alundum tube productivity, continuous acquisition time also extends to more than ten times of single alundum tube, this not only greatly reduces production cost and time cost, and provides a kind of feasible scheme for industrialized production.
It is to be understood that, although this specification is been described by according to embodiment, but the most each embodiment only comprises an independent technical scheme, this narrating mode of description is only for clarity sake, those skilled in the art should be using description as an entirety, technical scheme in each embodiment can also form, through appropriately combined, other embodiments that it will be appreciated by those skilled in the art that.
The a series of detailed description of those listed above is only for illustrating of the feasibility embodiment of the present invention; they also are not used to limit the scope of the invention, and all equivalent implementations or changes made without departing from skill of the present invention spirit should be included within the scope of the present invention.
Claims (10)
1. the device being used for growing carbon nanotube aerogel, it is characterised in that comprising:
Primary response chamber, it has an air inlet and the gas outlet being oppositely arranged with described air inlet；
Collecting box, is connected with the gas outlet in described primary response chamber；
Described primary response chamber is used for being catalyzed generation carbon nanotube aerogel, be provided with the collection device spinning axle and spinning on axle described in being arranged in described collecting box, described in spin axle and can drivingly be rotated so that the carbon nanotube aerogel that the catalysis of described primary response intracavity generates is wound on described collection device；
Wherein, at least one secondary response chamber connected with described primary response chamber also it is arranged with at described primary response intracavity, the described secondary response chamber air inlet near described primary response chamber is arranged, and the length in described secondary response chamber is less than the length in described primary response chamber in the axial direction in described primary response chamber.
Device for growing carbon nanotube aerogel the most according to claim 1, it is characterized in that, the described device for growing carbon nanotube aerogel is included in the most sheathed multiple secondary response chambeies in described primary response chamber, and be arranged in multiple secondary response chambeies the most from inside to outside in described primary response chamber, described primary response chamber axially on length and be gradually increased at primary response chamber sectional area radially.
Device for growing carbon nanotube aerogel the most according to claim 1, it is characterised in that arbitrary secondary response chamber is coated with fully up at described primary response chamber axle and arranges in the inner and adjacent secondary response chamber.
Device for growing carbon nanotube aerogel the most according to claim 1, it is characterised in that described primary response chamber and described secondary response chamber are tubulose, described primary response chamber and described secondary response chamber and are coaxially disposed.
Device for growing carbon nanotube aerogel the most according to claim 1, it is characterised in that the concordant setting of air inlet in the one end in described secondary response chamber and described primary response chamber.
Device for growing carbon nanotube aerogel the most according to claim 1, it is characterised in that there is space between described primary response chamber and described secondary response chamber, described space uses heat-preservation cotton to fill.
Device for growing carbon nanotube aerogel the most according to claim 1, it is characterised in that described primary response chamber overcoat horizontal electric resistance furnace.
Device for growing carbon nanotube aerogel the most according to claim 1, it is characterised in that the material in described primary response chamber and described secondary response chamber is corundum or quartzy or mullite.
Device for growing carbon nanotube aerogel the most according to claim 1, it is characterized in that, the described device for growing carbon nanotube aerogel also includes injection device, described injection device one in syringe pump, liquid ejector, ultrasonic atomizatio injection device.
Device for growing carbon nanotube aerogel the most according to claim 9, it is characterised in that be additionally provided with carbon source inlet and carrier gas inlet between described injection device and described primary response chamber.
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| CN111282763A (en) * | 2019-09-10 | 2020-06-16 | 沈健民 | Atomization device for carbon nanotube film production equipment |
| CN110937591B (en) * | 2019-11-08 | 2022-03-22 | 深圳烯湾科技有限公司 | Batch continuous production equipment for carbon nanotubes |
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| CN112251830B (en) * | 2020-10-22 | 2023-04-11 | 江西省纳米技术研究院 | Oriented carbon nanotube reinforced nylon composite material, and preparation method and application thereof |
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