CN113328038B - Preparation method of graphene-carbon nanotube heterojunction - Google Patents
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Abstract
The invention discloses a preparation method of a graphene-carbon nanotube heterojunction, which comprises the following steps: the method comprises the following steps of firstly, stripping single-layer graphene on ST-cut quartz by utilizing mechanical stripping. And step two, loading the single-walled carbon nanotube grown by the catalyst on the ST-cut quartz. Step three, transferring the obtained graphene-carbon nanotube heterojunction to SiO 2 On a/Si substrate. Step four, the SiO after the reaction 2 the/Si substrate was used to construct a field effect transistor, FET, of single-walled carbon nanotubes, and the electrical properties thereof were investigated. The preparation method is simple, the finished product quality is good, the carbon nano tube and the graphene are welded together at high temperature by utilizing the growth of the top end of the catalyst particle, and the graphene-carbon nano tube heterojunction containing the nano particles is successfully prepared.
Description
Technical Field
The invention relates to the field of nano material heterojunction, in particular to a preparation method of a graphene-carbon nano tube heterojunction.
Background
Since the discovery of low-dimensional carbon materials such as carbon nanotubes (SWNTs) and graphene, the low-dimensional carbon materials have been the hot point of research in the field of nanoscience due to their perfect conjugated structures and excellent physical properties. As information technology enters the post-molar age (More Moore), carbon nanotube-based devices are receiving More and More attention and are also considered to be one of the most potential competitors of (More Moore) nanoelectronic device materials. The economic society is continuously advanced, the chip is multifunctional, and the miniaturization development puts new requirements on semiconductor devices. The heterojunction is a basic core structure of a semiconductor device, and the energy band structure can be regulated and controlled through the heterojunction construction, so that the heterojunction obtains novel characteristics which are not available in a single material. Therefore, a heterojunction of the carbon nano tube and the graphene is constructed, and the heterojunction can be used for exploring the transmission of current carriers between an ideal two-dimensional material and a one-dimensional material.
The prior art is as follows: firstly, transferring a layer of carbon nanotube film on an insulating growth substrate, then transferring a layer of graphene layer on the insulating growth substrate, and carrying out patterning treatment on the graphene layer to obtain a heterojunction formed by the graphene and the carbon nanotube at the source end. The current state of the art has major drawbacks; the process of preparing the heterojunction is complex, the preparation cost is high, and the popularization value is low.
Disclosure of Invention
The invention aims to provide a preparation method of a heterojunction containing graphene and carbon nanotubes, and aims to solve the problems that the heterojunction preparation process at the present stage is complex, high in cost, difficult to popularize and difficult to realize industrial production.
In order to achieve the purpose, the invention adopts the following technical scheme: the invention provides a preparation method of a graphene-carbon nanotube heterojunction, which comprises the following steps:
step one, processing a growth substrate;
the method for treating the growth substrate comprises the following steps:
s1, ultrasonically 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 at 900 ℃ for 8 h, cooling to 300 ℃ for 10 h, and naturally cooling;
mechanically stripping (tape method) graphene on the treated growth substrate;
loading a catalyst on a growth base with graphene, and introducing hydrogen and a carbon source into a chemical vapor deposition system to grow the single-walled carbon nanotube;
and step four, cooling the system to obtain a finished product.
Step five, transferring the graphene-carbon nanotube heterojunction prepared in the step four to SiO 2 On a/Si substrate.
Step six, SiO reacted in the step three is used 2 the/Si substrate creates a Field Effect Transistor (FET) of single-walled carbon nanotubes and explores its electrical properties.
Further, in the first step, the growth substrate is one of ST-cut quartz, r-cut quartz, alpha alumina on a surface, alpha alumina on r surface and magnesium oxide.
Further, an ST-cut quartz substrate is preferable.
Further, the number of layers of graphene in the second step is 1-4, preferably 1.
Further, the kind of the catalyst precursor in the third step is Cu or Ni or Co or Ru or Rh.
Furthermore, the type of the catalyst precursor in the third step is preferably Cu, and the concentration is 0.05 mmol/L.
Further, Cu or Ni or Co or Ru or Rh is preferable, and the concentration is 0.05 mmol/L.
Further, the specific loading method for loading the catalyst in the third step is as follows: dipping a salt solution of the catalyst by using a sewing needle to scratch a catalyst strip on the pretreated substrate or spin-coating or drip-coating the salt solution of the catalyst on the surface of a growth substrate;
wherein, in the salt solution of the catalyst, the solute is hydroxide or salt of metal elements.
Further, ethanol as a carbon source was carried into the reaction chamber by using argon as a carrier gas at a flow rate of 10 to 500 sccm, preferably 30 sccm. The growth time can be 1 min-1 h, and preferably 20 min.
Further, the solute is CuCl 2 Or NiCl 2 (ii) a In the salt solution of the catalyst, the solvent is at least one of ethanol, water and acetone.
Further, the cooling process in the fourth step is specifically natural cooling or program-controlled cooling.
Further, the step five comprises the following processes:
S1，SiO 2 respectively ultrasonically cleaning the Si substrate in ultrapure water, acetone, ethanol and ultrapure water for 20 min, drying the substrate by using nitrogen, and cleaning the substrate for 15 min by using an oxygen plasma cleaning system;
s2, coating PMMA on ST-cut quartz by using a spin coater, wherein the spin coating time is 40S, drying for 3 min, and transferring to SiO by using HF solution with the mass concentration of 5% as a transfer solution 2 Drying a PMMA film (adhered graphene-carbon nano tube heterojunction) on a Si substrate for 2h by a hot bench 2 Soaking a PMMA film (adhered with a graphene-carbon nanotube heterojunction) on a Si substrate in acetone for 5 min to remove PMMA;
s3, using Electron Beam Lithography (EBL) on SiO 2 Positioning and evaporating Cr/Au on a Si substrate to prepare the FET device of the single-walled carbon nanotube;
and S4, electrically testing the prepared FET device by using the probe station.
In S3, Cr was 3 nm thick and Au was 60 nm thick.
Further, the thickness of the mechanical peeling in the second step was 0.4 nm.
The invention provides a semiconductor device containing a graphene-carbon nanotube heterojunction, which comprises an insulating growth substrate, graphene arranged on the insulating growth substrate, a carbon nanotube and catalyst nanoparticles, wherein one end of the carbon nanotube is abutted against the edge position of the graphene, and the connection node of the carbon nanotube and the graphene is fixed by welding the catalyst nanoparticles.
Further, the insulating growth substrate is SiO 2 a/Si substrate.
Further, still include the electrode, electrode one end laminating sets up on graphite alkene upper surface, electrode other end laminating sets up on insulating growth substrate.
Furthermore, the graphene growth substrate can further comprise two electrodes, wherein one end of the first electrode is attached to the upper surface of the graphene, and the other end of the first electrode is attached to the insulating growth substrate; one end of the second electrode is attached to the upper surface of the carbon nano tube, and the other end of the second electrode is attached to the insulating growth substrate.
The invention also provides field effect transistor devices containing horizontal arrays of high density single walled carbon nanotubes.
The invention also provides application of the horizontal array containing the high-density single-walled carbon nanotubes in preparing a field effect transistor device.
The invention has the beneficial effects that:
the preparation method of the graphene-carbon nanotube heterojunction provided by the invention comprises the steps of mechanically stripping single-layer graphene, growing a single-walled carbon nanotube by using the top end of a Cu catalyst, and welding graphene and the carbon nanotube by using catalyst particles at a high temperature to directly obtain the graphene-carbon nanotube heterojunction.
2, the preparation method of the graphene-carbon nanotube heterojunction provided by the invention firstly provides that a catalyst for growing the carbon nanotube is utilized to form a semiconductor device containing the graphene-carbon nanotube heterojunction.
3, the preparation method of the graphene-carbon nanotube heterojunction provided by the invention is used for carrying out electrical property tests on the novel graphene-carbon nanotube heterojunction with two different electrical properties (graphene (metalloid) -semiconductor tube junctions and graphene (metalloid) -metal tube junctions) to know the electrical properties of the novel graphene-carbon nanotube heterojunction.
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 structural diagram of a semiconductor device including a graphene-carbon nanotube heterojunction according to example 1.
Fig. 2 is a schematic structural view of a semiconductor device including a graphene-carbon nanotube heterojunction according to example 2.
Fig. 3 is a schematic flow diagram of a fabrication process for a semiconductor device containing a graphene-carbon nanotube heterojunction.
Fig. 4 is an output graph.
Fig. 5 is a transfer graph.
Detailed Description
The technical solutions of the present invention are described in detail by the following examples, which are merely 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.
Referring to fig. 1 to 4, in the present invention, a single-layer graphene mechanically exfoliated is deposited on a growth substrate, and then a single-walled carbon nanotube is grown on top of a Cu catalyst by a chemical vapor deposition method, a graphene-carbon nanotube heterojunction is prepared, and its electron transport properties are studied. The invention uses the single-layer graphene which is mechanically stripped as an obstacle to limit the growth of the single-walled carbon nanotube, and a graphene-carbon nanotube heterojunction is formed at the junction of the single-walled carbon nanotube and the single-walled carbon nanotube. The materials at the two ends of the heterojunction are connected by covalent bonds. Due to the different conductive properties of the semiconducting carbon nanotubes and graphene, there is a significant schottky barrier between the two, resulting in typical rectifying characteristics.
The invention provides a semiconductor device containing a graphene-carbon nanotube heterojunction, which is formed by using a catalyst for growing a carbon nanotube for the first time. Wherein the insulating growth substrate is SiO 2 a/Si substrate.
Example 1
A preparation method of a graphene-carbon nanotube heterojunction comprises the following steps:
step one, processing a growth substrate;
the method for treating the growth substrate comprises the following steps:
s1, in order to clean the ST-cut quartz substrate and repair lattice defects generated in the production and processing process of the growth substrate, the growth substrate is sequentially subjected to ultrasonic cleaning in ultrapure water, acetone, ethanol and ultrapure water, and the cleaning time is controlled to be 10min for each cleaning solution;
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 at 900 ℃ for 8 h, cooling to 300 ℃ for 10 h, and naturally cooling;
the growth substrate is one of ST-cut quartz, r-cut quartz, alpha alumina on a surface, alpha alumina on r surface and magnesium oxide. ST-cut quartz substrates are preferred.
And step two, mechanically stripping (tape method) graphene on the treated growth substrate, wherein the number of graphene layers is 1-4, and 1 layer is preferred.
Step three, loading a catalyst CuCl on one side of the substrate with the graphene 2 Then placing the graphene-carbon nanotube heterojunction in a chemical vapor deposition system, wherein a catalyst strip is vertical to the direction of gas flow, heating to 830 ℃, introducing 300 sccm argon for 5 min, introducing 300 sccm hydrogen, bubbling ethanol by using 35 sccm argon, growing for 30 min, closing the argon for ethanol blowing after the growth is finished, keeping the introduction of hydrogen and the rest of argon, naturally cooling to room temperature, and obtaining the graphene-carbon nanotube heterojunction on ST-cut quartz after the growth is finished;
further, the catalyst concentration was 0.05 mmol/L.
The specific loading method of the loaded catalyst is as follows: dipping the salt solution of the catalyst by a sewing needle to scratch catalyst strips on a pretreated substrate or spin-coating or dripping the salt solution of the catalyst on the surface of a growth substrate to scratch a plurality of catalyst strips.
Step four, transferring the graphene-carbon nanotube heterojunction prepared in the step three to SiO 2 On a/Si substrate.
The method comprises the following steps:
SiO 2 respectively ultrasonically cleaning the Si substrate in ultrapure water, acetone, ethanol and ultrapure water for 20 min, drying the substrate by using nitrogen, and cleaning the substrate for 15 min by using an oxygen plasma cleaning system;
s2, coating PMMA on ST-cut quartz by using a spin coater, wherein the spin coating time is 40S, drying is carried out for 3 min, and HF solution with the mass concentration of 5% is used asTransfer of the solution to SiO 2 Drying a PMMA film (adhered graphene-carbon nano tube heterojunction) on a Si substrate for 2h by a hot table 2 Soaking a PMMA film (adhered with a graphene-carbon nanotube heterojunction) on a Si substrate in acetone for 5 min to remove PMMA;
s3, using Electron Beam Lithography (EBL) on SiO 2 Positioning and evaporating Cr/Au on a Si substrate to prepare the FET device of the single-walled carbon nanotube;
s4, the prepared FET device was electrically tested using the probe station.
In S3, Cr was 3 nm thick and Au was 60 nm thick.
Further, the thickness of the mechanical peeling in the second step was 0.4 nm.
Fig. three is a schematic diagram of the process, fig. four is a device output curve, typical rectification behavior can be seen, and fig. five is a transfer curve of graphene and carbon nanotubes, demonstrating that the carbon nanotubes are semiconducting single-walled carbon nanotubes.
Example 2
The difference from example 1 is that: the CuCl used 2 Changing solution to NiCl 2 Has a concentration of 0.05 mmol/L of NiCl 2 After the/EtOH solution, the surface of the ST-cut quartz substrate with graphene is loaded with the Ni-containing catalyst.
Principle of preparation of heterojunction: the single-layer graphene is used as an obstacle to limit the growth of the single-walled carbon nanotube, and a graphene-carbon nanotube heterojunction is formed at the junction of the single-walled carbon nanotube and the single-walled carbon nanotube. Firstly, a layer of single-layer graphene is stripped on a growth substrate by using a tape method. Then, a metal catalyst is loaded on the substrate, and the carbon nano tube grows by utilizing a crystal lattice oriented growth mode, wherein the grown carbon nano tube is parallel to the crystal lattice direction. By utilizing the top growth mode of the carbon nano tube, the catalyst moves forwards along with the growth of the carbon nano tube until the catalyst touches the edge of the single-layer graphene, and the liquid metal catalyst can seamlessly weld the edge of the single-layer graphene and the carbon nano tube together at the high temperature of a CVD system to form a novel graphene-carbon nano tube heterojunction containing catalyst nano particles.
According to the invention, the band gap of the graphene is opened by a method for constructing a heterojunction. The heterojunction is composed of a semiconducting single-walled carbon nanotube and single-layer graphene, and the structure is shown in figure 2.
The application is distinguished from the prior art by the following features: by utilizing the characteristic of the growth of the top of the copper catalyst, the carbon nano tube directly grows on the substrate with the single-layer graphene, so that the heterojunction containing the catalyst nano particles can be obtained, and the two materials forming the heterojunction are connected in a chemical bond mode.
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 (2)
1. A preparation method of a graphene-carbon nanotube heterojunction is characterized by comprising the following steps: the method comprises the following steps:
step one, processing a growth substrate; the method for treating the growth substrate comprises the following steps:
s1, in order to clean the ST-cut quartz substrate and repair lattice defects generated in the production and processing process of the growth substrate, the growth substrate is sequentially subjected to ultrasonic cleaning in ultrapure water, acetone, ethanol and ultrapure water, and the cleaning time is controlled to be 10min for each cleaning solution;
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 at 900 ℃ for 8 h, cooling to 300 ℃ for 10 h, and naturally cooling;
mechanically stripping graphene on the treated growth substrate by using an adhesive tape method; the thickness of the mechanical stripping is 0.4 nm;
step three, loading a catalyst CuCl on one side of the substrate with the graphene 2 Then placing the mixture into a chemical vapor deposition system, heating the catalyst strip to 830 ℃ in a direction perpendicular to the gas flow, introducing 300 sccm argon for 5 min and 300 sccm hydrogen, finally bubbling 35 sccm argon into ethanol, growing for 30 min,after the growth is finished, closing argon gas for ethanol blowing, keeping hydrogen gas and the rest of argon gas continuously introduced, naturally cooling to room temperature, and obtaining the graphene-carbon nanotube heterojunction on ST-cut quartz after the growth is finished, wherein the concentration of the catalyst is 0.05 mmol/L;
step four, transferring the graphene-carbon nano tube heterojunction prepared in the step three to SiO 2 a/Si substrate;
the method comprises the following steps:
S1，SiO 2 respectively ultrasonically cleaning the Si substrate in ultrapure water, acetone, ethanol and ultrapure water for 20 min, drying the substrate by using nitrogen, and cleaning the substrate for 15 min by using an oxygen plasma cleaning system;
s2, coating PMMA on ST-cut quartz by using a spin coater, wherein the spin coating time is 40S, drying for 3 min, and transferring the PMMA film adhered with the graphene-carbon nano tube heterojunction to SiO by using an HF solution with the mass concentration of 5% as a transfer solution 2 On a Si substrate, drying for 2 hours by a hot bench,
obtaining the SiO adhered with the graphene-carbon nanotube heterojunction PMMA film 2 a/Si substrate, and the SiO 2 Soaking the Si substrate in acetone for 5 min to remove PMMA;
s3, using electron beam lithography to etch on SiO 2 Positioning and evaporating Cr/Au on a Si substrate to prepare the FET device of the single-walled carbon nanotube, wherein the thickness of Cr is 3 nm, and the thickness of Au is 60 nm;
s4, the prepared FET device was electrically tested using the probe station.
2. The method of claim 1, wherein the specific loading method for loading the catalyst in step three is: dipping a salt solution of the catalyst by using a sewing needle to scratch a catalyst strip on the pretreated substrate or spin-coating or drip-coating the salt solution of the catalyst on the surface of a growth substrate;
wherein, in the salt solution of the catalyst, the solute is hydroxide or salt of metal elements.
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