CN113213454A - Method for preparing single-walled carbon nanotube by taking graphene as catalyst - Google Patents
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- CN113213454A CN113213454A CN202110430294.1A CN202110430294A CN113213454A CN 113213454 A CN113213454 A CN 113213454A CN 202110430294 A CN202110430294 A CN 202110430294A CN 113213454 A CN113213454 A CN 113213454A
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Abstract
The invention discloses a method for preparing a single-walled carbon nanotube and an all-carbon heterojunction by taking graphene as a catalyst, which comprises the following steps of: s1, ultrasonic cleaning the growth substrate in ultrapure water, acetone, ethanol and ultrapure water in sequence; s2, drying with high-purity nitrogen; s3, putting the cleaned substrate into a muffle furnace, annealing at high temperature in air, heating to 900 ℃ for 2h, keeping the temperature at 900 ℃ for 8 h, cooling to 300 ℃ for 10 h, and naturally cooling; mechanically stripping graphene on the treated growth substrate, wherein the number of layers is 1-10; growing carbon nanotubes on the substrate deposited with the graphene, and introducing hydrogen and a carbon source into a chemical vapor deposition system to grow single-walled carbon nanotubes; and step four, manufacturing the all-carbon heterojunction provided by the invention into a field effect transistor device according to the following preparation flow. The single-walled carbon nanotube does not contain metal in the process, and can be used for preparing a field effect transistor device with stable performance.
Description
Technical Field
The invention relates to the field of single-walled carbon nanotube preparation, in particular to a method for preparing a single-walled carbon nanotube by taking graphene as a catalyst.
Background
Single-walled carbon nanotubes (SWNTs) are all composed of carbon atoms, and the geometric structure can be regarded as being formed by single-layer graphene curls, and the structure determines the properties, so that the single-walled carbon nanotubes have excellent electronic, mechanical and mechanical properties. Meanwhile, according to the curled structure, the single-walled carbon nanotube has three types of armchair type, sawtooth type and chirality; single-walled carbon nanotubes have a semiconductor type and a metal type (including a metalloid type and a metal type) in terms of electronic structure.
The SWNTs have great potential application value in the aspects of electronics, optical electronics, sensors, drug delivery, catalyst support, composite materials and the like. Theoretical and experimental studies have shown that controlled synthesis of SWNTs can be achieved to some extent by conscious selection of the catalyst.
At present, various metal catalysts have been developed to prepare single-walled carbon nanotubes controllably, such as Fe, Co, Ni, Au, Ag, Cu and Al and their alloys. However, metal species remaining in SWNTs products present significant disadvantages for both intrinsic property characterization (e.g., chemical, electronic and magnetic, thermal stability and toxicity) and application exploration (e.g., catalyst support, biology and medicine) that lead to SWNTs. These metal particle residues also have a number of adverse effects on SWNT-based electronic devices. And therefore often require time consuming and extensive post-processing before application. However, to date, it has been a difficult problem to completely remove metal catalysts from SWNTs samples without introducing defects and contamination. Therefore, the preparation of single-walled carbon nanotubes using non-metallic catalysts is highly desirable.
And preparing the semiconductor single-walled carbon nanotube by using a non-metallic catalyst SiC. The silicon carbide nano-particles obtained by the ion sputtering method are used as a catalyst, a carbon cap is formed by utilizing the self decomposition of trace atoms on the surface of the catalyst in the pretreatment process, and the high-activity metallic carbon cap is removed by utilizing the etching effect of hydrogen, so that the controllable growth of the semiconductor-enriched single-walled carbon nano-tube without metal impurities is realized.
The main problem of the prior art is that the metal catalyst is used for growing the single-walled carbon nanotube, so that metal residues are generated, and the performance of subsequent devices is influenced.
Disclosure of Invention
The invention aims to provide a method for preparing a single-walled carbon nanotube by taking graphene as a catalyst, and aims to solve the technical problem that the performance of a subsequent device is influenced because metal residues exist when the single-walled carbon nanotube grows by a metal catalyst.
In order to achieve the purpose, the invention adopts the following technical scheme: the invention provides a method for preparing a single-walled carbon nanotube by taking graphene as a catalyst,
step one, processing a growth substrate, comprising the following steps:
s1, ultrasonic cleaning the growth substrate in ultrapure water, acetone, ethanol and ultrapure water in sequence;
s2, drying by using high-purity nitrogen;
s3, putting the cleaned substrate into a muffle furnace, annealing at high temperature in air, heating to 900 ℃ for 2h, keeping the temperature of 900 ℃ for 8 h, cooling to 300 ℃ for 10 h, and naturally cooling;
mechanically stripping graphene on the treated growth substrate, wherein the number of layers is 1-10;
growing carbon nanotubes on the substrate deposited with the graphene, and introducing hydrogen and a carbon source into a chemical vapor deposition system to grow single-walled carbon nanotubes;
and step four, manufacturing the all-carbon heterojunction provided by the invention into a field effect transistor device according to the following preparation flow.
Further, in the step one, the growth substrate is SiO2The quartz crystal is made of/Si or ST-cut quartz or r-cut quartz or alpha alumina of a surface or alpha alumina of r surface or magnesium oxide.
Furthermore, the catalyst treatment and the growth of the single-walled carbon nanotube both need hydrogen with certain concentration and etching effect, the hydrogen flow is 30sccm to 300sccm,
further, the hydrogen flow rate is 100sccm to 300 sccm.
Further, in the second step, the graphene is mechanically stripped on the processed growth substrate, and the number of layers is 1-4.
Further, in the third step, the growth temperature is 600-900 ℃, specifically 800-850 ℃, and the growth time is 1 min-1 h.
Further, in the third step, the growth time is 10-30 min.
Further, in the chemical vapor deposition step, the carbon source is carbon-containing gas or carbon-containing liquid with large vapor pressure and easy cracking, and is C2H4 or ethanol or CH4 or isopropanol.
Further, ethanol is used as a carbon source. The ethanol carbon source was generated by bubbling an ethanol solution through argon.
Further, Electron Beam Lithography (EBL) is used on SiO2Positioning an all-carbon heterojunction on a/Si substrate and evaporating Cr/Au to prepare the field effect transistor device of the single-walled carbon nanotube, wherein the thickness of Cr is 3 nm, and the thickness of Au is 60 nm.
And further, electrically testing the prepared field effect transistor device by using the probe station.
The invention has the beneficial effects that:
the method for preparing the single-walled carbon nanotube by using the graphene as the catalyst, which is provided by the invention, has no report on the preparation of the single-walled carbon nanotube by using the graphene, and provides a brand new thought for the preparation of the single-walled carbon nanotube. And the process of preparing the single-walled carbon nanotube does not contain metal, and can be used for preparing a field effect transistor device with stable performance.
According to the method for preparing the single-walled carbon nanotube by using the graphene as the catalyst, the graphene is obtained by mechanical stripping, and the graphene with different layers can be grown into the single-walled carbon nanotube by adjusting the growth temperature and the growth atmosphere, so that the controllable growth of the single-walled carbon nanotube is realized.
And 3, the graphene obtained by mechanical stripping is used as a catalyst to controllably prepare the single-walled carbon nanotube, so that the preparation process is free of metal pollution and is suitable for constructing nano electronic devices.
And 4, the graphene is used as a catalyst to grow the single-walled carbon nanotube, so that an all-carbon heterojunction is directly formed, the process for preparing the heterojunction is simplified, and the method can be applied to the preparation of a field effect transistor.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the invention. The primary objects and other advantages of the invention may be realized and attained by the instrumentalities particularly pointed out in the specification.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings.
Fig. 1 is a schematic diagram of growing single-walled carbon nanotubes and forming an all-carbon heterojunction using graphene as a catalyst.
FIG. 2 is an SEM image of the growth results of example one.
Fig. 3a, 3b, and 3c are characterization graphs of the growth results in the first example, in which fig. 3a is an AFM image, fig. 3b is a height curve of graphene, and fig. 3c is a height curve of single-walled carbon nanotubes.
FIG. 4 is an SEM photograph showing the growth result in example two
Fig. 5a, 5b, and 5c are characterization graphs of the growth results in example two, in which fig. 5a is an AFM image, fig. 5b is a height curve of graphene, and fig. 5c is a height curve of single-walled carbon nanotubes.
FIGS. 6a and 6b are SEM images of the growth results in example three. FIGS. 6a and 6b are SEM images of different regions of the same growth substrate.
Fig. 7 is a schematic diagram of a device.
Fig. 8a-8d are device electrical test results. Fig. 8a is a graph of transfer curves of graphene and carbon nanotubes, fig. 8b and 8c are graphs of output curves of graphene and carbon nanotubes, respectively, and fig. 8d is a graph of output curves of junctions under different gate voltages.
Detailed Description
The technical solutions of the present invention are described in detail below by examples, and the following examples are only exemplary and can be used only for explaining and illustrating the technical solutions of the present invention, but not construed as limiting the technical solutions of the present invention.
For the first time, graphene is used as a catalyst to grow the single-walled carbon nanotube. The invention utilizes carbon atoms at the edge of graphene which is mechanically stripped on a growth substrate to form a carbon cap under the atmosphere of high-temperature hydrogen and a carbon source and then grow the single-walled carbon nanotube. Then, an all-carbon heterojunction is obtained, and the electrical properties of the heterojunction are explored.
The working principle is as follows: the invention adopts a chemical vapor deposition method to directly grow the single-walled carbon nanotube, obtains single-layer or multi-layer graphene on a growth substrate by using a mechanical stripping (adhesive tape) method, removes impurities at high temperature, utilizes hydrogen to etch the edge of the graphene into a carbon cap, and further performs the growth of the single-walled carbon nanotube in the atmosphere of a carbon source.
The invention provides a method for preparing a single-walled carbon nanotube by taking graphene as a catalyst,
step one, processing a growth substrate, comprising the following steps:
s1, ultrasonic cleaning the growth substrate in ultrapure water, acetone, ethanol and ultrapure water in sequence;
s2, drying by using high-purity nitrogen;
s3, putting the cleaned substrate into a muffle furnace, annealing at high temperature in air, heating to 900 ℃ for 2h, keeping the temperature of 900 ℃ for 8 h, cooling to 300 ℃ for 10 h, and naturally cooling; the growth substrate is SiO2The quartz crystal is made of/Si or ST-cut quartz or r-cut quartz or alpha alumina of a surface or alpha alumina of r surface or magnesium oxide.
Mechanically stripping graphene on the treated growth substrate, wherein the number of layers is 1-10; the number of layers is preferably 1 to 4.
Growing carbon nanotubes on the substrate deposited with the graphene, and introducing hydrogen and a carbon source into a chemical vapor deposition system to grow single-walled carbon nanotubes; the growth temperature is 600-900 ℃, particularly 800-850 ℃, and the growth time is 1 min-1 h. In a particular embodiment, the growth time is preferably 10-30 min.
And step four, manufacturing the all-carbon heterojunction provided by the invention into a field effect transistor device according to the following preparation flow.
The catalyst treatment and the growth of the single-walled carbon nanotube both need hydrogen with certain concentration and etching effect, and the hydrogen flow is 30sccm-300sccm, preferably 100sccm-300 sccm.
In the chemical vapor deposition step, the carbon source is carbon-containing gas or carbon-containing liquid which has high vapor pressure and is easy to crack and is C2H4Or ethanol or CH4Or isopropyl alcohol.
Wherein the carbon source is ethanol. The ethanol carbon source was generated by bubbling an ethanol solution through argon.
And positioning an all-carbon heterojunction on a SiO2/Si substrate by using an Electron Beam Lithography (EBL) technology and evaporating Cr/Au to prepare the field effect transistor device of the single-walled carbon nanotube, wherein the thickness of Cr is 3 nm, and the thickness of Au is 60 nm. And electrically testing the prepared field effect transistor device by using the probe station.
The semiconductor device containing the graphene-carbon nanotube heterojunction comprises electrodes, an insulating growth substrate, single-layer graphene and carbon nanotubes, wherein the single-layer graphene and the carbon nanotubes are arranged on the insulating growth substrate, one end of each carbon nanotube is abutted to the edge of the graphene, at least two electrodes are arranged on the substrate, and the two electrodes are arranged on the carbon nanotubes.
Example one
In SiO2and/Si substrate using single-layer graphene as catalyst to grow carbon nano tube. As shown in fig. 1.
The method comprises the following specific steps:
step one, selecting SiO2a/Si substrate, which is cut into 6mm x 6mm size, and is pretreated as follows:
1) ultrasonically cleaning a growth substrate in ultrapure water, acetone, ethanol and ultrapure water in sequence;
2) blowing the mixture by using high-purity nitrogen;
step two, treating the treated SiO2And mechanically stripping graphene on the Si growth substrate, wherein the number of layers is one. (height view as in FIG. 3 b)
And step three, growing the carbon nano tube on the substrate with the graphene.
And (4) placing the growth substrate with the single-layer graphene obtained in the step two in a chemical vapor deposition system, and heating to the growth temperature of 830 ℃ at the heating rate of 40 ℃/min under the protection of argon, wherein the flow of the argon is 300 sccm. And continuously introducing 100sccmH for 25min to reduce and separate out catalyst nanoparticles. And then introducing 50sccmAr/EtOH (Ar/EtOH refers to introducing ethanol liquid in the form of argon Ar bubbling) to start oriented growth of the single-walled carbon nanotube, wherein the growth time is 10min, after the growth is finished, stopping introducing the carbon source, keeping introducing hydrogen and argon continuously, and naturally cooling to room temperature to obtain the carbon nanotube provided by the invention. (as shown in FIG. 2)
Fig. 3a, 3b and 3c are characterization diagrams of growth results, wherein fig. 3a is an AFM diagram, fig. 3b is a height curve of graphene, and fig. 3c is a height curve of single-walled carbon nanotubes.
Example two
In SiO2and/Si substrate using three layers of graphene as catalyst to grow carbon nano tube. As shown with reference to fig. 4.
Step one, the same as step one of the first embodiment.
Step two, treating the treated SiO2The graphene is mechanically stripped on the/Si growth substrate, and the number of layers is three (the height diagram is shown in figure 5 b). Specifically, 5a, 5b, and 5c are characterization graphs of the growth results in example two, where fig. 5a is an AFM image, fig. 5b is a height curve of graphene, and fig. 5c is a height curve of single-walled carbon nanotubes.
And step three, growing the carbon nano tube on the substrate with the graphene.
And (4) placing the growth substrate with the single-layer graphene obtained in the step two in a chemical vapor deposition system, and heating to the growth temperature of 830 ℃ at the heating rate of 40 ℃/min under the protection of argon, wherein the flow of the argon is 300 sccm. And continuously introducing 100sccmH for 25min to reduce and separate out catalyst nanoparticles. And then introducing 40sccmAr/EtOH (Ar/EtOH refers to introducing ethanol liquid in the form of argon Ar bubbling) to start oriented growth of the single-walled carbon nanotube, wherein the growth time is 10min, after the growth is finished, stopping introducing the carbon source, keeping introducing hydrogen and argon continuously, and naturally cooling to room temperature to obtain the carbon nanotube provided by the invention, which is shown in figure 4.
EXAMPLE III
Growing a carbon nano tube on an ST-cut quartz substrate by using single-layer graphene as a catalyst.
Selecting an ST-cut quartz substrate, and pretreating the ST-cut quartz substrate, wherein the step of treating the growth substrate comprises the following steps:
1) ultrasonically cleaning a growth substrate in ultrapure water, acetone, ethanol and ultrapure water in sequence;
2) blowing the mixture by using high-purity nitrogen;
3) putting the cleaned substrate into a muffle furnace, annealing at high temperature in the air, heating to 900 ℃ for 2h, keeping the temperature of 900 ℃ for 8 h, cooling to 300 ℃ for 10 h, and naturally cooling;
and step two, mechanically stripping different layers of graphene on the processed ST-cut quartz growth substrate, wherein the number of the layers is 1-10.
And step three, growing the carbon nano tube on the substrate with the graphene.
And (4) placing the growth substrate with the single-layer graphene obtained in the step two in a chemical vapor deposition system, and heating to the growth temperature of 830 ℃ at the heating rate of 40 ℃/min under the protection of argon, wherein the flow of the argon is 300 sccm. And continuously introducing 100sccmH for 25min to reduce and separate out catalyst nanoparticles. And then introducing 30sccmAr/EtOH (Ar/EtOH refers to introducing ethanol liquid in the form of argon Ar bubbling) to start oriented growth of the single-walled carbon nanotube, wherein the growth time is 10min, after the growth is finished, stopping introducing the carbon source, keeping introducing hydrogen and argon continuously, and naturally cooling to room temperature to obtain the carbon nanotube provided by the invention, wherein the characterization is shown in FIGS. 6a and 6 b.
Example four
Electrical characterization of all-carbon heterojunctions
The all-carbon heterojunction provided by the invention is made into a field effect transistor device according to the following preparation process; as shown in fig. 7.
Using Electron Beam Lithography (EBL) to obtain SiO with all-carbon heterojunction in step one2Positioning an all-carbon heterojunction on a Si substrate and evaporating Cr/Au to prepare the field effect transistor device of the single-walled carbon nanotube, wherein the thickness of Cr is 3 nm, and the thickness of Au is 60 nm; preparation by using probe table pairThe field effect transistor device of (a) was electrically tested, and the results of the testing are shown in FIG. 8. As can be seen from the transfer curve of the carbon nanotube of FIG. 8a, the single-walled carbon nanotube tested was a semiconducting single-walled carbon nanotube (on-off ratio of about 10^ 6). As shown in fig. 8b, c, the output curves of the carbon nanotubes and graphene are symmetrical, and the linear behavior of the curves indicates the ohmic contact of the carbon nanotubes and graphene with the Au/Cr electrode. In contrast, the output curve across the junction (fig. 8 d) is highly non-linear and asymmetric with a rectification ratio of 280, showing the superiority of the device in other applications as a diode, etc.
The method provided by the invention utilizes carbon atoms at the edge of graphene which is mechanically stripped on a growth substrate to form a carbon cap under the atmosphere of high-temperature hydrogen and a carbon source and then grow the single-walled carbon nanotube. The controllable preparation of the single-walled carbon nanotube grown by the nonmetal catalyst graphene is realized.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that may be made by those skilled in the art within the technical scope of the present invention will be covered by the scope of the present invention.
Claims (10)
1. The method for preparing the single-walled carbon nanotube by taking the graphene as the catalyst is characterized by comprising the following steps of:
step one, processing a growth substrate, comprising the following steps:
s1, ultrasonic cleaning the growth substrate in ultrapure water, acetone, ethanol and ultrapure water in sequence;
s2, drying by using high-purity nitrogen;
s3, putting the cleaned substrate into a muffle furnace, annealing at high temperature in air, heating to 900 ℃ for 2h, keeping the temperature of 900 ℃ for 8 h, cooling to 300 ℃ for 10 h, and naturally cooling;
mechanically stripping graphene on the treated growth substrate, wherein the number of layers is 1-10;
growing carbon nanotubes on the substrate deposited with the graphene, and introducing hydrogen and a carbon source into a chemical vapor deposition system to grow single-walled carbon nanotubes;
and step four, obtaining a finished product of the all-carbon heterojunction.
2. The method of claim 1, wherein in step one, the growth substrate is SiO2The quartz crystal is made of/Si or ST-cut quartz or r-cut quartz or alpha alumina of a surface or alpha alumina of r surface or magnesium oxide.
3. The method of claim 1, wherein the catalyst treatment and the growth of the single-walled carbon nanotubes require hydrogen gas with a concentration of 30sccm to 300sccm for etching.
4. The method according to claim 3, wherein the hydrogen flow rate is 100sccm to 300 sccm.
5. The method of claim 1, wherein in the second step, the graphene is mechanically exfoliated on the treated growth substrate with 1-4 layers.
6. The method as claimed in claim 1, wherein the growth temperature in step three is 600-.
7. The method of claim 6, wherein in step three, the growth time is 10-30 min.
8. The method of claim 1, wherein the carbon source in the CVD process is a carbon-containing gas or a liquid having a relatively high vapor pressure and being easily cracked, and is C2H4Or ethanol or CH4Or isopropyl alcohol.
9. The method of claim 1, wherein the finished all-carbon heterojunction of step four is formed into a field effect transistor device using electron beam lithography on SiO2Positioning an all-carbon heterojunction on a/Si substrate and evaporating Cr/Au to prepare the field effect transistor device of the single-walled carbon nanotube, wherein the thickness of Cr is 3 nm, and the thickness of Au is 60 nm.
10. The method of claim 9, wherein the fabricated field effect transistor device is electrically tested using a probe station.
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| CN116544279A (en) * | 2023-04-30 | 2023-08-04 | 天津大学 | All-carbon graphene device and preparation method thereof |
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| CN111312830A (en) * | 2020-05-08 | 2020-06-19 | 南京晶碳纳米科技有限公司 | Carbon nanotube/graphene van der Waals heterojunction photoelectric device, construction method and application thereof |
| CN111943171A (en) * | 2020-08-21 | 2020-11-17 | 温州大学 | Controllable preparation method of high-density single-walled carbon nanotube horizontal array |
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| CN113759150A (en) * | 2021-09-09 | 2021-12-07 | 哈尔滨工业大学 | Method for KPFM in-situ test of electrical properties of two-dimensional material heterojunction under electric field coupling |
| CN116544279A (en) * | 2023-04-30 | 2023-08-04 | 天津大学 | All-carbon graphene device and preparation method thereof |
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