CN112420499A - Patterned alumina dielectric layer and grid based on screen printing, and preparation method and application thereof - Google Patents

Patterned alumina dielectric layer and grid based on screen printing, and preparation method and application thereof Download PDF

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CN112420499A
CN112420499A CN201910785990.7A CN201910785990A CN112420499A CN 112420499 A CN112420499 A CN 112420499A CN 201910785990 A CN201910785990 A CN 201910785990A CN 112420499 A CN112420499 A CN 112420499A
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dielectric layer
layer
alumina dielectric
screen printing
substrate
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CN112420499B (en
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张静
胡文平
段树铭
任晓辰
耿博文
高雄
汪涛
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Tianjin University
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    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
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    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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    • H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
    • H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
    • H01L21/02172—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides
    • H01L21/02175—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal
    • H01L21/02178—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal the material containing aluminium, e.g. Al2O3
    • H—ELECTRICITY
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    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
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    • H01L21/28079—Making conductor-insulator-semiconductor electrodes the insulator being formed after the semiconductor body, the semiconductor being silicon characterised by the conductor the final conductor layer next to the insulator being a single metal, e.g. Ta, W, Mo, Al
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    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • H01L21/28008—Making conductor-insulator-semiconductor electrodes
    • H01L21/28017—Making conductor-insulator-semiconductor electrodes the insulator being formed after the semiconductor body, the semiconductor being silicon
    • H01L21/28158—Making the insulator
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    • H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof  ; Multistep manufacturing processes therefor
    • H01L29/40—Electrodes ; Multistep manufacturing processes therefor
    • H01L29/41—Electrodes ; Multistep manufacturing processes therefor characterised by their shape, relative sizes or dispositions
    • H01L29/423—Electrodes ; Multistep manufacturing processes therefor characterised by their shape, relative sizes or dispositions not carrying the current to be rectified, amplified or switched
    • H01L29/42312—Gate electrodes for field effect devices
    • H01L29/42316—Gate electrodes for field effect devices for field-effect transistors
    • H01L29/4232—Gate electrodes for field effect devices for field-effect transistors with insulated gate
    • H01L29/42364—Gate electrodes for field effect devices for field-effect transistors with insulated gate characterised by the insulating layer, e.g. thickness or uniformity
    • H—ELECTRICITY
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    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof  ; Multistep manufacturing processes therefor
    • H01L29/40—Electrodes ; Multistep manufacturing processes therefor
    • H01L29/41—Electrodes ; Multistep manufacturing processes therefor characterised by their shape, relative sizes or dispositions
    • H01L29/423—Electrodes ; Multistep manufacturing processes therefor characterised by their shape, relative sizes or dispositions not carrying the current to be rectified, amplified or switched
    • H01L29/42312—Gate electrodes for field effect devices
    • H01L29/42316—Gate electrodes for field effect devices for field-effect transistors
    • H01L29/4232—Gate electrodes for field effect devices for field-effect transistors with insulated gate
    • H01L29/42372—Gate electrodes for field effect devices for field-effect transistors with insulated gate characterised by the conducting layer, e.g. the length, the sectional shape or the lay-out

Abstract

The invention discloses a patterned alumina dielectric layer and a grid based on screen printing, a preparation method and application thereof, wherein the preparation method comprises the following steps: immersing the alumina dielectric layer with limited growth in isopropanol, carrying out ultrasonic treatment for 5-10 minutes, drying, carrying out silk-screen printing on a layer of photoresist serving as an anti-corrosion layer on the alumina dielectric layer by adopting a silk-screen printing method, and curing for 1-2 minutes; and putting the obtained substrate into etching liquid until the alumina dielectric layer which is not covered by the anti-corrosion layer is etched, and cleaning the anti-corrosion layer to obtain the patterned alumina dielectric layer and the grid electrode. The preparation method provided by the invention is simple to operate, the patterned alumina dielectric layer and the grid electrode can be obtained by only two steps, various patterns can be simply and quickly obtained by printing the anti-corrosion layer by adopting a screen printing method, better conditions are provided for subsequent circuit design, and the method can be used for preparing complex circuits without the complex and time-consuming operation like the traditional photoetching and etching patterning technology.

Description

Patterned alumina dielectric layer and grid based on screen printing, and preparation method and application thereof
Technical Field
The invention belongs to the technical field of semiconductor thin film transistor preparation, and particularly relates to a patterned alumina dielectric layer and a patterned alumina gate based on screen printing, and a preparation method and application thereof.
Background
In recent years, Thin Film Transistors (TFTs) have become the core component of display driving backplanes in the flat panel display industry, and with the development of large-scale integrated circuit technology, the device size, including the thickness of the dielectric layer, is becoming smaller and smaller, and the trend of reduction follows moore's law. However, in the TFT device, most of the dielectric layers are based on silicon oxide materials, and as the thickness of the silicon oxide is reduced, the leakage current of the dielectric layer will gradually increase, which causes high energy consumption and heat dissipation problems of the device. In order to solve the related problems, a high dielectric constant (high-k) dielectric layer is used to replace silicon oxide to reduce gate leakage current and increase capacitance density, so that the preparation of a new high-k dielectric layer capable of replacing silicon oxide is the primary task to further improve the performance and integration of integrated circuits. High-k materials currently being the focus of research include AlOx、ZrO2、HfO2And the like. The common method for preparing the metal oxide is a sol-gel method or a physical vapor deposition method, and the organic substances used in the method are generally inflammable and toxic, and the temperature required for preparation is also high (over 400 ℃), which is not beneficial to realizing a flexible circuit. Compared with other materials and methods, the aluminum is used as an active metal, the aluminum oxide dielectric layer can be obtained by processing at room temperature through an electrochemical method, the operation of preparing the aluminum oxide dielectric layer through electrochemical anodic oxidation is simple, high-temperature heating is not needed, the cost is low, and the method is suitable for mass production. However, the existing anodic aluminum oxide growth technology enables aluminum oxide to completely cover the surface of aluminum, and secondary patterning etching needs to be carried out on the aluminum oxide to realize the construction of a complex circuit. Because the chemical properties of the aluminum oxide and the aluminum are closeThe complex protection process is needed for independently etching the aluminum oxide, so that the preparation cost is greatly increased, and the advantages of the anodic aluminum oxide method are limited.
In addition, semiconductor manufacturing is divided into wafer manufacturing and integrated circuit manufacturing, patterning technology is an essential part in integrated circuit manufacturing, and commonly used patterning technology comprises photoetching development and etching processes, a mask pattern is manufactured by using the photoetching development method, the operation is complex, a series of operations such as pretreatment, glue leveling, prebaking, alignment exposure, development, postbaking and the like are required, and a series of problems such as high energy consumption, high pollution, high cost and the like are caused. How to implement patterning by using a low-cost method instead of the photolithography process becomes a difficult problem.
Disclosure of Invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a method for fabricating a confined growth alumina dielectric layer with common gate contact sites, which enables patterning of the confined growth alumina dielectric layer (alumina) during anodization to create gate connection sites in an anodized alumina TFT-based integrated circuit without the need for a secondary etch of the alumina.
The invention also aims to provide the alumina dielectric layer with limited growth in the limited domain obtained by the preparation method.
It is another object of the present invention to provide the use of the above-described limited growth alumina dielectric layer in a field effect transistor.
Another object of the present invention is to provide a method for preparing a patterned alumina dielectric layer and a gate electrode based on screen printing.
Another object of the present invention is to provide a patterned alumina dielectric layer and a gate obtained by the above preparation method.
It is another object of the present invention to provide the use of the above-described patterned alumina dielectric layer and gate electrode in a field effect transistor.
The purpose of the invention is realized by the following technical scheme.
A method of making a confined growth alumina dielectric layer with a common gate contact site comprising the steps of:
1) vacuum deposition of a grid:
cleaning the substrate, drying the substrate, and evaporating an aluminum film with the thickness of 70-150nm on the substrate to be used as a grid;
in the step 1), the method for drying the substrate is blow-drying with nitrogen.
In the step 1), the substrate is a rigid substrate or a flexible substrate, the rigid substrate is a quartz plate or a glass slide, and the flexible substrate is polyethylene naphthalate (PEN) or polymethyl methacrylate (PMMA).
In the step 1), the purity of the nitrogen is 99.999%.
2) Printing a layer of photoresist material on the aluminum film by adopting a screen printing method as a mask, and curing for 1-2 minutes;
in the step 2), the screen used in the screen printing method is 300-500 meshes, and the moving speed of the scraper during screen printing is 5-20 mm/s.
In the step 2), the pattern of the mask is a rectangular photoresist layer arranged along a rectangular matrix, and the size of the rectangular photoresist layer is 300 μm × 300 μm.
In the step 2), the photoresist material is a positive photoresist material or a negative photoresist material.
In the step 2), the curing temperature is 40-80 ℃.
3) Electrochemical anodic oxidation:
taking the substrate as an anode, taking a conductive material as a cathode, soaking the anode and the cathode in electrolyte, applying constant current between the anode and the cathode to oxidize the aluminum film which is not covered by the mask in the step 2) to form aluminum oxide, and washing the mask by using an organic solvent to obtain the aluminum oxide dielectric layer with limited growth.
In the step 3), the conductive material is Pt, Au or graphite.
In the step 3), the density of the constant current is 0.007-0.07 mA/cm2。
In the step 3), the organic solvent is isopropanol, ethanol or dichloromethane.
The use of the above-described limited growth alumina dielectric layer in a field effect transistor.
In the technical scheme, an organic film is covered on the alumina dielectric layer of the alumina dielectric layer growing in the limited area, a mask is attached to the organic film, and a silver layer is evaporated in vacuum to be used as a source electrode and a drain electrode, so that the field effect transistor is obtained.
In the technical scheme, a mask is attached to the alumina dielectric layer grown in the limited area, organic matters are evaporated in vacuum to form an organic matter film, then the mask is attached, and a silver layer is evaporated in vacuum to be used as a source electrode and a drain electrode, so that the field effect transistor is obtained.
In the above technical solution, the organic thin film is made of C8-BTBT or C10-DNTT.
In the technical scheme, the mobility rate of the field effect transistor can be 2.6-3 cm2/(v*s)-1On/off ratio of 105～107。
The preparation method of the alumina dielectric layer with limited growth has the following beneficial effects:
1. the growth of alumina based on anodic oxidation can avoid the high-temperature heating requirement required by thermal growth or solvent-gel method and physical vapor deposition, reduce the production cost and be beneficial to large-scale production.
2. The preparation method of the invention is based on the preparation of the common gate connection site in the circuit and the alumina dielectric layer grown in the patterning limited area, the operation is simple, the secondary patterning etching of alumina is not needed, because the chemical properties of alumina and aluminum are close, if the alumina is etched separately, a complex protection process is needed, the preparation cost is greatly increased, compared with the method of thermally growing alumina and performing the secondary etching, the alumina obtained by the preparation method of the invention has low leakage current density and small variation range, and the performance is stable and excellent.
3. The surface roughness of the aluminum oxide dielectric layer obtained by the method is lower than 2nm, the surface is smooth, an excellent contact interface is provided for the subsequent preparation of a transistor, and better device properties are favorably obtained.
4. The substrate can be a rigid substrate or a flexible substrate, so that a rigid device or a flexible device can be prepared. When a flexible substrate is used, an electronic skin, flexible device can be made.
5. The preparation method of the invention has simple steps, obtains the grid connection sites required by the preparation circuit, and can form complex logic circuits, such as inverters, triggers and the like.
A preparation method of a patterned alumina dielectric layer and a grid based on screen printing comprises the following steps:
a) immersing the alumina dielectric layer grown in the limited area into isopropanol, carrying out ultrasonic treatment for 5-10 minutes, drying, carrying out silk-screen printing on a layer of photoresist serving as an anti-corrosion layer on the alumina dielectric layer by adopting a silk-screen printing method, and curing for 1-2 minutes;
in the step a), the drying is blow-drying with nitrogen.
In the step a), the purity of the nitrogen is 99.999%, the screen used in the screen printing method is 300-500 meshes, and the moving speed of the scraper during screen printing is 5-20 mm/s.
In the step a), the photoresist is a positive photoresist material or a negative photoresist material.
In the step a), the curing temperature is 40-80 ℃.
In the step a), the pattern of the resist layer is a photoresist layer arranged along a rectangular matrix, and the size of the photoresist layer is 700 μm × 700 μm.
b) Putting the substrate obtained in the step a) into etching liquid until the alumina dielectric layer which is not covered by the anti-corrosion layer is etched, and cleaning the anti-corrosion layer to obtain the patterned alumina dielectric layer and the grid electrode.
In the step b), the etching solution is a phosphoric acid aqueous solution, and the concentration of phosphoric acid in the etching solution is 60-90 wt%.
In the step b), the method for cleaning the resist layer comprises: firstly, adopting water to wash the etching solution, and then adopting an organic cleaning solution to wash the anti-corrosion layer, wherein the washing time is at least 10s, and the organic cleaning solution is isopropanol, ethanol or dichloromethane.
After said step b), a modification step is carried out: and soaking the patterned aluminum oxide dielectric layer and the grid electrode into the modification liquid for at least 2 hours, and then cleaning.
In the modification step, the modification liquid is an octadecyl phosphoric acid solution, and the solvent is isopropanol.
In the technical scheme, the concentration of octadecyl phosphate in the modification liquid is 2-4 mM.
In the modification step, isopropanol is adopted for cleaning, and the cleaning time is 5-10 min.
Use of the patterned alumina dielectric layer and gate electrode described above in a field effect transistor.
In the above technical solution, the method for manufacturing a field effect transistor comprises: and covering a layer of organic film on the patterned alumina dielectric layer and the alumina dielectric layer of the grid, attaching a mask plate on the organic film, and performing vacuum evaporation on a silver layer serving as a source electrode and a drain electrode to obtain the field effect transistor.
In the above technical solution, the method for manufacturing a field effect transistor comprises: attaching a mask plate on the patterned alumina dielectric layer and the alumina dielectric layer of the grid, carrying out vacuum evaporation on organic matters to form an organic matter film, attaching a mask plate, and carrying out vacuum evaporation on a silver layer serving as a source electrode and a drain electrode to obtain a field effect transistor; connecting a plurality of field effect transistors into a Pseudo-D inverter.
In the above technical solution, the organic thin film is made of C8-BTBT or C10-DNTT.
In the technical scheme, the mobility rate of the field effect transistor can be 3-5 cm2/(v*s)-1Average number of switching ratios is 106The Pseudo-D inverter gain is 75.
The preparation method of the patterned alumina dielectric layer and the grid based on the screen printing has the following beneficial effects:
1. the preparation method provided by the invention is simple to operate, the patterned alumina dielectric layer and the grid electrode can be obtained by only two steps, various patterns can be simply and quickly obtained by printing the anti-corrosion layer by adopting a screen printing method, better conditions are provided for subsequent circuit design, and the method can be used for preparing complex circuits without the complex and time-consuming operation like the traditional photoetching and etching patterning technology.
2. In the invention, a single medium-strong acid phosphoric acid solution is selected instead of a complex mixed solution, so that the danger of operation by using a strong acid is reduced, and the complex use steps required by using the strong acid are avoided. After the curing is completed, the substrate is immersed in the etching solution, and after the etching is completed, the substrate is cleaned by using an organic cleaning solution, and then the patterned dielectric layer and the patterned gate electrode are obtained, as shown in fig. 10.
3. The patterned alumina dielectric layer obtained by a series of operations has low leakage current density, small variation range and excellent property, is beneficial to obtaining better device performance, and the prepared TFT device and the Pseudo-D inverter have outstanding properties and can be applied to the manufacture of integrated circuits in the semiconductor industry.
Drawings
FIG. 1 is a flow chart of a method for preparing a confined growth alumina dielectric layer according to the present invention;
FIG. 2 is a schematic diagram of an electrochemical anodization apparatus in an embodiment of the present invention;
FIG. 3(a) is a schematic cross-sectional view after completion of step 2), and FIG. 3(b) is an optical image of a mask obtained after step 2) of example 2; FIG. 3(c) is an enlarged view of FIG. 3 (b);
FIG. 4(a) is a schematic cross-sectional view after step 3) is completed, and FIG. 4(b) is an optical picture of the alumina dielectric layer and the gate site obtained in step 3) of example 2; FIG. 4(c) is an enlarged view of FIG. 4 (b);
FIG. 5 is a graph of current versus voltage for different gate sites in example 2 of the present invention;
FIG. 6 is an AFM image of aluminum (left) and alumina (right) obtained in example 2 of the present invention;
FIG. 7 is a transfer characteristic curve of the C8-BTBT transistor fabricated in example 1 of the present invention;
FIG. 8 is a transfer characteristic curve of a C10-DNTT transistor prepared in example 2 of the present invention;
FIG. 9 is a flow chart of a method for forming a patterned alumina dielectric layer and a gate electrode according to the present invention;
FIG. 10(a) is a schematic cross-sectional view after step b) is completed, and FIG. 10(b) is an optical picture of the patterned alumina and the gate obtained in step b) of example 3; FIG. 10c) is an enlarged view of FIG. 10 (b);
FIG. 11 is a schematic view of a patterned alumina dielectric layer J-V in example 3 of the present invention;
FIG. 12 is a transfer curve of a single device in example 3 of the present invention;
FIG. 13 is a schematic view of a patterned alumina dielectric layer J-V in example 4 of the present invention;
FIG. 14 is a transfer curve of a single device in example 4 of the present invention;
fig. 15(a) schematic diagram of inverter structure design, (b) photo optics of inverter sample, (c) gain of inverter prepared based on the present invention.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
The purity of the nitrogen is 99.999 percent
Example 1
As shown in fig. 1, a method for preparing a confined growth alumina dielectric layer with a common gate contact site comprises the following steps:
1) vacuum deposition of a grid:
a substrate is prepared, the substrate being polyethylene naphthalate (PEN). Cleaning the substrate, drying the substrate by using nitrogen, and evaporating and coating a layer of aluminum film with the thickness of 100nm on the substrate to be used as a grid;
2) printing a layer of photoresist material on the aluminum film by a screen printing method to be used as a mask, and determining that the pattern is clearly printed, as shown in fig. 3(3(a), 3(b) and 3(c)), curing for 2 minutes at 60 ℃ (in order to reduce the corrosion of the electrolyte in an electrolytic cell to the pattern in the mask area, the mask needs to be cured); wherein the photoresist material is photoresist. The screen used in the screen printing method was 500 mesh, the squeegee moved at a speed of 20mm/s during screen printing, the mask pattern was a rectangular photoresist layer arranged along a rectangular matrix, and the dimensions of the rectangular photoresist layer were 300. mu. m.times.300. mu.m.
3) Electrochemical anodic oxidation:
using the substrate printed with the mask as an anode, graphite as a conductive material, and a conductive material as a cathode, and immersing the anode and the cathode in an electrolyte, as shown in FIG. 2, with a density of 0.07mA/cm was applied between the anode and the cathode2The anode immersed in the electrolyte solution is oxidized to form alumina by the oxidation reaction of the anode, and the alumina film not covered by the mask of step 2) is washed away by ethanol to obtain a confined growth alumina dielectric layer with a gate connection site, as shown in fig. 4(4(a), 4(b) and 4 (c)).
Preparing a flexible low-voltage C8-BTBT field effect transistor: the flexible alumina dielectric layer with limited-area growth prepared by the steps 1) -3) is coated with a layer of C8-BTBT film with the thickness of 27-30nm by a solution shearing method, then a mask plate (the mask plate is customized to Beijing New Bailey technology Co., Ltd., the width-length ratio is 3:1) is attached to the surface of the C8-BTBT film, silver with the thickness of 40nm is evaporated in vacuum to be used as a source electrode and a drain electrode, and the C8-BTBT transistor is obtained, wherein the channel width-length ratio is 3: 1. the electrical performance is tested on a Kerthley4200CSC of an electrical performance testing instrument, the transfer characteristic curve of the C8-BTBT transistor is shown in figure 7, the characteristic of a typical p-type field effect transistor is shown, the saturation voltage is as low as 5 volts, and the mobility of the prepared flexible low-voltage C8-BTBT transistor can reach 3cm2/(v*s)-1On-off ratio of 105. C8-BTBT has the following structural formula:
Figure BDA0002178035260000071
example 2
A method of making a confined growth alumina dielectric layer with a common gate contact site comprising the steps of:
1) vacuum deposition of a grid:
a substrate is prepared, the substrate being a glass slide. Cleaning the substrate, drying the substrate by using nitrogen, and evaporating and coating a layer of aluminum film with the thickness of 100nm on the substrate to be used as a grid;
2) printing a layer of photoresist material on the aluminum film by a screen printing method to be used as a mask, determining that the pattern is clearly printed, and curing for 2 minutes at 60 ℃ (the mask needs to be cured in order to reduce the corrosion of electrolyte in an electrolytic cell to the pattern in the mask area); wherein the photoresist material is photoresist. The screen used in the screen printing method was 500 mesh, the squeegee moved at a speed of 20mm/s during screen printing, the mask pattern was a rectangular photoresist layer arranged along a rectangular matrix, and the dimensions of the rectangular photoresist layer were 300. mu. m.times.300. mu.m. .
3) Electrochemical anodic oxidation:
using the substrate printed with the mask as an anode, preparing graphite as a conductive material, using the conductive material as a cathode, soaking the anode and the cathode in an electrolyte, and applying a density of 0.07mA/cm between the anode and the cathode2The anode soaked in the electrolyte generates oxidation reaction, the aluminum film which is not covered by the mask in the step 2) is oxidized to form aluminum oxide, and the mask is washed away by ethanol to obtain the alumina dielectric layer with the gate connection site and growing in a limited area.
Conducting tests on different gate connection sites of the prepared alumina dielectric layer with limited domain growth by using Keithley 4200CSC are shown in FIG. 5, and it can be found that different gate connection sites are mutually conducted to provide gates for preparing complex circuits such as inverters later. The roughness of the prepared aluminum oxide dielectric layer with limited growth and the surface of the grid site are measured by using a scanning probe microscope (AFM), as shown in FIG. 6, the root-mean-square roughness of aluminum and aluminum oxide is respectively 2.52 nm and 1.45nm, the surface is smooth, an excellent contact interface is provided for the subsequent preparation of a transistor, and better device properties are obtained.
Preparing a low-voltage C10-DNTT field effect thin film transistor: attaching a mask plate (the mask plate is customized to the Bairui technology emerging in Beijing) on the alumina dielectric layer with limited growth prepared by the steps 1) to 3)Technology ltd, width to length ratio 5: 1). Vacuum evaporating a 40nm thick C10-DNTT film, then attaching a mask plate (the mask plate is customized to Beijing New Bairui technology Co., Ltd., the width-length ratio is 3:1) to the surface of the C10-DNTT film, and vacuum evaporating 40nm thick silver as a source electrode and a drain electrode to obtain the C10-DNTT transistor, wherein the channel width-length ratio is 3: 1. the electrical performance is tested on an electrical performance test instrument Keithley 4200CSC, a transfer curve is shown in figure 8, the characteristic of a typical p-type field effect transistor is shown, the saturation voltage is low to 5 volts, and the mobility of the prepared C10-DNTT transistor can reach 2.6cm2/(v*s)-1On-off ratio of 107. The structural formula of C10-DNTT is as follows:
Figure BDA0002178035260000081
example 3
As shown in fig. 9, a method for preparing a patterned alumina dielectric layer and a gate electrode based on screen printing comprises the following steps:
a) immersing the alumina dielectric layer of the alumina dielectric layer with the limited growth obtained in the embodiment 2 in isopropanol, ultrasonically treating for 5 minutes, drying by using nitrogen, screen-printing a layer of photoresist on the alumina dielectric layer by adopting a screen printing method as an etch-resistant layer (ensuring that the pattern is clearly printed), and curing at 80 ℃ for 2 minutes, wherein the photoresist is a positive photoresist, the screen adopted in the screen printing method is 500 meshes, the moving speed of a scraper during screen printing is 20mm/s, the pattern of the etch-resistant layer is a photoresist layer arranged along a rectangular matrix, and the size of the photoresist layer is a square of 700 micrometers x 700 micrometers;
b) putting the substrate obtained in the step a) into an etching solution until the alumina dielectric layer which is not covered by the etching resistant layer is etched, and cleaning the etching resistant layer to obtain a patterned alumina dielectric layer and a grid electrode (the grid electrode and the patterned alumina dielectric layer positioned on the grid electrode), wherein the etching solution is a phosphoric acid aqueous solution, the concentration of phosphoric acid in the etching solution is 85 wt%, and the method for cleaning the etching resistant layer comprises the following steps: the etching solution is washed away by water, and then the anti-corrosion layer is washed away by isopropanol, wherein the washing time is 10 s.
The prepared dielectric layers were tested for leakage current density using Keithley 4200CSC, as shown in the current-voltage diagram of fig. 11, at low voltage, the leakage current density was below 10-8A/cm2The alumina has low leakage current density and small variation range, and shows stable and excellent performance.
Preparing a low-voltage C8-BTBT field effect transistor: coating a layer of C8-BTBT film with the thickness of 27-30nm on the patterned alumina dielectric layer prepared in the steps a) -b) by a solution shearing method, and then attaching a mask plate to the surface of the C8-BTBT film (the mask plate is customized to Beijing New Bairui technology Co., Ltd., the width-length ratio is 5: 1) and performing vacuum evaporation on silver with the thickness of 40nm as a source electrode and a drain electrode to obtain the C8-BTBT transistor, wherein the channel width-length ratio is 5: 1. when the electrical performance is tested on a Kerthley4200CSC of an electrical performance testing instrument, the transfer characteristic curve and the leakage current of the C8-BTBT transistor are shown in figure 12, and the mobility of the prepared flexible C8-BTBT transistor can reach 5cm2/(v*s)-1On-off ratio of 106. C8-BTBT has the following structural formula:
Figure BDA0002178035260000091
example 4
A preparation method of a patterned alumina dielectric layer and a grid based on screen printing comprises the following steps:
a) immersing the alumina dielectric layer of the alumina dielectric layer with the limited growth obtained in the embodiment 2 in isopropanol, ultrasonically treating for 5 minutes, drying by using nitrogen, screen-printing a layer of photoresist on the alumina dielectric layer by adopting a screen printing method as an etch-resistant layer (ensuring that the pattern is clearly printed), and curing at 80 ℃ for 2 minutes, wherein the photoresist is a positive photoresist, the screen adopted in the screen printing method is 500 meshes, the moving speed of a scraper during screen printing is 20mm/s, the pattern of the etch-resistant layer is a photoresist layer arranged along a rectangular matrix, and the size of the photoresist layer is a square of 700 micrometers x 700 micrometers;
b) putting the substrate obtained in the step a) into etching liquid until the alumina dielectric layer which is not covered by the corrosion-resistant layer is etched, cleaning the corrosion-resistant layer to obtain the patterned alumina dielectric layer and the grid electrode, wherein the etching liquid is phosphoric acid aqueous solution, the concentration of phosphoric acid in the etching liquid is 85 wt%, and the method for cleaning the corrosion-resistant layer comprises the following steps: the etching solution is washed away by water, and then the anti-corrosion layer is washed away by isopropanol, wherein the washing time is 10 s.
After step b), a modification step is carried out: and soaking the patterned alumina dielectric layer and the grid electrode in a modifying solution for 2 hours, and cleaning for 5 minutes by using isopropanol, wherein the modifying solution is an octadecyl phosphate solution, a solvent of the modifying solution is isopropanol, and the concentration of octadecyl phosphate in the modifying solution is 2 mM.
The leakage current density of the prepared dielectric layers was tested using Keithley 4200CSC and it was found that the leakage current density was below 10 at low voltage-9A/cm2And the leakage current is stable as shown in the current-voltage diagram of fig. 13.
Preparation of a Pseudo-D inverter: attaching a mask plate on the patterned alumina dielectric layer prepared in the steps a) to b). Vacuum evaporation is carried out to coat a C10-DNTT film with the thickness of 40nm, then a mask plate (the mask plate is customized in Beijing New Bairui technology Co., Ltd., the width-length ratio is customized according to circuit design) is attached to the surface of the C10-DNTT film, vacuum evaporation is carried out to coat 40nm silver as a source electrode and a drain electrode, 4C 10-DNTT field effect thin film transistors are obtained, and the width-length ratios of the mask plates of the 4C 10-DNTT field effect thin film transistors are sequentially 2: 1. 6: 1. 6: 1. 10: 1, connecting 4C 10-DNTT field effect thin film transistors to each other as shown in the structural design schematic diagram of the inverter in fig. 15(a) to obtain a Pseudo-D inverter, wherein as shown in fig. 15(a), the channel width-to-length ratio of the Pseudo-D inverter is 2 from top to bottom: 1. 6: 1. 6: 1. 10: 1. when the electrical performance is tested on a Keithley 4200CSC electrical performance test instrument, the transfer curve and the grid leakage current are shown in figure 14, and the mobility of the prepared C10-DNTT field effect thin film transistor can reach 3cm2/(v*s)-1On-off ratio of 106The Pseudo-D inverter gain can reach 75 as shown in FIG. 15 c.
Statement regarding sponsoring research or development
The invention obtains the fund support of China department of science and technology (approval numbers: 2016YFB0401100 and 2017YFA0204503), national science fund (51702297,51633006,51725304,51733004,51703159 and 51703160) and strategic focus research.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.

Claims (10)

1. A preparation method of a patterned alumina dielectric layer and a grid based on screen printing is characterized by comprising the following steps:
a) immersing the alumina dielectric layer with limited growth in isopropanol, carrying out ultrasonic treatment for 5-10 minutes, drying, carrying out silk-screen printing on a layer of photoresist serving as an anti-corrosion layer on the alumina dielectric layer by adopting a silk-screen printing method, and curing for 1-2 minutes;
b) placing the substrate obtained in the step a) into an etching solution until the alumina dielectric layer which is not covered by the anti-corrosion layer is etched, cleaning the anti-corrosion layer to obtain a patterned alumina dielectric layer and a grid electrode, wherein,
the preparation method of the alumina dielectric layer with limited growth comprises the following steps:
1) vacuum deposition of a grid: cleaning the substrate, drying the substrate, and evaporating an aluminum film with the thickness of 70-150nm on the substrate to be used as a grid;
2) printing a layer of photoresist material on the aluminum film by adopting a screen printing method as a mask, and curing for 1-2 minutes;
3) electrochemical anodic oxidation: taking the substrate as an anode, taking a conductive material as a cathode, soaking the anode and the cathode in electrolyte, applying constant current between the anode and the cathode to oxidize the aluminum film which is not covered by the mask in the step 2) to form aluminum oxide, and washing the mask by using an organic solvent to obtain the aluminum oxide dielectric layer with limited growth.
2. The method according to claim 1, wherein in the step a), the drying is blow-drying with nitrogen gas;
in the step a), the purity of the nitrogen is 99.999%, the screen used in the screen printing method is 300-500 meshes, and the moving speed of the scraper during screen printing is 5-20 mm/s;
in the step a), the photoresist is a positive photoresist material or a negative photoresist material;
in the step a), the curing temperature is 40-80 ℃;
in the step a), the pattern of the resist layer is a photoresist layer arranged along a rectangular matrix, and the size of the photoresist layer is 700 μm × 700 μm;
in the step b), the etching solution is a phosphoric acid aqueous solution, and the concentration of phosphoric acid in the etching solution is 60-90 wt%;
in the step b), the method for cleaning the resist layer comprises: firstly, washing the etching solution by using water, and then washing the anti-corrosion layer by using an organic cleaning solution, wherein the washing time is at least 10s, and the organic cleaning solution is isopropanol, ethanol or dichloromethane;
after said step b), a modification step is carried out: and soaking the patterned aluminum oxide dielectric layer and the grid electrode into the modification liquid for at least 2 hours, and then cleaning.
3. The method of claim 2, wherein in the step 1), the substrate is dried by blowing with nitrogen gas;
in the step 1), the substrate is a rigid substrate or a flexible substrate, the rigid substrate is a quartz plate or a glass slide, and the flexible substrate is polyethylene naphthalate or polymethyl methacrylate;
in the step 1), the purity of the nitrogen is 99.999 percent;
in the step 2), the screen adopted in the screen printing method is 300-500 meshes, and the moving speed of the scraper during screen printing is 5-20 mm/s;
in the step 2), the pattern of the mask is a rectangular photoresist material layer arranged along a rectangular matrix, and the size of the rectangular photoresist material layer is 300 microns multiplied by 300 microns;
in the step 2), the photoresist material is a positive photoresist material or a negative photoresist material;
in the step 2), the curing temperature is 40-80 ℃;
in the step 3), the conductive material is Pt, Au or graphite;
in the step 3), the density of the constant current is 0.007-0.07 mA/cm2；
In the step 3), the organic solvent is isopropanol, ethanol or dichloromethane.
4. The preparation method according to claim 2 or 3, wherein in the modification step, the modification solution is an octadecyl phosphate solution, the solvent is isopropanol, the concentration of octadecyl phosphate in the modification solution is 2-4 mM, isopropanol is used for cleaning, and the cleaning time is 5-10 min.
5. The patterned alumina dielectric layer and the gate obtained by the preparation method according to any one of claims 1 to 4.
6. Use of the patterned alumina dielectric layer and gate of claim 5 in field effect transistors and Pseudo-D inverters.
7. The use according to claim 6, wherein the field effect transistor is prepared by a method comprising: and covering a layer of organic film on the patterned alumina dielectric layer and the alumina dielectric layer of the grid, attaching a mask plate on the organic film, and performing vacuum evaporation on a silver layer serving as a source electrode and a drain electrode to obtain the field effect transistor.
8. The use according to claim 6, wherein the field effect transistor is prepared by a method comprising: attaching a mask plate on the patterned alumina dielectric layer and the alumina dielectric layer of the grid, carrying out vacuum evaporation on organic matters to form an organic matter film, attaching a mask plate, and carrying out vacuum evaporation on a silver layer serving as a source electrode and a drain electrode to obtain a field effect transistor; connecting a plurality of field effect transistors into a Pseudo-D inverter.
9. The use of claim 7 or 8, wherein the organic thin film is C8-BTBT or C10-DNTT.
10. The use according to claim 9, wherein the field effect transistor can have a mobility of 3-5 cm2/(v*s)-1Average number of switching ratios is 106The Pseudo-D inverter gain is 75.
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