CN104671230B - The continuous collection method of a kind of single wall carbon nano-tube film and special purpose device - Google Patents
The continuous collection method of a kind of single wall carbon nano-tube film and special purpose device Download PDFInfo
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- CN104671230B CN104671230B CN201510074790.2A CN201510074790A CN104671230B CN 104671230 B CN104671230 B CN 104671230B CN 201510074790 A CN201510074790 A CN 201510074790A CN 104671230 B CN104671230 B CN 104671230B
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Abstract
The present invention relates to controlled, the uniform collection technology of single wall carbon nano-tube film, the continuous collection method of the single wall carbon nano-tube film of a kind of floating catalytic agent method growth and special purpose device.Connect mounting ball valve switch and thin film collecting chamber in the design of chemical vapor carbon deposition nanotube growth furnace tail end, on the premise of not changing any growth conditions, collect high-quality single wall carbon nano-tube film directly, continuously on various film substrate surfaces.Under room temperature, room pressure condition, the single wall carbon nano-tube film that floating catalytic agent chemical vapour deposition technique grows is collected various substrate surface, by the regulation and control to sedimentation time, the control of growth parameter(s), it is achieved a few inches rank, density is controlled and the continuous collection of uniform single wall carbon nano-tube film.Thus, solve the technical barriers such as the lack of homogeneity that faced during current carbon nano-tube film is collected, draw ratio be little, size-constrained.
Description
Technical field
The present invention relates to controlled, the uniform collection technology of single wall carbon nano-tube film, be specially a kind of floating catalytic
The continuous collection method of the single wall carbon nano-tube film of agent method growth and special purpose device.
Background technology
SWCN, because of electricity, optics and the mechanical characteristic of its excellence, is suitable for preparing electrically conducting transparent thin
Film and flexible thin-film transistor circuit etc..Single wall carbon nano-tube film electronic device is in following Electronic Paper, flexibility
Battery, electronic tag, flexible and transparent show, even replaces the fields such as silicon-based semiconductor material be expected to have wide
Application prospect.
At present, the growth of floating catalytic agent chemical gaseous phase depositing process and the single wall carbon nano-tube film exhibition collected are utilized
Tempting photoelectric properties are shown.[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, i.e. single in floating catalytic growth
The exhaust end of wall carbon nano tube device installs syringe filter additional, and the SWCN of generation flows out growth with carrier gas
Device is also deposited on microporous filter membrane.Carbon nano-tube film on filter membrane can transfer to include plastics, glass,
In the substrates such as 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 presently, there are is: (1) filter caliber at air inlet and gas outlet occurs
Shrink and amplification can produce eddy current, affect SWCN and be uniformly distributed suprabasil；(2) substrate material
It is only limitted to porous membrane, needs to shift accordingly according to application, and transfer process can introduce pollutant effect
The intrinsic performance of CNT；(3) syringe filter is installed on exhaustor, and distance SWCN grows
Room is remote, and this causes high-quality big L/D ratio SWCN to be easily attached on the wall of pipeline；And it is collected thin
Single length of tube in film is shorter, this dramatically increases the contact resistance between CNT, and then causes
The performances such as the constructed carrier mobility of device, electrical conductivity reduce.Thus, how current subject matter is
Shorten the distance between collecting chamber and carbon nano tube growth room, avoid vortex phenomenon, it is achieved high length-diameter ratio, uniformly
The single wall carbon nano-tube film of distribution is collected, to meet high-quality, the demand of high-performance optical electrical part.
Summary of the invention
An object of the present invention is to provide the continuous collection method of a kind of high length-diameter ratio single wall carbon nano-tube film
With special purpose device, the SWCN draw ratio overcoming floating current catalyst chemical gas phase deposition method to collect is little
This technical barrier.
The two of the purpose of the present invention are to provide the list not limited by shapes of substrates, material under a kind of room temperature, normal pressure
The continuous collection method of wall carbon nano-tube film and special purpose device, overcome existing monolithic filter membrane collection method to limit to
The problem introducing pollutant in substrate kind and transfer process.
The three of the purpose of the present invention be to provide a kind of uniformly, the controlled single wall carbon nano-tube film of density continuous
Collection method and special purpose device, the carbon nano-tube film skewness overcoming current thin film collection method to exist is asked
Topic.
The technical scheme is that
The continuous collection method of a kind of single wall carbon nano-tube film, at chemical vapor carbon deposition nanotube growth furnace tail
End design and installation ball valve switch and thin film collecting chamber, on the premise of not changing any growth conditions, various thin
Film substrate surface collects high-quality carbon nano-tube film directly, continuously, by regulation sedimentation time, flow rate of carrier gas
Realize the collection of single wall carbon nano-tube film uniform, that thickness is controlled.
The film substrate of described single wall carbon nano-tube film continuously trapping system is unrestricted, and film substrate is many
Hole filter membrane, filter paper, PET class plastic-substrates, hard silicon chip or piezoid, the thin film collected is directly as thoroughly
Bright conductive film, transparency electrode or the channel material of photoelectric device thin film transistor (TFT).
The density of described single wall carbon nano-tube film is regulated and controled by acquisition time and flow rate of carrier gas, and thin film is saturating
Light rate uniform, controllable below 99%.
The special purpose device of the continuous collection method of described single wall carbon nano-tube film, this device includes chemical gaseous phase
Deposition of carbon nanotubes growth furnace, thin film collecting chamber, vacuum pump, water-circulating cooling device, concrete structure is as follows:
Arranging SWCN growth room in chemical vapor carbon deposition nanotube growth furnace, SWCN is raw
Long room is connected by supporting flange and flange switch seal with one end of ball valve switch, the other end of ball valve switch
The one end switched with thin film collecting chamber by supporting flange and flange is tightly connected, the other end of thin film collecting chamber
It is connected by supporting flange and flange switch seal with the one end in loop；One is extended at thin film collecting chamber rear portion
Gas outlet connects vacuum pump, and vacuum pump arranges vacuum pump air circuit breaker, and the extract system of vacuum pump is by vacuum pump
Air circuit breaker controls, and arranges film forming and collect fixing device, film substrate in thin film collecting chamber；The other end in loop
Communicate with SWCN growth room and the carrier gas outlet of chemical vapor carbon deposition nanotube growth furnace, single wall carbon
Outside nanotube and carrier gas outlet, water-circulating cooling device is set；Arrange three-way valve on described loop, bypass gas circuit is opened
Closing, two reduction of fractions to a common denominators of three-way valve do not communicate with loop, and the threeway of three-way valve is connected with gas outlet.
Described thin film collecting chamber is even footpath pipe or reducing pipe, is provided with groove for being positioned in its tube chamber
Film collects fixing device, and film forming is collected fixing device mobile film substrate that regulates in groove and received the position of thin film
Putting, the tabletting that film substrate is collected in fixing device by film forming is fixed.
Described ball valve switch, thin film collecting chamber respectively with the single wall in chemical vapor carbon deposition nanotube growth furnace
Carbon nano tube growth room not reducing is connected.
In described chemical vapor carbon deposition nanotube growth furnace, the SWCN of synthesis at the uniform velocity flow to carrier gas
Thin film collecting chamber, and be deposited in prefabricated film substrate, when thickness reaches requirement, closedown ball valve switch,
Open three-way valve, dismounting film forming collects fixing device, changes film substrate, opens vacuum pump and drain in device empty
Gas, open ball valve switch, by repeat the above steps, collect single wall carbon nano-tube film continuously.
The thin film collecting chamber of described SWCN is arranged on horizontal type or vertical chemical vapor deposition stove and carries out
Carbon nano-tube film is collected.
Described SWCN growth, collect during gas circuit conversion realized by three-way valve, it is ensured that body
Invariablenes pressure of liquid in system.
Described thin film collecting chamber connects vacuum extractor, discharges and enters from the external world because device for opening takes out substrate
The air entered.
The design philosophy of the present invention is:
The SWCN of floating catalytic agent chemical vapour deposition technique synthesis is under the carrying of carrier gas, by growth room
Flow to collecting chamber, be deposited on film forming in substrate.By regulation CNT at suprabasil sedimentation time, gas
Flows etc. realize the regulation to substrate surface SWCN density.Thin film is collected continuously can be by ball-cock device
And gas path three-way valve co-controlling, regulate air circuit breaker, can be real under not affecting carbon nano tube growth parameter
Now collect high-quality single wall carbon nano-tube film continuously.Collecting chamber is arranged on reacting furnace tail end, can realize high long
Footpath is than the collection of SWCN.Substrate is designed by draw-in groove and fixes thin film collection substrate, thus substrate material
Matter is unrestricted.Water cooling plant is had, it is ensured that the temperature constant of collecting chamber between growth room and collecting chamber.
Advantages of the present invention and providing the benefit that:
The continuous collection technique of the single wall carbon nano-tube film that 1, the present invention relates to and special purpose device, with the most universal
Use syringe filter subtraction unit compare, can realize more high-quality, big L/D ratio SWCN direct
Film forming.Deposition substrate is not had selectivity, i.e. can deposit single wall carbon nano-tube film in meaning substrate in office, receive
Collection thin-film process in will not in reacting furnace atmosphere produce any impact, it is ensured that the growth of SWCN and
It is independent that thin film collects two processes, and is independent of each other.
2, the quick detachable installation of apparatus of the present invention, adaptability is good, is mountable to different types ofization such as vertical, horizontal type
Learn gaseous phase deposition stove.The method overcome in the most commonly used chemically reacting furnace and utilize pin type after extraction catheter
Filter is collected CNT and is easily generated air stream turbulence effect, causes the phenomenon that thin film is uneven, and the method obtains
High-quality single wall carbon nano-tube film 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 receives
Nanotube growth stove；2, SWCN growth room；3, the carrier gas direction of airintake direction；4, flange is opened
Close；5, ball valve switch；6, film forming collects fixing device；7, film substrate；8, thin film collecting chamber；9, method
Blue switch；10, loop；11, vacuum pump；12, vacuum pump air circuit breaker；13, outgassing direction；14, three
Logical 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 microporous filter membrane.
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 collected on PET.
Fig. 6 is the typical scan electromicroscopic photograph of single wall carbon nano-tube film.In figure, (a) figure is light transmittance 97%
Single wall carbon nano-tube film；B () figure is the single wall carbon nano-tube film of light 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.
Detailed description of the invention
In a specific embodiment, the continuous collection method of single wall carbon nano-tube film of the present invention and special purpose device,
SWCN growth room tail end design and installation ball valve switch at single wall carbon nano-tube film continuously trapping system
With thin film collecting chamber, on the premise of not changing any growth conditions, at various substrate surfaces directly, closely,
Collect high-quality carbon nano-tube film continuously, can realize uniform, thick by regulation sedimentation time, flow rate of carrier gas etc.
Spend the collection of controlled single wall carbon nano-tube film.
The substrate that single wall carbon nano-tube film is collected is not limited by material and shape, and substrate can be: porous membrane,
Filter paper, PET class plastic-substrates, and the substrate such as hard silicon chip, piezoid.The thin film collected can be directly as
Transparent conductive film, transparency electrode, or the channel material of photoelectric device thin film transistor (TFT).Thus, eliminate
Loaded down with trivial details transfer step, decrease impurity and pollute and defect introduces, the application demand of multiple photoelectric device can be met.
The density of single wall carbon nano-tube film can be regulated and controled by acquisition time and flow rate of carrier gas, thin film light transmittance
Uniform, controllable below 99%；Owing to collecting in reacting furnace, air-flow is more stable, and single wall carbon nano-tube film has
There is the uniformity of excellence.
Thin film collecting chamber is arranged on SWCN growth room tail end, shortens SWCN from vitellarium
Flow to the distance of collecting region, it is to avoid high length-diameter ratio CNT deposits on tube wall, and cause collected
CNT draw ratio this technical barrier little of thin film, can be greatly reduced the contact resistance of CNT.
The diameter of thin film collecting chamber is variable, and i.e. according to device size needs, the thin film of design different-diameter is received
Collection room.Thin film collecting chamber is not required to the external force such as evacuation during collecting carbon nano-tube film, thus thin film is collected
Process does not change gas composition, pressure and SWCN growing environment in reaction system, which ensure that institute
The structural homogeneity of growing single-wall carbon nano tube and stability.
Single wall carbon nano-tube film collecting chamber may be mounted at horizontal type, the different types of chemical gaseous phase such as vertical deposition
Carbon nano-tube film collection is carried out on carbon nano tube growth stove (floating catalytic agent chemical vapour deposition reactor furnace),
Gas circuit conversion during SWCN growth, collection is realized by three-way valve, it is ensured that in system, pressure is permanent
Fixed.And, thin film collecting chamber connects vacuum extractor, can discharge because of device for opening taking-up substrate from outward
The air that boundary enters, it is ensured that reaction furnace gas is stable.
Below, by drawings and Examples describe in detail high-quality of the present invention, uniformly, the controlled single of density
Pipe thin film chemical vapor is prepared continuously and collects.
As it is shown in figure 1, single wall carbon nano-tube film continuously trapping system of the present invention, specifically include that chemical gaseous phase
Deposition of carbon nanotubes growth furnace 1, SWCN growth room 2, the carrier gas direction 3 of airintake direction, method
Blue switch 4, ball valve switch 5, film forming collect fixing device 6, film substrate 7, thin film collecting chamber 8, flange
Switch 9, loop 10, vacuum pump 11, vacuum pump air circuit breaker 12, outgassing direction 13, three-way valve 14, side
Road air circuit breaker 15, water-circulating cooling device 16, concrete structure is as follows:
Chemical vapor carbon deposition nanotube growth furnace 1 arranges SWCN growth room 2, single
Pipe growth room 2 is tightly connected by supporting flange and flange switch 4 with one end of ball valve switch 5, and ball valve is opened
One end that the other end of pass 5 is switched with thin film collecting chamber 8 by supporting flange and flange is tightly connected, thin film
The other end of collecting chamber 8 is tightly connected by supporting flange and flange switch 9 with the one end in loop 10.Thin
Film collecting chamber 8 rear portion is extended a gas outlet and is connected vacuum pump 11, vacuum pump 11 arranges vacuum pump gas circuit and opens
Closing 12, the extract system of vacuum pump 11 is controlled by vacuum pump air circuit breaker 12, is arranged in thin film collecting chamber 8
Film collects fixing device 6, film substrate 7.The other end in loop 10 and the list of SWCN growth room 2
Wall carbon nano tube and carrier gas outlet (the carrier gas direction 3 of airintake direction) communicate, SWCN and load
Outside gas outlet, water-circulating cooling device 16 is set.Three-way valve 14, bypass air circuit breaker are set on described loop 10
15, two reduction of fractions to a common denominators of three-way valve 14 do not communicate with loop 10, and the threeway of three-way valve 14 is connected with gas outlet (to go out
Gas direction 13), pipe influx, at three-way valve 14, arrives gas outlet.
Ball valve switch 5, thin film collecting chamber 8 respectively with the single wall in chemical vapor carbon deposition nanotube growth furnace 1
Carbon nano tube growth room 2 not reducing is connected, SWCN growth room 2 and the pipe of whole thin film collecting chamber 8
Being connected by dismountable flange between Kou, distance is shorter.Also by dismounting flange between ball valve switch 5 and pipe fitting
Connect, it is ensured that removing and installing flexibly between component.Thin film collecting chamber 8 can be even footpath pipe or reducing pipe,
Being provided with groove in it and collect fixing device 6 for placing film forming, film forming collects fixing device 6 can in tube chamber
In groove, movement regulates film substrate 7 and receives the position of thin film, and film substrate 7 is collected fixing dress by film forming
The tabletting put on 6 is fixed, it is ensured that do not loosen stable in film forming procedure.Chemical vapor carbon deposition nanotube grows
In stove 1, the SWCN of synthesis at the uniform velocity flow to thin film collecting chamber 8 with carrier gas, and is deposited on prefabricated thin film
In substrate 7, when thickness reaches requirement, close ball valve switch 5, open bypass air circuit breaker 15, be disassembled into
Film collects fixing device 6, changes film substrate 7, opens vacuum pump 11 and drain air in device, open ball valve
Switch 5, by repeat the above steps, can collect single wall carbon nano-tube film continuously.
During work, carbon source, catalyst precursor are passed through chemical vapor carbon deposition nanotube growth furnace 1 with carrier gas,
Catalyst precursor resolves into catalyst nano-particles in high temperature reaction zone, and then in SWCN growth room
Catalytic pyrolysis carbon source single-wall carbon nanotube synthesizing in 2.Generate SWCN under the carrying of carrier gas (with
The carrier gas direction 3 of airintake direction) and the cooling of water-circulating cooling device 16 under, entrance of lowering the temperature rapidly with carrier gas
Thin film collecting chamber device；Opening ball valve switch 5, close bypass air circuit breaker 15, gas enters into thin film and collects
Room 8 is internal, and SWCN is homogeneous film formation in film substrate 7, and film thickness reaches to set after requiring,
Close ball valve switch 5；Open bypass air circuit breaker 15, open quick release flange by flange switch 9, take out into
Film collects fixing device 6, takes out film substrate 7；Install new film substrate 7, open vacuum pump gas circuit and open
Pass 12, evacuation several seconds (generally 10～30 seconds) air-out, close vacuum pump air circuit breaker 12,
Repeat aforesaid operations and can realize continuous film collection.Whole collection process will not destroy the sealing of gas circuit, carbon
Nanotube growing environment etc., it is ensured that the homogeneity of carbon nanotube mass and stability；Thin film collecting region be room temperature,
Normal pressure, and film substrate 7 is to be fixed by draw-in groove, it is ensured that film substrate 7 material qualitative diversity.
The preparation of SWCN of the present invention uses conventional chemical vapor carbon nano tube growth stove, specifically
For: with hydrogen as carrier gas, methane as carbon source, ferrocene as catalyst precursor, elemental sulfur be growth promote
Agent, the mixture block of ferrocene and elemental sulfur is placed at reaction chamber air inlet 60～80 DEG C, and growth temperature is
1100℃；When SWCN enters continuous growth stage, carry out thin film collection.
Below, the practicality of the present invention is expanded on further by embodiment.
Embodiment 1
Use horizontal type chemical vapor carbon deposition nanotube growth furnace, chemical vapor carbon deposition nanotube growth furnace 1
Flow rate of carrier gas is 2000ml/min, and film substrate selects filter paper to be collected, and is put by the filter paper of a diameter of 50mm
Enter film forming and collect in fixing device 6, use film forming to collect the tabletting in fixing device 6 and fix the edge of filter paper,
After film forming is collected the pipe interior suitable location that fixing device 6 puts into thin film collecting chamber 8, film forming is collected fixing
Device 6 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, collection 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, open flange by flange switch 9, take out thin film base
Original pattern product, put into new filter paper substrate；Open ball valve switch 5, carry out thin film collection.As a comparison, respectively
Have collected growth time is 30 seconds, 1 minute, the film sample of 2 minutes.As shown in Figure 2, it can be seen that thin
Film color deepens with the increase of acquisition time, but three kinds of thin film are the most highly uniform.
Embodiment 2
Use vertical chemical vapor carbon deposition nanotube growth furnace, chemical vapor carbon deposition nanotube growth furnace 1
Flow rate of carrier gas is 4000ml/min, and film substrate selects microporous filter membrane to be collected.Repeat the experiment of embodiment 1
Step, have collected growth time respectively is 1 minute, 2 minutes, the film sample of 3 minutes, as shown in Figure 3.
Same as in Example 1, thin film color deepens with the increase of acquisition time, but three kinds of thin film are the most highly uniform.
Embodiment 3
Use vertical chemical vapor carbon deposition nanotube growth furnace, chemical vapor carbon deposition nanotube growth furnace 1
Flow rate of carrier gas is 1000ml/min, and film substrate selects aluminium foil to be collected.Repeat the experimental procedure of embodiment 1,
Have collected the film sample that growth time is 1 minute, as shown in Figure 4.With the aluminum not collecting carbon nano-tube film
Paper tinsel (left) is compared, and the aluminium foil being supported with carbon nano-tube film is a bit darkish in color (right).
Embodiment 4
Use vertical chemical vapor carbon deposition nanotube growth furnace, chemical vapor carbon deposition nanotube growth furnace 1
Flow rate of carrier gas is 500ml/min, and film substrate selects PET (polyethylene terephthalate) to carry out
Collect.Repeat the experimental procedure of embodiment 1, have collected the film sample that growth time is 1 minute, such as Fig. 5
Shown in, 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 light transmittance 97% and 92%, it can be seen that whether thick film (92%
Light transmittance) or thin film (97% light transmittance), SWCN is all uniformly distributed, be interleaved with each other and reticulate；
And single pipe range and straight (more than 20 μm), the high-quality of the SWCN collected by explanation.
Carry out the test of electrically conducting transparent performance in embodiment 4 for the single wall carbon nano-tube film utilizing PET to collect, sent out
Under the high transmission rate of present 93%, its square resistance is only 200 Ω/sq.More than test result indicate that, film forming is received
Collection fixing device 4 is that the uniform collection realizing single wall carbon nano-tube film provides excellent basis.
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 acquisition time be followed successively by 60 seconds, 30
Second, 10 seconds.Shrink rapidly in collection port owing to monolithic filter membrane syringe filter collection device exists air-flow, flow through
The air turbulence of filter membrane, causes collected uniformity of film poor, and along with the increase of thickness, this uneven
Property does not obtain any improvement.Fig. 9 is that the typical case of the single wall carbon nano-tube film utilizing syringe filter to collect sweeps
Retouch electromicroscopic photograph, it can be seen that the SWCN average length on thin film is short (80% < 5 μm), Er Qieduo
Bending, illustrates that longer path of collecting causes the SWCN collected second-rate.
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 uniformly, density is controlled, the continuous preparation of high-quality single wall carbon nano-tube film
With collection, for promote single wall carbon nano-tube film at photoelectricity such as transparent conductive film, field effect thin film transistor (TFT)s
The actual application in field is significant.
Claims (10)
1. the special purpose device collected continuously of a single wall carbon nano-tube film, it is characterised in that this device includes chemical vapor carbon deposition nanotube growth furnace, thin film collecting chamber, vacuum pump, water-circulating cooling device, and concrete structure is as follows:
Chemical vapor carbon deposition nanotube growth furnace arranges SWCN growth room, SWCN growth room is connected by supporting flange and flange switch seal with one end of ball valve switch, one end that the other end of ball valve switch is switched with thin film collecting chamber by supporting flange and flange is tightly connected, and the other end of thin film collecting chamber is connected by supporting flange and flange switch seal with the one end in loop；Extending a gas outlet at thin film collecting chamber rear portion and connect vacuum pump, vacuum pump arranges vacuum pump air circuit breaker, the extract system of vacuum pump is controlled by vacuum pump air circuit breaker, arranges film forming and collect fixing device, film substrate in thin film collecting chamber；The other end in loop communicates with SWCN growth room and the carrier gas outlet of chemical vapor carbon deposition nanotube growth furnace, arranges water-circulating cooling device outside the SWCN of SWCN growth room and carrier gas outlet；Arranging three-way valve, bypass air circuit breaker on described loop, two reduction of fractions to a common denominators of three-way valve do not communicate with loop, and the threeway of three-way valve is connected with gas outlet.
2. according to the special purpose device collected continuously of the single wall carbon nano-tube film described in claim 1, it is characterized in that, thin film collecting chamber is even footpath pipe or reducing pipe, it is provided with groove in its tube chamber and collects fixing device for placing film forming, film forming is collected fixing device mobile film substrate that regulates in groove and is received the position of thin film, and the tabletting that film substrate is collected in fixing device by film forming is fixed.
3. according to the special purpose device collected continuously of the single wall carbon nano-tube film described in claim 1, it is characterised in that ball valve switch, thin film collecting chamber are connected with the SWCN growth room not reducing in chemical vapor carbon deposition nanotube growth furnace respectively.
4. according to the special purpose device collected continuously of the single wall carbon nano-tube film described in claim 1, it is characterized in that, in chemical vapor carbon deposition nanotube growth furnace, the SWCN of synthesis at the uniform velocity flow to thin film collecting chamber with carrier gas, and be deposited in prefabricated film substrate, when thickness reaches requirement, close ball valve switch, open three-way valve, dismounting film forming collection fixing device, change film substrate, open vacuum pump and drain air in device, open ball valve switch, by repeat the above steps, collect single wall carbon nano-tube film continuously.
5. according to the special purpose device collected continuously of the single wall carbon nano-tube film described in claim 1, it is characterised in that the thin film collecting chamber of SWCN is arranged on horizontal type or vertical chemical vapor deposition stove and carries out carbon nano-tube film collection.
6. according to the special purpose device collected continuously of the single wall carbon nano-tube film described in claim 1, it is characterised in that the gas circuit conversion during SWCN growth, collection is realized by three-way valve, it is ensured that invariablenes pressure of liquid in system.
7., according to the special purpose device collected continuously of the single wall carbon nano-tube film described in claim 1, it is characterised in that thin film collecting chamber connects vacuum extractor, discharge the air entered because device for opening takes out substrate from the external world.
8. the continuous collection method of the single wall carbon nano-tube film utilizing special purpose device described in claim 1, it is characterized in that, at chemical vapor carbon deposition nanotube growth furnace tail end design and installation ball valve switch and thin film collecting chamber, on the premise of not changing any growth conditions, collection high-quality carbon nano-tube film direct on various film substrate surfaces, continuous, realizes the collection of single wall carbon nano-tube film uniform, that thickness is controlled by regulation sedimentation time, flow rate of carrier gas.
9. according to the continuous collection method of the single wall carbon nano-tube film described in claim 8, 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 piezoid, and the thin film collected is directly as transparent conductive film, transparency electrode or the channel material of photoelectric device thin film transistor (TFT).
10. according to the continuous collection method of the single wall carbon nano-tube film described in claim 8, it is characterised in that the density of single wall carbon nano-tube film is regulated and controled by acquisition time and flow rate of carrier gas, thin film light transmittance uniform, controllable below 99%.
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| CN109436916B (en) * | 2017-09-22 | 2020-05-15 | 中国科学院物理研究所 | Continuous collection method and device for carbon nanotube film |
| CN108277557B (en) * | 2018-02-28 | 2020-04-07 | 四川理工学院 | Continuous preparation system for spiral carbon nanofibers and carbon nanotubes |
| CN109443232B (en) * | 2018-12-29 | 2020-10-13 | 武汉华星光电技术有限公司 | Single-molecule substrate strain sensing device and preparation method thereof |
| CN110357073B (en) * | 2019-08-23 | 2022-03-15 | 哈尔滨工业大学 | Preparation method of gradient rigidity carbon nanotube sponge |
| CN112490322B (en) * | 2019-09-11 | 2023-04-07 | 中国科学院金属研究所 | Preparation method of flexible P-type single-walled carbon nanotube/N-type silicon heterojunction solar cell |
| CN114267492B (en) * | 2021-12-31 | 2023-07-25 | 大连工业大学 | Uniform transparent conductive film with long tube bundle carbon nano tubes and preparation method thereof |
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| US20110014446A1 (en) * | 2007-07-06 | 2011-01-20 | Takeshi Saito | Method for forming carbon nanotube film, film-forming apparatus, and carbon nanotube film |
| JP5327899B2 (en) * | 2008-02-29 | 2013-10-30 | 独立行政法人産業技術総合研究所 | Carbon nanotube film structure and manufacturing method thereof |
| JP5831966B2 (en) * | 2011-07-08 | 2015-12-16 | 国立研究開発法人産業技術総合研究所 | Method for producing a carbon nanotube aggregate in which single-walled carbon nanotubes and double-walled carbon nanotubes are mixed at an arbitrary ratio |
| CN102424375B (en) * | 2011-09-07 | 2013-11-13 | 钟国仿 | Preparation method for vertical carbon nanotube array |
| CN104098079A (en) * | 2013-04-11 | 2014-10-15 | 袁健飞 | Method for preparing carbon nanotube film through floating catalysis technology |
| CN104176722B (en) * | 2014-08-06 | 2016-05-18 | 北京航空航天大学 | High-intensity array drawing-off carbon nano-tube film of a kind of high orientation and preparation method thereof |
| CN104261384B (en) * | 2014-09-23 | 2016-06-01 | 中国科学院金属研究所 | The gas phase continuous production method of single wall carbon nano-tube film and special purpose device |
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