CN108767028B - Flexible solar-blind UV detector based on gallium oxide heterojunction structure and preparation method thereof - Google Patents
Flexible solar-blind UV detector based on gallium oxide heterojunction structure and preparation method thereof Download PDFInfo
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- H10F30/00—Individual radiation-sensitive semiconductor devices in which radiation controls the flow of current through the devices, e.g. photodetectors
- H10F30/10—Individual radiation-sensitive semiconductor devices in which radiation controls the flow of current through the devices, e.g. photodetectors the devices being sensitive to infrared radiation, visible or ultraviolet radiation, and having no potential barriers, e.g. photoresistors
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Abstract
本发明公开了一种基于氧化镓异质结结构的柔性日盲紫外探测器及其制备方法，包括玻璃纤维布衬底，设置于玻璃纤维布衬底上方的α‑Ga2O3薄膜，设置于α‑Ga2O3薄膜上方的α‑Ga2O3/β‑Ga2O3异质结纳米柱阵列，设置于α‑Ga2O3/β‑Ga2O3异质结纳米柱阵列间隙的α‑Ga2O3薄膜上方的β‑Ga2O3薄膜，以及Ti/Au薄膜电极；所述α‑Ga2O3/β‑Ga2O3异质结纳米柱阵列包括分布于α‑Ga2O3薄膜上方的α‑Ga2O3纳米柱阵列，包覆于α‑Ga2O3纳米柱外围的β‑Ga2O3外壳，α‑Ga2O3薄膜与β‑Ga2O3薄膜之间构成α‑Ga2O3/β‑Ga2O3异质结薄膜层；Ti/Au薄膜电极为两个，一个设置于α‑Ga2O3/β‑Ga2O3异质结纳米柱阵列上方，另一个设置于α‑Ga2O3薄膜上方。本发明的探测器反应灵敏，暗电流小，具有很好的紫外光电响应，在可穿戴设备、紫外线检测和智能纺织品等领域具有很大的应用前景。
The invention discloses a flexible solar-blind ultraviolet detector based on a gallium oxide heterojunction structure and a preparation method thereof, comprising a glass fiber cloth substrate, an α-Ga 2 O 3 film arranged above the glass fiber cloth substrate, α-Ga 2 O 3 /β-Ga 2 O 3 heterojunction nano-pillar array above α-Ga 2 O 3 thin film, arranged on α-Ga 2 O 3 /β-Ga 2 O 3 heterojunction nano-pillars a β-Ga 2 O 3 film over the α-Ga 2 O 3 film in the array gap, and a Ti/Au film electrode; the α-Ga 2 O 3 /β-Ga 2 O 3 heterojunction nanopillar array includes a distribution α-Ga 2 O 3 nanopillar array on top of α-Ga 2 O 3 film, β-Ga 2 O 3 shell wrapped around α-Ga 2 O 3 nanopillar, α-Ga 2 O 3 film and β-Ga 2 O 3 The α-Ga 2 O 3 /β-Ga 2 O 3 heterojunction thin film layer is formed between the -Ga 2 O 3 thin films; there are two Ti/Au thin film electrodes, and one is arranged on the α-Ga 2 O 3 /β-Ga 2 O 3 heterojunction nano-pillar array above, the other is arranged above the α-Ga 2 O 3 thin film. The detector of the invention has sensitive response, small dark current and good ultraviolet photoelectric response, and has great application prospects in the fields of wearable equipment, ultraviolet detection, smart textiles and the like.
Description
Technical Field
The invention belongs to the technical field of ultraviolet photoelectric detectors, and particularly relates to a flexible solar blind ultraviolet detector based on a gallium oxide heterojunction structure and a preparation method thereof.
Technical Field
At present, the wide bandgap semiconductor ultraviolet detector based on SiC, GaN and ZnO can not realize solar blind detection, is easily interfered by sunlight, has weak processing capability on weak signals, and is limited in application. And beta-Ga2O3Is a semiconductor material with deep ultraviolet property, has solar blind property, can detect ultraviolet light of 200-280nm, and can be used for manufacturingThe solar blind type deep ultraviolet photoelectric device is widely applied to the fields of high-voltage line corona detection, guidance, atmospheric environment quality monitoring, ultraviolet light communication, disaster weather forecast, interplanetary communication and the like.
Along with the promotion of people to electronic equipment demand, wearable electronic equipment's application is more and more extensive, and this type of electronic product needs flexible device, improves electronic equipment's convenience and the degree of freedom of design. The commonly used ultraviolet photoelectric detection device grows a semiconductor film on a rigid substrate, such as a silicon wafer, a sapphire substrate, a quartz substrate and the like, and the devices cannot be bent, so that the application range of the device is limited. Because most of the flexible substrates are macromolecular compounds at present and cannot bear high temperature, the flexible bending characteristic of the gallium oxide-based solar blind ultraviolet detector can be realized by selecting a high-temperature-resistant flexible substrate to prepare a gallium oxide material.
So far, there are few reports about flexible solar blind ultraviolet photodetectors, and although there are reports (chinese patent CN201710012296.2) of flexible gallium oxide nanoribbon based solar blind ultraviolet photodetectors, these detectors transfer the previously synthesized gallium oxide nanoribbon onto a flexible substrate, and have the disadvantages of difficult electrode manufacturing, poor stability, and insecure bonding with the substrate.
Therefore, research and development of different types of flexible photoelectric detectors are carried out, so that the flexible photoelectric detectors can be widely applied to different fields, and the flexible photoelectric detectors have important significance.
Disclosure of Invention
The invention aims to provide a flexible solar blind ultraviolet detector with high sensitivity, good stability, short response time and solar blind characteristic and a preparation method thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: comprises a glass fiber cloth substrate and alpha-Ga arranged above the glass fiber cloth substrate2O3A thin film provided on α -Ga2O3alpha-Ga over thin films2O3/β-Ga2O3A heterojunction nanopillar array arranged on the alpha-Ga2O3/β-Ga2O3alpha-Ga of heterojunction nano-pillar array gap2O3beta-Ga over thin films2O3A thin film, and a Ti/Au thin film electrode; the alpha-Ga2O3/β-Ga2O3The heterojunction nano-pillar array comprises a material distributed in alpha-Ga2O3alpha-Ga over thin films2O3Nanopillar array coated on alpha-Ga2O3beta-Ga around nano-column2O3Outer shell, alpha-Ga2O3Thin film and beta-Ga2O3alpha-Ga is formed between the films2O3/β-Ga2O3A heterojunction thin film layer; two Ti/Au thin film electrodes are arranged, one is arranged at the alpha-Ga2O3/β-Ga2O3One above the heterojunction nanopillar array and the other arranged on the alpha-Ga2O3Above the membrane.
In particular, the alpha-Ga2O3The film is arranged on a glass fiber cloth substrate and alpha-Ga2O3/β-Ga2O3Between heterojunction nanopillar arrays, alpha-Ga2O3/β-Ga2O3The distribution area of the heterojunction nano-pillar array is smaller than that of alpha-Ga2O3Film area of α -Ga2O3Ti/Au thin film electrode on thin film and alpha-Ga2O3/β-Ga2O3The heterojunction nano-pillar array is positioned in alpha-Ga2O3The same side of the film.
Further, the α -Ga2O3The thickness of the film is 0.5-1.0 μm; the alpha-Ga2O3/β-Ga2O3The diameter of the heterojunction nano-column is 100-200nm, and the height is 1.0-1.5 μm.
Specifically, the gallium metal layer is used as an autocatalyst for growing the gallium oxide nanosheet array, so that the gallium oxide with the nanorod array structure can be promoted to be formed, and the reaction time is shortened.
Preferably, the alpha-Ga2O3Thin film and alpha-Ga2O3The nano-pillars are of an integrated structure.
Specifically, the flexible solar blind ultraviolet detector based on the gallium oxide heterojunction structure can detect the solar blind ultraviolet light of 200-280nm, can be bent and folded, and can be applied to portable wearable ultraviolet detection equipment.
The invention also discloses a preparation method of the flexible solar blind ultraviolet detector based on the gallium oxide heterojunction structure, which is characterized by comprising the following steps of:
step one, cleaning a glass fiber cloth substrate, wherein the cleaning process is as follows: sequentially soaking the substrate in acetone, ethanol and deionized water, performing ultrasonic treatment for 10 minutes respectively, taking out, washing with deionized water, and drying with dry N2Air drying for later use;
placing the glass fiber cloth substrate on a heating table, setting the temperature of the heating table to be 100 ℃, placing a grain of Ga metal above the glass fiber cloth substrate, pressing the liquid Ga metal into a sheet by using a glass slide when the Ga metal is molten, and cooling to form a Ga metal sheet/glass fiber cloth substrate for later use;
step three, adding Ga2O3Placing the target material at the position of a target table of a magnetron sputtering deposition system, fixing the Ga metal sheet/glass fiber cloth substrate obtained in the step two on a sample support, and placing the sample support into a vacuum cavity;
step four, vacuumizing the vacuum cavity, introducing argon, adjusting the pressure in the vacuum cavity, introducing oxygen, heating the Ga metal sheet/glass fiber cloth substrate, and growing alpha-Ga on the gallium liquid drops on the surface of the gallium metal sheet in situ by utilizing a magnetron sputtering method2O3Nano column array, annealing, then heating continuously, making quick in-situ annealing to obtain alpha-Ga2O3/β-Ga2O3Heterojunction nanopillar array, and alpha-Ga2O3/β-Ga2O3A heterojunction thin film layer of Ga2O3The distance between the target material and the glass fiber cloth substrate is set to be 5 cm, and the pressure intensity of the evacuated cavity is 1 multiplied by 10-4Pa, introducing argon gas, regulating the pressure of the vacuum chamber to 0.8-1.0Pa, and regulating the pressure of the vacuum chamber to 103Pa；
Fifthly, utilizing a mask and passing radio frequencyThe alpha-Ga obtained in the step four by the magnetron sputtering technology2O3/β-Ga2O3Heterojunction nanopillar array and alpha-Ga2O3Depositing a layer of Ti/Au film electrode on each film, wherein the sputtering process conditions are as follows: the pressure of the evacuated cavity is 1 multiplied by 10-4Pa, the substrate temperature is room temperature, the working atmosphere is Ar gas, the working pressure is 0.8-1.0Pa, the sputtering power is 60-80W, and the sputtering time is 2 min. Specifically, the temperature for heating the Ga metal sheet/glass fiber cloth substrate in the fourth step is 400-.
Further, the temperature of the rapid annealing after the temperature rise in the fourth step is 700-800 ℃, and the annealing time is 10-20 minutes.
In the fourth step, the magnetron sputtering method is adopted to prepare the alpha-Ga2O3/β-Ga2O3Gallium oxide heterojunction nanopillar arrays. Forming gallium metal liquid drops on the surface of the gallium metal film under the high-temperature heating of 400-500 ℃, and growing alpha-Ga on the gallium metal liquid drops through magnetron sputtering2O3The nano-column array is formed by slowly oxidizing the gallium metal layer in the oxygen atmosphere to form alpha-Ga2O3A film; further rapidly heating to 700-800 deg.C, alpha-Ga2O3Conversion of the periphery of the nanopillars and films to beta-Ga2O3Form alpha-Ga2O3/β-Ga2O3A heterojunction nanopillar array. The gallium can be used as an autocatalyst to catalyze the gallium metal layer to form a gallium oxide nano material at high temperature, and on the other hand, the gallium metal layer is slowly oxidized to form a gallium oxide film which can be used as an array growth substrate, so that the formed gallium oxide nano columns are ordered and uniformly distributed.
The invention has the beneficial effects that:
1. the flexible solar blind ultraviolet detector based on the gallium oxide heterojunction structure has the advantages of stable performance, sensitive reaction, small dark current and solar blind photoelectric characteristic. alpha-Ga used2O3/β-Ga2O3The heterojunction nano-pillar array is uniform and ordered, and the size of the nano-pillar is controllable. Adopts the flexibility of glass fiber clothThe substrate makes the detector that forms flexible, collapsible, can be applied to fields such as wearable ultraviolet detection of portable.
2. The invention relates to a flexible solar blind ultraviolet detector based on a gallium oxide heterojunction structure, and alpha-Ga2O3/β-Ga2O3The diameter of the heterojunction nano-column is 100-200nm, and the photoelectric performance is better.
3. The flexible solar blind ultraviolet detector based on the gallium oxide heterojunction structure can detect the solar blind ultraviolet light of 200-280nm, can be bent and folded, and can be applied to ultraviolet detection equipment
4. The invention relates to a preparation method of a flexible solar blind ultraviolet detector based on a gallium oxide heterojunction structure, which adopts a magnetron sputtering method to synthesize a gallium oxide heterojunction nano-pillar array in situ to prepare alpha-Ga2O3/β-Ga2O3The method for the heterojunction nano-pillar array has the advantages of low cost, controllable process, large-area preparation and good repeatability.
5. The invention relates to a preparation method of a flexible solar blind ultraviolet detector based on a gallium oxide heterojunction structure, which is characterized in that a gallium oxide film and a gallium oxide nano-pillar array are directly prepared and formed on a glass fiber cloth flexible substrate to prepare an obtained MSSM type Ti/Au/alpha-Ga2O3/β-Ga2O3The flexible solar blind ultraviolet detector with the Ti/Au nano array has high stability and is firmly attached to the substrate; the preparation method has the advantages of strong process controllability, easy operation, stable and uniform thickness, flexibility and bendability.
Drawings
FIG. 1 is a schematic structural diagram of a flexible solar blind ultraviolet detector based on a gallium oxide heterojunction structure;
FIG. 2 is a view of alpha-Ga2O3/β-Ga2O3An XRD spectrum of the heterojunction nano-column array;
FIG. 3 is a view of α -Ga2O3/β-Ga2O3SEM photo of heterojunction nanometer column array;
FIG. 4 shows the bias voltage at-2V and the light intensity of a flexible solar blind ultraviolet detector based on a gallium oxide heterojunction structure is 50 muW/cm225 (c) ofI-t curves at 4nm and 365nm illumination.
Wherein: 1-a glass fiber cloth substrate; 2-alpha-Ga2O3A film; 3-alpha-Ga2O3A nanopillar; 4-beta-Ga2O3A housing; 5-beta-Ga2O3A film; 6-Ti/Au thin film electrodes; 7-alpha-Ga2O3/β-Ga2O3A heterojunction nanopillar array.
Detailed Description
The present invention now will be described more fully hereinafter with reference to the accompanying drawings, in which some, but not all embodiments of the invention are shown. The embodiments in the present invention, other embodiments obtained by persons skilled in the art without any inventive work, belong to the protection scope of the present invention.
Example 1
The preparation method of the flexible solar blind ultraviolet detector based on the gallium oxide heterojunction structure comprises the following steps:
(1) cleaning the glass fiber cloth substrate, wherein the cleaning process is as follows: sequentially soaking the substrate in acetone, ethanol and deionized water, performing ultrasonic treatment for 10 minutes respectively, taking out, washing with deionized water, and drying with dry N2Air drying for later use;
(2) placing a glass fiber cloth substrate on a heating table, setting the temperature of the heating table to be 100 ℃, placing a grain of Ga metal above the glass fiber cloth substrate, pressing liquid Ga metal into a sheet by using a glass slide after the Ga metal is melted, and cooling to form a Ga metal sheet/glass fiber cloth substrate for later use;
(3) ga (b) is2O3Placing the target material at the position of a target table of a magnetron sputtering deposition system, fixing the Ga metal sheet/glass fiber cloth substrate obtained in the step 2) on a sample support, and placing the sample support into a vacuum cavity;
(4) vacuumizing the cavity, introducing argon, adjusting the pressure in the vacuum cavity, introducing oxygen, heating the Ga metal sheet/glass fiber cloth substrate, and growing alpha-Ga on the gallium liquid drops on the surface of the Ga metal sheet in situ by using a magnetron sputtering method2O3Nano-column arrayAnnealing, then continuing to heat up, and carrying out rapid in-situ annealing to obtain alpha-Ga2O3/β-Ga2O3Heterojunction nanopillar array, and alpha-Ga2O3/β-Ga2O3A heterojunction thin film layer of Ga2O3The distance between the target material and the glass fiber cloth substrate is set to be 5 cm, and the pressure intensity of the evacuated cavity is 1 multiplied by 10-4Pa, introducing argon gas, regulating the pressure of the vacuum chamber to 1.0Pa, introducing oxygen gas, and regulating the pressure of the vacuum chamber to 103Pa; heating the Ga metal sheet/glass fiber cloth substrate at 450 ℃, sputtering power of 80W and sputtering time of 1 hour; the temperature of the rapid annealing after the temperature rise is 700 ℃, and the annealing time is 10 minutes.
(5) Utilizing a mask and adopting a radio frequency magnetron sputtering technology to obtain alpha-Ga obtained in the step (4)2O3/β-Ga2O3Heterojunction nanopillar array and alpha-Ga2O3Depositing a layer of Ti/Au film electrode on each film, wherein the sputtering process conditions are as follows: the pressure of the evacuated cavity is 1 multiplied by 10-4Pa, the substrate temperature is room temperature, the working atmosphere is Ar gas, the working pressure is 1.0Pa, the sputtering power is 80W, and the sputtering time is 2 min.
The flexible solar blind ultraviolet detector based on the gallium oxide heterojunction structure and shown in the structure of figure 1 is prepared and comprises a glass fiber cloth substrate and alpha-Ga arranged above the glass fiber cloth substrate 12O3Film 2 of alpha-Ga2O3alpha-Ga over film 22O3/β-Ga2O3A heterojunction nanopillar array 7 arranged on the alpha-Ga2O3/β-Ga2O3alpha-Ga of heterojunction nano-pillar array 7 gap2O3beta-Ga over film 22O3A thin film 3, and a Ti/Au thin film electrode 4; the alpha-Ga2O3/β-Ga2O3The heterojunction nano-pillar array comprises a material distributed in alpha-Ga2O3alpha-Ga over film 22O3Nanopillar array coated on alpha-Ga2O3beta-Ga around nano-column 32O3 Outer casing 4，α-Ga2O3Film 2 and beta-Ga2O3alpha-Ga is formed between the films 32O3/β-Ga2O3A heterojunction thin film layer; two Ti/Au thin-film electrodes 6 are arranged, one is arranged at alpha-Ga2O3/β-Ga2O3One is arranged above the heterojunction nano-pillar array 7 and the other is arranged above the alpha-Ga2O3Above the membrane 2.
In this example, step (4) was carried out to prepare α -Ga by magnetron sputtering2O3/β-Ga2O3Gallium oxide heterojunction nanopillar arrays. Forming gallium metal liquid drops on the surface of the gallium metal film under the high-temperature heating of 450-500 ℃, and growing alpha-Ga on the gallium metal liquid drops through magnetron sputtering2O3The nano-column array is formed by slowly oxidizing the gallium metal layer in the oxygen atmosphere to form alpha-Ga2O3A film; further rapidly heating to 700-800 deg.C, alpha-Ga2O3Conversion of the periphery of the nanopillars and films to beta-Ga2O3Form alpha-Ga2O3/β-Ga2O3A heterojunction nanopillar array. The gallium can be used as an autocatalyst to catalyze the gallium metal layer to form a gallium oxide nano material at high temperature, and on the other hand, the gallium metal layer is slowly oxidized to form a gallium oxide film which can be used as an array growth substrate, so that the formed gallium oxide nano columns are ordered and uniformly distributed.
XRD analysis was carried out on the sample obtained in step (4) by heating at 450 ℃ to find that the diffraction peaks of (104), (110), (113), (116) and (300) in the figure were α -Ga2O3Characteristic peaks of the phases (FIG. 2), no characteristic peaks of other impurities were found, indicating that alpha-Ga was first grown on the flexible glass fiber substrate2O3A material. In the XRD pattern of the sample obtained after annealing at the temperature of quickly raising the temperature to 700 ℃ in the step (4), the diffraction peaks of the crystal faces of (-401), (-202), (111), (-311), (400), (-501) and (512) are found to correspond to beta-Ga2O3Characteristic peaks of the phases, the rest diffraction peaks being alpha-Ga2O3Material, indicating that the obtained sample is alpha-Ga2O3/β-Ga2O3A heterojunction structure material. Will be described in detail(4) The obtained sample is observed in a scanning electron microscope, and the nano-column grows uniformly, as shown in figure 3, which shows that alpha-Ga2O3/β-Ga2O3The diameter of the heterojunction nano-column is 100-200nm, the height is 1.0-1.5 μm, and the nano-column array substrate layer is alpha-Ga2O3The thickness of the film is 0.5-1.0 μm. alpha-Ga2O3The nano-column is calcined rapidly at high temperature to make alpha-Ga2O3Is oxidized to form a layer of beta-Ga2O3And forming a heterojunction structure.
For the Ti/Au/alpha-Ga obtained in the step (4)2O3/β-Ga2O3And carrying out photoelectric performance test on the/Ti/Au nano array flexible solar blind ultraviolet detection device. FIG. 4 shows the bias voltage at-2V and the light intensity at 50. mu.W/cm2I-t curves measured by turning the lamp off without turning the lamp on and off under 254nm and 365nm illumination. The device showed good reproducibility by repeated testing for 4I-t cycles. Under dark conditions, the detector has a dark current of-3 nA, when the light intensity is 50 μ W/cm2After the irradiation of 254nm ultraviolet light, the current is rapidly increased to-66 nA, and the light-dark ratio Iphoto/IdarkReach 22 and high sensitivity. Under the same illumination intensity, the obtained Ti/Au/alpha-Ga is subjected to ultraviolet light of 365nm2O3/β-Ga2O3The flexible solar blind ultraviolet detector with the Ti/A heterojunction nano array is used for carrying out photoelectric detection, and no photocurrent response is found, so that the flexible ultraviolet detector has the solar blind characteristic, can work outdoors without being interfered by sunlight, and is expected to be widely applied to the fields of portable wearing equipment, intelligent textiles and the like.
Example 2
The preparation method of the flexible solar blind ultraviolet detector based on the gallium oxide heterojunction structure comprises the following steps:
(1) cleaning the glass fiber cloth substrate, wherein the cleaning process is as follows: sequentially soaking the substrate in acetone, ethanol and deionized water, performing ultrasonic treatment for 10 minutes respectively, taking out, washing with deionized water, and drying with dry N2Air drying for later use;
(2) placing a glass fiber cloth substrate on a heating table, setting the temperature of the heating table to be 100 ℃, placing a grain of Ga metal above the glass fiber cloth substrate, pressing liquid Ga metal into a sheet by using a glass slide after the Ga metal is melted, and cooling to form a Ga metal sheet/glass fiber cloth substrate for later use;
(3) ga (b) is2O3Placing the target material at the position of a target table of a magnetron sputtering deposition system, fixing the Ga metal sheet/glass fiber cloth substrate obtained in the step 2) on a sample support, and placing the sample support into a vacuum cavity;
(4) vacuumizing the cavity, introducing argon, adjusting the pressure in the vacuum cavity, introducing oxygen, heating the Ga metal sheet/glass fiber cloth substrate, and growing alpha-Ga on the gallium liquid drops on the surface of the Ga metal sheet in situ by using a magnetron sputtering method2O3Nano column array, annealing, then heating continuously, making quick in-situ annealing to obtain alpha-Ga2O3/β-Ga2O3Heterojunction nanopillar array in which Ga2O3The distance between the target material and the glass fiber cloth substrate is set to be 5 cm, and the pressure intensity of the evacuated cavity is 1 multiplied by 10- 4Pa, introducing argon gas, regulating the pressure of the vacuum chamber to 1.0Pa, introducing oxygen gas, and regulating the pressure of the vacuum chamber to 103Pa; heating the Ga metal sheet/glass fiber cloth substrate at 450 ℃, wherein the sputtering power is 70W, and the sputtering time is 1 hour; the temperature of the rapid annealing after the temperature rise is 750 ℃, and the annealing time is 10 minutes.
(5) Utilizing a mask and adopting a radio frequency magnetron sputtering technology to obtain alpha-Ga obtained in the step (4)2O3/β-Ga2O3Heterojunction nanopillar array and alpha-Ga2O3Depositing a layer of Ti/Au film electrode on each film, wherein the sputtering process conditions are as follows: the pressure of the evacuated cavity is 1 multiplied by 10-4Pa, the substrate temperature is room temperature, the working atmosphere is Ar gas, the working pressure is 1.0Pa, the sputtering power is 80W, and the sputtering time is 2 min.
The crystal structure, chemical composition, morphology and solar-blind ultraviolet photoelectric characteristics of the obtained heterojunction nanopillar array are similar to those of example 1.
Example 3
The preparation method of the flexible solar blind ultraviolet detector based on the gallium oxide heterojunction structure comprises the following steps:
(1) cleaning the glass fiber cloth substrate, wherein the cleaning process is as follows: sequentially soaking the substrate in acetone, ethanol and deionized water, performing ultrasonic treatment for 10 minutes respectively, taking out, washing with deionized water, and drying with dry N2Air drying for later use;
(2) placing a glass fiber cloth substrate on a heating table, setting the temperature of the heating table to be 100 ℃, placing a grain of Ga metal above the glass fiber cloth substrate, pressing liquid Ga metal into a sheet by using a glass slide after the Ga metal is melted, and cooling to form a Ga metal sheet/glass fiber cloth substrate for later use;
(3) ga (b) is2O3Placing the target material at the position of a target table of a magnetron sputtering deposition system, fixing the Ga metal sheet/glass fiber cloth substrate obtained in the step 2) on a sample support, and placing the sample support into a vacuum cavity;
(4) vacuumizing the cavity, introducing argon, adjusting the pressure in the vacuum cavity, introducing oxygen, heating the Ga metal sheet/glass fiber cloth substrate, and growing alpha-Ga on the gallium liquid drops on the surface of the Ga metal sheet in situ by using a magnetron sputtering method2O3Nano column array, annealing, then heating continuously, making quick in-situ annealing to obtain alpha-Ga2O3/β-Ga2O3Heterojunction nanopillar array in which Ga2O3The distance between the target material and the glass fiber cloth substrate is set to be 5 cm, and the pressure intensity of the evacuated cavity is 1 multiplied by 10- 4Pa, introducing argon gas, regulating the pressure of the vacuum chamber to 1.0Pa, introducing oxygen gas, and regulating the pressure of the vacuum chamber to 103Pa; heating the Ga metal sheet/glass fiber cloth substrate at 400 ℃, sputtering power of 70W and sputtering time of 1 hour; the temperature of the rapid annealing after the temperature rise is 700 ℃, and the annealing time is 20 minutes.
(5) Utilizing a mask and adopting a radio frequency magnetron sputtering technology to obtain alpha-Ga obtained in the step (4)2O3/β-Ga2O3Heterojunction nanopillar array and alpha-Ga2O3Depositing a layer of Ti/Au thin film electrode on each thin film, wherein, sputtering process stripsA piece: the pressure of the evacuated cavity is 1 multiplied by 10-4Pa, the substrate temperature is room temperature, the working atmosphere is Ar gas, the working pressure is 1.0Pa, the sputtering power is 80W, and the sputtering time is 2 min.
Example 4
The preparation method of the flexible solar blind ultraviolet detector based on the gallium oxide heterojunction structure comprises the following steps:
(1) cleaning the glass fiber cloth substrate, wherein the cleaning process is as follows: sequentially soaking the substrate in acetone, ethanol and deionized water, performing ultrasonic treatment for 10 minutes respectively, taking out, washing with deionized water, and drying with dry N2Air drying for later use;
(2) placing a glass fiber cloth substrate on a heating table, setting the temperature of the heating table to be 100 ℃, placing a grain of Ga metal above the glass fiber cloth substrate, pressing liquid Ga metal into a sheet by using a glass slide after the Ga metal is melted, and cooling to form a Ga metal sheet/glass fiber cloth substrate for later use;
(3) ga (b) is2O3Placing the target material at the position of a target table of a magnetron sputtering deposition system, fixing the Ga metal sheet/glass fiber cloth substrate obtained in the step 2) on a sample support, and placing the sample support into a vacuum cavity;
(4) vacuumizing the cavity, introducing argon, adjusting the pressure in the vacuum cavity, introducing oxygen, heating the Ga metal sheet/glass fiber cloth substrate, and growing alpha-Ga on the gallium liquid drops on the surface of the Ga metal sheet in situ by using a magnetron sputtering method2O3Nano column array, annealing, then heating continuously, making quick in-situ annealing to obtain alpha-Ga2O3/β-Ga2O3Heterojunction nanopillar array in which Ga2O3The distance between the target material and the glass fiber cloth substrate is set to be 5 cm, and the pressure intensity of the evacuated cavity is 1 multiplied by 10- 4Pa, introducing argon gas, regulating the pressure of the vacuum chamber to 1.0Pa, introducing oxygen gas, and regulating the pressure of the vacuum chamber to 103Pa; heating the Ga metal sheet/glass fiber cloth substrate at 500 ℃, sputtering power of 80W and sputtering time of 1.5 hours; the temperature of the rapid annealing after the temperature rise is 800 ℃, and the annealing time is 20 minutes.
(5) Utilizing a mask and adopting a radio frequency magnetron sputtering technology to obtain alpha-Ga obtained in the step (4)2O3/β-Ga2O3Heterojunction nanopillar array and alpha-Ga2O3Depositing a layer of Ti/Au film electrode on each film, wherein the sputtering process conditions are as follows: the pressure of the evacuated cavity is 1 multiplied by 10-4Pa, the substrate temperature is room temperature, the working atmosphere is Ar gas, the working pressure is 1.0Pa, the sputtering power is 80W, and the sputtering time is 2 min.
Example 5
As shown in figure 1, the flexible solar blind ultraviolet detector based on the gallium oxide heterojunction structure comprises a glass fiber cloth substrate and alpha-Ga arranged above the glass fiber cloth substrate 12O3Film 2 of alpha-Ga2O3alpha-Ga over film 22O3/β-Ga2O3A heterojunction nanopillar array 7 arranged on the alpha-Ga2O3/β-Ga2O3alpha-Ga of heterojunction nano-pillar array 7 gap2O3beta-Ga over film 22O3A thin film 3, and a Ti/Au thin film electrode 4; the alpha-Ga2O3/β-Ga2O3The heterojunction nano-pillar array comprises a material distributed in alpha-Ga2O3alpha-Ga over film 22O3Nanopillar array coated on alpha-Ga2O3beta-Ga around nano-column 32O3Outer shell 4, alpha-Ga2O3Film 2 and beta-Ga2O3alpha-Ga is formed between the films 32O3/β-Ga2O3A heterojunction thin film layer; two Ti/Au thin-film electrodes 6 are arranged, one is arranged at alpha-Ga2O3/β-Ga2O3One is arranged above the heterojunction nano-pillar array 7 and the other is arranged above the alpha-Ga2O3Above the membrane 2.
The alpha-Ga2O3The film 2 is positioned on the glass fiber cloth substrate 1 and alpha-Ga2O3/β-Ga2O3Between heterojunction nanopillar arrays 7, alpha-Ga2O3/β-Ga2O3Distribution area of heterojunction nano-pillar array 7Less than alpha-Ga2O3Area of the thin film 2, set at alpha-Ga2O3Ti/Au thin film electrode 6 and alpha-Ga on the thin film 22O3/β-Ga2O3The heterojunction nano-pillar array 7 is positioned in alpha-Ga2O3The same side of the film 2.
The alpha-Ga2O3Film 2 and alpha-Ga2O3The nano-pillars are of an integrated structure.
Further, the α -Ga2O3/β-Ga2O3The diameter of the heterojunction nano-column is 100-200nm, and the height is 1.0-1.5 μm; the alpha-Ga2O3The thickness of the film 2 is 0.5 to 1.0. mu.m.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Any modification, equivalent replacement or improvement made by the ordinary skilled in the art based on the above description and within the method and principle of the present invention shall be included in the protection scope of the present invention. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (6)
1. The preparation method of the flexible solar blind ultraviolet detector based on the gallium oxide heterojunction structure is characterized by comprising the following steps of:
step one, cleaning a glass fiber cloth substrate, wherein the cleaning process is as follows: sequentially soaking the substrate in acetone, ethanol and deionized water, performing ultrasonic treatment for 10 minutes respectively, taking out, washing with deionized water, and drying with dry N2Air drying for later use;
placing the glass fiber cloth substrate on a heating table, setting the temperature of the heating table to be 100 ℃, placing a grain of Ga metal above the glass fiber cloth substrate, pressing the liquid Ga metal into a sheet by using a glass slide when the Ga metal is molten, and cooling to form a Ga metal sheet/glass fiber cloth substrate for later use;
step three, adding Ga2O3Target materialPlacing the Ga metal sheet/glass fiber cloth substrate obtained in the step two on a sample support and placing the Ga metal sheet/glass fiber cloth substrate into a vacuum cavity;
step four, vacuumizing the vacuum cavity, introducing argon, adjusting the pressure in the vacuum cavity, introducing oxygen, heating the Ga metal sheet/glass fiber cloth substrate, and growing alpha-Ga on the gallium liquid drops on the surface of the gallium metal sheet in situ by utilizing a magnetron sputtering method2O3Nano column array, annealing, then heating continuously, making quick in-situ annealing to obtain alpha-Ga2O3/β-Ga2O3Heterojunction nanopillar array, and alpha-Ga2O3/β-Ga2O3A heterojunction thin film layer of Ga2O3The distance between the target material and the glass fiber cloth substrate is set to be 5 cm, and the pressure intensity of the evacuated cavity is 1 multiplied by 10-4Pa, introducing argon gas, regulating the pressure of the vacuum chamber to 0.8-1.0Pa, and regulating the pressure of the vacuum chamber to 103Pa；
Step five, utilizing a mask and adopting a radio frequency magnetron sputtering technology to obtain the alpha-Ga obtained in the step four2O3/β-Ga2O3Heterojunction nanopillar array and alpha-Ga2O3Depositing a layer of Ti/Au film electrode on each film, wherein the sputtering process conditions are as follows: the pressure of the evacuated cavity is 1 multiplied by 10-4Pa, the substrate temperature is room temperature, the working atmosphere is Ar gas, the working pressure is 0.8-1.0Pa, the sputtering power is 60-80W, and the sputtering time is 2 min; the prepared flexible solar blind ultraviolet detector based on the gallium oxide heterojunction structure comprises a glass fiber cloth substrate and alpha-Ga arranged above the glass fiber cloth substrate2O3A thin film provided on α -Ga2O3alpha-Ga over thin films2O3/β-Ga2O3A heterojunction nanopillar array arranged on the alpha-Ga2O3/β-Ga2O3alpha-Ga of heterojunction nano-pillar array gap2O3beta-Ga over thin films2O3A thin film, and a Ti/Au thin film electrode;
the alpha-Ga2O3Thickness of the filmThe degree is 0.5-1.0 μm; the alpha-Ga2O3/β-Ga2O3The diameter of the heterojunction nano-column is 100-200nm, and the height is 1.0-1.5 μm.
2. The method for preparing a flexible solar-blind ultraviolet detector based on a gallium oxide heterojunction structure according to claim 1, wherein the alpha-Ga2O3The film is arranged on a glass fiber cloth substrate and alpha-Ga2O3/β-Ga2O3Between heterojunction nanopillar arrays, alpha-Ga2O3/β-Ga2O3The distribution area of the heterojunction nano-pillar array is smaller than that of alpha-Ga2O3Film area of α -Ga2O3Ti/Au thin film electrode on thin film and alpha-Ga2O3/β-Ga2O3The heterojunction nano-pillar array is positioned in alpha-Ga2O3The same side of the film.
3. The method for preparing a flexible solar-blind ultraviolet detector based on a gallium oxide heterojunction structure according to claim 1, wherein the alpha-Ga2O3Thin film and alpha-Ga2O3The nano-pillars are of an integrated structure.
4. The method according to claim 1, wherein the Ga metal sheet/glass fiber cloth substrate is heated at 400-500 ℃, the sputtering power is 60-80W, and the sputtering time is 1-1.5 hours.
5. The method as claimed in claim 1, wherein the temperature of the rapid in-situ annealing after the temperature rise in the fourth step is 700-800 ℃, and the annealing time is 10-20 minutes.
6. Flexible solar blind ultraviolet detector based on gallium oxide heterojunction structure prepared on the basis of the preparation method according to any one of claims 1 to 5, characterized in that: the prepared flexible solar blind ultraviolet detector based on the gallium oxide heterojunction structure comprisesA glass fiber cloth substrate, and alpha-Ga arranged above the glass fiber cloth substrate2O3A thin film provided on α -Ga2O3alpha-Ga over thin films2O3/β-Ga2O3A heterojunction nanopillar array arranged on the alpha-Ga2O3/β-Ga2O3alpha-Ga of heterojunction nano-pillar array gap2O3beta-Ga over thin films2O3A thin film, and a Ti/Au thin film electrode; the alpha-Ga2O3/β-Ga2O3The heterojunction nano-pillar array comprises a material distributed in alpha-Ga2O3alpha-Ga over thin films2O3Nanopillar array coated on alpha-Ga2O3beta-Ga around nano-column2O3Outer shell, alpha-Ga2O3Thin film and beta-Ga2O3alpha-Ga is formed between the films2O3/β-Ga2O3A heterojunction thin film layer; two Ti/Au thin film electrodes are arranged, one is arranged at the alpha-Ga2O3/β-Ga2O3One above the heterojunction nanopillar array and the other arranged on the alpha-Ga2O3Above the membrane.
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| CN111463297B (en) * | 2020-04-16 | 2021-10-12 | 杭州紫芯光电有限公司 | Solar blind ultraviolet detector based on flexible titanium metal wire/gallium oxide nano array and preparation method thereof |
| CN112382691B (en) * | 2020-10-16 | 2022-05-17 | 华南师范大学 | Self-powered detector containing gallium nitride/gallium oxide nanopillar array and preparation method thereof |
| CN113659020B (en) * | 2021-02-26 | 2023-06-02 | 松山湖材料实验室 | Solar-blind ultraviolet detector, preparation method thereof, and solar-blind ultraviolet detection method |
| RU207743U1 (en) * | 2021-07-16 | 2021-11-15 | Александр Вячеславович Цымбалов | SOLAR BLIND UV DETECTOR |
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