CN108163840B - Carbon nanotube purification method, thin film transistor and preparation method - Google Patents
Carbon nanotube purification method, thin film transistor and preparation method Download PDFInfo
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having potential barriers
- H10K10/40—Organic transistors
- H10K10/46—Field-effect transistors, e.g. organic thin-film transistors [OTFT]
- H10K10/462—Insulated gate field-effect transistors [IGFETs]
- H10K10/466—Lateral bottom-gate IGFETs comprising only a single gate
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/20—Carbon compounds, e.g. carbon nanotubes or fullerenes
- H10K85/221—Carbon nanotubes
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Abstract
The invention provides a purification method of a carbon nano tube, which comprises the following steps: adding a single-walled carbon nanotube mixed with a metallic single-walled carbon nanotube and a semiconducting single-walled carbon nanotube into an organic solvent containing a small molecular compound, and performing ultrasonic dispersion to obtain a carbon nanotube suspension; and centrifuging the carbon nano tube suspension to remove the sediment of the carbon nano tube suspension to obtain the supernatant of the semiconductor single-walled nano tube. The invention also provides a preparation method of the thin film transistor, which comprises the following steps: forming a bottom gate and a bottom gate insulating layer covering the bottom gate on a substrate; forming an active layer on the bottom gate insulating layer by using a semiconducting single-walled nanotube supernatant; forming a source electrode and a drain electrode at opposite ends of the active layer, respectively; and sequentially forming a top gate insulating layer, a top gate and a passivation layer on the source electrode and the drain electrode. The invention also provides a thin film transistor.
Description
Technical Field
The invention relates to the technical field of display manufacturing, in particular to a carbon nano tube purification method, a thin film transistor and a preparation method.
Background
In recent years, Carbon nano Thin Film transistors (CNT-TFTs) have attracted many researchers in the display field due to their characteristics of high mobility, high transparency, and high elasticity.
Generally, CNT-TFTs are prepared from network-like carbon nanotube films. Wherein, during the synthesis process, the Single-Walled Carbon Nanotube (SWCNT) has metallic Single-Walled Carbon Nanotube (m-SWCNT) and semiconducting Single-Walled Carbon Nanotube (sc-SWCNT) mixed. The m-SWCNT is used for preparing nano-scale electrodes, the sc-SWCNT is a conductive channel with high mobility and on-off ratio, the band gaps of the sc-SWCNT with different diameters are different, and the difference of the band gap distribution width can cause the conductive performance of the prepared CNT-TFT to be greatly reduced.
Disclosure of Invention
The invention aims to provide a carbon nano tube purification method for preparing a carbon nano thin film transistor with a high-performance field effect.
The invention also provides a carbon nano-film transistor and a preparation method thereof.
The purification method of the carbon nano tube comprises the following steps:
adding a single-walled carbon nanotube mixed with a metallic single-walled carbon nanotube and a semiconducting single-walled carbon nanotube into an organic solvent containing a small molecular compound, and performing ultrasonic dispersion to obtain a carbon nanotube suspension;
and centrifuging the carbon nano tube suspension to remove the sediment of the carbon nano tube suspension, thereby obtaining the supernatant of the semiconductor single-walled carbon nano tube.
The method comprises the following steps of adding a single-walled carbon nanotube mixed with a metallic single-walled carbon nanotube and a semiconducting single-walled carbon nanotube into an organic solvent containing a small molecular compound, and performing ultrasonic dispersion under the condition of an ice water bath in the process of obtaining a carbon nanotube suspension.
And centrifuging the carbon nanotube suspension in a centrifuge in the process of centrifuging the carbon nanotube suspension to remove sediments of the carbon nanotube suspension to obtain a supernatant of the semiconductor single-walled carbon nanotube.
Wherein, the purification method of the carbon nano tube comprises the following steps:
dissolving carbon nanotubes prepared by an electric arc method in a toluene solution containing small molecular compounds, and ultrasonically dispersing for 20-40 min under the ice-water bath condition to obtain a carbon nanotube suspension, wherein the mass ratio of the carbon nanotubes to the small molecular compounds is 1-3;
and centrifuging the carbon nano tube suspension at a high speed for 20-40 min under the centrifugal force of 20-30 kg to remove the sediment of the carbon nano tube suspension, thus obtaining the supernatant of the semiconductor single-walled carbon nano tube.
Wherein the small molecule compound comprises 1, 4-bis (anthracene-9-methylthio) -p-xylene, 1- (pyrene-1-methoxyl) -4- (anthracene-1-methoxyl) -p-xylene, 1- (pyrene-1-methylthio) -4- (pyrene-1-methylthio) -p-xylene, and 1- (benzopyrene-1-methoxyl) -4- (benzopyrene-1-methoxyl) -p-xylene.
The preparation method of the thin film transistor comprises the following steps:
forming a bottom gate and a bottom gate insulating layer covering the bottom gate on a substrate;
forming an active layer on the bottom gate insulating layer by using a semi-conductive single-walled carbon nanotube supernatant;
forming a source electrode and a drain electrode at opposite ends of the active layer, respectively;
and sequentially forming a top gate insulating layer, a top gate and a passivation layer on the source electrode and the drain electrode.
After a bottom gate and a bottom gate insulating layer covering the bottom gate are formed on a substrate, the substrate is soaked and washed by organic solution and dried at 50-100 ℃.
Wherein, in the process of forming an active layer on the bottom gate insulating layer by using a supernatant of semiconductor single-walled carbon nanotubes, the active layer is formed by a pulling deposition mode.
Wherein the process of forming the active layer on the bottom gate insulating layer with the supernatant of the semiconducting single-walled carbon nanotubes is performed in an atmosphere filled with a protective gas.
The thin film transistor of the invention comprises:
a bottom gate and a bottom gate insulating layer formed in sequence on the substrate;
an active layer formed on the bottom gate insulating layer, the active layer being made of the carbon nanotube purified in claim 1;
the source electrode and the drain electrode are positioned at two ends of the active layer;
the top gate insulating layer, the top gate and the passivation layer cover the source electrode and the drain electrode;
and a contact hole.
According to the semiconductor carbon nano tube obtained by adopting the single-walled carbon nano tube purification method, the band gap distribution of the semiconductor carbon nano tube obtained by purification is narrow, so that the high-purity semiconductor carbon nano tube is used as an active layer to prepare the carbon nano film transistor with the high-performance field effect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of the purification method of single-walled carbon nanotubes according to the present invention.
Fig. 2 is a flow chart of a method for manufacturing a thin film transistor according to the present invention.
Fig. 3 is a film structure diagram of the thin film transistor according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a method for purifying semiconducting single-walled carbon nanotubes, comprising:
s101, adding the single-walled carbon nanotube mixed with the metallic single-walled carbon nanotube and the semiconductor single-walled carbon nanotube into an organic solvent containing a small molecular compound, and performing ultrasonic dispersion to obtain a carbon nanotube suspension.
Specifically, the single-walled carbon nanotube may be prepared by a laser evaporation method, an arc discharge method, or a chemical vapor deposition method, and the like, and the single-walled carbon nanotube includes a metallic single-walled carbon nanotube and a semiconducting single-walled carbon nanotube. The semiconducting carbon nanotube is coated by a small molecular compound dissolved in an organic solvent, wherein the general formula of the small molecular compound is Polycyclic Aromatic Hydrocarbon-Benzene ring-Polycyclic Aromatic Hydrocarbon (PAH-B-PAH), and the chemical structural general formula of the small molecular compound is as follows:
the polycyclic aromatic hydrocarbons (PAN), i.e., R1 and R2 in the above general structural formula, include but are not limited to polycyclic aromatic hydrocarbons within five benzene rings such as pyrene, anthracene, benzopyrene, naphthalene, tetracene, phenanthrene, and rylene, and the chemical structural formula of the polycyclic aromatic hydrocarbons is as follows:
specifically, the PAH-B-PAH includes but is not limited to 1, 4-bis (anthracene-9-methylthio) -p-xylene, 1- (pyrene-1-methoxy) -4- (anthracene-1-methoxy) -p-xylene, 1- (pyrene-1-methylthio) -4- (pyrene-1-methylthio) -p-xylene, 1- (benzopyrene-1-methoxy) -4- (benzopyrene-1-methoxy) -p-xylene, and the specific chemical structural formula of the small molecule compound is as follows:
organic solvents that can dissolve small molecule compounds include, and are not limited to, toluene solutions. The method comprises the following steps of carrying out ultrasonic dispersion on an organic solvent of a mixed oil single-walled carbon nanotube and a small molecular compound under the condition of ice-water bath, effectively preventing a large amount of volatilization of the organic solvent in the ultrasonic process, and after the small molecular compound and the single-walled carbon nanotube are subjected to ultrasonic dispersion incubation in the organic solvent, selectively wrapping and compounding the small molecular compound and a semiconducting single-walled carbon nanotube to enhance the solubility and the dispersibility of the semiconducting single-walled carbon nanotube in the organic solvent. In the embodiment, the carbon nanotube prepared by an arc method is dissolved in a toluene solution containing a small molecular compound, and ultrasonic dispersion is performed for 20-40 min under the condition of ice-water bath to obtain a carbon nanotube suspension, wherein the mass ratio of the carbon nanotube to the small molecular compound is 1-3.
Preferably, in this example, 4mg of carbon nanotubes prepared by the arc method are dissolved in 20ml of toluene solution containing 2mg of small molecule compound, and ultrasonically dispersed for 30min under the condition of ice water bath, so as to obtain a carbon nanotube suspension.
S102, performing centrifugal treatment on the carbon nanotube suspension to remove sediments of the carbon nanotube suspension, and obtaining a semi-conductive single-walled carbon nanotube supernatant.
Specifically, after the carbon nanotube suspension is centrifuged at a high speed in a centrifuge, metallic single-walled carbon nanotubes and amorphous carbide precipitate at the bottom of the solution, while semiconducting single-walled carbon nanotubes are wrapped by a small molecular compound and dissolved in an organic solvent, so that the separation of the metallic single-walled carbon nanotubes and the semiconducting single-walled carbon nanotubes can be realized by separating a supernatant and a bottom precipitate. The supernatant can be taken out from the centrifuge tube, and metallic single-walled carbon nanotubes and amorphous carbon impurities in the solution at the bottom are removed, so that high-content semiconductor single-walled carbon nanotubes are obtained and used for constructing the carbon nanotube thin film transistor. In this embodiment, after the carbon nanotube suspension is subjected to high-speed centrifugation for 20 to 40 minutes under a centrifugal force of 20 to 30kg, a supernatant is taken out of the centrifugal tube by using an injector, and metallic single-walled carbon nanotubes and amorphous carbon impurities at the bottom of the centrifugal tube are removed, so as to obtain a high-content semiconductor single-walled carbon nanotube solution.
Referring to fig. 2, the present invention further provides a method for manufacturing a thin film transistor, including:
s201, forming a bottom gate and a bottom gate insulating layer covering the bottom gate on a substrate.
Specifically, the substrate includes, but is not limited to, a quartz substrate, a glass substrate, or a flexible plastic substrate. In this embodiment, the substrate is a glass substrate, a first metal film is formed by sputtering a Mo film and then a Cu film on the glass substrate by pvd, a Mo/Cu bottom gate is formed by photolithography, and a 200nm thick SiO layer is formed on the bottom gate by plasma enhanced chemical deposition2Using the silicon nitride as a bottom gate insulating layer, soaking and washing the silicon nitride in acetone, methanol and isopropanol to remove impurities, and heating the silicon nitride at 50-100 DEG CAnd (5) drying. Wherein the material of the bottom gate electrode includes, but is not limited to, one or more conductive materials such as Al, Ag, Cu, Mo or Ti, and the material of the bottom gate insulating layer includes, but is not limited to, SiO2、Al2O3、SiNx、HfO2Or ionic gels, etc. The formation method of the bottom gate and the gate insulating layer includes, but is not limited to, a Deposition method such as Plasma Enhanced Chemical Vapor Deposition (PECVD).
And S202, forming an active layer on the bottom gate insulating layer by using a supernatant of the semiconducting single-walled carbon nanotubes.
In this embodiment, the single-walled nanotube supernatant is prepared by the method for purifying semiconductor single-walled carbon nanotubes, the substrate prepared in S201 is immersed in the semiconductor single-walled nanotube supernatant in a glove box filled with a protective gas, a uniform carbon nanotube active layer is formed by a multi-time lift-and-deposition technique, and then a carbon nanotube channel is etched by a photolithography technique and an oxygen plasma and placed in an electron beam evaporation machine.
And S203, respectively forming a source electrode and a drain electrode at two opposite ends of the active layer.
In this embodiment, an electron evaporation technology is used to plate a Mo film on the bottom gate insulating layer, then a Cu film is evaporated, and then a Mo film is evaporated to form a second metal layer composed of a Mo/Cu/Mo three-layer film, and the second metal layer is patterned by a photolithography technology to form the source and drain electrodes. The source and drain electrodes are made of one or more conductive materials including but not limited to Al, Ag, Cu, Mo or Ti.
And S204, sequentially forming a top gate insulating layer, a top gate and a passivation layer on the source electrode and the drain electrode.
In this example, a 300nm thick SiO film was coated on the sample prepared in step S203 by chemical vapor deposition2The film is used as a top gate insulating layer; under the action of shadow mask, evaporating a Mo film and then evaporating a Cu film, the Mo/Cu film forming the topA partial gate; followed by chemical vapor deposition to coat with SiO2As a passivation layer. The forming method of the top gate insulating layer and the passivation layer includes chemical vapor deposition or physical vapor deposition, and the forming thickness of the top gate insulating layer is not particularly limited, which is based on the technical features of the technical staff in the field that can achieve the object of the present invention. The material of the top gate insulating layer includes, but is not limited to, SiO2、Al2O3、SiNx、HfO2Or ionic gel, the material of the top gate includes and is not limited to one or more conductive materials such as Al, Ag, Cu, Mo or Ti, the material of the passivation layer includes and is not limited to SiO2Phosphosilicate glass, Si3N4Or Al2O3And the like.
And further, coating photoresist, exposing, etching and removing photoresist on the top gate insulating layer in sequence to prepare a contact hole, so as to obtain the double-gate carbon nano thin film transistor.
In the preparation process of the thin film transistor, the high-purity semiconductive carbon nanotube is adopted to prepare the active layer, so that the carbon nanotube thin film transistor with high-performance field effect is prepared.
Referring to fig. 3, the present invention further provides a thin film transistor 100, which is prepared by the above method for preparing a thin film transistor and is used to prepare a display panel. As shown in fig. 3, the thin film transistor 100 includes: a bottom gate electrode 20 and a bottom gate insulating layer 30 sequentially formed on the substrate 10; an active layer 40 formed on the bottom gate insulating layer 30; source and drain electrodes 50 positioned at both ends of the active layer 40; a top gate insulating layer 60, a top gate electrode 70, a passivation layer 80 covering the source and drain electrodes 50; and contact hole 90.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. A method for purifying carbon nanotubes, comprising:
adding a single-walled carbon nanotube mixed with a metallic single-walled carbon nanotube and a semiconducting single-walled carbon nanotube into an organic solvent containing a small molecular compound, and performing ultrasonic dispersion to obtain a carbon nanotube suspension;
centrifuging the carbon nano tube suspension to remove the sediment of the carbon nano tube suspension to obtain the supernatant of the semiconductor single-walled carbon nano tube, wherein the general formula of the micromolecular compound is shown in the specification
R1 is a condensed-ring aromatic hydrocarbon formed by connecting n benzene rings, n is less than or equal to 5, R2 is a condensed-ring aromatic hydrocarbon formed by connecting m benzene rings, and m is less than or equal to 5.
2. The method for purifying carbon nanotubes as claimed in claim 1, wherein the ultrasonic dispersion is performed under the condition of an ice water bath in the process of adding the single-walled carbon nanotubes mixed with the metallic single-walled carbon nanotubes and the semiconducting single-walled carbon nanotubes into an organic solvent containing a small molecular compound and performing ultrasonic dispersion to obtain a carbon nanotube suspension.
3. The method for purifying carbon nanotubes according to claim 1, wherein the suspension of carbon nanotubes is centrifuged in a centrifuge during the centrifugation of the suspension to remove the deposit of the suspension of carbon nanotubes and obtain a supernatant of semiconducting single-walled carbon nanotubes.
4. The method for purifying carbon nanotubes according to any one of claims 1 to 3, wherein the method for purifying carbon nanotubes comprises:
dissolving carbon nanotubes prepared by an electric arc method in a toluene solution containing small molecular compounds, and ultrasonically dispersing for 20-40 min under the ice-water bath condition to obtain a carbon nanotube suspension, wherein the mass ratio of the carbon nanotubes to the small molecular compounds is 1-3;
and centrifuging the carbon nano tube suspension at a high speed for 20-40 min under the centrifugal force of 20-30 kg to remove the sediment of the carbon nano tube suspension, thus obtaining the supernatant of the semiconductor single-walled carbon nano tube.
5. The method for purifying carbon nanotubes according to claim 1, wherein the small molecule compound comprises 1, 4-bis (anthracene-9-methylthio) -p-xylene, 1- (pyrene-1-methoxy) -4- (anthracene-1-methoxy) -p-xylene, 1- (pyrene-1-methylthio) -4- (pyrene-1-methylthio) -p-xylene, 1- (benzopyrene-1-methoxy) -4- (benzopyrene-1-methoxy) -p-xylene.
6. A method for manufacturing a thin film transistor includes:
forming a bottom gate and a bottom gate insulating layer covering the bottom gate on a substrate;
forming an active layer on the bottom gate insulating layer by using the supernatant of the semiconducting single-walled carbon nanotubes prepared by the method for purifying carbon nanotubes of any one of claims 1 to 5;
forming a source electrode and a drain electrode at opposite ends of the active layer, respectively;
and sequentially forming a top gate insulating layer, a top gate and a passivation layer on the source electrode and the drain electrode.
7. The method of manufacturing a thin film transistor according to claim 6, wherein after forming a bottom gate electrode and a bottom gate insulating layer covering the bottom gate electrode on a substrate, the substrate is rinsed by soaking in an organic solution and dried at 50 ℃ to 100 ℃.
8. The method of manufacturing a thin film transistor according to claim 6, wherein the active layer is formed by a lift-off deposition process during the formation of the active layer on the bottom gate insulating layer using a supernatant of semiconducting single-walled carbon nanotubes.
9. The method of manufacturing a thin film transistor according to claim 6, wherein the forming of the active layer on the bottom gate insulating layer using a supernatant of semiconducting single-walled carbon nanotubes is performed in an atmosphere filled with a protective gas.
10. A thin film transistor, comprising:
a bottom gate and a bottom gate insulating layer formed in sequence on the substrate;
an active layer formed on the bottom gate insulating layer, the active layer being made of the carbon nanotube purified in claim 1;
the source electrode and the drain electrode are positioned at two ends of the active layer;
the top gate insulating layer, the top gate and the passivation layer cover the source electrode and the drain electrode;
and a contact hole.
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| CN109256467B (en) * | 2018-09-07 | 2022-08-26 | 苏州希印纳米科技有限公司 | High-performance single-walled carbon nanotube thin film transistor and preparation method thereof |
| CN111864069A (en) * | 2019-04-26 | 2020-10-30 | 京东方科技集团股份有限公司 | Thin film transistor, preparation method thereof and display device |
| CN110395715B (en) * | 2019-09-04 | 2021-05-11 | 中国科学院福建物质结构研究所 | Method for purifying carbon nanohorn |
| CN112993041B (en) * | 2021-02-03 | 2023-03-24 | 重庆先进光电显示技术研究院 | Liquid crystal display panel, thin film transistor and manufacturing method thereof |
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| CN107298436A (en) * | 2016-04-07 | 2017-10-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | The method for obtaining high-purity semi-conductive single-walled carbon nanotubes |
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