CN111276573B - Based on amorphous (GaLu)2O3Solar blind ultraviolet detector of film - Google Patents
Based on amorphous (GaLu)2O3Solar blind ultraviolet detector of film Download PDFInfo
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Abstract
The invention discloses a non-crystal (GaLu) -based glass fiber reinforced plastic composite material2O3A solar blind ultraviolet detector of a film and a preparation method thereof. The detector sequentially comprises an m-plane sapphire substrate, an active layer and a pair of parallel metal electrodes from bottom to top; the active layer is amorphous (GaLu)2O3A film. The invention utilizes Lu2O3And Ga2O3Formation (GaLu)2O3Alloy to increase Ga2O3Optical bandgap of (1), higher bandgap (GaLu)2O3The film can effectively reduce the dark current of the device and enable the cut-off wavelength to be blue-shifted to be within 280 nm. In addition, the invention grows amorphous (GaLu) on the m-plane sapphire2O3The film has a plurality of dangling bonds and surface states, and the dangling bonds and the surface states can serve as recombination centers to accelerate the response speed of the device. Benefit from this, amorphous (GaLu)2O3Thin film devices vs. pure Ga2O3The device greatly improves the detection capability of the device to deep ultraviolet light.
Description
Technical Field
The invention belongs to the field of medicineThe invention belongs to the technical field of conductor detectors, and particularly relates to a solar blind ultraviolet detector with an MSM structure, in particular to a solar blind ultraviolet detector based on amorphous (GaLu)2O3A high-gain solar-blind ultraviolet detector of a film and a preparation method thereof.
Background
Because the deep ultraviolet part (200-280 nm) in sunlight can be strongly absorbed by an ozone layer before reaching the surface of the earth, the solar blind ultraviolet photoelectric detector has the characteristics of strong anti-interference capability, high sensitivity and the like when working on the surface of the earth. The method has very important application in military and civil fields of missile early warning, ultraviolet communication, fire prevention and control, environmental monitoring and the like. Compared with the traditional vacuum ultraviolet photomultiplier, the solar blind ultraviolet photoelectric detector based on the wide-bandgap semiconductor material has the characteristics of small size, high gain, low energy consumption and the like, and becomes the focus of research and competition of various countries in the world. Wherein the research is mainly focused on MgZnO, AlGaN and Ga2O3The semiconductor material with the same width forbidden band. However, to realize solar blind ultraviolet detection, the band gap of the active layer semiconductor material must be larger than 4.4eV, and MgZnO and AlGaN significantly degrade the crystal quality while increasing the band gap to 4.4eV by increasing the Mg and Al contents, respectively, and greatly reduce the electrical properties and stability of the device.
The present application has been made for the above reasons.
Disclosure of Invention
Ga2O3The material is a semiconductor material with a direct band gap of 4.9eV, has high exciton confinement energy at room temperature, has good physical and chemical stability, and is an ideal solar blind ultraviolet detection material.
Since the forbidden band width of pure gallium oxide is 4.9eV, Ga is2O3The peak value response of the basic solar blind ultraviolet photoelectric detector is about 255 nm. Then the wavelength responsivity cut-off wavelength is more than 280nm, namely the device also has obvious response to ultraviolet light in UVB wave band. Because the ultraviolet light intensity of the solar blind wave band on the ground is very weak, the influence of background noise can be well weakened by reducing the dark current of the device. Based on the analysis of the above problems, the present invention adoptsLu with wider band gap2O3(5.5eV) with Ga2O3(4.9eV) formation (GaLu)2O3Alloy to increase Ga2O3The band gap of the semiconductor device can further reduce the dark current of the device and blue shift the cut-off wavelength. In addition, the m-plane sapphire is used as the substrate, because the m-plane sapphire and Ga2O3The lattice mismatch rate is large, so that amorphous sapphire (GaLu) grows on the m-plane2O3A film. Amorphous at the same time (GaLu)2O3Many dangling bonds and surface states exist in the film, and the dangling bonds and the surface states can serve as recombination centers to accelerate the response speed of the device. Benefit from this, amorphous (GaLu)2O3Thin film devices vs. pure Ga2O3The device greatly improves the detection capability of the device to deep ultraviolet light.
In addition, the metal-semiconductor-metal (MSM) structure detector is particularly beneficial to surface light absorption, has the advantages of simple structure, high efficiency, convenience in integration and the like, and can regulate and control the performance of the obtained detector by controlling parameters such as metal types, channel widths and the like. Therefore, the invention selects and utilizes m-plane sapphire to prepare the amorphous-based (GaLu)2O3High gain solar blind UV detector of thin film.
The invention aims to provide a non-crystal (GaLu) -based glass fiber reinforced composite material2O3A solar blind ultraviolet detector of a film and a preparation method thereof. The invention utilizes Lu3+The doping of the gallium oxide film improves the band gap of the gallium oxide film and enables the film to be amorphous, thereby leading the cut-off wavelength blue shift of the gallium oxide solar blind ultraviolet detector, obviously reducing the dark current and the relaxation time, and greatly improving the detection capability of the gallium oxide solar blind ultraviolet detector on the deep ultraviolet.
In order to achieve the first object of the present invention, the present invention adopts the following technical solutions:
amorphous (GaLu) -based2O3The solar blind ultraviolet light detector of film, the detector includes m face sapphire substrate, active layer, a pair of parallel metal electrode from supreme down in proper order, wherein: the active layer is amorphous (GaLu)2O3A film.
Further, according to the technical scheme, the thickness of the active layer is 150-300 nm.
Further, according to the technical scheme, the thickness of the parallel metal electrodes is 30-70 nm.
Further, according to the technical scheme, the distance between the parallel metal electrodes is 10-100 mu m.
Further, in the above technical solution, the parallel metal electrode material may be any one of Pt, Au, Al, or ITO, and is preferably Au.
It is another object of the present invention to provide the amorphous-based (GaLu) as described above2O3A method of making a thin film solar blind uv detector, said method comprising the steps of:
(1) taking m-plane sapphire as a substrate for film growth, ultrasonically cleaning the substrate by using a cleaning solution, drying the substrate by using nitrogen, and immediately placing the substrate in a vacuum chamber;
(2) use (GaLu)2O3Depositing the ceramic target on the surface of the m-surface sapphire substrate pretreated in the step (1) by adopting a pulse laser ablation deposition, magnetron sputtering or electron beam evaporation method to form amorphous (GaLu)2O3A film;
(3) by evaporation or photolithography, in said (GaLu)2O3Preparing a pair of parallel metal electrodes on the surface of the film to obtain the amorphous-based (GaLu)2O3A film solar blind uv detector.
Further, in the above technical scheme, the cleaning solution in step (1) includes acetone, ethanol, and deionized water, and the ultrasonic cleaning time is preferably 15 min.
Further, the technical proposal is that the amorphous (GaLu) in the step (2)2O3The film is prepared by a pulse laser ablation deposition method, and the specific process comprises the following steps:
utilization (GaLu)2O3Ceramic is used as a target material, the temperature of the substrate is controlled to be 300-800 ℃, the energy of Pulse laser is 200-600 mJ/Pulse, the oxygen pressure is 1-8 Pa, and amorphous (GaLu) is formed by deposition on the surface of the m-plane sapphire substrate pretreated in the step (1)2O3A film.
Further, the above technical solution, step (2) said (GaLu)2O3The ceramic target is prepared by adopting a solid-phase sintering method, and the specific method comprises the following steps:
(a) the molar ratio of the components is 95: 5 ratio of Ga2O3、Lu2O3Uniformly mixing the powder, adding ultrapure water, uniformly mixing again, and placing in a ball milling tank for ball milling to obtain mixed powder;
(b) drying the mixed powder in a vacuum drying oven, cooling to room temperature, grinding, and pressing into round pieces;
(c) in the air atmosphere, putting the wafer obtained in the step (b) into a vacuum tube furnace, and firing at 1000-1500 ℃ for 1-4 h to obtain the (GaLu)2O3A ceramic.
Furthermore, in the above technical scheme, the temperature of the vacuum drying oven in the step (b) is 120 ℃, and the drying time is 12 hours.
The principle of the invention is as follows:
the invention utilizes Lu2O3Has an ultra-wide band gap (5.5eV) greater than Ga2O3Band gap of (4.9eV), so that Lu2O3And Ga2O3Formation (GaLu)2O3Alloys, i.e. Lu3+Partially substituted Ga2O3Ga (1) in3+Thereby increasing Ga2O3The optical bandgap of (1). Of higher band gap (GaLu)2O3The film can effectively reduce the dark current of the device and enable the cut-off wavelength to be blue-shifted to be within 280 nm. In addition, the m-plane sapphire is used as the substrate, because the m-plane sapphire and Ga2O3The lattice mismatch rate is large, so that amorphous sapphire (GaLu) grows on the m-plane2O3A film. Because the bond energy of the Lu-O bond is larger than that of the Ga-O bond, the introduction of Lu can greatly reduce the oxygen vacancy in the film and accelerate the response speed of the device; amorphous at the same time (GaLu)2O3Many dangling bonds and surface states exist in the film, and the dangling bonds and the surface states can serve as recombination centers to further accelerate the response speed of the device. Benefit from this, amorphous (GaLu)2O3Thin film devices vs. pure Ga2O3The device greatly improves the detection capability of the device to deep ultraviolet light.
The invention has the beneficial effects that:
1. through Lu2O3Has an ultra-wide band gap (5.5eV) greater than Ga2O3Band gap of (4.9eV), so that Lu2O3And Ga2O3Formation (GaLu)2O3Alloying to increase Ga2O3The optical bandgap of (1). In addition, m-plane sapphire and Ga2O3Large lattice mismatch rate, and amorphous sapphire (GaLu) grown on m-plane2O3A film.
2. Higher bandgap (GaLu)2O3The carrier concentration in the film is lower, so that the dark current of the solar blind ultraviolet photoelectric detector can be effectively reduced, and the cut-off wavelength can be blue-shifted.
3. Because the bond energy of the Lu-O bond is larger than that of the Ga-O bond, the introduction of Lu can greatly reduce the oxygen vacancy in the film and accelerate the response speed of the device; amorphous at the same time (GaLu)2O3Many dangling bonds and surface states exist in the film, and the dangling bonds and the surface states can serve as recombination centers to further accelerate the response speed of the device. Benefit from this, amorphous (GaLu)2O3Thin film devices vs. pure Ga2O3The device greatly improves the detection capability of the device to deep ultraviolet light.
4. The solar blind ultraviolet photoelectric detector with the MSM structure has simple structure and manufacturing process, and in addition, the detector has excellent detection capability on deep ultraviolet light with 245nm wavelength, extremely small dark current and high response speed.
Drawings
FIG. 1 is a non-crystal (GaLu) base of the present invention2O3The structural schematic diagram of a solar blind ultraviolet detector of the film;
FIG. 2 is amorphous (GaLu) prepared in example 1 of the present invention2O3And (3) a film XRD full spectrum.
FIG. 3 shows amorphous (GaLu) in example 1 of the present invention2O3Basic solar blindAn I-V curve of the ultraviolet photoelectric detector;
FIG. 4 shows amorphous (GaLu) in example 1 of the present invention2O3A response rate graph of a solar-based blind ultraviolet photodetector;
FIG. 5 shows a single crystal (GaLu) in example 2 of the present invention2O3A response rate graph of a solar-based blind ultraviolet photodetector;
FIG. 6 shows amorphous β -Ga prepared in example 3 of the present invention2O3A film XRD full spectrogram;
FIG. 7 shows a graph based on β -Ga in example 3 of the present invention2O3I-V curve of solar blind ultraviolet detector of the film;
FIG. 8 shows a graph based on β -Ga in example 3 of the present invention2O3Response rate graph of solar blind ultraviolet detector of the film;
FIG. 9 shows amorphous (GaLu) -based particles in example 1 of the present invention2O3Thin film solar blind UV detector and beta-Ga based UV detector of example 32O3And (3) testing the spectral responsivity of the solar blind ultraviolet detector of the film.
FIG. 10 shows amorphous (GaLu) in example 4 of the present invention2O3A response rate graph of a solar-based blind ultraviolet photodetector;
FIG. 11 shows amorphous (GaLu) in example 5 of the present invention2O3A response rate graph of a solar-based blind ultraviolet photodetector;
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The embodiment is implemented on the premise of the technical scheme of the invention, and a detailed implementation mode and a specific operation process are given, but the protection scope of the invention is not limited to the following embodiment.
Various modifications to the precise description of the invention will be readily apparent to those skilled in the art from the information contained herein without departing from the spirit and scope of the appended claims. It is to be understood that the scope of the invention is not limited to the procedures, properties, or components defined, as these embodiments, as well as others described, are intended to be merely illustrative of particular aspects of the invention. Indeed, various modifications of the embodiments of the invention which are obvious to those skilled in the art or related fields are intended to be covered by the scope of the appended claims.
For a better understanding of the invention, and not as a limitation on the scope thereof, all numbers expressing quantities, percentages, and other numerical values used in this application are to be understood as being modified in all instances by the term "about". Accordingly, unless expressly indicated otherwise, the numerical parameters set forth in the specification and attached claims are approximations that may vary depending upon the desired properties sought to be obtained. At the very least, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.
The sapphire substrate used in each of the following examples of the present invention was one whose main component was alumina (Al)2O3)，m-Al2O3Representing m-plane sapphire. The thickness of the sapphire substrate is preferably 0.35-0.45 mm.
Example 1
As shown in FIG. 1, the amorphous (GaLu) -based glass of the present embodiment2O3The solar blind ultraviolet light detector of film, the detector includes m face sapphire substrate, active layer, a pair of parallel metal electrode from supreme down in proper order, wherein: the active layer is amorphous (GaLu)2O3And the parallel metal electrode is made of Au. The thickness of the substrate is 0.43mm, the thickness of the active layer is 120nm, the thickness of the parallel metal electrodes is 50nm, and the distance between the parallel metal electrodes is 10 microns.
The above-mentioned amorphous-based (GaLu)2O3The solar blind ultraviolet detector of the film is prepared by the following method, comprising the following steps:
step 1: prepared by adopting a solid-phase sintering method (GaLu)2O3Ternary ceramic target material
1.1 in molar ratio Ga2O3：Lu2O395: 5, weighing 8.995g Ga2O3Powder and 1.005g Lu2O3Mixing the powder, adding 15g of deionized water, then placing the mixture into a ball milling tank (zirconia ceramic balls are used as a ball milling medium) in a planetary ball mill, and carrying out ball milling for 4 hours to obtain mixed powder;
1.2, placing the mixed powder in a vacuum drying oven, carrying out vacuum drying for 12h at the temperature of 110 ℃, taking out, naturally cooling to room temperature, screening out zirconium balls, adding 1g of deionized water, fully and uniformly grinding by using a grinding bowl, and pressing into round blank sheets with the diameter of 27.5mm and the thickness of 2mm by using a tablet press under the pressure of 8M Pa;
1.3 the slab was placed in a crucible in a vacuum tube furnace and powder of the same composition (15.0000g) was placed around it. Heating the tube furnace to 1300 ℃ and keeping the temperature for 3h, and then naturally cooling to room temperature to obtain the (GaLu)2O3A ternary ceramic target material.
2.1 preparation of (GaLu) in step 12O3The ternary ceramic target material is used as a laser ablation target material, is put into a vacuum chamber together with a sapphire substrate with m surfaces which is respectively subjected to ultrasonic cleaning for 15min by acetone, absolute ethyl alcohol, deionized water and the like, and is vacuumized to 10 DEG- 4Pa；
2.2 after the temperature of the substrate reaches 700 ℃, introducing oxygen to ensure that the air pressure is maintained at 6Pa in the whole film deposition process; then starting the substrate and the target table to rotate, setting the output energy of the laser to be 300mJ/pulse and the pulse repetition frequency to be 5Hz, and starting the laser to deposit the film. After deposition for 30min, closing oxygen and heating, and finally, naturally cooling the sample to room temperature in vacuum and taking out;
2.3 placing the obtained film on a mask plate and installing the film into a vacuum cavity of a vacuum evaporator, then installing a tungsten boat and placing an evaporation source, namely 0.2g of metal Au, closing the vacuum cavity, starting a mechanical pump, a front-stage valve and a molecular pump, and pumping the vacuum degree to 10-4And below Pa, starting an evaporation power supply, slowly increasing the current until the metal Au melts and then keeping the current constant, and opening a baffle to start evaporation. Metal evaporation is finishedThen slowly reducing current, closing evaporation source, closing molecular pump, front valve and mechanical pump, and opening air valve to obtain the amorphous-based (GaLu)2O3A film solar blind uv detector.
FIG. 2 shows the amorphous phase (GaLu) prepared in this example2O3The full spectrum of the film. As shown in the figure, there were no diffraction peaks other than those of the m-plane sapphire substrate, indicating that this example succeeded in obtaining amorphous (GaLu)2O3A film. FIG. 3 shows the amorphous-based (GaLu) prepared in this example2O3The I-V curve of the solar blind ultraviolet detector of the film can be obviously seen to be nonlinear under illumination, which indicates Au and amorphous (GaLu)2O3Forming a schottky contact therebetween. Fig. 4 is a time current response curve of the device at 10V operating voltage. As can be seen from FIG. 4, the dark current of the device is very low (I) under a bias voltage of 10Vdark0.4pA) much smaller than the single crystal β -Ga based on c-plane sapphire substrate prepared in example 32O3Dark current of base detector (10.6 pA). This is because Lu2O3And Ga2O3Formation (GaLu)2O3Alloys, i.e. Lu3+The doping of Ga broadens2O3Thereby enabling a wider band gap (GaLu)2O3The dark current of the base detector is significantly reduced. At the same time, we use a bi-exponential relaxation equation
Fitting the curve to obtain the relaxation response time tau of the deviced2Is only 20ms, much faster than pure Ga2O3Relaxation response time (τ) of base detectord20.661 s). This is because m-plane sapphire and Ga are used2O3The lattice mismatch rate is large, so that amorphous sapphire (GaLu) grows on the m-plane2O3A film. Because the bond energy of the Lu-O bond is larger than that of the Ga-O bond, the introduction of Lu can greatly reduce the oxygen vacancy in the film and accelerate the response speed of the device; amorphous at the same time (GaLu)2O3The film has many dangling keys and watchAnd the planar state can be used as a recombination center to further accelerate the response speed of the device. FIG. 8 is amorphous (GaLu)2O3And single crystal beta-Ga2O3Wavelength responsivity curve of base detector benefiting from (GaLu)2O3Relatively wider band gap, amorphous (GaLu)2O3The peak response wavelength of the base detector is equivalent to single crystal beta-Ga2O3The peak response wavelength of the base detector is blue shifted. In conclusion, amorphous (GaLu)2O3Relative to single crystal beta-Ga2O3The base detector has lower dark current, obviously accelerated recovery speed and shorter peak response wavelength, and shows more sensitive and rapid detection capability to solar blind ultraviolet light.
Example 2 (comparative example)
A single crystal-based (GaLu) of this example2O3The solar blind ultraviolet light detector of film, the detector includes c face sapphire substrate, active layer, a pair of parallel metal electrode from supreme down in proper order, wherein: the active layer is (GaLu)2O3The thin film is characterized in that the parallel metal electrodes are made of Au, the thickness of the substrate is 0.43mm, the thickness of the active layer is 150nm, the thickness of the parallel metal electrodes is 55nm, and the distance between the parallel metal electrodes is 10 micrometers.
The above-mentioned embodiment is based on a single crystal (GaLu)2O3The solar blind ultraviolet detector of the film is prepared by the following method, comprising the following steps:
step 1: prepared by the same solid-phase sintering method as in example 1 (GaLu)2O3Ternary ceramic target material
2.1 preparation of (GaLu) in step 12O3The ternary ceramic target material is used as a laser ablation target material, is loaded into a vacuum chamber together with a sapphire substrate which is respectively subjected to ultrasonic cleaning for 15min by acetone, absolute ethyl alcohol, deionized water and the like, and is vacuumized to 10 DEG-4Pa；
2.2 after the temperature of the substrate reaches 700 ℃, introducing oxygen to ensure that the air pressure is maintained at 4Pa in the whole film deposition process; then starting the substrate and the target table to rotate, setting the output energy of the laser to be 300mJ/pulse and the pulse repetition frequency to be 5Hz, and starting the laser to deposit the film. After deposition for 30min, closing oxygen and heating, and finally, naturally cooling the sample to room temperature in vacuum and taking out;
2.3 placing the obtained film on a mask plate and installing the film into a vacuum cavity of a vacuum evaporator, then installing a tungsten boat and placing an evaporation source, namely 0.2g of metal Au, closing the vacuum cavity, starting a mechanical pump, a front-stage valve and a molecular pump, and pumping the vacuum degree to 10-4And below Pa, starting an evaporation power supply, slowly increasing the current until the metal Au melts and then keeping the current constant, and opening a baffle to start evaporation. Slowly reducing current after metal evaporation, closing evaporation source, closing molecular pump, front valve and mechanical pump, and opening air valve to obtain single crystal (GaLu)2O3A film solar blind uv detector.
A voltage of 10V was applied between the electrodes of the device fabricated in this example and the surface of the sample was irradiated with monochromatic light for photoelectric property test. The results show that the ratio of light to dark current (I)light/Idark300) is much smaller than the optical dark current ratio 9000 of the device of example 1; device relaxation response time τd240ms is lower than 20ms in example 1 because of the amorphous (GaLu)2O3Many dangling bonds and surface states exist in the film, and the dangling bonds and the surface states can serve as recombination centers to accelerate the response speed of the device. Moreover, the amorphous film has many defects causing amorphous (GaLu)2O3Film detector gain much larger than crystalline state (GaLu)2O3Gain of the thin film detector. The test results are shown in FIG. 5.
Example 3 (comparative example)
A catalyst based on beta-Ga of this example2O3The solar blind ultraviolet light detector of film, the detector includes c face sapphire substrate, active layer, a pair of parallel metal electrode from supreme down in proper order, wherein: the active layer is beta-Ga2O3A film, the parallel metal electrode material is Au, and the linerThe thickness of the bottom is 0.43mm, the thickness of the active layer is 150nm, the thickness of the parallel metal electrodes is 55nm, and the distance between the parallel metal electrodes is 10 μm.
This example is based on beta-Ga as described above2O3The solar blind ultraviolet detector of the film is prepared by the following method, comprising the following steps:
step 1: preparation of Ga by solid-phase sintering2O3Ceramic target material
1.1 weighing 10g Ga2O3Adding 15g of deionized water into the powder, then placing the powder into a ball milling tank (zirconia ceramic balls are used as a ball milling medium) in a planetary ball mill, and carrying out ball milling for 4 hours to obtain uniformly dispersed powder;
1.2, placing the powder in a vacuum drying oven, carrying out vacuum drying for 12h at the temperature of 110 ℃, taking out, naturally cooling to room temperature, screening out zirconium balls, adding 1g of deionized water, fully and uniformly grinding by using a grinding bowl, and pressing into round blank sheets with the diameter of 27.5mm and the thickness of 2mm by using a tablet press under the pressure of 8M Pa;
1.3 the slab was placed in a crucible in a vacuum tube furnace and powder of the same composition (15.0000g) was placed around it. Heating the tube furnace to 1300 ℃ and preserving the heat for 3h, and then naturally cooling to room temperature to obtain the Ga2O3A ceramic target material.
2.1 Ga prepared in step 12O3Ceramic target material as laser ablation target material, loading into vacuum chamber together with sapphire substrate respectively ultrasonically cleaned with acetone, anhydrous alcohol and deionized water for 15min, and vacuumizing to 10%-4Pa；
2.2 after the temperature of the substrate reaches 700 ℃, introducing oxygen to ensure that the air pressure is maintained at 4Pa in the whole film deposition process; then starting the substrate and the target table to rotate, setting the output energy of the laser to be 300mJ/pulse and the pulse repetition frequency to be 5Hz, and starting the laser to deposit the film. After deposition for 30min, closing oxygen and heating, and finally, naturally cooling the sample to room temperature in vacuum and taking out;
2.3 placing the obtained film on a mask plate and installing the film into a vacuum cavity of a vacuum evaporator, then installing a tungsten boat and placing an evaporation source, namely 0.2g of metal Au, closing the vacuum cavity, starting a mechanical pump, a front-stage valve and a molecular pump, and pumping the vacuum degree to 10-4And below Pa, starting an evaporation power supply, slowly increasing the current until the metal Au melts and then keeping the current constant, and opening a baffle to start evaporation. Slowly reducing current after metal evaporation, closing the evaporation source, closing the molecular pump, the front-stage valve and the mechanical pump, and opening the air valve to finally obtain the beta-Ga-based solar cell2O3A film solar blind uv detector.
Ga obtained from the example2O3The XRD full spectrum of the thin film is shown in FIG. 6, except for three diffraction peaks (0003), (0006) and (0009) of the c-plane sapphire substrate, there are only three diffraction peaks respectively located near 18.9 degrees, 38.3 degrees and 59.1 degrees, and comparison Ga2O3As can be seen from the standard XRD spectrum (JCPDS File No.41-1103), these three diffraction peaks represent Ga respectively2O3(-201), (-402) and (-603) planes, indicating that this example successfully produced beta-Ga in the (-201) orientation2O3A film. A voltage of 10V was applied between the electrodes of the device fabricated in this example and the surface of the sample was irradiated with monochromatic light for photoelectric property test. The result shows that the device has dark current Idark10.6pA, relaxation response time τd2It was 0.661 s. It can be seen that the dark current of the device is significantly higher than that of the amorphous (GaLu)2O3The thin film device is a gain-based detector, and has slower response speed and lower responsivity. And amorphous (GaLu)2O3Peak response wavelength of device relative to single crystal Ga2O3A blue shift occurs. Embodies the amorphous (GaLu)2O3The base detector has more excellent solar blind ultraviolet detection capability. The test results are shown in fig. 7, 8 and 9, respectively.
Example 4
One of the embodiments is based on amorphous (GaLu)2O3The solar blind ultraviolet detector of the film, the said detector includes m-plane sapphire substrate, has from the bottom to the top sequentiallyA source layer, a pair of parallel metal electrodes, wherein: the active layer is amorphous (GaLu)2O3The thin film is characterized in that the parallel metal electrode is made of Al, the thickness of the substrate is 0.43mm, the thickness of the active layer is 150nm, the thickness of the parallel metal electrode is 50nm, and the distance between the parallel metal electrodes is 50 micrometers.
The above-mentioned amorphous-based (GaLu)2O3The solar blind ultraviolet detector of the film is prepared by the following method, comprising the following steps:
step 1: prepared by the same solid-phase sintering method as in example 1 (GaLu)2O3A ternary ceramic target material.
Step 2: utilization (GaLu)2O3Solar blind ultraviolet detector prepared from ternary ceramic target material
2.1 preparation of (GaLu) in step 12O3The ternary ceramic target material is used as a laser ablation target material, is loaded into a vacuum chamber together with a sapphire substrate which is respectively subjected to ultrasonic cleaning for 15min by acetone, absolute ethyl alcohol, deionized water and the like, and is vacuumized to 10 DEG-4Pa；
2.2 after the temperature of the substrate is 500 ℃, introducing oxygen to ensure that the air pressure is maintained at 1Pa in the whole film deposition process; then starting the substrate and the target table to rotate, setting the output energy of the laser to be 300mJ/pulse and the pulse repetition frequency to be 5Hz, and starting the laser to deposit the film. After deposition for 30min, closing oxygen and heating, and finally, naturally cooling the sample to room temperature in vacuum and taking out;
2.3 placing the obtained film on a mask plate and installing the film into a vacuum cavity of a vacuum evaporator, then installing a tungsten boat and placing an evaporation source, namely 0.10g of metal Al, closing the vacuum cavity, starting a mechanical pump, a front valve and a molecular pump, and pumping the vacuum degree to 10-4And (4) below Pa, starting an evaporation power supply, slowly increasing the current until the current is kept constant after the metal Al is melted, and opening a baffle to start evaporation. Slowly reducing current after metal evaporation, closing evaporation source, closing molecular pump, front valve and mechanical pump, and opening air valve to obtain the amorphous-based (GaLu)2O3Solar blind with filmAn ultraviolet light detector.
A voltage of 10V was applied between the electrodes of the device fabricated in this example and the surface of the sample was irradiated with monochromatic light for photoelectric property test. The test result shows that the dark current of the device is extremely low (I)dark0.2pA), the dark current ratio is 9000. It can be seen that the device also exhibits better performance at lower operating voltages. The test results are shown in fig. 10, respectively.
Example 5
One of the embodiments is based on amorphous (GaLu)2O3The solar blind ultraviolet light detector of film, the detector includes m face sapphire substrate, active layer, a pair of parallel metal electrode from supreme down in proper order, wherein: the active layer is amorphous (GaLu)2O3The thin film is characterized in that the parallel metal electrode is made of Au, the thickness of the substrate is 0.43mm, the thickness of the active layer is 300nm, the thickness of the parallel metal electrode is 70nm, and the distance between the parallel metal electrodes is 100 micrometers.
The above-mentioned amorphous-based (GaLu)2O3The solar blind ultraviolet detector of the film is prepared by the following method, comprising the following steps:
step 1: prepared by the same solid-phase sintering method as in example 1 (GaLu)2O3A ternary ceramic target material.
Step 2: utilization (GaLu)2O3Solar blind ultraviolet detector prepared from ternary ceramic target material
2.1 preparation of (GaLu) in step 12O3The ternary ceramic target material is used as a laser ablation target material, is loaded into a vacuum chamber together with a sapphire substrate which is respectively subjected to ultrasonic cleaning for 15min by acetone, absolute ethyl alcohol, deionized water and the like, and is vacuumized to 10 DEG-4Pa；
2.2 after the temperature of the substrate reaches 700 ℃, introducing oxygen to ensure that the air pressure is maintained at 4Pa in the whole film deposition process; then starting the substrate and the target table to rotate, setting the output energy of the laser to be 600mJ/pulse and the pulse repetition frequency to be 5Hz, and starting the laser to deposit the film. After deposition for 30min, closing oxygen and heating, and finally, naturally cooling the sample to room temperature in vacuum and taking out;
2.3 placing the obtained film on a mask plate and installing the film into a vacuum cavity of a vacuum evaporator, then installing a tungsten boat and placing an evaporation source, namely 0.20g of metal Au, closing the vacuum cavity, starting a mechanical pump, a front valve and a molecular pump, and pumping the vacuum degree to 10-4And below Pa, starting an evaporation power supply, slowly increasing the current until the metal Au melts and then keeping the current constant, and opening a baffle to start evaporation. Slowly reducing current after metal evaporation, closing evaporation source, closing molecular pump, front valve and mechanical pump, and opening air valve to obtain the amorphous-based (GaLu)2O3A film solar blind uv detector.
A voltage of 10V was applied between the electrodes of the device fabricated in this example and the surface of the sample was irradiated with monochromatic light for photoelectric property test. The test result shows that the dark current of the device is extremely low (I)dark2pA), the dark current ratio was 5000. This is because the thin film becomes thicker, the carrier concentration in the thin film increases; in addition, the test bias voltage is increased, and the noise of the device is increased. Which in turn results in a decrease in the light-to-dark current ratio. The test results are shown in fig. 11, respectively.
Claims (9)
1. Amorphous (GaLu) -based2O3The solar blind ultraviolet detector of film, its characterized in that: the detector includes m face sapphire substrate, active layer, a pair of parallel metal electrode from supreme down in proper order, wherein: the active layer is amorphous (GaLu)2O3A film.
2. Amorphous-based (GaLu) according to claim 12O3The solar blind ultraviolet detector of film, its characterized in that: the thickness of the m-plane sapphire substrate is 0.35-0.45 mm.
3. Amorphous-based (GaLu) according to claim 12O3The solar blind ultraviolet detector of film, its characterized in that: the thickness of the active layer is 150-300 nm.
4. Amorphous-based (GaLu) according to claim 12O3The solar blind ultraviolet detector of film, its characterized in that: the thickness of the parallel metal electrode is 30-70 nm.
5. Amorphous-based (GaLu) according to claim 12O3The solar blind ultraviolet detector of film, its characterized in that: the distance between the parallel metal electrodes is 10-100 mu m.
6. Amorphous-based (GaLu) according to claim 12O3The solar blind ultraviolet detector of film, its characterized in that: the parallel metal electrode material may be any one of Pt, Au, Al, or ITO.
7. Amorphous-based (GaLu) according to claim 12O3The preparation method of the solar blind ultraviolet detector of the film is characterized by comprising the following steps: the method comprises the following steps:
(1) taking m-plane sapphire as a substrate for film growth, ultrasonically cleaning the substrate by using a cleaning solution, drying the substrate by using nitrogen, and immediately placing the substrate in a vacuum chamber of a pulse laser deposition system;
(2) depositing the pretreated m-plane sapphire substrate surface in the step (1) by adopting a pulse laser ablation deposition, magnetron sputtering or electron beam evaporation method to form amorphous (GaLu)2O3A film;
(3) by vapor deposition or photolithography, on the amorphous (GaLu)2O3Preparing a pair of parallel metal electrodes on the surface of the film to obtain the amorphous-based (GaLu)2O3A film solar blind uv detector.
8. Amorphous-based (GaLu) according to claim 72O3The preparation method of the solar blind ultraviolet detector of the film is characterized by comprising the following steps: the amorphous phase (GaLu) in step (2)2O3The film is prepared by a pulse laser ablation deposition method, and the specific process comprises the following steps:
utilization (GaLu)2O3Ceramic is used as a target material, the temperature of the substrate is controlled to be 300-800 ℃, the energy of Pulse laser is 200-600 mJ/Pulse, the oxygen pressure is 1-8 Pa, and the amorphous silicon (GaLu) is formed by deposition on the surface of the m-plane sapphire substrate pretreated in the step (1)2O3A film.
9. Amorphous-based (GaLu) according to claim 82O3The preparation method of the solar blind ultraviolet detector of the film is characterized by comprising the following steps: (GaLu) described in step (2)2O3The ceramic target is prepared by adopting a solid-phase sintering method, and the specific method comprises the following steps:
(a) the molar ratio of the components is 95: 5 ratio of Ga2O3、Lu2O3Uniformly mixing the powder, adding ultrapure water, uniformly mixing again, and placing in a ball milling tank for ball milling to obtain mixed powder;
(b) drying the mixed powder in a vacuum drying oven, cooling to room temperature, grinding, and pressing into round pieces;
(c) in the air atmosphere, putting the wafer obtained in the step (b) into a vacuum tube furnace, and firing at 1000-1500 ℃ for 1-4 h to obtain the (GaLu)2O3A ceramic.
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