CN104671230A - Continuous collecting method of single-walled carbon nanotube film and special device - Google Patents
Continuous collecting method of single-walled carbon nanotube film and special device Download PDFInfo
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Abstract
The invention relates to a controllable uniform collecting technology of a single-walled carbon nanotube film and particularly relates to a continuous collecting method of the single-walled carbon nanotube film growing by virtue of a floating catalyst method and a special device. A connect installation ball valve switch and a film collecting chamber are designed and connected to the tail end of a chemical vapor deposition carbon nanotube growth furnace. On the premise that any growing conditions are not changed, high quality single-walled carbon nanotube films are directly and continuously collected on the surfaces of various film substrates. The single-walled carbon nanotube films growing by virtue of the chemical vapor deposition method by using the floating catalyst under conditions of normal temperature and pressure are collected to the surfaces of various substrates. The single-walled carbon nanotube films which are in inch grade, controllable in density and uniform are continuously collected by regulating the deposition time and growing parameters. Therefore, the technical problems that the existing carbon nanotube film collecting process is poor in uniformity, small in draw ratio, limited in size and the like are solved.
Description
Technical field
The present invention relates to controlled, the uniform collection technology of single wall carbon nano-tube film, be specially continuous collection method and the special purpose device of the single wall carbon nano-tube film of a kind of floating catalytic agent method growth.
Background technology
Single Walled Carbon Nanotube, because of the electricity of its excellence, optics and mechanical characteristic, is suitable for preparing transparent conductive film and flexible thin-film transistor circuit etc.Single wall carbon nano-tube film electron device is expected to have broad application prospects in the field such as Electronic Paper, flexible battery, electronic tag, flexible and transparent display, even replacement silicon-based semiconductor material in future.
At present, the single wall carbon nano-tube film utilizing floating catalytic agent chemical gaseous phase depositing process to grow and to collect illustrates tempting photoelectric properties.[document 1, Sun DM, Timmermans MY, Tian Y, Nasibulin AG, Kauppinen EI, Kishimoto S, Mizutani T, OhnoY, NatureNanotechnology, 2011,6 (3) 156-161; Document 2, Sun DM, Timmermans MY, Kaskela A, Nasibulin AG, Kishimoto S, Mizutani T, Kauppinen EI, Ohno Y, Nature Communications, 2013,4:2302.].The collection device of its design is pin type filtering with microporous membrane collection device, and namely install syringe filter additional at the exhaust side of floating catalytic growing single-wall carbon nano tube device, the Single Walled Carbon Nanotube of generation goes out growing apparatus with carrier gas stream and is deposited on millipore filtration.Carbon nano-tube film on filter membrane can be transferred in substrates such as comprising plastics, glass, quartz, silicon chip and metal.[document 3, Nasibulin AG, Kaskela A, Mustonen K, Anisimov AS, Ruiz V, Kivsto S, Rackauskas S, Timmermans MY, Pudas, M, Aitchison B, Kauppinen M, Brown DP, Okhotnikov, OG, Kauppinen EI, ACS Nano, 2011,5 (4), 3214-3221].
The subject matter that the method exists at present is: (1) strainer to shrink and amplification can produce eddy current at inlet mouth and air outlet place caliber, affects Single Walled Carbon Nanotube and is uniformly distributed suprabasil; (2) substrate material is only limitted to porous membrane, needs to carry out corresponding transfer according to application, and can introduce the intrinsic performance of pollutant effect carbon nanotube in transfer process; (3) syringe filter is installed on vapor pipe, and distance Single Walled Carbon Nanotube growth room is far away, and this causes high-quality big L/D ratio Single Walled Carbon Nanotube to be easily attached on the wall of pipeline; And single length of tube in collected film is shorter, this dramatically increases the contact resistance between carbon nanotube, and then causes the performance such as carrier mobility, specific conductivity of constructed device to reduce.Thus, current subject matter how to shorten distance between collecting chamber and carbon nano tube growth room, avoids vortex phenomenon, realizes high length-diameter ratio, equally distributed single wall carbon nano-tube film is collected, to meet the demand of high quality, high-performance optical electrical part.
Summary of the invention
An object of the present invention is the continuous collection method and the special purpose device that provide a kind of high length-diameter ratio single wall carbon nano-tube film, overcomes Single Walled Carbon Nanotube length-to-diameter ratio this technical barrier little that floating current catalyst chemical gas phase deposition method is collected.
Two of object of the present invention is not subject to continuous collection method and the special purpose device of the single wall carbon nano-tube film of shapes of substrates, material restriction under being to provide a kind of normal temperature, normal pressure, overcome the problem that existing monolithic filter membrane collection method is confined to introduce in substrate kind and transfer process pollutent.
Three of object of the present invention be to provide a kind of evenly, the continuous collection method of the controlled single wall carbon nano-tube film of density and special purpose device, overcome the carbon nano-tube film skewness problem that current thin film collection method exists.
Technical scheme of the present invention is:
A kind of continuous collection method of single wall carbon nano-tube film, at chemical vapor carbon deposition nanotube growth stove tail end design and installation ball valve switch and film collecting chamber, under the prerequisite not changing any growth conditions, directly, continuously high quality carbon nano-tube film is collected, the collection of the single wall carbon nano-tube film that depositing time, flow rate of carrier gas realize evenly by regulating, thickness is controlled on various film substrate surface.
The film substrate of described single wall carbon nano-tube film continuously trapping system is unrestricted, film substrate is porous membrane, filter paper, PET class plastic-substrates, hard silicon chip or quartz plate, and the film collected is directly as the channel material of transparent conductive film, transparency electrode or photoelectric device thin film transistor.
The density of described single wall carbon nano-tube film is regulated and controled by collection time and flow rate of carrier gas, film transmittance uniform, controllable below 99%.
The special purpose device of the continuous collection method of described single wall carbon nano-tube film, this device comprises chemical vapor carbon deposition nanotube growth stove, film collecting chamber, vacuum pump, water-circulating cooling device, and concrete structure is as follows:
In chemical vapor carbon deposition nanotube growth stove, Single Walled Carbon Nanotube growth room is set, Single Walled Carbon Nanotube growth room is connected by supporting flange and flange switch seal with one end of ball valve switch, the other end of ball valve switch is tightly connected by one end of supporting flange and flange switch and film collecting chamber, and the other end of film collecting chamber is connected by supporting flange and flange switch seal with the one end in loop; Extend an air outlet at film collecting chamber rear portion and connect vacuum pump, vacuum pump is arranged vacuum pump air circuit breaker, the air-bleed system of vacuum pump is controlled by vacuum pump air circuit breaker, arranges film forming and collect stationary installation, film substrate in film collecting chamber; The other end in loop exports with the Single Walled Carbon Nanotube growth room of chemical vapor carbon deposition nanotube growth stove and carrier gas and communicates, Single Walled Carbon Nanotube and carrier gas outlet arranged outside water-circulating cooling device; Described loop is arranged T-valve, bypass air circuit breaker, two reduction of fractions to a common denominators of T-valve do not communicate with loop, and the threeway of T-valve is connected with air outlet.
Described film collecting chamber is even footpath pipe or reducing pipe, be provided with groove in its tube chamber to be used for placing film forming collection stationary installation, film forming collects stationary installation mobile position regulating film substrate to receive film in groove, and the compressing tablet that film substrate is collected in stationary installation by film forming is fixed.
Described ball valve switch, film collecting chamber respectively with the Single Walled Carbon Nanotube growth room in chemical vapor carbon deposition nanotube growth stove not reducing be connected.
The Single Walled Carbon Nanotube of synthesizing in described chemical vapor carbon deposition nanotube growth stove at the uniform velocity flow to film collecting chamber with carrier gas, and be deposited in prefabricated film substrate, when thickness reaches requirement, close ball valve switch, open T-valve, dismantle film forming collection stationary installation, change film substrate, open vacuum pump and drain air in device, open ball valve switch, by repeating above-mentioned steps, collect single wall carbon nano-tube film continuously.
The film collecting chamber of described Single Walled Carbon Nanotube is arranged on horizontal type or vertical chemical vapor deposition stove and carries out carbon nano-tube film collection.
Gas circuit conversion in described Single Walled Carbon Nanotube growth, collection process is realized by T-valve, invariablenes pressure of liquid in guarantee system.
Described film collecting chamber is connected with vacuum extractor, discharges the air entered from the external world because opening unit takes out substrate.
Design philosophy of the present invention is:
The Single Walled Carbon Nanotube of floating catalytic agent chemical Vapor deposition process synthesis, under the carrying of carrier gas, flows to collecting chamber by growth room, is deposited on film forming in substrate.The adjustment to substrate surface Single Walled Carbon Nanotube density is realized in suprabasil depositing time, airshed etc. by regulating carbon nanotube.Film is collected continuously and by ball-cock device and gas path three-way valve co-controlling, can be regulated air circuit breaker, can collect high-quality single wall carbon nano-tube film continuously not affecting realization under carbon nano tube growth parameter.Collecting chamber is arranged on Reaktionsofen tail end, can realize the collection of high length-diameter ratio Single Walled Carbon Nanotube.Substrate fixes film by draw-in groove design and collects substrate, and thus substrate material is unrestricted.There is water cooling plant between growth room and collecting chamber, ensure that the homo(io)thermism of collecting chamber.
Advantage of the present invention and beneficial effect are:
The continuous collection technique of the single wall carbon nano-tube film that 1, the present invention relates to and special purpose device, compared with the syringe filter subtraction unit generally adopted at present, can realize the direct formation of film at surface of more high quality, big L/D ratio Single Walled Carbon Nanotube.Selectivity is not had to deposition substrate, namely meaning substrate in office can deposit single wall carbon nano-tube film, collect in thin-film process and can not produce any impact to the atmosphere in Reaktionsofen, it is independent that the growth of bonding wall carbon nano tube and film collect two processes, and be independent of each other.
2, the quick detachable installation of apparatus of the present invention, adaptability is good, can be installed on vertical, the chemical vapor deposition stove that horizontal type etc. are dissimilar.The method overcome generally to adopt at present and chemically utilize syringe filter to collect carbon nanotube after extraction catheter in Reaktionsofen easily to produce air stream turbulence effect, cause the phenomenon that film is uneven, the high quality single wall carbon nano-tube film that the method obtains can meet the photoelectric device application demand of different field.
Accompanying drawing explanation
Fig. 1 is single wall carbon nano-tube film continuously trapping system schematic diagram.In figure, 1, chemical vapor carbon deposition nanotube growth stove; 2, Single Walled Carbon Nanotube growth room; 3, the carrier gas direction of airintake direction; 4, flange switch; 5, ball valve switch; 6, film forming collects stationary installation; 7, film substrate; 8, film collecting chamber; 9, flange switch; 10, loop; 11, vacuum pump; 12, vacuum pump air circuit breaker; 13, outgassing direction; 14, T-valve; 15, bypass air circuit breaker; 16, water-circulating cooling device.
Fig. 2 is the single wall carbon nano-tube film optical photograph collected on filter paper.
Fig. 3 is the single wall carbon nano-tube film optical photograph collected on millipore filtration.
Fig. 4 is the single wall carbon nano-tube film optical photograph collected on aluminium foil.
Fig. 5 is the single wall carbon nano-tube film optical photograph that PET collects.
Fig. 6 is the typical scan electromicroscopic photograph of single wall carbon nano-tube film.In figure, (a) figure is the single wall carbon nano-tube film of transmittance 97%; B () figure is the single wall carbon nano-tube film of transmittance 92%.
Fig. 7 is the device that syringe filter collects single wall carbon nano-tube film.
Fig. 8 is the single wall carbon nano-tube film optical photograph that syringe filter is collected.
Fig. 9 is the single wall carbon nano-tube film stereoscan photograph that syringe filter is collected.
Embodiment
In a specific embodiment, the continuous collection method of single wall carbon nano-tube film of the present invention and special purpose device, at Single Walled Carbon Nanotube growth room tail end design and installation ball valve switch and the film collecting chamber of single wall carbon nano-tube film continuously trapping system, under the prerequisite not changing any growth conditions, directly, closely, continuously high quality carbon nano-tube film is collected, by the collection of the adjustment single wall carbon nano-tube film that depositing time, flow rate of carrier gas etc. can realize evenly, thickness is controlled at various substrate surface.
The substrate that single wall carbon nano-tube film is collected does not limit by material and shape, and substrate can be: porous membrane, filter paper, PET class plastic-substrates, and the substrate such as hard silicon chip, quartz plate.The film collected can directly as transparent conductive film, transparency electrode, or the channel material of photoelectric device thin film transistor.Thus, eliminate loaded down with trivial details transfer step, decrease contaminating impurity and defect introducing, the application demand of multiple photoelectric device can be met.
The density of single wall carbon nano-tube film regulates and controls by collection time and flow rate of carrier gas, film transmittance uniform, controllable below 99%; Owing to collecting in Reaktionsofen, air-flow is more stable, and single wall carbon nano-tube film has excellent homogeneity.
Film collecting chamber is arranged on Single Walled Carbon Nanotube growth room tail end, shorten Single Walled Carbon Nanotube flows to collecting region distance from vitellarium, avoid high length-diameter ratio carbon nanotube to deposit on tube wall, and the carbon nanotube length-to-diameter ratio of the collected film caused this technical barrier little, significantly can reduce the contact resistance of carbon nanotube.
The diameter of film collecting chamber is variable, namely according to device size needs, and the film collecting chamber of design different diameter.Film collecting chamber does not need external force such as vacuumizing in collection carbon nano-tube film process, thus film collection process does not change gas composition in reaction system, pressure and Single Walled Carbon Nanotube growing environment, which ensure that structural homogeneity and the stability of institute's growing single-wall carbon nano tube.
Single wall carbon nano-tube film collecting chamber can be arranged on horizontal type, the dissimilar chemical vapor carbon deposition nanotube growth stove (floating catalytic agent chemical vapour deposition reactor furnace) such as vertical and carry out carbon nano-tube film collection, gas circuit conversion in Single Walled Carbon Nanotube growth, collection process is realized by T-valve, invariablenes pressure of liquid in guarantee system.And film collecting chamber is connected with vacuum extractor, the air entered from the external world because opening unit takes out substrate can be discharged, ensure that reaction furnace gas is stablized.
Below, by drawings and Examples describe in detail high quality of the present invention, evenly, the controlled single wall carbon nano-tube film gas phase continuous production of density and collection.
As shown in Figure 1, single wall carbon nano-tube film continuously trapping system of the present invention, mainly comprise: the carrier gas direction 3 of chemical vapor carbon deposition nanotube growth stove 1, Single Walled Carbon Nanotube growth room 2, airintake direction, flange switch 4, ball valve switch 5, film forming collect stationary installation 6, film substrate 7, film collecting chamber 8, flange switch 9, loop 10, vacuum pump 11, vacuum pump air circuit breaker 12, outgassing direction 13, T-valve 14, bypass air circuit breaker 15, water-circulating cooling device 16, and concrete structure is as follows:
In chemical vapor carbon deposition nanotube growth stove 1, Single Walled Carbon Nanotube growth room 2 is set, Single Walled Carbon Nanotube growth room 2 is tightly connected by supporting flange and flange switch 4 with one end of ball valve switch 5, the other end of ball valve switch 5 is tightly connected by one end of supporting flange and flange switch and film collecting chamber 8, and the other end of film collecting chamber 8 and the one end in loop 10 are tightly connected by supporting flange and flange switch 9.Extend an air outlet at film collecting chamber 8 rear portion and connect vacuum pump 11, vacuum pump 11 is arranged vacuum pump air circuit breaker 12, the air-bleed system of vacuum pump 11 is controlled by vacuum pump air circuit breaker 12, arranges film forming and collect stationary installation 6, film substrate 7 in film collecting chamber 8.The other end in loop 10 exports with the Single Walled Carbon Nanotube of Single Walled Carbon Nanotube growth room 2 and carrier gas, and (the carrier gas direction 3 of airintake direction) communicates, Single Walled Carbon Nanotube and carrier gas outlet arranged outside water-circulating cooling device 16.Described loop 10 is arranged T-valve 14, bypass air circuit breaker 15, two reduction of fractions to a common denominators of T-valve 14 do not communicate with loop 10, and the threeway of T-valve 14 is connected with air outlet (outgassing direction 13), and pipe influx, in T-valve 14 place, arrives air outlet.
Ball valve switch 5, film collecting chamber 8 respectively with the Single Walled Carbon Nanotube growth room 2 in chemical vapor carbon deposition nanotube growth stove 1 not reducing be connected, be connected by dismountable flange between Single Walled Carbon Nanotube growth room 2 with the mouth of pipe of whole film collecting chamber 8, distance is shorter.Also by dismantling Flange joint between ball valve switch 5 and pipe fitting, ensure that removing and installing flexibly between component.Film collecting chamber 8 can be even footpath pipe or reducing pipe, be provided with groove in it to be used for placing film forming collection stationary installation 6, film forming is collected stationary installation 6 and can be moved to regulate film substrate 7 to receive the position of film in tube chamber in groove, the compressing tablet that film substrate 7 is collected in stationary installation 6 by film forming is fixed, and ensures not loosen in film process to stablize.In chemical vapor carbon deposition nanotube growth stove 1, the Single Walled Carbon Nanotube of synthesis at the uniform velocity flow to film collecting chamber 8 with carrier gas, and be deposited in prefabricated film substrate 7, when thickness reaches requirement, close ball valve switch 5, open bypass air circuit breaker 15, dismantle film forming collection stationary installation 6, change film substrate 7, open vacuum pump 11 and drain air in device, open ball valve switch 5, by repeating above-mentioned steps, single wall carbon nano-tube film can be collected continuously.
During work, carbon source, catalyst precursor pass into chemical vapor carbon deposition nanotube growth stove 1 with carrier gas, catalyst precursor resolves into catalyst nano-particles in high temperature reaction zone, so in Single Walled Carbon Nanotube growth room 2 catalytic pyrolysis carbon source single-wall carbon nanotube synthesizing.Under the cooling of the Single Walled Carbon Nanotube (the carrier gas direction 3 with airintake direction) and the water-circulating cooling device 16 under the carrying of carrier gas that generate, lower the temperature rapidly with carrier gas and enter film collecting chamber device; Open ball valve switch 5, close bypass air circuit breaker 15, it is inner that gas enters into film collecting chamber 8, and Single Walled Carbon Nanotube is homogeneous film formation in film substrate 7, and film thickness closes ball valve switch 5 after reaching setting requirement; Open bypass air circuit breaker 15, open quick release flange by flange switch 9, take out film forming and collect stationary installation 6, take out film substrate 7; Install new film substrate 7, open vacuum pump air circuit breaker 12, vacuumize several seconds (being generally 10 ~ 30 seconds) exhausted air, close vacuum pump air circuit breaker 12, repeat aforesaid operations and can realize continuous film collection.Whole collection process can not destroy the stopping property, carbon nano tube growth environment etc. of gas circuit, ensure that homogeneity and the stability of carbon nanotube mass; Film collecting region is normal temperature, normal pressure, and film substrate 7 is fixed by draw-in groove, ensure that film substrate 7 material qualitative diversity.
The preparation of Single Walled Carbon Nanotube of the present invention adopts conventional chemical vapor carbon nano tube growth stove, be specially: using hydrogen as carrier gas, methane is carbon source, ferrocene is catalyst precursor, elemental sulfur is growth stimulant, the mixture block of ferrocene and elemental sulfur is placed in reaction chamber inlet mouth 60 ~ 80 DEG C and locates, and growth temperature is 1100 DEG C; When Single Walled Carbon Nanotube enters continuous growth phase, carry out film collection.
Below, practicality of the present invention is set forth further by embodiment.
Embodiment 1
Adopt horizontal type chemical vapor carbon deposition nanotube growth stove, the flow rate of carrier gas of chemical vapor carbon deposition nanotube growth stove 1 is 2000ml/min, film substrate selects filter paper to collect, be that the filter paper of 50mm is put into film forming and collected stationary installation 6 by diameter, the film forming compressing tablet collected in stationary installation 6 is used to fix the edge of filter paper, after film forming collection stationary installation 6 is put into the pipe interior suitable location of film collecting chamber 8, film forming is collected stationary installation 6 and is fixed by pipe interior draw-in groove.First, open ball valve switch 5, close vacuum pump air circuit breaker 12 and bypass air circuit breaker 15, collect single wall carbon nano-tube film; After collection terminates, close ball valve switch 5, open vacuum pump air circuit breaker 12 and bypass air circuit breaker 15, opened flange by flange switch 9, take out film substrate sample, put into new filter paper substrate; Open ball valve switch 5, carry out film collection.As a comparison, have collected the film sample that growth time is 30 seconds, 1 minute, 2 minutes respectively.As shown in Figure 2, can see that film color deepens with the increase of collection time, but three kinds of films are all very even.
Embodiment 2
Adopt vertical chemical vapor carbon deposition nanotube growth stove, the flow rate of carrier gas of chemical vapor carbon deposition nanotube growth stove 1 is 4000ml/min, and film substrate selects millipore filtration to collect.Repeat the experimental procedure of embodiment 1, have collected the film sample that growth time is 1 minute, 2 minutes, 3 minutes respectively, as shown in Figure 3.Identical with embodiment 1, film color deepens with the increase of collection time, but three kinds of films are all very even.
Embodiment 3
Adopt vertical chemical vapor carbon deposition nanotube growth stove, the flow rate of carrier gas of chemical vapor carbon deposition nanotube growth stove 1 is 1000ml/min, and film substrate selects aluminium foil to collect.Repeat the experimental procedure of embodiment 1, have collected the film sample that growth time is 1 minute, as shown in Figure 4.Compared with the aluminium foil (left side) not collecting carbon nano-tube film, the aluminium foil being supported with carbon nano-tube film is a bit darkish in color (right side).
Embodiment 4
Adopt vertical chemical vapor carbon deposition nanotube growth stove, the flow rate of carrier gas of chemical vapor carbon deposition nanotube growth stove 1 is 500ml/min, and film substrate selects PET (polyethylene terephthalate) to collect.Repeat the experimental procedure of embodiment 1, have collected the film sample that growth time is 1 minute, as shown in Figure 5, illustrate its high light transmittance.
The typical scan electron micrograph of single wall carbon nano-tube film as shown in Figure 6, Fig. 6 (a) and Fig. 6 (b) is respectively the single wall carbon nano-tube film of transmittance 97% and 92%, no matter can see it being thick film (92% transmittance) or film (97% transmittance), Single Walled Carbon Nanotube is all uniformly distributed, it is netted to be woven into mutually; And single pipe range and straight (more than 20 μm), the high quality of the Single Walled Carbon Nanotube collected by explanation.Test for the single wall carbon nano-tube film utilizing PET to collect has carried out electrically conducting transparent performance in embodiment 4, find that, under the high transmission rate of 93%, its square resistance is only 200 Ω/sq.Above experimental result shows, film forming is collected stationary installation 4 and provided good basis for the uniform collection realizing single wall carbon nano-tube film.
As comparative example, monolithic filter membrane syringe filter collection device (Fig. 7) general before employing, collect single wall carbon nano-tube film, optical photograph as shown in Figure 8, from left to right collection time be followed successively by 60 seconds, 30 seconds, 10 seconds.Shrink rapidly, flow through the air turbulence of filter membrane because monolithic filter membrane syringe filter collection device exists air-flow collecting mouth, cause collected uniformity of film poor, and along with the increase of thickness, this ununiformity does not obtain any improvement.Fig. 9 is the typical scan electromicroscopic photograph of the single wall carbon nano-tube film utilizing syringe filter to collect, the Single Walled Carbon Nanotube mean length short (80%<5 μm) on film can be seen, and bend, illustrate that the Single Walled Carbon Nanotube that longer collection path causes collecting is second-rate. more
Embodiment result shows, the gas phase continuous film forming technology of the single wall carbon nano-tube film that the present invention proposes, achieve under normal pressure, room temperature condition evenly, the continuous production of controlled, the high quality single wall carbon nano-tube film of density and collection, significant in the practical application of the photoelectric fields such as transparent conductive film, field-effect thin film transistor for promotion single wall carbon nano-tube film.
Claims (10)
1. the continuous collection method of a single wall carbon nano-tube film, it is characterized in that, at chemical vapor carbon deposition nanotube growth stove tail end design and installation ball valve switch and film collecting chamber, under the prerequisite not changing any growth conditions, directly, continuously high quality carbon nano-tube film is collected, the collection of the single wall carbon nano-tube film that depositing time, flow rate of carrier gas realize evenly by regulating, thickness is controlled on various film substrate surface.
2. according to the continuous collection method of single wall carbon nano-tube film according to claim 1, it is characterized in that, the film substrate of single wall carbon nano-tube film continuously trapping system is unrestricted, film substrate is porous membrane, filter paper, PET class plastic-substrates, hard silicon chip or quartz plate, and the film collected is directly as the channel material of transparent conductive film, transparency electrode or photoelectric device thin film transistor.
3. according to the continuous collection method of single wall carbon nano-tube film according to claim 1, it is characterized in that, the density of single wall carbon nano-tube film is regulated and controled by collection time and flow rate of carrier gas, film transmittance uniform, controllable below 99%.
4. a special purpose device for the continuous collection method of single wall carbon nano-tube film according to claim 1, is characterized in that, this device comprises chemical vapor carbon deposition nanotube growth stove, film collecting chamber, vacuum pump, water-circulating cooling device, and concrete structure is as follows:
In chemical vapor carbon deposition nanotube growth stove, Single Walled Carbon Nanotube growth room is set, Single Walled Carbon Nanotube growth room is connected by supporting flange and flange switch seal with one end of ball valve switch, the other end of ball valve switch is tightly connected by one end of supporting flange and flange switch and film collecting chamber, and the other end of film collecting chamber is connected by supporting flange and flange switch seal with the one end in loop; Extend an air outlet at film collecting chamber rear portion and connect vacuum pump, vacuum pump is arranged vacuum pump air circuit breaker, the air-bleed system of vacuum pump is controlled by vacuum pump air circuit breaker, arranges film forming and collect stationary installation, film substrate in film collecting chamber; The other end in loop exports with the Single Walled Carbon Nanotube growth room of chemical vapor carbon deposition nanotube growth stove and carrier gas and communicates, Single Walled Carbon Nanotube and carrier gas outlet arranged outside water-circulating cooling device; Described loop is arranged T-valve, bypass air circuit breaker, two reduction of fractions to a common denominators of T-valve do not communicate with loop, and the threeway of T-valve is connected with air outlet.
5. according to the special purpose device of the continuous collection of single wall carbon nano-tube film according to claim 4, it is characterized in that, film collecting chamber is even footpath pipe or reducing pipe, be provided with groove in its tube chamber to be used for placing film forming collection stationary installation, film forming collects stationary installation mobile position regulating film substrate to receive film in groove, and the compressing tablet that film substrate is collected in stationary installation by film forming is fixed.
6., according to the special purpose device of the continuous collection of single wall carbon nano-tube film according to claim 4, it is characterized in that, ball valve switch, film collecting chamber respectively with the Single Walled Carbon Nanotube growth room in chemical vapor carbon deposition nanotube growth stove not reducing be connected.
7. according to the special purpose device of the continuous collection of single wall carbon nano-tube film according to claim 4, it is characterized in that, the Single Walled Carbon Nanotube of synthesizing in chemical vapor carbon deposition nanotube growth stove at the uniform velocity flow to film collecting chamber with carrier gas, and be deposited in prefabricated film substrate, when thickness reaches requirement, close ball valve switch, open T-valve, dismantle film forming collection stationary installation, change film substrate, open vacuum pump and drain air in device, open ball valve switch, by repeating above-mentioned steps, collect single wall carbon nano-tube film continuously.
8. according to the special purpose device of the continuous collection of single wall carbon nano-tube film according to claim 4, it is characterized in that, the film collecting chamber of Single Walled Carbon Nanotube is arranged on horizontal type or vertical chemical vapor deposition stove and carries out carbon nano-tube film collection.
9. according to the special purpose device of the continuous collection of single wall carbon nano-tube film according to claim 4, it is characterized in that, the gas circuit conversion in Single Walled Carbon Nanotube growth, collection process is realized by T-valve, invariablenes pressure of liquid in guarantee system.
10. according to the special purpose device of the continuous collection of single wall carbon nano-tube film according to claim 4, it is characterized in that, film collecting chamber is connected with vacuum extractor, discharges the air entered from the external world because opening unit takes out substrate.
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| CN108277557A (en) * | 2018-02-28 | 2018-07-13 | 四川理工学院 | A kind of spiral nanometer carbon fiber, the continuous preparation system of carbon nanotube |
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| CN109436916A (en) * | 2017-09-22 | 2019-03-08 | 中国科学院物理研究所 | A kind of continuous collection method and device of carbon nano-tube film |
| CN110357073A (en) * | 2019-08-23 | 2019-10-22 | 哈尔滨工业大学 | A kind of preparation method of gradient rigidity carbon nanotube sponge |
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| CN114267492A (en) * | 2021-12-31 | 2022-04-01 | 大连工业大学 | Uniform and transparent conductive film with long-tube-bundle carbon nanotubes and preparation method thereof |
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