CN114725284A - Carbon nano tube thin film transistor and manufacturing method thereof - Google Patents
Carbon nano tube thin film transistor and manufacturing method thereof Download PDFInfo
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/20—Changing the shape of the active layer in the devices, e.g. patterning
- H10K71/231—Changing the shape of the active layer in the devices, e.g. patterning by etching of existing layers
- H10K71/233—Changing the shape of the active layer in the devices, e.g. patterning by etching of existing layers by photolithographic etching
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- H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having a potential-jump barrier or a surface barrier
- H10K10/40—Organic transistors
- H10K10/46—Field-effect transistors, e.g. organic thin-film transistors [OTFT]
- H10K10/462—Insulated gate field-effect transistors [IGFETs]
- H10K10/464—Lateral top-gate IGFETs comprising only a single gate
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- H—ELECTRICITY
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- H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having a potential-jump barrier or a surface barrier
- H10K10/40—Organic transistors
- H10K10/46—Field-effect transistors, e.g. organic thin-film transistors [OTFT]
- H10K10/462—Insulated gate field-effect transistors [IGFETs]
- H10K10/484—Insulated gate field-effect transistors [IGFETs] characterised by the channel regions
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- H—ELECTRICITY
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/20—Changing the shape of the active layer in the devices, e.g. patterning
- H10K71/211—Changing the shape of the active layer in the devices, e.g. patterning by selective transformation of an existing layer
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- H—ELECTRICITY
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
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Abstract
The invention belongs to the field of research, development and application of novel carbon nanotube thin film transistors, and particularly relates to a carbon nanotube thin film transistor and a manufacturing method thereof. The manufacturing method provided by the invention comprises the following steps: manufacturing a source electrode and a drain electrode of a transistor on a substrate based on the high-density carbon nanotube film; sticking a photosensitive dry film on the surface of the carbon nanotube film by adopting a film covering technology, and realizing the patterning of the carbon nanotube film by adopting a photoetching technology; transferring the low-density carbon nanotube film, and manufacturing a channel by a dry film laminating and photoetching technology; preparing a gate insulating layer by a spin-on curing process; carrying out insulating layer windowing on the gate insulating layer; transferring the high-density carbon nanotube film, and manufacturing the grid electrode by dry film coating and photoetching technology. The invention realizes the preparation of the carbon nano tube thin film transistor by utilizing the dry film process and the photoetching process, has simple process, realizes the preparation of large-area devices under normal pressure, saves the process cost, and has good electrical property and mechanical property.
Description
The application is a divisional application with application date of 2017, 06 and 05, application number of 201710411464.5 and invention name of 'a carbon nano tube thin film transistor based on a photosensitive dry film process and a manufacturing method'.
Technical Field
The invention relates to the research and development and application fields of novel carbon nanotube thin film transistors, in particular to a carbon nanotube thin film transistor and a manufacturing method thereof.
Background
Since being discovered, carbon nanotubes have become one of the most promising semiconductor channel materials for thin film transistors in the field of flexible electronics due to their excellent optical, electrical, and mechanical properties. In the last decades, scientists and researchers have conducted intensive and intensive research on the application of flexible carbon nanotube thin film transistor devices in integrated circuits, active matrix displays, sensors, etc., and have effectively promoted the development of carbon nanotube thin film transistors in the field of flexible electronic devices. However, the photoresist, which is the main body of the patterning process, needs to be spin-coated on a target substrate by a spin coater in view of its own liquid properties, and a patterned coating layer is formed by a photolithography process. Therefore, the area of the prepared device is directly limited by the size of the spin coater, and becomes one of the main bottlenecks of the continuous development of the carbon nanotube thin film transistor in the field of large-area flexible electronics.
Disclosure of Invention
The invention aims to provide a carbon nanotube thin film transistor and a manufacturing method thereof, which simplify the preparation process of preparing the carbon nanotube thin film transistor by using the traditional photoresist, solve the limitations of the traditional photoresist on flexibility and large area and realize the large-scale preparation of all-carbon nanotube thin film transistor devices.
The technical scheme of the invention is as follows:
a manufacturing method of a carbon nano tube thin film transistor comprises the following steps:
(1) manufacturing a source electrode and a drain electrode of a transistor on a substrate based on the high-density carbon nanotube film;
(2) sticking a photosensitive dry film on the surface of the carbon nanotube film by adopting a film covering technology, and realizing the patterning of the carbon nanotube film by adopting a photoetching technology;
(3) transferring the low-density carbon nanotube film, and manufacturing a channel by a dry film laminating and photoetching technology;
(4) preparing a gate insulating layer by a spin-on curing process;
(5) carrying out insulating layer windowing on the gate insulating layer;
(6) transferring the high-density carbon nanotube film, and manufacturing a grid electrode by using a dry film laminating and photoetching technology;
the source electrode, the drain electrode and the grid electrode are formed by 8-12 high-density carbon nanotube films per mu m; the semiconductor channel is made of a low-density carbon nanotube film material with 0.4-0.6 carbon nanotubes per mu m;
the carbon nano tube film is a random carbon nano tube network collected by a floating catalytic chemical vapor deposition method, and the preparation method comprises the following steps: under the condition that the temperature is 1100 +/-50 ℃, injecting ferrocene catalyst solution into a reaction cavity through an injector at a constant speed, and reacting with carbon source gas to generate a carbon nano tube; collecting the generated carbon nanotubes at the air outlet end by using a high-flux nitrocellulose membrane, thereby obtaining a carbon nanotube film which is randomly distributed;
in the photosensitive dry film process, the adhesion degree of a dry film and a substrate is adjusted by controlling the speed, the pressure and the temperature of a roller of a laminating machine, so that the stability of the dry film is improved; wherein the speed of the roller is 0.5-2.0 m/min, the pressure is 0.5-1.5 bar, and the temperature is 100-150 ℃.
Preferably, before the source electrode and the drain electrode are manufactured in the step (1), demolding is carried out, and a demolding agent adopted in demolding is a sodium hydroxide solution; the concentration of the release agent is 2.5%; the temperature of the release agent is 70 ℃; the demolding time is 5 min.
Preferably, the speed of the roller of the laminator is 1.5m/min, the pressure is 1.0bar, and the temperature is 130 ℃.
Preferably, in the photosensitive dry film process, the change of the morphology is observed by exposure and development through an optical microscope, post-treatment is carried out after the exposure is finished, and standing is carried out before the development is carried out.
Preferably, the exposure time is 4.5-14 s, baking is carried out after the exposure is finished, the baking time is 30-150 s, the baking temperature is 90-140 ℃, and the standing time is 10-30 min.
Preferably, the exposure time is 10s, the baking time is 90s, the baking temperature is 120 ℃, and the standing time after exposure is 15 min.
The invention also provides the carbon nanotube thin film transistor prepared by the preparation method in the scheme, and the device of the carbon nanotube thin film transistor comprises a substrate, and a source electrode, a drain electrode, a semiconductor channel, a gate insulating layer and a gate electrode which are arranged on the substrate, wherein the source electrode, the drain electrode, the gate electrode and the semiconductor channel are made of carbon nanotube thin film materials.
Preferably, the structure type of the carbon nanotube thin film transistor device is a bottom gate type, a buried gate type or a top gate type.
Preferably, the substrate is a flexible substrate, and the material of the gate insulating layer is a polymer material.
Preferably, the material of the flexible substrate is polyethylene naphthalate, and the polymer material is polymethyl methacrylate.
The design idea of the invention is as follows:
the method utilizes the film coating property of the photosensitive dry film, adopts a film coating machine to directly stick the photosensitive dry film on the target substrate under the heating condition, and replaces photoresist and spin coating processes to prepare the carbon nano tube thin film transistor. The invention utilizes the photosensitive property of the photosensitive dry film, adopts the photoetching process to realize the imaging of the device structure and the carbon nanotube film, and utilizes the standing after exposure to realize the imaging with higher precision. The invention realizes the pure stripping of the photosensitive dry film at 70 ℃ by using the stripping property of the dry film and adopting 1.5-2.5 wt% of sodium hydroxide solution.
The invention has the advantages and beneficial effects that:
1. compared with the traditional photoresist semiconductor process, the manufacturing method of the carbon nanotube thin film transistor greatly simplifies the process flow; meanwhile, the electrical property of the carbon nano tube thin film transistor is effectively protected by the pure stripping of the photosensitive dry film.
2. Compared with liquid photoresist, the photosensitive dry film provided by the invention is low in cost and uniform in thickness, has good adhesion force with a plurality of substrates, and can realize large-area large-scale preparation of the carbon nanotube thin film transistor.
3. According to the invention, the photosensitive dry film is used for replacing photoresist to prepare the flexible carbon nanotube thin film transistor device, the photosensitive dry film is tightly pasted on the flexible substrate and the surface of the carbon nanotube thin film by regulating the speed, the temperature and the pressure of the roller of the film laminating machine, the patterning is completed by matching with the photoetching process, the process flow is simplified, and an ideal device structure is obtained. Meanwhile, the prepared all-carbon nanotube thin film transistor device has good electrical properties, and shows wide application prospects of the photosensitive dry film in the fields of large areas, low cost and flexible printed semiconductor devices.
Drawings
FIG. 1 is a basic process for fabricating an all-carbon nanotube thin film transistor by the photo-sensitive dry film process according to the present invention;
FIG. 2 is a microscopic optical photograph of a top gate type all-carbon nanotube thin film transistor fabricated on a PEN substrate by a photo-sensitive dry film process;
FIG. 3 is a macroscopic view of a top gate type all carbon nanotube thin film transistor fabricated on a PEN substrate by a photo-sensitive dry film process;
FIGS. 4 to 5 are scanning electron micrographs of carbon nanotube films of the electrode (FIG. 4) and the channel (FIG. 5);
FIG. 6 shows a single carbon nanotube TFT on a PEN substrate at VdsTransfer characteristic curve at-1V, wherein the abscissa represents the gate-source voltage Vgs(V) the ordinate represents the source-drain current Ids(A);
FIG. 7 shows a plurality of carbon nanotube thin film transistor devices on a PEN substrate at VdsTransfer characteristic curve at-1V, wherein the abscissa represents the gate-source voltage Vgs(V) the ordinate represents the source-drain current Ids(A);
FIG. 8 shows the same CNT TFT device on a PEN substrate at different VgsOutput characteristic curve of the following, in which the abscissa represents the source-drain voltage Vds(V) the ordinate represents the source-drain current Ids(A);
FIG. 9 shows the same CNT TFT device on a PEN substrate at different VdsTransfer characteristic curve of (1), wherein the abscissa represents the applied gate voltage Vgs(V) the ordinate represents the source-drain current Ids(A);
FIG. 10 shows On-off ratio (On-off) and carrier Mobility (cm) of a multiple carbon nanotube TFT device On a PEN substrate2Vs);
FIG. 11 is a photo of an inverter, wherein VDDRepresenting a supply voltage, IN representing an input voltage, OUT representing an output voltage, and GND representing a ground terminal;
fig. 12 is a performance test curve of the inverter, in (v) is an input voltage, out (v) is an output voltage, and Gain is an ordinate.
Detailed Description
In the specific implementation process, the method for preparing the all-carbon nanotube thin film transistor by using the photosensitive dry film process comprises the following steps:
the speed, temperature and pressure of the laminator rollers need to be verified, the speed, temperature and pressure of the laminator rollers are different for different laminators and different dry films, and the optimal conditions for the photosensitive dry films are optimized by using the photosensitive dry films and specifications of the U.S. dupont company. Firstly, exploring parameters of a photosensitive dry film by adopting a control variable method for three variables of speed, temperature and pressure of a roller of a laminating machine; then, exposing, developing and observing the change of the appearance of the film through an optical microscope, wherein after exposure, post-treatment is needed, and standing is needed before developing; finally, the optimal parameters of the photosensitive dry film are determined, the adhesion degree of the dry film and the substrate can be adjusted by controlling the speed, the pressure and the temperature of a roller of the laminating machine, and the stability of the dry film is improved.
In addition to considering some parameters of the laminator, it is also necessary to consider the following parameters, such as: exposure time, baking after exposure (including baking time and temperature), standing time after exposure, concentration, temperature and time of the release agent, and the like.
In a specific experiment, in order to realize higher-precision patterning of the carbon nanotube film, the following attempts are respectively adopted:
three variables of the laminator were optimized, such as: respectively trying at 100 deg.C, 110 deg.C, 120 deg.C, 130 deg.C, 140 deg.C and 150 deg.C to obtain optimal temperature of 130 deg.C; the speed and pressure of the rollers were 1.5m/min and 1.0bar, respectively.
The exposure time was optimized, and 4.5s, 6s, 8s, 10s, 12s, 14s, and the like were tried, respectively, to obtain the optimal exposure time of 10 s.
The baking time and temperature after exposure were optimized by trying 90 deg.C, 100 deg.C, 110 deg.C, 120 deg.C, 130 deg.C, 140 deg.C and 30s, 60s, 90s, 120s, 150s, etc., respectively, to obtain the optimum temperature and time of 120 deg.C, 90 s.
For the standing time after exposure, 10min, 15min, 20min, 30min, 1h, 2h, 5h and 24h were tried respectively, and it was found that the difference of the development effect was small when the standing time was more than 15min, and in order to save the process time, the optimum standing time was selected to be 15 min.
For the concentration of the release agent, the temperature and the time of release, the following were tried: the weight concentration of the sodium hydroxide is respectively 1.5%, 2%, 2.5%, 3%, 4%, 5%, 10%, etc., the temperature is respectively 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃, etc., and the demoulding time is respectively 2min, 3min, 4min, 5min, 6min, 7min, 10min, etc. In order to realize the overlay, gold marks need to be made on a polyethylene naphthalate (PEN) substrate, and the gold marks are easy to fall off in sodium hydroxide with high concentration, so that the optimal conditions are 2.5%, 70 ℃ and 5 min.
In order to further illustrate the present invention, the feasibility of the method for fabricating a carbon nanotube thin film transistor based on a photosensitive dry film process of the present invention is further demonstrated by the following figures and examples, which should not be construed as limiting the scope of the present invention.
Example 1
(1) Usually, 5nm titanium and 50nm gold are used for making the mark, but in this embodiment, 50nm gold is only evaporated on PEN for making the mark, because titanium is active, and sodium hydroxide solution reacts with the dry film when peeling off the dry film, so that the mark is peeled off.
(2) As shown in fig. 1, the basic flow of fabricating an all-carbon nanotube thin film transistor device is as follows: first, source and drain electrodes (source and drain); secondly, channeling; thirdly, insulating layer; fourthly, windowing the insulating layer; and fifthly, grid electrode. The device is constituted by: the substrate is a PEN flexible substrate, the gate insulating layer is made of polymer materials (such as polymethyl methacrylate (PMMA)) and the source electrode, the drain electrode, the gate electrode and the semiconductor channel are all carbon nanotube films, the only difference is that the three electrodes adopt high-density (8-12 pieces/mu m) carbon nanotube films, and the channel adopts low-density (0.4-0.6 pieces/mu m) carbon nanotube films.
The carbon nano tube film is a random carbon nano tube network collected by a floating catalytic chemical vapor deposition method, and the preparation method comprises the following steps: under the condition that the temperature is 1100 ℃, slowly and uniformly injecting a ferrocene catalyst solution into a reaction cavity through an injector, and reacting with a carbon source gas to generate a carbon nano tube; and collecting the generated carbon nanotubes at the air outlet end by using a high-flux nitrocellulose membrane (the high-flux nitrocellulose membrane is a nitrate mixed cellulose filter membrane with the aperture of 0.45 micrometer), thereby obtaining the carbon nanotube membrane with random distribution.
(3) The carbon nanotube thin film transistor device structure types comprise: a bottom gate type, a buried gate type, and a top gate type. Taking a top gate carbon nanotube thin film transistor as an example, firstly transferring a high-density carbon nanotube thin film on a PEN substrate, and manufacturing a source electrode and a drain electrode of the transistor on the substrate based on the high-density carbon nanotube thin film; and sticking a photosensitive dry film on the surface of the carbon nanotube film by adopting a film covering technology, and realizing the imaging of the carbon nanotube by adopting a photoetching technology to finish a source drain electrode.
(4) Transferring the low-density carbon nanotube film on the PEN substrate, and manufacturing a channel by dry film coating and photoetching technology.
(5) And preparing the gate insulating layer by processes of spin coating and curing PMMA and the like.
(6) Transferring a high-density carbon nanotube film on a PEN substrate, manufacturing a grid electrode by a dry film laminating and photoetching technology, and finally obtaining the structure of the all-carbon nanotube film transistor as shown in figure 2. Carbon nanotube thin film transistors have excellent electrical properties including low operating voltage, higher current-to-switching ratio, and small gate leakage current. Wherein the working voltage is-40V, and the current on-off ratio is 105~106Gate leakage current of 10-11~10-12A。
In this embodiment, the ultraviolet lithography patterning process is replaced with a photosensitive dry film patterning process, a coating technique is used to coat a photosensitive dry film on the surface of the carbon nanotube film, and the patterning of the carbon nanotube film is achieved by the lithography technique. Therefore, the dry film is used for replacing photoresist, the process flow is simplified, the cost is saved, and the flexible large-area large-scale preparation of the carbon nanotube thin film transistor is realized.
As shown in fig. 3, the top gate type all-carbon nanotube thin film transistor prepared by the photosensitive dry film process on the PEN substrate has good flexibility and high transparency as seen from a macroscopic optical photograph.
As shown in fig. 4 to 5, it can be seen from the scanning electron microscope photographs of the carbon nanotube films of the electrode and the channel that the electrode material is the carbon nanotube film with higher density, and the channel is the carbon nanotube film with lower density without any metal material.
As shown in FIGS. 6-7, the single carbon nanotube thin film transistor and the multiple carbon nanotube thin film transistor devices on the PEN substrate are at VdsTransfer at-1VThe characteristic curve shows that the retardation of the carbon nanotube thin film transistor is very small, and the uniformity is good.
As shown in FIG. 8, the same carbon nanotube TFT device on the PEN substrate is operated at different VgsThe output characteristic curve shows that the grid source voltage VgsAt constant value, source-drain current IdsAnd source-drain voltage VdsThe relationship (2) of (c).
As shown in FIG. 9, the same carbon nanotube TFT device on the PEN substrate has different VdsThe transfer characteristic curves below show that the current switching ratio remains substantially constant.
As shown in fig. 10, according to the distribution diagram of the on-off ratio and the carrier mobility of the multiple carbon nanotube thin film transistor devices on the PEN substrate, the on-off ratio of the devices is high and the uniformity of the devices is good.
As shown in fig. 11, it can be seen from the photo of the inverter that the inverter is composed of two carbon nanotube thin film transistors that share the same source and are shorted to the gate of one transistor.
As shown in fig. 12, it can be seen from the performance test curve of the all-carbon inverter that the inverter has good inversion capability and gain index (maximum value is 17).
The embodiment result shows that the invention provides the manufacturing method of the carbon nanotube thin film transistor based on the photosensitive dry film process, the large-scale preparation of the large-area, low-cost and flexible carbon nanotube thin film transistor is completed under normal pressure, and the manufacturing method has important significance for promoting the progress of the carbon nanotube thin film in the fields of large-scale preparation and application of all-carbon nanotube thin film transistor devices.
Claims (10)
1. A manufacturing method of a carbon nano tube thin film transistor is characterized by comprising the following steps:
(1) manufacturing a source electrode and a drain electrode of a transistor on a substrate based on the high-density carbon nanotube film;
(2) sticking a photosensitive dry film on the surface of the carbon nanotube film by adopting a film coating technology, and realizing the imaging of the carbon nanotube film by adopting a photoetching technology;
(3) transferring the low-density carbon nanotube film, and manufacturing a channel by a dry film laminating and photoetching technology;
(4) preparing a gate insulating layer by a spin-on curing process;
(5) carrying out insulating layer windowing on the gate insulating layer;
(6) transferring the high-density carbon nanotube film, and manufacturing a grid electrode by using a dry film laminating and photoetching technology;
the source electrode, the drain electrode and the grid electrode are formed by 8-12 high-density carbon nano tube films per mu m; the semiconductor channel is made of a low-density carbon nanotube film material with 0.4-0.6 carbon nanotubes per mu m;
the carbon nano tube film is a random carbon nano tube network collected by a floating catalytic chemical vapor deposition method, and the preparation method comprises the following steps: under the condition that the temperature is 1100 +/-50 ℃, injecting ferrocene catalyst solution into a reaction cavity through an injector at a constant speed, and reacting with carbon source gas to generate a carbon nano tube; collecting the generated carbon nanotubes at the air outlet end by using a high-flux nitrocellulose membrane, thereby obtaining a carbon nanotube film which is randomly distributed;
in the photosensitive dry film process, the adhesion degree of a dry film and a substrate is adjusted by controlling the speed, the pressure and the temperature of a roller of a laminating machine, so that the stability of the dry film is improved; wherein the speed of the roller is 0.5-2.0 m/min, the pressure is 0.5-1.5 bar, and the temperature is 100-150 ℃.
2. The manufacturing method according to claim 1, wherein before the source electrode and the drain electrode are manufactured in step (1), demolding is performed, and a demolding agent used for demolding is a sodium hydroxide solution; the concentration of the release agent is 2.5%; the temperature of the release agent is 70 ℃; the demolding time is 5 min.
3. The method of claim 1, wherein the laminator rollers are at a speed of 1.5m/min, a pressure of 1.0bar, and a temperature of 130 ℃.
4. The manufacturing method according to claim 1, wherein in the photosensitive dry film process, the change in morphology is observed by exposure, development, and an optical microscope, and the post-treatment is performed after the exposure is completed and the standing is performed before the development is performed.
5. The method according to claim 4, wherein the exposure time is 4.5 to 14 seconds, the baking is performed after the exposure is completed, the baking time is 30 to 150 seconds, the baking temperature is 90 to 140 ℃, and the standing time is 10 to 30 min.
6. The method of claim 5, wherein the exposure time is 10s, the baking time is 90s, the baking temperature is 120 ℃, and the standing time is 15 min.
7. The carbon nanotube thin film transistor manufactured by the manufacturing method of any one of claims 1 to 6, wherein the device structure of the carbon nanotube thin film transistor comprises a substrate and a source electrode, a drain electrode, a semiconductor channel, a gate insulating layer and a gate electrode which are arranged on the substrate, wherein the source electrode, the drain electrode and the gate electrode are formed by high-density carbon nanotube thin films with 8-12 carbon atoms/μm; the semiconductor channel is made of a low-density carbon nanotube film material with 0.4-0.6 carbon nanotubes/micrometer.
8. The carbon nanotube thin film transistor of claim 7, wherein the structure type of the carbon nanotube thin film transistor device is a bottom gate type, a buried gate type, or a top gate type.
9. The carbon nanotube thin film transistor according to claim 7, wherein the substrate is a flexible substrate, and the material of the gate insulating layer is a polymer material.
10. The carbon nanotube thin film transistor of claim 9, wherein the flexible substrate is polyethylene naphthalate and the polymer material is polymethyl methacrylate.
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