CN111755576A - Amorphous gallium oxide etching method and application in three-terminal device and array imaging system - Google Patents
Amorphous gallium oxide etching method and application in three-terminal device and array imaging system Download PDFInfo
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- CN111755576A CN111755576A CN201910245457.1A CN201910245457A CN111755576A CN 111755576 A CN111755576 A CN 111755576A CN 201910245457 A CN201910245457 A CN 201910245457A CN 111755576 A CN111755576 A CN 111755576A
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- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 title claims abstract description 172
- 229910001195 gallium oxide Inorganic materials 0.000 title claims abstract description 172
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- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims abstract description 86
- 238000001039 wet etching Methods 0.000 claims abstract description 28
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- 229910052594 sapphire Inorganic materials 0.000 claims description 6
- 239000010980 sapphire Substances 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 230000005855 radiation Effects 0.000 claims description 5
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- 229910052681 coesite Inorganic materials 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 229910052906 cristobalite Inorganic materials 0.000 claims description 3
- 230000005284 excitation Effects 0.000 claims description 3
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 claims description 3
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- 229910052682 stishovite Inorganic materials 0.000 claims description 3
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 3
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 5
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
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- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 description 1
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- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/20—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof such devices or parts thereof comprising amorphous semiconductor materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/08—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors
- H01L31/10—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors characterised by potential barriers, e.g. phototransistors
- H01L31/101—Devices sensitive to infrared, visible or ultraviolet radiation
- H01L31/112—Devices sensitive to infrared, visible or ultraviolet radiation characterised by field-effect operation, e.g. junction field-effect phototransistor
- H01L31/113—Devices sensitive to infrared, visible or ultraviolet radiation characterised by field-effect operation, e.g. junction field-effect phototransistor being of the conductor-insulator-semiconductor type, e.g. metal-insulator-semiconductor field-effect transistor
- H01L31/1136—Devices sensitive to infrared, visible or ultraviolet radiation characterised by field-effect operation, e.g. junction field-effect phototransistor being of the conductor-insulator-semiconductor type, e.g. metal-insulator-semiconductor field-effect transistor the device being a metal-insulator-semiconductor field-effect transistor
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
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- Manufacturing & Machinery (AREA)
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Abstract
The invention discloses an amorphous gallium oxide etching method and application thereof in a three-terminal device and an array imaging system, wherein the etching method comprises the following steps: carrying out selective wet etching on amorphous gallium oxide by using a solution of 0.04-25% of tetramethylammonium hydroxide (TMAH); the temperature of the selective wet etching is between 20 and 100 ℃.
Description
Technical Field
The invention relates to the technical field of lithium battery materials, in particular to an amorphous gallium oxide etching method and application thereof in a three-terminal device and an array imaging system.
Background
In recent years, a wide bandgap oxide semiconductor material gallium oxide (Ga)2O3) Because of the advantages of band gap as high as 4.9eV, stable chemical and thermal properties, the material has very important application prospects in the fields of deep ultraviolet detection, high-energy radiation detection, photocatalysis, solar cells, gas sensing, power devices and the like, and is widely concerned by more and more scientific researchers. However, most of the currently reported gallium oxide photodetectors adopt a two-terminal device structure, and have the following problems: without bagThe patterning process including the gallium oxide active layer brings adverse effects on effectively isolating pixel points of the array device, reducing dark current, improving imaging quality and the like; in addition, the device has a continuous photoconductive phenomenon, thereby seriously affecting the response frequency of the device and the practical application thereof. Research has shown that in a three terminal device with gate modulation (such as a thin film transistor), the persistent photoconduction of the device can be effectively suppressed by applying a gate pulse. Therefore, it is very significant and urgently required to fabricate a three-terminal device based on gallium oxide. However, if the gallium oxide channel layer is not patterned, the device usually exhibits a large gate leakage current, which is not favorable for improving the light-dark ratio of the device; in addition, when the three-terminal device is applied to other conventional occasions, the larger grid leakage current is not beneficial to realizing the energy-saving target.
The solution of the above problems places a pressing need for patterning of gallium oxide materials and devices. Patterning is generally achieved by an etching method, which generally includes dry etching and wet etching, and wet etching is further classified into chemical etching and electrochemical etching, wherein chemical etching is widely adopted due to the advantages of low cost (expensive vacuum plasma equipment and the like commonly used in dry etching are not needed), controllable etching rate, simplicity in operation, wide application range and the like.
The chemical etching solution of the gallium oxide material which is disclosed at present mainly comprises various strong acids and strong bases, and specifically comprises the following components:
1. etching using hydrofluoric acid (HF) solution (phys. stat. sol. (c),2008,5, 3116);
2. high temperature etching using concentrated nitric acid (phys. stat. sol. (c),2008,5, 3116);
3. high temperature etching (RSC adv.,2018,8,6544) using sodium hydroxide (NaOH) solution;
4. high temperature etching (jpn. j. appl. phys.,2009,48,040208) was performed using a concentrated phosphoric acid (H3PO4) and concentrated sulfuric acid (H2SO4) solution.
However, the above method can etch gallium oxide and simultaneously corrode and denature the photoresist, so that the photoresist cannot be removed by acetone or even an etching barrier layer cannot be formed. That is, the existing gallium oxide chemical etching technology has the problem of incompatibility with the photoetching process. Therefore, it is very important and practical to find a chemical etching method for gallium oxide material that is easy and convenient to operate, stable in process, low in cost, and has a high etching selectivity ratio for other materials (i.e. gallium oxide is stably etched while other materials are rarely or hardly etched).
Disclosure of Invention
The invention aims to provide an amorphous gallium oxide etching method which has the advantages of stable process, low cost, good compatibility with a photoetching process and high etching selection ratio to other materials, is used for solving the problems in the prior art, and simultaneously provides the application of the amorphous gallium oxide etching method in a three-terminal device and an array imaging system.
In order to achieve the above object, in a first aspect, an embodiment of the present invention provides an amorphous gallium oxide etching method, including:
carrying out selective wet etching on amorphous gallium oxide by using a solution of 0.04-25% of tetramethylammonium hydroxide (TMAH); the temperature of the selective wet etching is between 20 and 100 ℃.
In a second aspect, an embodiment of the present invention provides a process method for a gallium oxide-based three-terminal device, where the process method includes:
growing an amorphous gallium oxide film channel layer;
manufacturing a masking layer for wet etching on the amorphous gallium oxide thin film channel layer to form a pre-patterned amorphous gallium oxide thin film channel layer;
carrying out selective wet etching on the pre-patterned amorphous gallium oxide thin film channel layer by using a TMAH solution with the concentration of 0.04-25% to obtain a patterned amorphous gallium oxide thin film channel layer; the temperature of the selective wet etching is between 20 and 100 ℃;
and preparing an electrode on the patterned amorphous gallium oxide thin film channel layer so as to form the gallium oxide-based three-terminal device.
Preferably, the method further comprises, before the growing the amorphous gallium oxide thin film channel layer or after the obtaining the patterned amorphous gallium oxide thin film channel layer, the method further comprising:
and preparing a gate insulating layer.
In a third aspect, an embodiment of the present invention provides a gallium oxide-based three-terminal device prepared by the process method according to the second aspect:
the gallium oxide base three-terminal device is a bottom gate structure device, and the profile structure sequentially comprises from bottom to top: the transistor comprises a substrate, a gate electrode, a gate insulating layer, an amorphous gallium oxide thin film channel layer, a source electrode and a drain electrode; alternatively, the first and second electrodes may be,
the gallium oxide-based three-terminal device is a top gate structure device, and the profile structure sequentially comprises from bottom to top: the transistor comprises a substrate, a source electrode, a drain electrode, an amorphous gallium oxide thin film channel layer, a gate insulating layer and a gate electrode.
Preferably, the amorphous gallium oxide channel layer is: an oxide thin film active layer exists that is photo-electrically responsive under excitation by incident solar blind ultraviolet or X-ray radiation.
Preferably, the substrate is one of a rigid substrate or a flexible organic substrate, and the thickness of the substrate is 0.01-1 mm; the rigid substrate comprises one of Si, sapphire and quartz glass; the flexible organic substrate comprises one or a combination of a plurality of polyethylene naphthalate, polyethylene terephthalate, polyimide, polymethyl methacrylate, polydimethylsiloxane, polyvinyl chloride, polycarbonate, polystyrene or organic glass;
the thickness of the amorphous gallium oxide film channel layer is 20-100 nanometers;
the electrode materials of the source electrode, the drain electrode and the gate electrode are one or more of ITO, Ti/Au, Al, Cr, silver, copper or molybdenum, and the thickness is 0.02-0.3 micrometer;
the material of the gate insulating layer comprises Al2O3、SiO2、Y2O3、HfO2、ZrO2、Ta2O5、Si3N4One or more of AlN or polyvinylpyrrolidone with a thickness of0.002 to 0.3 μm.
In a fourth aspect, an embodiment of the present invention provides a processing method for a two-terminal array imaging device, including:
growing an amorphous gallium oxide film on a substrate;
manufacturing a masking layer for wet etching on the amorphous gallium oxide film to form a pre-patterned amorphous gallium oxide film;
carrying out selective wet etching on the pre-patterned amorphous gallium oxide film by using a TMAH solution with the concentration of 0.04-25% to obtain a patterned amorphous gallium oxide film; the temperature of the selective wet etching is between 20 and 100 ℃;
and preparing a collecting electrode on the patterned amorphous gallium oxide film so as to form the two-end array imaging device.
In a fifth aspect, an embodiment of the present invention provides a two-terminal array imaging device manufactured by the process method according to the fourth aspect.
Preferably, the substrate is one of a rigid substrate or a flexible organic substrate, and the thickness of the substrate is 0.01-1 mm; the rigid substrate comprises one of Si, sapphire and quartz glass; the flexible organic substrate comprises one or a combination of a plurality of polyethylene naphthalate, polyethylene terephthalate, polyimide, polymethyl methacrylate, polydimethylsiloxane, polyvinyl chloride, polycarbonate, polystyrene or organic glass;
the thickness of the amorphous gallium oxide film is 30 nanometers to 2 micrometers;
the electrode material of the collecting electrode is one or more of ITO, Ti/Au, Al, Cr, silver, copper or molybdenum.
In a sixth aspect, the embodiment of the present invention provides an array imaging system formed by the two-terminal array imaging device according to the fifth aspect.
The technological method of the gallium oxide-based three-terminal device has the advantages of stable technology, convenience in operation, low cost, compatibility with a photoetching technology and the like, and the etching rate is uniform. The etched surface is smooth, and the photoresist is etched,The etching selection ratio of materials such as ITO, Ti/Au, Cr, silver, copper, molybdenum and the like is high. The gallium oxide-based three-terminal device prepared by the process method of the invention has the advantages that the grid leakage current is obviously inhibited from 10-6A falls to 10-10A can be reduced by 4 orders of magnitude; the array imaging system prepared by the process method can effectively isolate the pixel points of the array device, reduce the dark current, improve the imaging quality and have higher sensitivity and resolution.
Drawings
The technical solutions of the embodiments of the present invention are further described in detail with reference to the accompanying drawings and embodiments.
FIG. 1 is a cross-sectional view of an amorphous gallium oxide film etched with hydrofluoric acid using a Scanning Electron Microscope (SEM) according to an embodiment of the present invention;
FIG. 2 is a cross-sectional view of an amorphous gallium oxide film etched with TMAH aqueous solution under SEM according to an embodiment of the present invention;
FIG. 3 is a schematic flow chart of TMAH solution etching of amorphous gallium oxide material according to the embodiment of the present invention;
fig. 4 is a graph showing the variation of the etching rate of the TMAH aqueous solution to two amorphous gallium oxide materials with different stoichiometric ratios at 27 degrees celsius according to the embodiment of the present invention along with the concentration of the TMAH aqueous solution;
FIG. 5 is a graph showing the variation of the etching rate of TMAH aqueous solution with a volume concentration of 0.12% to two amorphous gallium oxide materials with different stoichiometric ratios with the etching temperature according to the embodiment of the present invention;
FIG. 6 is a graph comparing the transfer characteristics of a three-terminal device with and without amorphous gallium oxide;
FIG. 7 is a graph comparing gate leakage current of a three-terminal device with and without amorphous gallium oxide etched according to an embodiment of the present invention;
FIG. 8 is a graph comparing transfer characteristic curves of amorphous gallium oxide-based three-terminal thin film transistor devices provided by embodiments of the present invention with or without 254nm ultraviolet radiation;
fig. 9 is a time response curve of the amorphous gallium oxide-based three-terminal thin film transistor device provided by the embodiment of the present invention under irradiation of ultraviolet light with source-drain voltage of 10V and 254 nm;
fig. 10 is a graph showing the photoresponse of an amorphous gallium oxide-based three-terminal thin film transistor device under 254nm ultraviolet irradiation to suppress continuous photoconduction by applying gate pulses;
fig. 11 is a schematic structural diagram of an amorphous gallium oxide-based two-terminal array imaging device according to an embodiment of the present invention;
fig. 12 is a diagram of an amorphous gallium oxide-based two-terminal array imaging device according to an embodiment of the present invention.
Detailed Description
The embodiment of the invention provides an amorphous gallium oxide etching method and application thereof in a three-terminal device and an array imaging system.
The invention relates to an amorphous gallium oxide etching method, which is to carry out selective wet etching on amorphous gallium oxide by using a solution of tetramethyl ammonium hydroxide (TMAH) with the concentration of 0.04-25%; the temperature of the selective wet etching is between 20 and 100 degrees celsius. The complete process of etching can be as shown in fig. 3. Of course, fig. 3 is merely a schematic process diagram and does not show that the actual topography produced by etching is exactly the same as that shown in the figure.
The reaction principle of etching the amorphous gallium oxide film by the TMAH aqueous solution is as follows:
Ga2O3+2(CH3)4NOH＝2(CH3)4NGaO2+H2O。
the masking layer for selective etching can be photoresist, TMAH aqueous solution is used for etching the amorphous gallium oxide film, and the etching selectivity ratio of the photoresist is high. In addition, the etching selectivity ratio of materials such as ITO, Ti/Au, Cr, silver, copper, molybdenum and the like is high, so that the method has good application prospect in the preparation process of the gallium oxide-based device.
The etching method provided by the embodiment of the invention can be particularly applied to the technical process of the gallium oxide-based three-terminal device and is used for preparing the gallium oxide-based three-terminal device. The method specifically comprises the following steps:
growing an amorphous gallium oxide thin film channel layer on a substrate, and manufacturing a masking layer for wet etching on the amorphous gallium oxide thin film channel layer to form a pre-patterned amorphous gallium oxide thin film channel layer; selectively wet etching the pre-patterned amorphous gallium oxide film channel layer by using a TMAH solution with the concentration of 0.04% to 25% to obtain a patterned amorphous gallium oxide film channel layer, wherein the temperature of the selective wet etching is between 20 ℃ and 100 ℃; and preparing an electrode on the patterned amorphous gallium oxide thin film channel layer so as to form the gallium oxide-based three-terminal device.
The preparation of the gate insulating layer in the device can be that before the amorphous gallium oxide thin film channel layer grows or after the graphical amorphous gallium oxide thin film channel layer is obtained, the device with a bottom gate structure or the device with a top gate structure can be obtained by correspondingly adjusting the process sequence.
Wherein, bottom gate structure device, the section structure includes from bottom to top in proper order: the transistor comprises a substrate, a gate electrode, a gate insulating layer, an amorphous gallium oxide thin film channel layer, a source electrode and a drain electrode.
Top gate structure device, the section structure includes from bottom to top in proper order: the transistor comprises a substrate, a source electrode, a drain electrode, an amorphous gallium oxide thin film channel layer, a gate insulating layer and a gate electrode.
The amorphous gallium oxide channel layer of the prepared device is as follows: an oxide thin film active layer with photoelectric response exists under the excitation of incident solar blind ultraviolet or X-ray radiation; the thickness of the amorphous gallium oxide thin film channel layer is preferably 20 nm to 100 nm.
The substrate can be one of a rigid substrate or a flexible organic substrate, and the thickness of the substrate is 0.01-1 mm; the rigid substrate comprises one of Si, sapphire, quartz glass and the like; the flexible organic substrate comprises one or a combination of a plurality of polyethylene naphthalate, polyethylene terephthalate, polyimide, polymethyl methacrylate, polydimethylsiloxane, polyvinyl chloride, polycarbonate, polystyrene or organic glass;
the electrode materials of the source electrode, the drain electrode and the gate electrode are one or more of ITO, Ti/Au, Al, Cr, silver, copper or molybdenum, and the thickness of the electrode materials is 0.02-0.3 micrometer;
the material of the gate insulating layer includes Al2O3、SiO2、Y2O3、HfO2、ZrO2、Ta2O5、Si3N4One or more of AlN or polyvinylpyrrolidone, and the like, and the thickness of the mixture is 0.002-0.3 micron.
The gallium oxide-based three-terminal device prepared by the process method of the invention has the advantages that the grid leakage current is obviously inhibited from 10-6A falls to 10-10A can be reduced by 4 orders of magnitude. The gallium oxide-based three-terminal device effectively inhibits continuous photoconduction by applying grid pulses, and the dark current can reach 10 instantly-12Of the order of a.
The etching method of the embodiment of the invention can also be specifically applied to the technical process of the two-end array imaging device and used for preparing the gallium oxide-based three-end device. The method specifically comprises the following steps:
growing an amorphous gallium oxide film on a substrate; manufacturing a masking layer for wet etching on the amorphous gallium oxide film to form a pre-patterned amorphous gallium oxide film; carrying out selective wet etching on the pre-patterned amorphous gallium oxide film by using a TMAH solution with the concentration of 0.04-25% to obtain a patterned amorphous gallium oxide film; wherein the temperature of the selective wet etching is between 20 ℃ and 100 ℃; and preparing a collecting electrode on the patterned amorphous gallium oxide film so as to form the two-end array imaging device.
In a specific embodiment, the substrate can be one of a rigid substrate or a flexible organic substrate, and the thickness is 0.01-1 mm; the rigid substrate comprises one of Si, sapphire, quartz glass and the like; the flexible organic substrate comprises one or a combination of a plurality of polyethylene naphthalate, polyethylene terephthalate, polyimide, polymethyl methacrylate, polydimethylsiloxane, polyvinyl chloride, polycarbonate, polystyrene or organic glass;
the thickness of the amorphous gallium oxide film is 30 nanometers to 2 micrometers;
the electrode material of the collecting electrode is one or more of ITO, Ti/Au, Al, Cr, silver, copper or molybdenum.
The two-end array imaging device can be integrated to form an array imaging system. The array imaging system prepared by the process method can effectively isolate the pixel points of the array device, reduce the dark current, improve the imaging quality and have higher sensitivity and resolution.
The present invention is further illustrated by the following specific examples.
Example 1
The embodiment provides a chemical etching method of an amorphous gallium oxide material.
Firstly, growing an amorphous gallium oxide film with the thickness of 450 nanometers by using a radio frequency magnetron sputtering method under the condition of introducing oxygen, then making a pattern by using an ultraviolet photoetching process, respectively etching by using hydrofluoric acid commonly used in the prior art and a TMAH aqueous solution adopted by the invention, and finally measuring an etching profile by using a scanning electron microscope. As shown in fig. 1, hydrofluoric acid is used for etching the semiconductor device, so that the anisotropy degree is poor, the lateral underetching is serious, the transferred pattern is distorted, the resolution of array imaging is reduced, the size of a channel of a three-terminal device is changed, and the performance of the device is seriously influenced; as shown in FIG. 2, TMAH etching has good anisotropy, transverse undercutting phenomenon is negligible, transferred pattern quality is good, and device quality can be ensured
Example 2
The embodiment provides a chemical etching method of an amorphous gallium oxide material.
Firstly, growing an amorphous gallium oxide film with the thickness of 450 nanometers by using a radio frequency magnetron sputtering method under the condition of not introducing oxygen, then using photoresist as a mask, etching the film by using TMAH aqueous solution with the volume concentration of 2.4% at the temperature of 27 ℃, wherein the etching time is 40 seconds, 80 seconds and 120 seconds, finally measuring the etching depth by using a step profiler, and calculating the etching rate to be 2.2 nm/s.
Example 3
The embodiment provides a chemical etching method of an amorphous gallium oxide material.
Firstly, growing an amorphous gallium oxide film with the thickness of 450 nanometers by using a radio frequency magnetron sputtering method under the condition of not introducing oxygen, then using photoresist as a mask, etching the film by using TMAH aqueous solution with the volume concentration of 0.24% at the temperature of 27 ℃, wherein the etching time is 60 seconds, 120 seconds and 180 seconds, finally measuring the etching depth by using a step profiler, and calculating the etching rate to be 1.8 nm/s.
Example 4
The embodiment provides a chemical etching method of an amorphous gallium oxide material.
Firstly, growing an amorphous gallium oxide film with the thickness of 450 nanometers by using a radio frequency magnetron sputtering method under the condition of not introducing oxygen, then using photoresist as a mask, etching the film by using TMAH aqueous solution with the volume concentration of 0.12% at 27 ℃, respectively etching for 75 seconds, 150 seconds and 225 seconds, finally respectively measuring the etching depth by using a step profiler, and calculating the etching rate to be 1.5 nm/s.
Example 5
The embodiment provides a chemical etching method of an amorphous gallium oxide material.
Firstly, growing an amorphous gallium oxide film with the thickness of 450 nanometers by using a radio frequency magnetron sputtering method under the condition of not introducing oxygen, then using photoresist as a mask, etching the film by using TMAH aqueous solution with the volume concentration of 0.048% at the temperature of 27 ℃, wherein the etching time is 100 seconds, 200 seconds and 300 seconds, finally measuring the etching depth by using a step profiler, and calculating the etching rate to be 1.1 nm/s. Bonding of
In examples 1, 2, 3 and 4, curves of the rate of solution etching of amorphous gallium oxide films sputter-grown without introducing oxygen at 27 ℃ according to the volume concentration of TMAH aqueous solution were drawn, wherein the curves without introducing oxygen are shown by dashed lines in FIG. 4.
Example 6
The embodiment provides a chemical etching method of an amorphous gallium oxide material.
Firstly, growing an amorphous gallium oxide film with the thickness of 450 nanometers by using a radio frequency magnetron sputtering method under the condition of introducing oxygen, then using photoresist as a mask, etching the film by using TMAH aqueous solution with the volume concentration of 2.4% at the temperature of 27 ℃, wherein the etching time is 50 seconds, 100 seconds and 150 seconds, finally measuring the etching depth by using a step profiler, and calculating the etching rate to be 0.79 nm/s.
Example 7
The embodiment provides a chemical etching method of an amorphous gallium oxide material.
Firstly, growing an amorphous gallium oxide film with the thickness of 450 nanometers by using a radio frequency magnetron sputtering method under the condition of introducing oxygen, then using photoresist as a mask, etching the film by using TMAH aqueous solution with the volume concentration of 0.24% at the temperature of 27 ℃, wherein the etching time is 60 seconds, 120 seconds and 180 seconds, finally measuring the etching depth by using a step profiler, and calculating the etching rate to be 0.65 nm/s.
Example 8
The embodiment provides a chemical etching method of an amorphous gallium oxide material.
Firstly, growing an amorphous gallium oxide film with the thickness of 450 nanometers by using a radio frequency magnetron sputtering method under the condition of introducing oxygen, then using photoresist as a mask, etching the film by using TMAH aqueous solution with the volume concentration of 0.12% at the temperature of 27 ℃, wherein the etching time is 80 seconds, 160 seconds and 240 seconds, finally measuring the etching depth by using a step profiler, and calculating the etching rate to be 0.58 nm/s.
Example 9
The embodiment provides a chemical etching method of an amorphous gallium oxide material.
Firstly growing an amorphous gallium oxide film with the thickness of 450 nanometers by using a radio frequency magnetron sputtering method under the condition of introducing oxygen, then using photoresist as a mask, etching the film by using TMAH aqueous solution with the volume concentration of 0.048% at the temperature of 27 ℃, wherein the etching time is 90 seconds, 180 seconds and 270 seconds, finally measuring the etching depth by using a step profiler, and calculating the etching rate to be 0.49 nm/s. With reference to examples 5, 6, 7 and 8, a curve of the rate of the amorphous gallium oxide film sputter-grown under the condition of solution etching and oxygen introduction at 27 ℃ along with the volume concentration of the TMAH aqueous solution is plotted, as shown by the solid line in fig. 4.
Example 10
The embodiment provides a chemical etching method of an amorphous gallium oxide material.
Firstly, growing an amorphous gallium oxide film with the thickness of 450 nanometers by using a radio frequency magnetron sputtering method under the condition of not introducing oxygen, then using photoresist as a mask, etching the film by using TMAH aqueous solution with the volume concentration of 0.12% at 60 ℃, respectively etching for 10 seconds, 20 seconds and 30 seconds, finally respectively measuring the etching depth by using a step profiler, and calculating the etching rate to be 10.2 nm/s.
Example 11
The embodiment provides a chemical etching method of an amorphous gallium oxide material.
Firstly, growing an amorphous gallium oxide film with the thickness of 450 nanometers by using a radio frequency magnetron sputtering method under the condition of not introducing oxygen, then using photoresist as a mask, etching the film by using TMAH aqueous solution with the volume concentration of 0.12% at 40 ℃, respectively etching for 40 seconds, 80 seconds and 120 seconds, finally respectively measuring the etching depth by using a step profiler, and calculating the etching rate to be 3.1 nm/s.
Example 12
The embodiment provides a chemical etching method of an amorphous gallium oxide material.
Firstly, growing an amorphous gallium oxide film with the thickness of 450 nanometers by using a radio frequency magnetron sputtering method under the condition of not introducing oxygen, then using photoresist as a mask, etching the film by using TMAH aqueous solution with the volume concentration of 0.12% at 27 ℃, respectively etching for 60 seconds, 120 seconds and 180 seconds, finally respectively measuring the etching depth by using a step profiler, and calculating the etching rate to be 1.5 nm/s. With reference to examples 9, 10 and 11, the curve of the rate of the amorphous gallium oxide film sputter-grown under the condition of etching with TMAH aqueous solution with volume concentration of 0.12% and without introducing oxygen gas as a function of temperature is plotted, as shown by the dotted line in fig. 5.
Example 13
The embodiment provides a chemical etching method of an amorphous gallium oxide material.
Firstly, growing an amorphous gallium oxide film with the thickness of 450 nanometers by using a radio frequency magnetron sputtering method under the condition of introducing oxygen, then using photoresist as a mask, etching the film by using TMAH aqueous solution with the volume concentration of 0.12% at 60 ℃, respectively etching for 10 seconds, 20 seconds and 30 seconds, finally respectively measuring the etching depth by using a step profiler, and calculating the etching rate to be 9.84 nm/s.
Example 14
The embodiment provides a chemical etching method of an amorphous gallium oxide material.
Firstly, growing an amorphous gallium oxide film with the thickness of 450 nanometers by using a radio frequency magnetron sputtering method under the condition of introducing oxygen, then using photoresist as a mask, etching the film by using TMAH aqueous solution with the volume concentration of 0.12% at 40 ℃, respectively etching for 40 seconds, 80 seconds and 120 seconds, finally respectively measuring the etching depth by using a step profiler, and calculating the etching rate to be 2.83 nm/s.
Example 15
The embodiment provides a chemical etching method of an amorphous gallium oxide material.
Firstly, growing an amorphous gallium oxide film with the thickness of 450 nanometers by using a radio frequency magnetron sputtering method under the condition of introducing oxygen, then using photoresist as a mask, etching the film by using TMAH aqueous solution with the volume concentration of 0.12% at 27 ℃, respectively etching for 100 seconds, 200 seconds and 300 seconds, finally respectively measuring the etching depth by using a step profiler, and calculating the etching rate to be 0.58 nm/s. With reference to examples 12, 13 and 14, the rate of amorphous gallium oxide thin film sputter-grown under the condition of etching with TMAH aqueous solution having a volume concentration of 0.12% and introducing oxygen gas was plotted as a function of temperature, as shown by the solid line in fig. 5.
The above embodiments of the present invention have studied the etch rate under two conditions, i.e., the elemental composition of the etched amorphous gallium oxide material includes the in-stoichiometry ratio and the off-stoichiometry ratio.
Example 16
The embodiment provides an amorphous gallium oxide thin film transistor prepared by a selective chemical etching method. The device adopts a bottom gate structure, and the channel part is in an interdigital shape.
The preparation method of the thin film transistor comprises the following steps: chromium with the thickness of 30nm is grown on a quartz substrate by adopting a magnetron sputtering technology to be used as a bottom gate electrode; patterning the bottom gate electrode by using a chromium etching solution through an ultraviolet lithography process; growing an alumina film with the thickness of 100nm by adopting an ALD method; patterning the alumina by using concentrated phosphoric acid at 70 ℃ through an ultraviolet lithography process; growing an amorphous gallium oxide film with the thickness of 25nm by adopting a radio frequency magnetron sputtering technology; patterning the amorphous gallium oxide film at 60 ℃ by using TMAH aqueous solution with volume concentration of 0.24% through an ultraviolet lithography process; an ITO source-drain electrode with the thickness of 100nm is grown by adopting a radio frequency magnetron sputtering technology, and the source-drain electrode is patterned by combining an ultraviolet lithography process with a lift-off method.
The transfer characteristic and the output characteristic of the device are tested. Fig. 6 shows the transfer characteristic curves of the thin film transistor of the amorphous gallium oxide material etched by gallium oxide and not etched by gallium oxide, and the comparison shows that the device etched by gallium oxide shows typical transfer characteristics, and the device not etched by gallium oxide has poor transfer characteristics. FIG. 7 shows the gate leakage curves of the TFT with and without the amorphous gallium oxide material etched with gallium oxide, the gate leakage of the device etched with gallium oxide being maintained at 10-10And the leakage current of the grid electrode of the device which is not etched by the gallium oxide is very large.
Example 17
The embodiment provides a three-terminal photoelectric detector made of an amorphous gallium oxide material by a selective chemical etching method. The device structure and fabrication flow were consistent with example 16.
The transfer characteristic curve of the test device under 254nm ultraviolet irradiation, and fig. 8 shows the transfer characteristic curve of the prepared amorphous gallium oxide three-terminal photodetector under 254nm ultraviolet irradiation. When the grid voltage is 0V, the light-dark ratio of the device can reach 106Magnitude.
Example 18
The embodiment provides a three-terminal photoelectric detector made of an amorphous gallium oxide material. The device structure and fabrication flow were consistent with example 16.
The test device is irradiated by 254nm ultraviolet lightTime response curve of (2). Fig. 9 shows a curve of source-drain current of the prepared amorphous gallium oxide three-terminal photodetector changing with ultraviolet light switching under 254nm ultraviolet light irradiation, and the device shows repeatable light response characteristics with repeated switching of ultraviolet light; FIG. 10 shows that by applying a grid forward pulse to the photodetector, the persistent photoconduction is significantly suppressed and the current is momentarily reduced to 10-10Magnitude.
Example 19
The embodiment provides preparation of an array imaging device made of amorphous gallium oxide materials.
The device structure is shown in fig. 11. The imaging system integrates multiple discrete gallium oxide ultraviolet sensors together, with the individual sensors taking the shape of interdigitated fingers. The physical diagram is shown in FIG. 12.
The preparation method of the imaging device comprises the following steps: growing an amorphous gallium oxide film with the thickness of 150nm on a quartz substrate by using a magnetron sputtering technology; patterning gallium oxide by using TMAH aqueous solution with volume concentration of 0.24% through an ultraviolet lithography process; an ITO source-drain electrode with the thickness of 100nm is grown by adopting a radio frequency magnetron sputtering technology, and the electrode is patterned by combining an ultraviolet photoetching technology with a lift-off method.
The imaging system has the advantages of discrete pixel points, low dark current, low noise, good imaging quality, and very high sensitivity and resolution.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. An amorphous gallium oxide etching method is characterized by comprising the following steps:
carrying out selective wet etching on amorphous gallium oxide by using a solution of 0.04-25% of tetramethylammonium hydroxide (TMAH); the temperature of the selective wet etching is between 20 and 100 ℃.
2. A process method of a gallium oxide-based three-terminal device is characterized by comprising the following steps:
growing an amorphous gallium oxide film channel layer;
manufacturing a masking layer for wet etching on the amorphous gallium oxide thin film channel layer to form a pre-patterned amorphous gallium oxide thin film channel layer;
carrying out selective wet etching on the pre-patterned amorphous gallium oxide thin film channel layer by using a TMAH solution with the concentration of 0.04-25% to obtain a patterned amorphous gallium oxide thin film channel layer; the temperature of the selective wet etching is between 20 and 100 ℃;
and preparing an electrode on the patterned amorphous gallium oxide thin film channel layer so as to form the gallium oxide-based three-terminal device.
3. The process of claim 2, further comprising, before said growing an amorphous gallium oxide thin film channel layer or after said obtaining a patterned amorphous gallium oxide thin film channel layer:
and preparing a gate insulating layer.
4. The gallium oxide-based three-terminal device prepared by the process method according to claim 2, wherein the gallium oxide-based three-terminal device is a bottom-gate structure device, and the cross-sectional structure sequentially comprises from bottom to top: the transistor comprises a substrate, a gate electrode, a gate insulating layer, an amorphous gallium oxide thin film channel layer, a source electrode and a drain electrode; alternatively, the first and second electrodes may be,
the gallium oxide-based three-terminal device is a top gate structure device, and the profile structure sequentially comprises from bottom to top: the transistor comprises a substrate, a source electrode, a drain electrode, an amorphous gallium oxide thin film channel layer, a gate insulating layer and a gate electrode.
5. The gallium oxide-based three-terminal device according to claim 4, wherein the amorphous gallium oxide channel layer is: an oxide thin film active layer exists that is photo-electrically responsive under excitation by incident solar blind ultraviolet or X-ray radiation.
6. The gallium oxide-based three-terminal device according to claim 4,
the substrate is one of a rigid substrate or a flexible organic substrate, and the thickness of the substrate is 0.01-1 mm; the rigid substrate comprises one of Si, sapphire and quartz glass; the flexible organic substrate comprises one or a combination of a plurality of polyethylene naphthalate, polyethylene terephthalate, polyimide, polymethyl methacrylate, polydimethylsiloxane, polyvinyl chloride, polycarbonate, polystyrene or organic glass;
the thickness of the amorphous gallium oxide film channel layer is 20-100 nanometers;
the electrode materials of the source electrode, the drain electrode and the gate electrode are one or more of ITO, Ti/Au, Al, Cr, silver, copper or molybdenum, and the thickness is 0.02-0.3 micrometer;
the material of the gate insulating layer comprises Al2O3、SiO2、Y2O3、HfO2、ZrO2、Ta2O5、Si3N4One or more of AlN or polyvinylpyrrolidone with a thickness of 0.002-0.3 μm.
7. A process method of a two-terminal array imaging device is characterized by comprising the following steps:
growing an amorphous gallium oxide film on a substrate;
manufacturing a masking layer for wet etching on the amorphous gallium oxide film to form a pre-patterned amorphous gallium oxide film;
carrying out selective wet etching on the pre-patterned amorphous gallium oxide film by using a TMAH solution with the concentration of 0.04-25% to obtain a patterned amorphous gallium oxide film; the temperature of the selective wet etching is between 20 and 100 ℃;
and preparing a collecting electrode on the patterned amorphous gallium oxide film so as to form the two-end array imaging device.
8. A two-terminal array imaging device fabricated according to the process of claim 7.
9. The two-terminal array imaging device of claim 8,
the substrate is one of a rigid substrate or a flexible organic substrate, and the thickness of the substrate is 0.01-1 mm; the rigid substrate comprises one of Si, sapphire and quartz glass; the flexible organic substrate comprises one or a combination of a plurality of polyethylene naphthalate, polyethylene terephthalate, polyimide, polymethyl methacrylate, polydimethylsiloxane, polyvinyl chloride, polycarbonate, polystyrene or organic glass;
the thickness of the amorphous gallium oxide film is 30 nanometers to 2 micrometers;
the electrode material of the collecting electrode is one or more of ITO, Ti/Au, Al, Cr, silver, copper or molybdenum.
10. An arrayed imaging system comprising a plurality of two-terminal arrayed imaging devices of claim 9.
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