CN109585593B - Spontaneous polarization field enhanced ultraviolet light detector based on BeZnOS quaternary alloy and preparation method thereof - Google Patents
Spontaneous polarization field enhanced ultraviolet light detector based on BeZnOS quaternary alloy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a spontaneous polarization field enhanced ultraviolet detector based on a BeZnOS quaternary alloy and a preparation method thereof. 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 a BeZnOS quaternary alloy film with an m surface, and the parallel metal electrodes are perpendicular to the c-axis direction of the BeZnOS quaternary alloy film. According to the invention, the epitaxial m-surface BeZnOS film is grown on the single crystal m-surface sapphire, the metal electrode vertical to the c axis of the film is evaporated, the separation of photon-generated carriers is promoted by fully utilizing the superposition enhancement of a spontaneous polarization electric field and an external electric field, and the light detection capability is enhanced. In addition, the ultraviolet light detector with the MSM structure has the advantages of simple structure, simple manufacturing process, high detection capability on ultraviolet light with the wavelength of 300nm, high response speed, small dark current and stable performance.
Description
Technical Field
The invention belongs to the technical field of semiconductor detectors, particularly relates to an ultraviolet detector with an MSM structure, and more particularly relates to a spontaneous polarization field enhanced ultraviolet detector based on a BeZnOS quaternary alloy and a preparation method thereof.
Background
The BeZnOS quaternary alloy is a semiconductor material with wide forbidden band and high visible light transmission, and can be used for an ultraviolet to solar dead zone light-emitting device or a light detection device. As the BeZnOS quaternary alloy has a hexagonal wurtzite structure like a ZnO crystal, the interior of the BeZnOS quaternary alloy is alternately arranged by O (S) atomic planes and Zn (Be) atomic planes, and Zn (Be) -O (S) bonds have polarity, and a large amount of regularly arranged Zn (Be) -O (S) bonds cause the BeZnOS to have a spontaneous polarization field in the c-axis direction, the spontaneous electric field polarization existing in the whole BeZnOS crystal can effectively promote the separation and the transportation of photo-generated carriers, so that a spontaneous polarization field enhancement type detector developed based on the m-plane BeZnOS quaternary film theoretically has more excellent detection capability than a common c-plane BeZnOS film-based detector. When a bezmos thin film is grown on m-plane sapphire by the PLD method, the surface of the thin film is m-plane, the c-axis of the thin film is perpendicular to the c-axis direction of sapphire, and the c-axis direction of the thin film is parallel to the surface, so that a spontaneous polarization electric field exists in the entire thin film in the direction parallel to the surface (c-axis).
The metal-semiconductor-metal (MSM) structure detector has the advantages of simple structure, high detection efficiency and the like, and the performance of the obtained detector can be regulated and controlled by controlling parameters such as metal types, channel widths and the like. When parallel electrodes perpendicular to the c axis of the film are designed and manufactured on the surface of the m-plane BeZnOS film, the enhanced MSM ultraviolet detector can be obtained by utilizing the spontaneous polarization electric field of the film.
In addition, the prior art with publication number CN 102412334 a discloses an ultraviolet light detector based on a BeZnO MSM structure and a preparation method thereof, where the detector includes a substrate and an epitaxial layer grown on the substrate, the epitaxial layer includes a stress buffer layer and a BeZnO doping layer disposed on the stress buffer layer, and an electrode with an interdigital structure or a gap structure is plated on the BeZnO doping layer. However, this technique is to improve the crystal quality by interposing a buffer layer between the active layer and the substrate, which greatly increases the complexity of the process. In addition, the technology only directly prepares the film into the detector and does not consider the polarity of the film. If c-plane sapphire is used as a substrate, and the obtained c-plane BeZnO is a polar plane epitaxial layer, a quantum Stark effect can be generated on a quantum well light-emitting device, namely an in-plane spontaneous polarization field can spatially separate electrons and holes, the recombination probability of carriers is reduced, and therefore the light-emitting intensity is reduced, and meanwhile, the spontaneous polarization field can bend an energy band at the quantum well, so that the band gap is reduced, and the light-emitting wavelength is lengthened, namely red shift occurs.
The inventor of the present application has filed a patent application with the name of "a BeZnOS compound semiconductor material, a preparation method and an application thereof (with the publication number of CN 105734491A)" in the previous period, wherein a quaternary compound semiconductor material is prepared from BeO and ZnS according to a proportion, and the effects of freely regulating and controlling a ZnO band gap and the like are realized through the synergistic effect of composite substitution of Be and S, and the BeZnOS quaternary compound prepared by the invention can Be used for an ultraviolet-to-solar dead zone light-emitting device or a light detection device.
The present application is proposed after further intensive research, development and innovation based on the above work of the inventors.
Disclosure of Invention
The invention aims to provide a spontaneous polarization field enhanced ultraviolet detector based on a BeZnOS quaternary alloy and a preparation method thereof. According to the invention, the separation and transportation of photon-generated carriers are effectively promoted by utilizing the self-generating field in the BeZnOS alloy film along the c-axis direction, so that the m-surface BeZnOS-based ultraviolet light detector is constructed.
In order to achieve the first object of the present invention, the present invention adopts the following technical solutions:
the utility model provides a spontaneous polarization field enhancement mode ultraviolet photodetector based on four-element alloy of BeZnOS, the detector includes m face sapphire substrate, active layer, a pair of parallel metal electrode from bottom to top in proper order, wherein: the active layer is a BeZnOS quaternary alloy film with an m surface, and the parallel metal electrodes are perpendicular to the c-axis direction of the BeZnOS quaternary alloy film.
Further, according to the technical scheme, the thickness of the m-plane sapphire substrate is 0.35-0.45 mm.
Further, according to the technical scheme, the thickness of the active layer is 80-160 nm.
Further, according to the technical scheme, the thickness of the parallel metal electrodes is 30-60 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 Au, Ag, or Al, and is preferably Al.
The invention also aims to provide a preparation method of the spontaneous polarization field enhanced ultraviolet light detector based on the BeZnOS quaternary alloy, which 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 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 an m-surface BeZnOS quaternary alloy film;
(3) determining the c-axis direction of the m-surface BeZnOS quaternary alloy film prepared in the step (2) by using a four-circle single crystal X-ray diffractometer XRD;
(4) and (3) manufacturing a pair of parallel metal electrodes on the surface of the BeZnOS quaternary alloy film in the direction vertical to the c axis by using an evaporation method or a photoetching method to obtain the spontaneous polarization field enhanced ultraviolet detector based on the BeZnOS quaternary alloy.
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, in the technical scheme, the m-surface BeZnOS quaternary alloy film in the step (2) is prepared by a pulse laser ablation deposition method, and the specific process is as follows:
and (2) using BeZnOS ceramic as a target material, controlling the substrate temperature to be 100-800 ℃, controlling the Pulse laser energy to be 200-600 mJ/Pulse and the oxygen pressure to be 0-10 Pa, and depositing on the surface of the m-surface sapphire substrate pretreated in the step (1) to form a BeZnOS quaternary alloy film.
Further, in the above technical scheme, the bezmos ceramic target material in step (2) is prepared by a solid-phase sintering method, which specifically comprises the following steps:
(a) the molar ratio of the components is 99: 1-70: 30, uniformly mixing ZnS and BeO 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) and (3) in an argon atmosphere, taking sulfur powder as a deoxidant, placing the wafer obtained in the step (b) into a vacuum tube furnace, and firing for 2-5 h at 1100-1400 ℃ to obtain the BeZnOS ceramic.
Furthermore, in the above technical scheme, the temperature of the vacuum drying oven in the step (b) is 110 ℃, and the drying time is 10 hours.
The parallel electrode of the MSM ultraviolet light detector provided by the invention is vertical to the c-axis direction of the thin film crystal so as to obtain the enhancement effect of the spontaneous polarization field.
The principle of the invention is as follows:
according to the invention, after Be and S jointly substitute ZnO, the two atoms are complementary, so that the doping of the two atoms can Be simultaneously promoted, and the crystal quality and the band gap regulation range of the alloy can Be more simply and effectively improved.
The method comprises the steps of firstly depositing a BeZnOS film on a m-plane sapphire substrate by using a pulse laser deposition method. The film obtained at this time is BeZnOS with m-plane orientation, has no polarity on the surface, and is used as an active layer of a detector. For the BeZnOS with m-plane orientation, the c axis is parallel to the surface of the film, the polarity exists along the c axis direction of the film crystal, and when parallel metal electrodes are evaporated on the surface of the film in the direction vertical to the c axis of the crystal, a spontaneous polarization electric field parallel to the surface exists inside the film, namely an active layer. When the detector works under an external electric field, when the direction of the external electric field is consistent with the direction of a spontaneous polarization field in the film, the separation and transportation of photon-generated carriers can be accelerated by the superposition of the two fields, so that the response speed and the detection capability of the photoelectric detector are improved.
The invention has the beneficial effects that:
1. by using the BeZnOS quaternary ZnO alloy wide bandgap semiconductor material for the photoelectric detector, better film crystallization quality can be obtained, and lower detection cut-off wavelength can be obtained.
2. An epitaxial m-surface BeZnOS film is grown on a single crystal m-surface sapphire, a metal electrode vertical to the c axis of the film is evaporated, the separation and transmission of photon-generated carriers are enhanced by fully utilizing the superposition effect of a spontaneous polarization electric field and an external electric field, and the optical detection capability is enhanced.
3. The BeZnOS quaternary ZnO alloy semiconductor material can be grown by adopting various methods such as conventional pulse laser ablation deposition, magnetron sputtering, electron beam evaporation and the like, the electrode material can adopt metal aluminum, gold, silver and the like, and the shape of the electrode and the width of a channel can be freely adjusted and optimized. The electrode of the invention can be made by vapor deposition or photolithography. The evaporation method has simple process and is convenient for large-scale preparation; the photolithography is very useful for the development of high-precision, micro-scale devices.
4. The ultraviolet light detector with the MSM structure has the advantages of simple structure, simple manufacturing process and low raw material cost, and the detector prepared by the invention has good detection capability on ultraviolet light with the wavelength of 300nm, and has the advantages of high response speed, small dark current and stable performance.
Drawings
FIG. 1 is a schematic structural diagram of a spontaneous polarization field enhanced ultraviolet light detector based on a BeZnOS quaternary alloy of the present invention;
FIG. 2 is an I-V curve of a spontaneous polarization enhanced photodetector obtained in example 1 of the present invention;
FIG. 3 is a graph of the response rate of a spontaneous polarization enhanced photodetector made in example 1 of the present invention;
FIG. 4 is an I-V curve of a spontaneous polarization enhanced photodetector obtained in example 2 of the present invention;
FIG. 5 is a graph of the response rate of a spontaneous polarization enhanced photodetector made in example 2 of the present invention;
FIG. 6 is an I-V curve of a non-spontaneous-polarization enhanced photodetector obtained in example 3 of the present invention;
FIG. 7 is a graph of the response rate of a non-spontaneous-polarization enhanced photodetector obtained in example 3 of the present invention;
FIG. 8 shows the results of the spectral responsivity test of the spontaneous polarization enhanced photodetector obtained in example 2 of the present invention.
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 contains oxygen as a main componentAluminium (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 detector of the present embodiment based on a BeZnOS quaternary alloy and having a spontaneous polarization field enhancement type ultraviolet light detector sequentially includes, from bottom to top, an m-plane sapphire substrate, an active layer, and a pair of parallel metal Al electrodes, where: the active layer is a BeZnOS quaternary alloy film with an m surface, and the parallel metal electrodes are perpendicular to the c-axis direction of the BeZnOS quaternary alloy film. The thickness of the substrate is 0.43mm, the thickness of the active layer is 120nm, the thickness of the Al electrode is 50nm, and the distance between the parallel electrodes is 10 microns.
The spontaneous polarization field enhanced ultraviolet detector based on the BeZnOS quaternary alloy is prepared by the following method, and comprises the following steps:
step 1: BeZnOS quaternary ceramic target material prepared by adopting solid-phase sintering method
1.1 by molar ratio ZnS: BeO 95: weighing 55.558g of ZnS powder and 7.504g of BeO powder, mixing, adding 39g of deionized water, placing in a ball milling tank (zirconia ceramic balls are used as a ball milling medium) in a planetary ball mill, and 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 10h at the temperature of 110 ℃, taking out, naturally cooling to room temperature, screening out zirconia balls, adding 6g of ethanol, fully and uniformly grinding by using a mortar grinding machine, 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 10M Pa;
1.3 the slab was placed in a crucible in a vacuum tube furnace, and around it was placed a powder (15.0000g) of the same composition and a high purity sulfur powder (3.3000 g). And (4) vacuumizing the vacuum tube furnace to 0.1Pa, introducing high-purity argon, and repeating for 3 times. And (3) heating the tube furnace to 1300 ℃ under the protective atmosphere, preserving the temperature for 2h, and naturally cooling to room temperature to obtain the BeZnOS quaternary ceramic target material.
Step 2: preparation of ultraviolet light detector by using BeZnOS quaternary ceramic target material
2.1 taking the BeZnOS quaternary ceramic target material prepared in the step 1 as a laser ablation target material, loading the laser ablation target material and a substrate which is respectively subjected to ultrasonic cleaning for 15min by acetone, absolute ethyl alcohol, deionized water and the like into a vacuum chamber, and vacuumizing to 10 DEG-4Pa；
2.2 starting the substrate to heat, adjusting the temperature of the substrate to 700 ℃, and introducing oxygen to ensure that the air pressure is maintained at 2Pa 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 400mJ/pulse, setting the pulse repetition frequency to be 5Hz, starting laser deposition for 30min, then closing oxygen and substrate heating, and finally naturally cooling the sample to room temperature in vacuum and taking out the sample from the vacuum chamber;
2.3 the c-axis direction of the film was determined by XRD scanning and marked on the back of the sample. Installing the film and the mask plate in a vacuum cavity of a vacuum evaporation machine, enabling an electrode channel to be vertical to a c axis of a sample, placing a tungsten boat in an evaporation source, namely 0.2g of metal aluminum, closing the vacuum cavity, starting a mechanical pump, a front-stage valve and a molecular pump, and pumping the vacuum degree to 10-4Pa. And (3) starting an evaporation power supply after reaching the vacuum degree, keeping the temperature at 400 ℃ for 2min, slowly increasing the current until the current is kept constant after the metal aluminum is melted, opening a baffle plate until the metal is evaporated, slowly reducing the current, closing an evaporation source, closing a molecular pump, a front-stage valve and a mechanical pump, and opening an air valve to obtain the target MSM ultraviolet detector.
A voltage of 10V was applied between the electrodes of the device fabricated in this example to conduct a photoelectric test. The result shows that the device has obvious detection capability and quick response speed to ultraviolet light. Fast response time tau of devicer1And τd1Respectively at 0.28s and 0.11s, and the test results are shown in fig. 2 and fig. 3, respectively.
Example 2
The utility model provides a spontaneous polarization field enhancement mode ultraviolet photodetector based on four-element alloy of BeZnOS, the detector includes m face sapphire substrate, active layer, a pair of parallel metal Al electrode from supreme down in proper order, wherein: the active layer is a BeZnOS quaternary alloy film with an m surface, and the parallel metal electrodes are perpendicular to the c-axis direction of the BeZnOS quaternary alloy film. The thickness of the substrate is 0.43mm, the thickness of the active layer is 90nm, the thickness of the electrode is 55nm, and the distance between the parallel electrodes is 10 mu m.
The spontaneous polarization field enhanced ultraviolet detector based on the BeZnOS quaternary alloy is prepared by the following method, and comprises the following steps:
step 1: BeZnOS quaternary ceramic target material prepared by adopting solid-phase sintering method
1.1 by molar ratio ZnS: BeO 85: weighing 49.710g of ZnS powder and 22.511g of BeO powder, mixing, adding 36g of deionized water, placing in a ball milling tank (zirconia ceramic balls are used as a ball milling medium) in a planetary ball mill, and 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 10h at the temperature of 110 ℃, taking out, naturally cooling to room temperature, screening out zirconia balls, adding 6g of ethanol, fully and uniformly grinding by using a mortar grinding machine, 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 10M Pa;
1.3 the slab was placed in a crucible in a vacuum tube furnace, and around it was placed a powder (15.0000g) of the same composition and a high purity sulfur powder (3.3000 g). And (4) vacuumizing the vacuum tube furnace to 0.1Pa, introducing high-purity argon, and repeating for 3 times. And (3) heating the tube furnace to 1200 ℃ under the protective atmosphere, preserving the temperature for 5h, and naturally cooling to room temperature to obtain the BeZnOS quaternary ceramic target material.
Step 2: preparation of ultraviolet light detector by using BeZnOS quaternary ceramic target material
2.1 taking the BeZnOS quaternary ceramic target material prepared in the step 1 as a laser ablation target material, loading the laser ablation target material and a substrate which is respectively subjected to ultrasonic cleaning for 15min by acetone, absolute ethyl alcohol, deionized water and the like into a vacuum chamber, and vacuumizing to 10 DEG-4Pa；
2.2 starting the substrate to heat, adjusting the temperature of the substrate to 400 ℃, and 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 250mJ/pulse, setting the pulse repetition frequency to be 5Hz, starting laser deposition for 60min, then closing oxygen and substrate heating, and finally naturally cooling the sample to room temperature in vacuum and taking out the sample from the vacuum chamber;
2.3 the sample obtained in the step 2 is scanned by XRD to determine the c-axis direction of the film, and the back of the sample is marked. And (3) mounting the film and the interdigital electrode mask plate in a vacuum cavity of a vacuum evaporation machine, so that an electrode channel is vertical to the c axis of the sample. Installing tungsten boat, putting into evaporation source-metal aluminum 0.2g, closing vacuum chamber, starting mechanical pump, front valve and molecular pump, pumping vacuum to 10 degree- 4Pa. And (3) starting an evaporation power supply after the vacuum degree is reached, increasing the current to the state that the metal aluminum is melted at the speed of 100A/min, opening a baffle plate until the metal is evaporated, slowly reducing the current, closing an evaporation source, closing a molecular pump, a pre-stage valve and a mechanical pump, and opening an air valve. The instrument was closed and the sample removed.
A voltage of 10V was applied between the electrodes of the device fabricated in this example to conduct a photoelectric test. The result shows that the device has obvious detection capability and quick response speed to ultraviolet light. Fast response time tau of devicer1And τd1Respectively 0.19s and 0.21s, and the response wave band is in the ultraviolet region, and the test results are respectively shown in fig. 4, fig. 5 and fig. 8.
Example 3 (comparative example)
The utility model provides a there is not spontaneous polarization field enhancement mode ultraviolet photodetector based on four-element alloy of BeZnOS, the detector includes m face sapphire substrate, active layer, a pair of parallel metal Al electrode from supreme down in proper order, wherein: the active layer is a BeZnOS quaternary alloy film with an m surface, and the parallel metal electrodes are parallel to the c-axis direction of the BeZnOS quaternary alloy film. The thickness of the substrate is 0.43mm, the thickness of the active layer is 90nm, the thickness of the electrode is 60nm, and the distance between the parallel electrodes is 10 microns.
The above-mentioned no-spontaneous-polarization-field enhanced ultraviolet light detector based on the BeZnOS quaternary alloy of this embodiment is prepared by the following method, including the following steps:
step 1: BeZnOS quaternary ceramic target material prepared by adopting solid-phase sintering method
1.1 by molar ratio ZnS: BeO 92: weighing 53.803g of ZnS powder and 18.065g of BeO powder, mixing, adding 39g of deionized water, placing in a ball milling tank (zirconia ceramic balls are used as a ball milling medium) in a planetary ball mill, and 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 10h at the temperature of 110 ℃, taking out, naturally cooling to room temperature, screening out zirconia balls, adding 6g of ethanol, fully and uniformly grinding by using a mortar grinding machine, 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 10M Pa;
1.3 the slab was placed in a crucible in a vacuum tube furnace, and around it was placed a powder (15.0000g) of the same composition and a high purity sulfur powder (3.3000 g). And (4) vacuumizing the vacuum tube furnace to 0.1Pa, introducing high-purity argon, and repeating for 3 times. And (3) heating the tube furnace to 1300 ℃ under the protective atmosphere, preserving the temperature for 2h, and naturally cooling to room temperature to obtain the BeZnOS quaternary ceramic target material.
Step 2, preparing the ultraviolet detector by using the BeZnOS quaternary ceramic target material
2.1 taking the BeZnOS quaternary ceramic target material prepared in the step 1 as a laser ablation target material, loading the laser ablation target material and a substrate which is respectively subjected to ultrasonic cleaning for 15min by acetone, absolute ethyl alcohol, deionized water and the like into a vacuum chamber, and vacuumizing to 10 DEG-4Pa；
2.2 starting the substrate to heat, adjusting the temperature of the substrate to 400 ℃, and 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 400mJ/pulse, the pulse repetition frequency to be 5Hz and the number of pulses to be 9000, starting laser deposition for 30min, then closing oxygen and substrate heating, and finally naturally cooling the sample to room temperature in vacuum and taking out the sample from the vacuum chamber;
2.3 using four-circle single crystal XRD to scan the (103) plane of the sample obtained in the step 2, determining the c direction of the sample and marking. Installing a sample and a mask plate to enable an electrode to be parallel to a c axis, installing a tungsten boat, then placing an evaporation source, namely 0.3g of metal aluminum, into the tungsten boat, closing a vacuum cavity, starting a mechanical pump, a front-stage valve and a molecular pump, and pumping the vacuum cavity to 10 degrees-4Pa. After reaching the vacuum degree, the evaporation power supply is started at the speed of 100A/minAnd increasing the current until the metal aluminum is melted, opening the baffle plate until the metal is evaporated, slowly reducing the current, closing the evaporation source, closing the molecular pump, the pre-stage valve and the mechanical pump, and opening the air valve. And (5) closing the instrument after the vacuum cavity is filled with air, and taking out the sample to obtain the target light detector.
A voltage of 10V was applied between the electrodes of the device fabricated in this example to conduct a photoelectric test. The result shows that the device has a slower response speed to ultraviolet light relative to a spontaneous polarization field enhanced detector. Fast response time tau of devicer1And τd1Respectively at 0.30s and 0.46s, and the test results are shown in fig. 6 and fig. 7, respectively.
Example 4
The spontaneous polarization field enhancement type ultraviolet light detector based on the BeZnOS quaternary alloy comprises an m-plane sapphire substrate, an active layer and a pair of parallel metal Au electrodes from bottom to top in sequence, wherein: the active layer is a BeZnOS quaternary alloy film with an m surface, and the parallel metal electrodes are perpendicular to the c-axis direction of the BeZnOS quaternary alloy film. The thickness of the substrate is 0.43mm, the thickness of the active layer is 80nm, the thickness of the electrode is 30nm, and the distance between the parallel electrodes is 30 μm.
The spontaneous polarization field enhanced ultraviolet detector based on the BeZnOS quaternary alloy is prepared by the following method, and comprises the following steps:
step 1: the same solid-phase sintering method as in example 1 was used to prepare a bezmos quaternary ceramic target.
Step 2, preparing the ultraviolet detector by using the BeZnOS quaternary ceramic target material
2.1 taking the BeZnOS quaternary ceramic target material prepared in the step 1 as a laser ablation target material, loading the laser ablation target material and a substrate which is respectively subjected to ultrasonic cleaning for 15min by acetone, absolute ethyl alcohol, deionized water and the like into a vacuum chamber, and vacuumizing to 10 DEG-4Pa；
2.2 starting the substrate to heat, adjusting the temperature of the substrate to 100 ℃, and introducing oxygen to ensure that the air pressure is maintained at 8Pa 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 200mJ/pulse, setting the pulse repetition frequency to be 5Hz, starting laser deposition for 10min, then closing oxygen and substrate heating, and finally naturally cooling the sample to room temperature in vacuum and taking out the sample from the vacuum chamber;
2.3 the c-axis direction of the film was determined by XRD scanning and marked on the back of the sample. Installing the film and the mask plate in a vacuum cavity of a vacuum evaporation machine, enabling an electrode channel to be vertical to a c axis of a sample, placing an evaporation source, namely metal Au0.2g, after installing a tungsten boat, closing the vacuum cavity, starting a mechanical pump, a front-stage valve and a molecular pump, and pumping the vacuum degree to 10-4Pa. And (3) starting an evaporation power supply after reaching the vacuum degree, keeping the temperature at 400 ℃ for 2min, slowly increasing the current until the current is kept constant after the metal Au is melted, opening a baffle plate until the metal is evaporated, slowly reducing the current, closing an evaporation source, closing a molecular pump, a pre-stage valve and a mechanical pump, and opening an air valve to obtain the target MSM ultraviolet detector.
Example 5
The spontaneous polarization field enhancement type ultraviolet light detector based on the BeZnOS quaternary alloy comprises an m-plane sapphire substrate, an active layer and a pair of parallel metal Pt electrodes from bottom to top in sequence, wherein: the active layer is a BeZnOS quaternary alloy film with an m surface, and the parallel metal electrodes are perpendicular to the c-axis direction of the BeZnOS quaternary alloy film. The thickness of the substrate is 0.43mm, the thickness of the active layer is 160nm, the thickness of the electrode is 30nm, and the distance between the parallel electrodes is 60 mu m.
The above-mentioned spontaneous polarization field enhanced ultraviolet light detector based on the BeZnOS quaternary alloy of this embodiment is prepared by the following method, including the following steps:
step 1: the same solid-phase sintering method as in example 1 was used to prepare a bezmos quaternary ceramic target.
Step 2, preparing the ultraviolet detector by using the BeZnOS quaternary ceramic target material
2.1 taking the BeZnOS quaternary ceramic target material prepared in the step 1 as a laser ablation target material, loading the laser ablation target material and a substrate which is respectively subjected to ultrasonic cleaning for 15min by acetone, absolute ethyl alcohol, deionized water and the like into a vacuum chamber, and vacuumizing to 10 DEG-4Pa；
2.2 starting the substrate to heat, adjusting the temperature of the substrate to 800 ℃, and introducing oxygen to ensure that the air pressure is maintained at 10Pa 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, setting the pulse repetition frequency to be 5Hz, starting laser deposition for 40min, then closing oxygen and substrate heating, and finally naturally cooling the sample to room temperature in vacuum and taking out the sample from the vacuum chamber;
2.3 the c-axis direction of the film was determined by XRD scanning and marked on the back of the sample. Installing the film and the mask plate in a vacuum cavity of a vacuum evaporation machine, enabling an electrode channel to be vertical to a c axis of a sample, placing a tungsten boat in an evaporation source, namely metal Ag0.2g, closing the vacuum cavity, starting a mechanical pump, a front-stage valve and a molecular pump, and pumping the vacuum degree to 10-4Pa. And (3) starting an evaporation power supply after reaching the vacuum degree, keeping the temperature at 400 ℃ for 2min, slowly increasing the current until the current is constant after the metal Ag is melted, opening a baffle plate until the metal is evaporated, slowly reducing the current, closing an evaporation source, closing a molecular pump, a pre-stage valve and a mechanical pump, and opening an air valve to obtain the target MSM ultraviolet detector.
Claims (9)
1. A spontaneous polarization field enhancement type ultraviolet detector based on a BeZnOS quaternary alloy is 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 a BeZnOS quaternary alloy film with an m surface, and the parallel metal electrodes are perpendicular to the c-axis direction of the BeZnOS quaternary alloy film.
2. The BeZnOS quaternary alloy-based spontaneous polarization field enhanced ultraviolet light detector as claimed in claim 1, wherein: the thickness of the m-plane sapphire substrate is 0.35-0.45 mm.
3. The BeZnOS quaternary alloy-based spontaneous polarization field enhanced ultraviolet light detector as claimed in claim 1, wherein: the thickness of the active layer is 80-160 nm.
4. The BeZnOS quaternary alloy-based spontaneous polarization field enhanced ultraviolet light detector as claimed in claim 1, wherein: the thickness of the parallel metal electrode is 30-60 nm.
5. The BeZnOS quaternary alloy-based spontaneous polarization field enhanced ultraviolet light detector as claimed in claim 1, wherein: the distance between the parallel metal electrodes is 10-100 mu m.
6. The BeZnOS quaternary alloy-based spontaneous polarization field enhanced ultraviolet light detector as claimed in claim 1, wherein: the parallel metal electrode material may be any one of Au, Ag, or Al.
7. The method for preparing the spontaneous polarization field enhanced ultraviolet light detector based on the BeZnOS quaternary alloy as claimed in claim 1, wherein: 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 a m-surface BeZnOS quaternary alloy film 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;
(3) determining the c-axis direction of the m-surface BeZnOS quaternary alloy film prepared in the step (2) by using a four-circle single crystal X-ray diffractometer;
(4) and forming a pair of parallel metal electrodes on the surface of the BeZnOS quaternary alloy film in the direction vertical to the c axis by using an evaporation method or a photoetching method to obtain the spontaneous polarization field enhanced ultraviolet detector based on the BeZnOS quaternary alloy.
8. The method for preparing the spontaneous polarization field enhanced ultraviolet light detector based on the BeZnOS quaternary alloy as claimed in claim 7, wherein: the m-surface BeZnOS quaternary alloy film in the step (2) is prepared by adopting a pulse laser ablation deposition method, and the specific process is as follows:
and (2) using BeZnOS ceramic as a target material, controlling the substrate temperature to be 100-800 ℃, controlling the Pulse laser energy to be 200-600 mJ/Pulse and the oxygen pressure to be 0-10 Pa, and depositing on the surface of the m-surface sapphire substrate pretreated in the step (1) to form a BeZnOS quaternary alloy film.
9. The method for preparing the spontaneous polarization field enhanced ultraviolet light detector based on the BeZnOS quaternary alloy as claimed in claim 8, wherein: the BeZnOS 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 99: 1-70: 30, uniformly mixing ZnS and BeO 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) and (3) in an argon atmosphere, taking sulfur powder as a deoxidant, placing the wafer obtained in the step (b) into a vacuum tube furnace, and firing for 2-5 h at 1100-1400 ℃ to obtain the BeZnOS ceramic.
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