CN105585000B - A kind of method for preparing no dispersant semi-conductive single-walled carbon nanotubes film - Google Patents
A kind of method for preparing no dispersant semi-conductive single-walled carbon nanotubes film Download PDFInfo
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Abstract
Present invention is disclosed a kind of method for preparing no dispersant semi-conductive single-walled carbon nanotubes film, this method comprises the following steps：Dispersion soln one is made in single-walled carbon nanotube and conjugated polymer dispersant common distribution in organic solvent one；Centrifugal treating dispersion soln one, collect supernatant and filter, obtain being coated with the semi-conductive single-walled carbon nanotubes of dispersant；Organic solvent two is provided, cleaning is coated with the semi-conductive single-walled carbon nanotubes of conjugated polymer dispersant；Organic solvent three is provided, the semi-conductive single-walled carbon nanotubes after above-mentioned cleaning are subjected to scattered obtained dispersion soln two；By dispersion soln two coated in acquisition in a substrate without dispersant semi-conductive single-walled carbon nanotubes film.Compared with prior art, what is be prepared by the method for the present invention can show the intrinsic performance of single-walled carbon nanotube without dispersant semi-conductive single-walled carbon nanotubes film, be applicable to the preparation of high-performance carbon nanotube thin-film semiconductor device.
Description
Technical field
The invention belongs to carbon nanotube technology field, more particularly to one kind to prepare the semi-conductive single-walled carbon nanometer of no dispersant
The method of pipe film.
Background technology
Single-walled carbon nanotube（single-walled carbonnanotubes:SWNTS）One as a kind of most prospect
Tie up semi-conducting material and obtain greatly concern in electronic applications.Single-walled carbon nanotube includes the single-walled carbon nanotube of metallicity
（m-SWCNTS）And semi-conductive single-walled carbon nanotubes（s-SWCNTS）, wherein, semi-conductive single-walled carbon nanotubes（s-
SWCNTs）There are more research and application in molectronics and photoelectricity field.
Under normal circumstances because semi-conductive single-walled carbon nanotubes have larger specific surface area, easily there is the shape reunited
State, therefore ground extensively by researcher by the monodispersed semi-conductive single-walled carbon nanotubes of effect acquisition of dispersant
Study carefully.But dispersant is helping semi-conductive single-walled carbon nanotubes monodispersed while can also have a strong impact on the semiconductive of preparation
Single wall carbon nano-tube film device performance.Therefore, the semi-conductive single-walled carbon nanotubes film of no dispersant is obtained for high property
The application of energy semi-conductive single-walled carbon nanotubes thin-film device has great importance.
The method that dispersant is removed in solution at present mainly goes to realize from the angle of MOLECULE DESIGN.Stanford Univ USA
Professor Bao Zhenan adds trifluoroacetic acid in the solution by designing the conjugated polymer with hydrogen bond so that and hydrogen bond is destroyed, point
Powder conjugated polymer separates from CNT.But herein handle during CNT purity can seriously by
The influence of dispersant.At present, received it is not yet reported that crossing and successfully preparing monodispersed semi-conductive single-walled carbon by the above method
Mitron film.
The content of the invention
It is an object of the invention to provide a kind of preparation for solving above-mentioned technical problem without the semi-conductive single-walled carbon of dispersant
The method of nano-tube film.
To solve an above-mentioned goal of the invention, it is thin that present invention offer one kind prepares no dispersant semi-conductive single-walled carbon nanotubes
The method of film, this method comprise the following steps：
S1, by single-walled carbon nanotube and conjugated polymer dispersant common distribution in organic solvent one be made dispersion soln
One；
S2, centrifugal treating dispersion soln one, collect supernatant and by supernatant liquid filtering, obtain being coated with conjugated polymers
The semi-conductive single-walled carbon nanotubes of thing dispersant；
S3, offer can dissolve the organic solvent two of conjugated polymer dispersant, and cleaning is coated with conjugated polymer point
The semi-conductive single-walled carbon nanotubes of powder；
S4, organic solvent three is provided, the semi-conductive single-walled carbon nanotubes after above-mentioned cleaning are carried out into scattered be made disperses
Solution two；
S5, a substrate is provided, dispersion soln two is used into immersion or spraying or spin coating proceeding coating on the substrate,
Obtained in the substrate without dispersant semi-conductive single-walled carbon nanotubes film.
As a further improvement on the present invention, the conjugated polymer dispersant is polycarbazole, and the organic solvent one is
Toluene or 1-METHYLPYRROLIDONE, the organic solvent two are dimethylbenzene or hexamethylene, and the organic solvent three is chloroform or three
Chloromethanes.
As a further improvement on the present invention, " single-walled carbon nanotube and conjugated polymer dispersant are total to the step by S1
Dispersion soln one " is made specially with being dispersed in organic solvent one：
Single-walled carbon nanotube, conjugated polymer dispersant are mixed with toluene or 1-METHYLPYRROLIDONE, at ultrasonic disperse
Reason, ultrasonic power 20W-100W, dispersion soln one is made.
As a further improvement on the present invention, the centrifugal rotational speed in the step S2 is 10000g ~ 1000000g, and the time is
0.5 h~20 h。
As a further improvement on the present invention, filtered, be coated with using teflon membrane filter in the step S2
The semi-conductive single-walled carbon nanotubes of conjugated polymer dispersant are stayed on filter membrane, and partly conjugated polymeric dispersant passes through filter opening
It is filtered.
As a further improvement on the present invention, " S3 is provided can dissolve the organic molten of conjugated polymer dispersant to the step
The semi-conductive single-walled carbon nanotubes for being coated with conjugated polymer dispersant are cleaned in agent two, obtain semi-conductive single-walled carbon and receive
Mitron " is specially：
The semi-conductive single-walled carbon nanotubes for being coated with conjugated polymer dispersant are immersed in dimethylbenzene or hexamethylene
In alkane, centrifugal treating, centrifugal rotational speed 10000-200000g, being precipitated as being collected into are semi-conductive single-walled again for first decentralized processing
CNT.
As a further improvement on the present invention, the substrate is cleaned before being applied by dispersion soln two with toluene or acetone
And dry.
As a further improvement on the present invention, before step S4, repeat step S3 is for several times.
As a further improvement on the present invention, the S2 steps also include：The partly conjugated polymer being filtered is put again
Enter in step S1, reuse.
As a further improvement on the present invention, the single-walled carbon nanotube uses chemical vapour deposition technique or arc discharge method
Or prepared by laser evaporization method.
Because above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：
1st, by the present invention method prepare can carbon pipe without dispersant semi-conductive single-walled carbon nanotubes film
Film shows the intrinsic performance of carbon pipe；
2nd, the carbon pipe film can have good contact with metal electrode；
3rd, can be directly using technique sides such as immersion, spraying, spin coatings without dispersant semi-conductive single-walled carbon nanotubes solution
Method large area prepares high performance carbon pipe thin-film device so that carbon pipe thin-film device removes dispersant without subsequent treatment.
Brief description of the drawings
Fig. 1 is method and step of the preparation without dispersant semi-conductive single-walled carbon nanotubes film in an embodiment of the present invention
Flow chart；
Fig. 2 a are that the semi-conductive single-walled carbon that conjugated polymer dispersant is coated with an embodiment of the present invention is received
Mitron cleaned with dimethylbenzene before UV-vis absorption spectrum figure；
Fig. 2 b are Fig. 2 a partial enlarged drawings；
Fig. 2 c are that the semi-conductive single-walled carbon that conjugated polymer dispersant is coated with an embodiment of the present invention is received
Mitron cleaned with dimethylbenzene after UV-vis absorption spectrum figure；
Fig. 3 is the semi-conductive single-walled carbon nanometer that conjugated polymer dispersant is coated with an embodiment of the present invention
The front and rear Raman spectrum comparison diagram of effective dimethylbenzene cleaning；
Fig. 4 a are that the semi-conductive single-walled carbon that conjugated polymer dispersant is coated with an embodiment of the present invention is received
AFM figures before mitron cyclohexane；
Fig. 4 b are that the semi-conductive single-walled carbon that conjugated polymer dispersant is coated with an embodiment of the present invention is received
The height phase diagram of CNT on AFM before mitron cyclohexane；
Fig. 5 a are that the semi-conductive single-walled carbon that conjugated polymer dispersant is coated with an embodiment of the present invention is received
AFM figures after mitron cyclohexane；
Fig. 5 b are that the semi-conductive single-walled carbon that conjugated polymer dispersant is coated with an embodiment of the present invention is received
The height phase diagram of CNT on AFM before mitron cyclohexane.
Embodiment
Below with reference to embodiment shown in the drawings, the present invention will be described in detail.But these embodiments are simultaneously
The present invention is not limited, structure that one of ordinary skill in the art is made according to these embodiments, method or functionally
Conversion is all contained in protection scope of the present invention.
Join an a kind of tool of method for preparing no dispersant semi-conductive single-walled carbon nanotubes film of Fig. 1 introductions present invention
Body embodiment, this method specifically include following steps：
S1, by single-walled carbon nanotube and conjugated polymer dispersant common distribution in organic solvent one be made dispersion soln
One.Specifically, single-walled carbon nanotube is that the single wall carbon that chemical vapour deposition technique or arc discharge method or laser evaporization method grow is received
Mitron, wherein, single-walled carbon nanotube includes metallic single-wall carbon nano-tube and semi-conductive single-walled carbon nanotubes；Conjugated polymer
Dispersant is polycarbazole；Organic solvent one is toluene or 1-METHYLPYRROLIDONE（NMP）.By single-walled carbon nanotube, polycarbazole with
Toluene or 1-METHYLPYRROLIDONE（NMP）Mixing, ultrasonic disperse processing, ultrasonic power be 20W-100W, the time for 0.5h ~
2h, dispersion soln one is made.
S2, centrifugal treating dispersion soln one, collect supernatant and by supernatant liquid filtering, obtain being coated with conjugated polymers
The semi-conductive single-walled carbon nanotubes of thing dispersant.By the above-mentioned centrifugal treating of dispersion soln one, centrifugal rotational speed be 10000 g ~
1000000 g, time are the h of 0.5 h ~ 20, collect supernatant, then again handle supernatant liquid filtering, filtered using polytetrafluoroethylene (PTFE)
Membrane filtration, the semi-conductive single-walled carbon nanotubes for being coated with conjugated polymer dispersant are stayed on filter membrane, the list of metallicity
Wall carbon nano tube and most of conjugated polymer dispersant are filtered by filter opening, especially, the conjugated polymers being filtered
Thing dispersant and the single-walled carbon nanotube of metallicity can be reentered into S1 steps, are reused conjugated polymer therein and are disperseed
Agent.
S3, offer can dissolve the organic solvent two of conjugated polymer dispersant, and conjugated polymers are coated with for cleaning
The semi-conductive single-walled carbon nanotubes of thing dispersant, obtain semi-conductive single-walled carbon nanotubes.Preferably, organic solvent two is two
Toluene or hexamethylene, dimethylbenzene or hexamethylene have to the dissolubility of conjugated polymer dispersant and semi-conductive single-walled carbon nanotubes
Difference, the conjugated polymer dispersant for being wrapped in semi-conductive single-walled carbon nanotubes surface can be dissolved.Conjugation will be coated with
The semi-conductive single-walled carbon nanotubes of polymeric dispersant are immersed in dimethylbenzene or hexamethylene, first decentralized processing, then centrifuge place
Reason, centrifugal rotational speed 10000-200000g, what is be collected into is precipitated as semi-conductive single-walled carbon nanotubes.In order to by conjugated polymers
Thing dispersant washes away as far as possible, needs to be repeated several times as this step 1.
Join shown in Fig. 2 a-2c, Fig. 2 a are the semi-conductive single-walled carbon nanotubes for being coated with conjugated polymer dispersant
The contrast of front and rear UV-vis absorption spectrum figure is cleaned with dimethylbenzene, 300-500nm region can be with from absorption spectrum
Find out, the conjugated polymer dispersant before being cleaned with dimethylbenzene is considerably beyond the scope of absorption spectrum test, cleaning
Later dispersant reduces a lot, and conjugated polymer dispersant is 2 with semi-conductive single-walled carbon nanotubes absorptance：1, this
Individual ratio can either ensure that semi-conductive single-walled carbon nanotubes keep monodisperse status in organic solvent, and and can causes on carbon pipe
The conjugated polymer dispersant of parcel is seldom.
Join Fig. 3, can be seen that from being cleaned with dimethylbenzene in front and rear Raman spectrum comparison diagram, it is generally the case that 1594cm-1's
Peak represents the characteristic absorption peak of carbazole quasi-molecule, after the absworption peak disappearance explanation of carbazole quasi-molecule is cleaned with dimethylbenzene after cleaning
The conjugated polymer dispersant of semi-conductive single-walled carbon nanotubes surface parcel is seldom；In addition, the drift condition at G peaks is often
The state that dispersant is wrapped on carbon pipe can be reflected, the film G peaks after cleaning are offset to high wave number（Blue shift）, also say
Understand that the conjugated polymer dispersant of the semi-conductive single-walled carbon nanotubes surface parcel after being cleaned with dimethylbenzene is seldom.
S4, organic solvent three is provided, semi-conductive single-walled carbon nanotubes are subjected to scattered obtained dispersion soln two.It is preferred that
Ground, organic solvent three is chloroform or dichloromethane, with chloroform or dichloromethane come dispersion steps under the booster action of ultrasonic wave
Dispersion soln two is made in the precipitation obtained in S3.
Join Fig. 4 a-4b, the single-walled carbon nanotube caliber used in present embodiment is 1.5nm, due to conjugated polymer point
The parcel of powder, semi-conductive single-walled carbon nanotubes often show 2.0nm or so caliber；Join Fig. 5 a-5b, pass through S3, S4
The semi-conductive single-walled carbon nanotubes that step obtains, its caliber is consistent with the single-walled carbon nanotube caliber wrapped up without dispersant,
For 1.5nm, illustrate that by the above method the pure semi-conductive single-walled carbon nanotubes in surface can be obtained.
S5, a substrate is provided, dispersion soln two is used into immersion or spraying or spin coating proceeding coating on the substrate,
Obtained in the substrate without dispersant semi-conductive single-walled carbon nanotubes film.In the present embodiment, it is preferable that will cut
Good silicon base is immersed directly in dispersion soln two, you can the semi-conductive single-walled carbon nanotubes film without dispersant is obtained,
Different according to the time of immersion, the density of the semi-conductive single-walled carbon nanotubes film of resulting no dispersant is also different.Separately
Outside, the silicon base of well cutting also first can be cleaned and dried with toluene or acetone, be soaked in the solution placed into step S4 after diluting
Bubble.
In order to preferably illustrate the present invention, the specific reality of no dispersant carbon nano-tube film preparation method more presented below
Apply example.
Embodiment 1
1st, the single-walled carbon nanotube that 50 mg conjugated polymers dispersants and 5 mg use chemical vapour deposition technique to prepare is weighed
It is put into beaker, then adds 100 ml toluene, be made into mixed solution；
2nd, above-mentioned mixed solution is ultrasonically treated, power setting 100W, time 0.5h, after ultrasound at centrifugation
Reason, centrifugal rotational speed are arranged to 10000g, and the time is 20 h.After the completion of centrifugation, supernatant is collected, the use of filter opening is 0.1 micron
Teflon membrane filter filtering supernatant, the semi-conductive single-walled carbon nanotubes for being coated with conjugated polymer dispersant stay in
On filter membrane, the single-walled carbon nanotube of partly conjugated polymeric dispersant and metallicity is filtered by filter opening；
3rd, by filter membrane semiconductor-on-insulator single envelope in a large amount of xylene solvents, the ultrasonic 10min in waters,
So that a large amount of conjugated polymer dispersants are dissolved in xylene solvent, half an hour is then centrifuged again, centrifugal rotational speed is arranged to
10000g, collect precipitation.
The precipitation being collected into is dissolved with a large amount of xylene solvents again, then passes through the effect solid-liquid point of centrifugation
From collection precipitation；
4th, after repeating above-mentioned step clean with tetrahydrofuran 3-4 times, divided under the booster action of ultrasonic wave with chloroform
Dissipate precipitation.
The silicon base of well cutting is soaked in solution in step 4, nothing point can be obtained according to the difference of soak time
The semi-conductive single-walled carbon nanotubes film of the different densities of powder.
Embodiment 2
1st, the single-walled carbon nanotube that 50 mg conjugated polymers dispersants and 100mg are prepared using arc discharge method is weighed to put
Enter in beaker, then add 100 ml 1-METHYLPYRROLIDONEs（NMP）, it is made into mixed solution；
2nd, above-mentioned mixed solution is ultrasonically treated, power setting 20W, time 2h, centrifugal treating after ultrasound, from
Heart rotating speed is arranged to 1000000g, and the time is 0.5 h.After the completion of centrifugation, supernatant is collected, the use of filter opening is 0.025 micron
Teflon membrane filter filtering supernatant, the semi-conductive single-walled carbon nanotubes for being coated with conjugated polymer dispersant stay in
On filter membrane, the single-walled carbon nanotube of partly conjugated polymeric dispersant and metallicity is filtered by filter opening；
3rd, by filter membrane semiconductor-on-insulator single envelope in a large amount of cyclohexane solvents, the ultrasonic 30min in waters,
So that a large amount of conjugated polymer dispersants are dissolved in cyclohexane solvent, half an hour is then centrifuged again, centrifugal rotational speed is arranged to
200000g, collect precipitation.
The precipitation being collected into is dissolved with a large amount of cyclohexane solvents again, then passes through the effect solid-liquid point of centrifugation
From collection precipitation；
4th, after repeating the above-mentioned step with cyclohexane 3-4 times, under the booster action of ultrasonic wave with dichloromethane come
Scattered precipitation.
Solution in step 4 is spin-coated in the silicon base of well cutting, according to spin-coating time, the difference of spin speed
Obtain the semi-conductive single-walled carbon nanotubes film of the different densities without dispersant.
It should be appreciated that although the present specification is described in terms of embodiments, not each embodiment only includes one
Individual independent technical scheme, this narrating mode of specification is only that those skilled in the art will should say for clarity
For bright book as an entirety, the technical scheme in each embodiment may also be suitably combined to form those skilled in the art can
With the other embodiment of understanding.
Those listed above is a series of to be described in detail only for feasibility embodiment of the invention specifically
Bright, they simultaneously are not used to limit the scope of the invention, all equivalent implementations made without departing from skill spirit of the present invention
Or change should be included in the scope of the protection.
Claims (9)
- A kind of 1. method for preparing no dispersant semi-conductive single-walled carbon nanotubes film, it is characterised in that this method include with Lower step：S1, by single-walled carbon nanotube and conjugated polymer dispersant common distribution in organic solvent one be made dispersion soln one, The conjugated polymer dispersant is polycarbazole, and the organic solvent one is toluene or 1-METHYLPYRROLIDONE；S2, centrifugal treating dispersion soln one, collect supernatant and by supernatant liquid filtering, obtain being coated with conjugated polymer point The semi-conductive single-walled carbon nanotubes of powder；S3, offer can dissolve the organic solvent two of conjugated polymer dispersant, and cleaning is coated with conjugated polymer dispersant Semi-conductive single-walled carbon nanotubes, the organic solvent two is dimethylbenzene or hexamethylene；S4, organic solvent three is provided, the semi-conductive single-walled carbon nanotubes after above-mentioned cleaning are subjected to scattered obtained dispersion soln Two, the organic solvent three is chloroform or dichloromethane；S5, a substrate is provided, dispersion soln two is coated on the substrate, described using immersion or spraying or spin coating proceeding Obtained in substrate without dispersant semi-conductive single-walled carbon nanotubes film.
- 2. method of the preparation without dispersant semi-conductive single-walled carbon nanotubes film according to claim 1, its feature exist In " single-walled carbon nanotube and conjugated polymer dispersant common distribution are made scattered to the step by S1 in organic solvent one Solution one " is specially：Single-walled carbon nanotube, conjugated polymer dispersant are mixed with toluene or 1-METHYLPYRROLIDONE, ultrasonic disperse processing, surpassed Acoustical power is 20W-100W, and dispersion soln one is made.
- 3. method of the preparation without dispersant semi-conductive single-walled carbon nanotubes film according to claim 1, its feature exist It is 10000g ~ 1000000g in, the centrifugal rotational speed in the step S2, the time is the h of 0.5 h ~ 20.
- 4. method of the preparation without dispersant semi-conductive single-walled carbon nanotubes film according to claim 3, its feature exist In being filtered in the step S2 using teflon membrane filter, be coated with the semiconductive list of conjugated polymer dispersant Wall carbon nano tube is stayed on filter membrane, and partly conjugated polymeric dispersant is filtered by filter opening.
- 5. method of the preparation without dispersant semi-conductive single-walled carbon nanotubes film according to claim 4, its feature exist In " cleaning of organic solvent two that S3 offers can dissolve conjugated polymer dispersant is coated with conjugated polymer to the step The semi-conductive single-walled carbon nanotubes of dispersant, obtain semi-conductive single-walled carbon nanotubes " be specially：The semi-conductive single-walled carbon nanotubes for being coated with conjugated polymer dispersant are immersed in-dimethylbenzene or hexamethylene In, first decentralized processing centrifugal treating, centrifugal rotational speed 10000-200000g again, what is be collected into is precipitated as semi-conductive single-walled carbon Nanotube.
- 6. method of the preparation without dispersant semi-conductive single-walled carbon nanotubes film according to claim 1, its feature exist In the substrate is cleaned and dried with toluene or acetone before being applied by dispersion soln two.
- 7. method of the preparation without dispersant semi-conductive single-walled carbon nanotubes film according to claim 1, its feature exist In before step S4, repeat step S3 is for several times.
- 8. method of the preparation without dispersant semi-conductive single-walled carbon nanotubes film according to claim 4, its feature exist In the S2 steps also include：The partly conjugated polymer being filtered is placed into step S1, recycling.
- 9. method of the preparation without dispersant semi-conductive single-walled carbon nanotubes film according to claim 1, its feature exist In the single-walled carbon nanotube is prepared using chemical vapour deposition technique or arc discharge method or laser evaporization method.
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| CN110980694A (en) * | 2019-12-06 | 2020-04-10 | 中国科学院空间应用工程与技术中心 | Preparation method of ultrahigh-purity semiconductive carbon nanotube solution |
| CN111056526B (en) * | 2019-12-30 | 2024-05-03 | 中国科学院空间应用工程与技术中心 | Method for preparing semiconductor carbon nano tube array film |
| CN111348641B (en) * | 2020-03-16 | 2022-12-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for replacing single-walled carbon nanotube solution system |
| CN112174118B (en) * | 2020-10-14 | 2022-04-22 | 西安交通大学 | Separation method of large-diameter semiconductor single-walled carbon nanotubes |
| CN112591735B (en) * | 2020-12-23 | 2022-07-26 | 北京大学 | Method for purifying semiconductor type single-walled carbon nanotube |
| CN116178886A (en) * | 2022-11-17 | 2023-05-30 | 湘潭大学 | Method for depositing semiconductor carbon nano tube film by utilizing light-driven polymer and semiconductor carbon nano tube film |
| CN117361512B (en) * | 2023-12-06 | 2024-02-20 | 苏州烯晶半导体科技有限公司 | Method for controlling density of parallel array of carbon nano tube |
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