CN110255533A - The method and its product and application of semi-conductive single-walled carbon nanotubes are prepared based on phenylating method of modifying - Google Patents

The method and its product and application of semi-conductive single-walled carbon nanotubes are prepared based on phenylating method of modifying Download PDF

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CN110255533A
CN110255533A CN201910531490.0A CN201910531490A CN110255533A CN 110255533 A CN110255533 A CN 110255533A CN 201910531490 A CN201910531490 A CN 201910531490A CN 110255533 A CN110255533 A CN 110255533A
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walled carbon
phenylating
carbon nanotubes
semi
substrate
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CN110255533B (en
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胡悦
王赢
钱金杰
黄少铭
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Wenzhou University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/159—Carbon nanotubes single-walled
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/16—Preparation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/168—After-treatment
    • C01B32/174—Derivatisation; Solubilisation; Dispersion in solvents
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00—Structure or properties of carbon nanotubes
    • C01B2202/02—Single-walled nanotubes

Abstract

The invention discloses the method that semi-conductive single-walled carbon nanotubes are prepared based on phenylating method of modifying and its product and applications.The semi-conductive single-walled carbon nanotubes the preparation method is as follows: (1) using chemical vapor deposition (CVD) in ST-cut grown on quartz single-walled carbon nanotube.(2) single-walled carbon nanotube grown in ST-cut quartz is transferred to SiO2/ Si substrate.(3) by above-mentioned SiO2/ Si substrate is immersed in benzoyl peroxide solution, with being dried with nitrogen and irradiating under raman laser after taking-up, is finally cleaned and is used with isopropanol and be dried with nitrogen.By the SiO after above-mentioned reaction2The field effect transistor of/Si substrate building single-walled carbon nanotube, the results showed that the semi-conductive single-walled carbon nanotubes purity that the method is prepared is higher than 90%.This method is convenient and efficient, reduces the influence of various negative factors brought by traditional separation method to a certain extent, proposes a kind of new research direction for the control preparation of semi-conductive single-walled carbon nanotubes.

Description

Based on phenylating method of modifying prepare semi-conductive single-walled carbon nanotubes method and its Product and application
Technical field
The present invention relates to technical field of micro nano material preparation, and in particular to semi-conductive single-walled carbon nanotubes, especially Refer to the method and its product and application that semi-conductive single-walled carbon nanotubes are prepared based on phenylating method of modifying.
Background technique
Single-walled carbon nanotube has perfect conjugated structure and excellent physical property, since 1991 by Japanese Scientists Since Iijima has found, one of the hot spot to study in nano science field has been become.Due to the excellent electricity of single-walled carbon nanotube, It is wide that the performances such as optics and mechanics have it in numerous areas such as nanometer electronic device, energy conversion, bio-sensing and composite materials Wealthy application prospect.Especially in nano-electron field, many studies have shown that, silicon base CMOS (complementary metal oxide semiconductor, Complementary Metal Oxide Semiconductor) technology in the year two thousand twenty or so is up to its limit, for number not In more alternative materials, carbon nanotube is uniquely can be by reducing device until 5 nanometer nodes continue raising system entirety The material of performance.But the single-walled carbon nanotube usually synthesized is semi-conductive single-walled carbon nanotubes and metallic single-wall carbon nanometer The mixture of pipe, wherein about containing 1/3 metallic single-wall carbon nano-tube.Due to only having semi-conductive single-walled carbon nanotubes to device The building of part contributes, and the presence of metallic single-wall carbon nano-tube will be greatly reduced the performance of these devices, therefore obtains and can use The semi-conductive single-walled carbon nanotubes array of high density single-wall carbon nano tube part is constructed, to semi-conductive single-walled carbon nanotubes Property and its device performance research have very important value and significance.
Summary of the invention
It is partly led the technical problem to be solved by the embodiment of the invention is that providing a kind of prepare based on phenylating method of modifying The method of body single-walled carbon nanotube.This process employs benzoyl peroxides generated under the irradiation of raman laser phenyl and with Single-walled carbon nanotube reacts.Due to the difference of metal/semiconductor single-walled carbon nanotube reactivity, we be can choose Property with metallic single-wall carbon nano-tube carry out phenylating react, so that it is changed into transistor, to make whole single wall carbon Semiconducting behavior is presented in nanotube.
To achieve the above object, the technical scheme is that invention provides and a kind of prepares semi-conductive single-walled carbon nanometer The method of pipe, comprising:
Step S1 is using chemical vapor deposition (CVD) in ST-cut grown on quartz single-walled carbon nanotube；
The step S1 single-walled carbon nanotube grown in ST-cut quartz is transferred to SiO by step S22In/Si substrate；
Step S3 is by the SiO in step S22/ Si substrate is immersed in benzoyl peroxide solution, is taken out and is blown with nitrogen It is dry, it then is allowed to react with the irradiation of 532nm raman laser, is finally cleaned and used with ethyl alcohol and be dried with nitrogen；
Step S1 includes the following steps:
Before growing single-wall carbon nano tube, the ST-cut quartz is pre-processed；
The pretreatment of ST-cut quartz: respectively it is cleaned by ultrasonic 20min in ultrapure water, acetone, ethyl alcohol and ultrapure water, is dried with nitrogen Afterwards, constant temperature 8h after rising to 1100 DEG C by room temperature in 3h, then 300 DEG C are cooled in 15h, then be naturally cooling to room temperature；
The catalyst of iron, cobalt, nickel, copper as growing single-wall carbon nano tube preferentially selects iron herein.Iron/ethanol solution Content be 0.01-0.1mmol/L, preferably 0.05mmol/L；
In the chemical vapor deposition step method, carbon source is carbonaceous gas or vapour pressure is larger and what is easily cracked contains carbon liquid Body, concretely C2H4, ethyl alcohol, CH4Or isopropanol, ethyl alcohol is preferentially selected herein, and ethyl alcohol carbon source is by bubbling argon ethyl alcohol What solution generated；
The gas flow of carbon source is 10sccm-500sccm, preferentially selects 35sccm herein；
Reducing atmosphere is hydrogen atmosphere；The gas flow of hydrogen is 30-500sccm, preferential herein to select 300sccm；
Carrier gas used in reducing atmosphere is argon gas；The air flow rate of the carrier gas is 50-500sccm, herein preferential choosing Use 300sccm；
Growth temperature is 600 DEG C -900 DEG C, and specially 840 DEG C, growth time is 1min~1h, specially 30min；
Step S1 further includes following steps: after the chemical vapor deposition step, system being cooled down；The cooling tool Body is that Temperature fall or process control cool down.
Step S2 includes the following steps:
Before shifting single-walled carbon nanotube, by the SiO2/ Si substrate is pre-processed；
SiO2/ Si substrate is respectively cleaned by ultrasonic 20min in ultrapure water, acetone, ethyl alcohol and ultrapure water, after being dried with nitrogen, uses Oxygen plasma cleaning system cleans 5-20min, preferably 15min；
PMMA, spin-coating time 20-60s, preferably 40s are coated on ST-cut quartz using sol evenning machine, and is dried, the time For 1-5min, preferably 3min；
Using HF as transfer solution, HF concentration of polymer solution be 1%-10%, preferably 5%；
It is transferred to SiO2PMMA film (adhesion single-walled carbon nanotube) is dried by thermal station in/Si substrate, and drying time is 1h-4h, preferably 2h；
SiO2PMMA film (adhesion single-walled carbon nanotube) impregnates in acetone in/Si substrate, removes PMMA, soaking time For 1min-10min, preferably 5min；
Step S3 includes the following steps:
By above-mentioned SiO2/ Si substrate is immersed in benzoyl peroxide solution, solution concentration 0.1mmol/L-1mmol/ L, preferably 0.5mmol/L, soaking time 10min-60min, preferably 30min, 532nm laser power are 0.5mW-5mW, preferably 2mW, irradiation time 10s-2min, preferably 1min；
The semi-conductive single-walled carbon nanotubes of the modification of phenylating prepared by the present invention include the following steps:
Using electron beam lithography (EBL) in SiO2It is positioned in/Si substrate and Cr/Au is deposited to prepare single The FET device of pipe, Cr with a thickness of 1-5nm, preferably 3nm, Au with a thickness of 30-80nm, preferably 60nm.
Electrical testing is carried out using FET device of the probe station to preparation, the results showed that the semiconductive that the method is prepared Single wall carbon nano pipe purity is higher than 90%.
Single-walled carbon nanotube phenylating is a kind of novel carbon pipe " separation " method, is different from traditional method, the method Selection does not remove metal tube, and only makes it that semiconducting behavior be presented, thus make whole single-walled carbon nanotube that semiconductive be presented, The visible experimental data of the embodiment of the present invention of the specific effect of the present invention.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this Some embodiments of invention, for those of ordinary skill in the art, without any creative labor, according to These attached drawings obtain other attached drawings and still fall within scope of the invention.
Fig. 1 single-walled carbon nanotube shows phenylating schematic diagram；
Wherein, (Fig. 2 a, Fig. 2 b) single single-walled carbon nanotube FET device SEM image, (Fig. 2 c) is in V by Fig. 2dsWhen=1V Typical case I before and after single single-walled carbon nanotube phenylatingds-VgCurve, (Fig. 2 d, Fig. 2 e) single-walled carbon nanotube horizontal array FET Device SEM image, (Fig. 2 f) is in VdsTypical case I before and after single-walled carbon nanotube horizontal array phenylating when=1Vds-VgCurve, (figure 2g, Fig. 2 h) single wall carbon nano-tube film FET device SEM image, (Fig. 2 i) is in VdsSingle wall carbon nano-tube film phenylating when=1V Front and back typical case Ids-VgCurve；
Fig. 3 wherein I before and after (Fig. 3 a) single-walled carbon nanotube horizontal array phenylatingon/IoffRatio statistics, (Fig. 3 b, Fig. 3 c) Raman spectrum before and after single-walled carbon nanotube phenylating；
Fig. 4 wherein typical case I before (Fig. 4 a) single-walled carbon nanotube phenylating, after phenylating and after annealingds-VgCurve, (figure 4b, Fig. 4 c, Fig. 4 d) before single-walled carbon nanotube phenylating, Raman spectrum after phenylating and after annealing.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, the present invention is made into one below in conjunction with attached drawing Step ground detailed description.
Embodiment 1
Single single-walled carbon nanotube phenylating modification
(1) SiO is selected2Substrate of/Si the substrate as carbon nano tube growth, successively in ultrapure water, acetone, ethyl alcohol and ultrapure Respectively it is cleaned by ultrasonic 20min in water, after being dried with nitrogen, cleans 15min with oxygen plasma cleaning system；
(2) in SiO2In the load on one side of/Si substrate then catalyst Fe is placed in chemical gas-phase deposition system, catalyst Band is warming up to 950 DEG C perpendicular to airflow direction, is passed through 300sccm argon gas 5min, 300sccm hydrogen, finally uses 35sccm argon Gas bell ethyl alcohol grows 30min, after the completion of growth, closes the argon gas of drum ethyl alcohol, hydrogen and remaining argon gas is kept to continue to lead to Enter, be down to room temperature naturally, so far air-flow directional single-wall carbon nanotube growth terminates.
Fig. 2 a, 2b are the SEM images of single single-walled carbon nanotube FET device, and Fig. 2 c is in VdsSingle single wall carbon when=1V Typical case I before and after nanotube phenylatingds-VgCurve becomes having as the result is shown after metallic single-wall carbon nano-tube phenylating and partly lead The single-walled carbon nanotube of body performance.
Embodiment 2
The modification of single-walled carbon nanotube horizontal array phenylating
(1) select substrate of the ST-cut quartz substrate as carbon nano tube growth, successively ultrapure water, acetone, ethyl alcohol and Respectively it is cleaned by ultrasonic 20min in ultrapure water, then is dried up with high pure nitrogen.The substrate cleaned up is put into Muffle furnace, in air High annealing, 3h are raised to 900 DEG C, are cooled to 300 DEG C in 900 DEG C of constant temperature 8h, then 15h, Temperature fall is cooling, this process is used to repair The multiple lattice defect due to being generated in process of manufacture.
(2) upper catalyst Fe is loaded in ST-cut quartz to be then placed in chemical gas-phase deposition system, be warming up to 840 DEG C, It is passed through 300sccm argon gas 5min, 300sccm hydrogen, finally uses 35sccm bubbling argon ethyl alcohol, grows 30min, growth is completed Afterwards, the argon gas of drum ethyl alcohol is closed, keeps hydrogen and remaining argon gas to continue to be passed through, is down to room temperature naturally.
(3) single-walled carbon nanotube on ST-cut quartz is transferred to SiO2In/Si substrate, field effect transistor is constructed, Carry out electrical performance testing.Fig. 2 d, 3e are the SEM images of single-walled carbon nanotube horizontal array FET device, and Fig. 2 f is in Vds=1V When single-walled carbon nanotube horizontal array phenylating before and after typical Ids-VgCurve, as the result is shown after single-walled carbon nanotube phenylating Semiconducting behavior is presented.Fig. 3 a is I before and after single-wall carbon nanotube array phenylatingon/IoffRatio statistics, shows this phenylating side Method prepares the semi-conductive single-walled carbon nanotubes horizontal array of 90% or more purity.Fig. 3 b, 3c are single-walled carbon nanotube phenyl Change front and back Raman spectrum, single-walled carbon nanotube is without the peak D before phenylating, it was demonstrated that single-walled carbon nanotube is flawless before reacting.And Occurs the peak D after reaction, D/G is stronger, illustrates that single-walled carbon nanotube realizes phenylating；
Embodiment 3
The modification of single wall carbon nano-tube film phenylating
(1) SiO is selected2Substrate of/Si the substrate as carbon nano tube growth, successively in ultrapure water, acetone, ethyl alcohol and ultrapure Respectively it is cleaned by ultrasonic 20min in water, after being dried with nitrogen, cleans 15min with the particles cleaning system such as oxygen；
(2) in SiO2In the load of/Si substrate then catalyst Fe is placed in chemical gas-phase deposition system, is warming up to 840 DEG C, it is passed through 300sccm argon gas 5min, 300sccm hydrogen, finally uses 35sccm bubbling argon ethyl alcohol, 30min is grown, has grown Cheng Hou closes the argon gas of drum ethyl alcohol, keeps hydrogen and remaining argon gas to continue to be passed through, is down to room temperature naturally.
Fig. 2 g, 3h are the SEM images of single wall carbon nano-tube film FET device, and Fig. 2 i is in VdsSingle when=1V Typical case I before and after pipe film phenylatingds-VgCurve becomes after showing single wall carbon nano-tube film phenylating with semiconducting behavior Single wall carbon nano-tube film.
Single-walled carbon nanotube after phenylating is made annealing treatment, Fig. 4 a be single-walled carbon nanotube phenylating before, phenyl After change and annealing after typical case Ids-VgCurve, Cong Tuzhong is we have found that single-walled carbon nanotube is restored to original property after annealing. Fig. 4 b, 4c, 4d be phenylating before, Raman spectrum after phenylating and after annealing, Cong Tuzhong we have found that the peak D disappears after annealing, Single-walled carbon nanotube restores to the original state again.
The above disclosure is only the preferred embodiments of the present invention, cannot limit the right model of the present invention with this certainly It encloses, therefore equivalent changes made in accordance with the claims of the present invention, is still within the scope of the present invention.

Claims (10)

1. a kind of method for preparing semi-conductive single-walled carbon nanotubes based on phenylating method of modifying, it is characterised in that including following Step:
S1, growing single-wall carbon nano tube is being gone up in substrate using chemical vapour deposition technique；
S2, the single-walled carbon nanotube grown in step S1 is transferred to SiO2In/Si substrate；
S3, by the SiO with single-walled carbon nanotube in step S22/ Si substrate is immersed in benzoyl peroxide solution, is taken out Afterwards with being dried with nitrogen and being irradiated under raman laser, generates phenyl and react with single-walled carbon nanotube, finally use isopropanol It cleans and uses and be dried with nitrogen, obtain the semi-conductive single-walled carbon nanotubes of phenylating modification.
2. a kind of side for preparing semi-conductive single-walled carbon nanotubes based on phenylating method of modifying according to claim 1 Method, it is characterised in that: by SiO in step S32/ Si substrate is immersed in benzoyl peroxide solution, concentration 0.1mmol/L- 1mmol/L, soaking time 10min-60min irradiate under 532nm raman laser, power density 0.5mW-4mW, irradiation Time is 10s-2min.
3. a kind of side for preparing semi-conductive single-walled carbon nanotubes based on phenylating method of modifying according to claim 1 Method, it is characterised in that: the material of the substrate in the step S1 is r-cut quartz, ST-cut quartz, SiO2/ Si, r face α oxidation Aluminium, the face a alpha-aluminium oxide or magnesia.
4. a kind of side for preparing semi-conductive single-walled carbon nanotubes based on phenylating method of modifying according to claim 1 Method, it is characterised in that: substrate described in step S1 is ST-cut quartz, is carrying out chemical vapour deposition technique growing single-wall carbon Pre-treatment is also carried out before nanotube, which is: successively each ultrasound in ultrapure water, acetone, ethyl alcohol and ultrapure water 20min is cleaned, then is dried up with high pure nitrogen, the substrate cleaned up is put into Muffle furnace, air high temperature annealing, 3h is raised to 900 DEG C, 300 DEG C are cooled in 900 DEG C of constant temperature 8h, then 15h, Temperature fall is cooling.
5. a kind of side for preparing semi-conductive single-walled carbon nanotubes based on phenylating method of modifying according to claim 1 Method, it is characterised in that: catalyst precursor used by chemical vapour deposition technique is Fe, Co, Ni, Cu, Au in step S1, Mo, Zn, W, Ru, Cr, Rh, V, Ti, Al, Mg or Pd, concentration are metal/ethanol solution content 0.05mmol/L.
6. a kind of side for preparing semi-conductive single-walled carbon nanotubes based on phenylating method of modifying according to claim 1 Method, it is characterised in that: chemical deposition, at 840 DEG C, 300sccm argon will be carried out by substrate of ST-cut quartz in the step S1 Gas is grown under 300sccm hydrogen, and ethyl alcohol is to do carrier gas by argon gas to carry it into reaction cavity as carbon source, and flow is 10~500sccm, growth time can be 1min~1h.
7. a kind of side for preparing semi-conductive single-walled carbon nanotubes based on phenylating method of modifying according to claim 1 Method, it is characterised in that: SiO in step S22/ Si substrate is also pre-processed before carrying out transfer single-walled carbon nanotube, side Method is respectively to be cleaned by ultrasonic 20min in ultrapure water, acetone, ethyl alcohol and ultrapure water, after being dried with nitrogen, cleans system with oxygen plasma System cleaning 5-20min.
8. a kind of side for preparing semi-conductive single-walled carbon nanotubes based on phenylating method of modifying according to claim 1 Method, it is characterised in that: using HF as the solution of transfer in step S2, HF concentration of polymer solution is 1%-10%.
9. a kind of semi-conductive single-walled carbon nanotubes of the modification of the phenylating as prepared by one of claim 1-8 method.
10. a kind of semi-conductive single-walled carbon nanotubes based on phenylating as claimed in claim 9 modification construct single wall in building Application on the field effect transistor of carbon nanotube.
CN201910531490.0A 2019-06-19 2019-06-19 Method for preparing semiconductor single-walled carbon nanotube based on phenylation modification method, product and application thereof Active CN110255533B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113328038A (en) * 2021-04-21 2021-08-31 温州大学 Preparation method of graphene-carbon nanotube heterojunction

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120171103A1 (en) * 2009-06-26 2012-07-05 Nanyang Technological University Method for modifying electrical properties of carbon nanotubes

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120171103A1 (en) * 2009-06-26 2012-07-05 Nanyang Technological University Method for modifying electrical properties of carbon nanotubes

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113328038A (en) * 2021-04-21 2021-08-31 温州大学 Preparation method of graphene-carbon nanotube heterojunction
CN113328038B (en) * 2021-04-21 2022-08-30 温州大学 Preparation method of graphene-carbon nanotube heterojunction

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