CN114566566A - Aluminum nitride solar blind photoelectric detector and preparation method thereof - Google Patents
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- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/184—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof the active layers comprising only AIIIBV compounds, e.g. GaAs, InP
- H01L31/1856—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof the active layers comprising only AIIIBV compounds, e.g. GaAs, InP comprising nitride compounds, e.g. GaN
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Abstract
An aluminum nitride solar blind photoelectric detector and a preparation method thereof belong to the technical field of semiconductor photoelectric detection. The method comprises the steps of taking c-plane sapphire as a substrate, growing an aluminum nitride film on the substrate by adopting a reactive radio frequency magnetron sputtering technology, then improving the crystallization quality of the aluminum nitride film in a face-to-face annealing mode, preparing a metal interdigital electrode on the aluminum nitride film in a magnetron sputtering or electron beam evaporation mode, and finally obtaining the aluminum nitride solar blind photodetector. The aluminum nitride detector prepared by the invention has higher response to solar blind band light with the wavelength less than 210nm, the photocurrent of the detector under 50V bias voltage reaches 291nA, and the responsivity is 0.51A/W. The method has the advantages of simple process flow, low cost and suitability for batch production, and the prepared aluminum nitride detector can be applied to the field of solar blind photoelectric detection.
Description
Technical Field
The invention belongs to the technical field of semiconductor photoelectric detection, and particularly relates to an aluminum nitride solar blind photoelectric detector and a preparation method thereof.
Background
In the process of the sunlight irradiating the earth, the deep ultraviolet light with the wavelength less than 280nm is almost completely absorbed by the atmosphere and cannot reach the earth surface, so that the sunlight shielding zone is called a solar blind zone. Because the sunlight reaching the ground has little interference on the solar blind detection, the solar blind detector can work all weather, has extremely high signal-to-noise ratio, and is widely applied to a plurality of fields, such as missile tail flame early warning, flame control detection, ultraviolet communication and the like. At present, a few photoelectric detectors working in the solar dead zone wave band have high preparation cost, and cannot be produced in batches and applied in large scale.
The aluminum nitride is used as a third generation ultra-wide forbidden band semiconductor material, the forbidden band width is about 6.2eV, the absorptivity is high, the theoretical cut-off wavelength is about 200nm, and the aluminum nitride is suitable for the detection field of solar blind band light. The method for growing the high-quality aluminum nitride material mainly comprises the following steps: metal Organic Chemical Vapor Deposition (MOCVD), physical vapor transport, molecular beam epitaxy, and the like. A subject group of the Proc. Jianghong Star, university of Texas, USA, grows an aluminum nitride material with a cutoff wavelength of about 207nm by using a MOCVD method using trimethylaluminum and ammonia gas as sources, and prepares an aluminum nitride solar blind photodetector with a responsivity of about 0.4A/W (Li J, Fan Z Y, Dahal R, et al.200nm deep ultraviolet detectors based on AlN [ J ]. Applied Physics Letters,2006,89(21):213510) at a bias of 100V. However, MOCVD equipment is very expensive, the requirement on the growth temperature of aluminum nitride is high, a general MOCVD system generally cannot meet the requirement on the growth temperature of aluminum nitride, the equipment needs to be specially modified, and the preparation process is complex.
In order to reduce the cost for preparing the aluminum nitride detector, the adopted aluminum nitride growth equipment and raw materials are as economical and cheap as possible, the process flow for preparing the detector is as simple as possible, and the requirement that the device has high responsivity is met, so that the aluminum nitride detector is suitable for batch production.
Disclosure of Invention
The invention aims to provide an aluminum nitride solar blind photoelectric detector which is low in cost, easy to operate, safe, reliable and high in responsivity and a preparation method thereof. The method takes a high-purity aluminum target and high-purity nitrogen with low cost as sources, adopts a reaction radio frequency magnetron sputtering method to grow an aluminum nitride film on a c-plane sapphire substrate, then improves the crystallization quality of the aluminum nitride film by a high-temperature face-to-face annealing method, and finally prepares the interdigital electrode by a magnetron sputtering or electron beam evaporation method.
As shown in fig. 4, the aluminum nitride solar blind photodetector according to the present invention is composed of a c-plane sapphire substrate, a high quality aluminum nitride thin film, and metal interdigital electrodes.
The invention relates to a preparation method of an aluminum nitride solar blind photoelectric detector, which comprises the following steps:
(1) sequentially ultrasonically cleaning a c-surface sapphire substrate by using acetone, ethanol and deionized water, and then blowing the substrate by using high-purity nitrogen for later use;
(2) growing an aluminum nitride film on the c-plane sapphire substrate obtained in the step (1) by using a reactive radio frequency magnetron sputtering method for 60-120 min, wherein an aluminum source is a high-purity aluminum target (the purity is more than or equal to 99.95%), a working gas is high-purity nitrogen (the purity is more than or equal to 99.999%), the sputtering pressure is 0.3-0.5 Pa, the radio frequency power is 225-250W, the sputtering temperature is 350-450 ℃, and the thickness of the obtained aluminum nitride film is 300-600 nm;
(3) carrying out face-to-face thermal annealing treatment on the aluminum nitride film prepared in the step (2), wherein the annealing temperature is 1500-1600 ℃, the annealing atmosphere is high-purity nitrogen (the purity is more than or equal to 99.999%) and the annealing time is 60-120 min; the face-to-face thermal annealing treatment is to cut the aluminum nitride film prepared in the step (2) and the substrate into two parts, attach and compact the surface on which the aluminum nitride film grows face to make the aluminum nitride film contact closely, and then carry out high-temperature annealing;
(4) and (3) depositing metal layers of gold, aluminum, titanium, silver, molybdenum, chromium or nickel and the like on the annealed aluminum nitride film in the step (3) by using a magnetron sputtering or electron beam evaporation method, wherein the thickness of the metal layers is 100-400 nm, and then preparing the interdigital electrode by using a photoetching process, wherein the finger width and the finger spacing are both 5-100 mu m, so that the aluminum nitride solar blind photoelectric detector is prepared.
The invention has the advantages that: (1) the process flow is simple, and the cost of instruments, materials and substrates used in the experiment is low; (2) large-area and high-quality aluminum nitride films can be obtained and applied to the mass production of detectors; (3) the prepared aluminum nitride solar blind photoelectric detector has high responsivity, high response speed and good switching repeatability.
The principle of the invention is as follows: (1) the principle of in-situ growth of the aluminum nitride film is as follows: nitrogen in the cavity is ionized into nitrogen ions and electrons by a strong electric field, the electrons do cycloidal motion under the combined action of the electric field and the magnetic field and collide with other nitrogen atoms to ionize new nitrogen ions and secondary electrons, the nitrogen ions are accelerated by the electric field and then shoot to an aluminum target and bombard the aluminum target, and high-energy aluminum particles escape from the surface of the target and react with the nitrogen to generate aluminum nitride and are attached to a sapphire substrate; (2) the "face-to-face" annealing principle of aluminum nitride films: the aluminum nitride material is extremely easy to decompose at high temperature, and the decomposition of the aluminum nitride at high temperature can be inhibited by using a face-to-face annealing method, crystal grains in the film are recrystallized and arranged, defects and crystal boundaries are eliminated, and the crystallization quality of the film is obviously improved; (3) the working principle of the aluminum nitride solar blind photoelectric detector is as follows: when deep ultraviolet light with the wavelength less than the cut-off wavelength of the aluminum nitride irradiates the surface of the detector, electrons in the aluminum nitride jump from a valence band to a conduction band to generate a large number of electron-hole pairs, and the electrons are separated under the action of an external bias and collected by electrodes on two sides to generate photocurrent.
Drawings
FIG. 1: the method adopts a principle schematic diagram of growing the aluminum nitride film by a reactive radio frequency magnetron sputtering method;
FIG. 2: the method of the invention is a schematic diagram of the process of annealing the aluminum nitride films in a face-to-face way;
FIG. 3: raman spectrum (fig. a) and XRD spectrum (fig. b) of the aluminum nitride thin film prepared in the step (3) of example 1;
FIG. 4: a schematic structural diagram of the aluminum nitride solar-blind photodetector prepared in example 1;
FIG. 5: example 1 ultraviolet absorption spectrum of the aluminum nitride thin film prepared in the step (3);
FIG. 6: I-V characteristic curve (a) and switching characteristic curve (b) of the aluminum nitride solar blind photodetector prepared in example 1.
Detailed Description
Example 1
(1) Selecting c-plane sapphire as a substrate material, firstly ultrasonically cleaning the substrate in acetone for 10min to remove organic matters on the surface, then ultrasonically cleaning in absolute ethyl alcohol for 10min to remove the acetone, then ultrasonically cleaning in deionized water for 10min to remove the ethyl alcohol, and finally drying by using high-purity nitrogen.
(2) As shown in fig. 1, an aluminum target (purity 99.9995%) is fixed on a target holder connected with a cathode of a radio frequency magnetron sputtering apparatus, then the c-plane sapphire substrate cleaned in step (1) is fixed on a sample holder connected with an anode above the aluminum target, the sample is blocked by a baffle plate, and the target distance between the aluminum target and the sapphire substrate is adjusted to 6 cm. Pumping the background vacuum degree in the growth chamber to 5.0 × 10 by using a mechanical pump and a molecular pump-4Pa. Then, 60sccm of nitrogen (purity: 99.9995%) was introduced into the growth chamber, and the pressure in the growth chamber was adjusted to 1 Pa. And turning on the radio frequency source, setting the default sputtering power to be 75W, and clicking a start button to start the glow in the automatic tuning mode. Regulating the sputtering power to 250W after glow stabilization, reducing the pressure in the growth chamber to 0.3Pa, and startingThe substrate heating power supply set the heating temperature to 400 ℃. And after the pre-sputtering is carried out for 30min, starting the substrate to rotate at the substrate rotation speed of 10rps, removing the baffle, starting the formal sputtering, wherein the formal sputtering time is 120min, stopping the sample by using the baffle after the formal sputtering is finished, and then sequentially closing each system. And taking out the sample after the substrate is automatically cooled to obtain the aluminum nitride film with the thickness of about 600 nm.
(3) And (3) cutting the aluminum nitride film obtained in the step (2) and the lining into two halves, as shown in figure 2, tightly attaching the surfaces on which the aluminum nitride films grow together on a graphite table in a face-to-face manner, pressing the sapphire substrate by using a small graphite block to enable the aluminum nitride films to be in close contact, and then placing the sapphire substrate in a chamber of an annealing furnace. Pumping the background vacuum degree in the chamber to 1Pa by using a mechanical pump and a Roots pump, and introducing high-purity nitrogen (the purity is more than 99.999%) with the flow of 200sccm into the chamber to maintain the pressure in the chamber to be about 200 Pa. The annealing furnace is heated in a mode of generating eddy current by the induction coil, and real-time temperature is calibrated and feedback adjusted by infrared rays emitted by the infrared temperature measuring probe. And (3) raising the temperature in the annealing furnace chamber to 1600 ℃, maintaining for 120min, then carrying out voltage cooling and automatic cooling, and taking out the sample to obtain the high-quality aluminum nitride film on the sapphire substrate. The Raman spectrum is shown in FIG. 3(a), E2(high) vibration peak was located at 661.9cm-1Half peak width of only 7.5cm-1. The XRD pattern is shown in figure 3(b), the 2 theta diffraction peak of the (0002) crystal face is positioned at 36.05 degrees, and the half-value width is only 0.17 degrees. The UV-VIS absorption spectrum of this film is shown in FIG. 5, with a cut-off wavelength of about 205 nm.
(4) And (3) depositing a layer of metal aluminum with the thickness of about 300nm on the aluminum nitride film obtained in the step (3) by using electron beam evaporation, preparing an interdigital electrode by using a photoetching process, wherein the width and the distance between the interdigital electrodes are both 100 mu m, and finally obtaining the aluminum nitride solar blind photoelectric detector.
(5) When the aluminum nitride solar blind photodetector obtained in the step (4) is tested by using a light source with the wavelength of 189.4nm, as shown in fig. 6, the photocurrent of the aluminum nitride solar blind photodetector under the bias voltage of 50V is as high as 291nA, the responsivity of the aluminum nitride solar blind photodetector is 0.51A/W, the aluminum nitride solar blind photodetector has very good switching repeatability, and the rising time and the falling time of the aluminum nitride solar blind photodetector are 243ms and 115ms respectively.
Claims (6)
1. A preparation method of an aluminum nitride solar blind photoelectric detector comprises the following steps:
(1) sequentially ultrasonically cleaning a c-surface sapphire substrate by using acetone, ethanol and deionized water, and then drying by using high-purity nitrogen;
(2) growing an aluminum nitride film on the c-plane sapphire substrate obtained in the step (1) by using a reactive radio frequency magnetron sputtering method for 60-120 min, wherein an aluminum source is a high-purity aluminum target, a working gas is high-purity nitrogen, the sputtering pressure is 0.3-0.5 Pa, the radio frequency power is 225-250W, the sputtering temperature is 350-450 ℃, and the thickness of the obtained aluminum nitride film is 300-600 nm;
(3) carrying out face-to-face thermal annealing treatment on the aluminum nitride film prepared in the step (2), wherein the annealing temperature is 1500-1600 ℃, the annealing atmosphere is high-purity nitrogen (the purity is more than or equal to 99.999%) and the annealing time is 60-120 min;
(4) and (4) depositing metal layers such as gold, aluminum, titanium, silver, molybdenum, chromium or nickel and the like on the annealed aluminum nitride film in the step (3) by using a magnetron sputtering or electron beam evaporation method, wherein the thickness of the metal layers is 100-400 nm, and then preparing the interdigital electrode by using a photoetching process, wherein the finger width and the finger spacing are both 5-100 mu m, so that the aluminum nitride solar blind photodetector is prepared.
2. The method for preparing an aluminum nitride solar-blind photodetector as claimed in claim 1, wherein: and preparing the aluminum nitride film by adopting a reactive radio frequency magnetron sputtering method.
3. The method for preparing an aluminum nitride solar-blind photodetector as claimed in claim 1, wherein: the purity of the high-purity nitrogen is more than 99.999 percent.
4. The method for preparing an aluminum nitride solar-blind photodetector as claimed in claim 1, wherein: the purity of the high-purity aluminum target material is more than 99.95 percent.
5. The method for preparing an aluminum nitride solar blind photodetector as claimed in claim 1, wherein: the face-to-face thermal annealing treatment is to cut the aluminum nitride film prepared in the step (2) and the substrate into two halves, attach and compact the side on which the aluminum nitride film is grown face-to-face to make the aluminum nitride films more closely contact, and then anneal.
6. An aluminum nitride solar blind photoelectric detector is characterized in that: is prepared by the method of any one of claims 1 to 5.
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| CN115295401A (en) * | 2022-08-25 | 2022-11-04 | 松山湖材料实验室 | Aluminum nitride single crystal composite substrate, preparation method thereof and ultraviolet light-emitting device |
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| US11049993B1 (en) * | 2019-12-26 | 2021-06-29 | National Chung-Shan Institute Of Science And Technology | Method for preparing aluminum nitride-zinc oxide ultraviolet detecting electrode |
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| CN101280412A (en) * | 2007-12-29 | 2008-10-08 | 电子科技大学 | Aluminum nitride piezoelectric film and preparation thereof |
| US20180204722A1 (en) * | 2015-09-11 | 2018-07-19 | Mie University | Method for manufacturing nitride semiconductor substrate |
| CN108447945A (en) * | 2017-12-29 | 2018-08-24 | 西安电子科技大学 | Blind type flexibility ultraviolet light detector based on aluminium nitride film |
| CN108878588A (en) * | 2018-06-28 | 2018-11-23 | 西安电子科技大学 | The preparation method of gallium nitride base photodetector based on graphene insert layer structure |
| US11049993B1 (en) * | 2019-12-26 | 2021-06-29 | National Chung-Shan Institute Of Science And Technology | Method for preparing aluminum nitride-zinc oxide ultraviolet detecting electrode |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115295401A (en) * | 2022-08-25 | 2022-11-04 | 松山湖材料实验室 | Aluminum nitride single crystal composite substrate, preparation method thereof and ultraviolet light-emitting device |
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