CN115274891A - Vacuum ultraviolet photoelectric detector and preparation method thereof - Google Patents
Vacuum ultraviolet photoelectric detector and preparation method thereof Download PDFInfo
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- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/0304—Inorganic materials including, apart from doping materials or other impurities, only AIIIBV compounds
- H01L31/03044—Inorganic materials including, apart from doping materials or other impurities, only AIIIBV compounds comprising a nitride compounds, e.g. GaN
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- H01L31/101—Devices sensitive to infrared, visible or ultraviolet radiation
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- 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
The invention discloses a vacuum ultraviolet photoelectric detector and a preparation method thereof, wherein the preparation method comprises the following steps: preparing an aluminum nitride crystal by adopting a physical vapor transport method; preparing a substrate, and depositing and forming a bottom electrode on the surface of the substrate; placing the aluminum nitride crystal on the bottom electrode; transferring the prepared graphene onto the aluminum nitride crystal; and depositing to form a top electrode on the upper area of the graphene. The vacuum ultraviolet photoelectric detector is manufactured on the basis of the aluminum nitride crystal, the aluminum nitride crystal is manufactured by adopting a physical vapor transport method, a substrate for bearing the growth of the aluminum nitride crystal is not needed in the process of manufacturing the vacuum ultraviolet detector, the production cost is reduced, the selectivity of a bottom electrode is increased, and meanwhile, graphene is used as a transparent window to increase the photosensitive area.
Description
Technical Field
The invention relates to the technical field of photoelectric detection, in particular to a vacuum ultraviolet photoelectric detector and a preparation method thereof.
Background
Ultraviolet detection has wide application in the fields of military, civil and scientific research, such as fire detection, missile tracking, environment monitoring, biological detection, ultraviolet astronomy, ultraviolet communication and the like, and is increasingly emphasized. Vacuum ultraviolet (VUV, vacuum Ultra-Violet) refers to the ultraviolet spectrum with a wavelength of less than 200 nm. Due to strong absorption of the atmosphere, vacuum deep ultraviolet electromagnetic radiation belongs to the ultraviolet region of solar blindness, does not exist in human society in a natural state, and signal detection of the vacuum deep ultraviolet electromagnetic radiation has natural low background noise conditions.
The aluminum nitride material has an ultra-wide electronic band gap of 6.2eV, corresponds to a vacuum ultraviolet wavelength of about 200nm, and is an excellent photosensitive material for vacuum ultraviolet detection. In recent years, vacuum ultraviolet detectors based on aluminum nitride have also been developed, but aluminum nitride films have been obtained mainly using epitaxial methods. Thus, there are problems in that the cost is high and the device structure is limited.
Disclosure of Invention
The invention mainly aims to provide a vacuum ultraviolet photoelectric detector and a preparation method thereof, and aims to solve the problems of high preparation cost and limited device structure of the conventional vacuum ultraviolet photoelectric detector.
In order to achieve the above object, the present invention provides a method for manufacturing a vacuum ultraviolet photodetector, the method comprising:
preparing an aluminum nitride crystal by adopting a physical vapor transport method;
preparing a substrate, and depositing and forming a bottom electrode on the surface of the substrate;
placing the aluminum nitride crystal on the bottom electrode;
transferring the prepared graphene onto the aluminum nitride crystal;
and depositing to form a top electrode in the upper area of the graphene.
Alternatively, the temperature range for preparing the aluminum nitride crystal is 1900-2300 ℃.
Optionally, the morphology of the aluminum nitride crystals comprises at least one of nanowires, microwires, nanosheets, and bulk crystals.
Optionally, the substrate is made of at least one of an electronic glass substrate, sapphire, silicon dioxide, plastic and quartz plate.
Optionally, the bottom electrode is made of metal, graphene or indium tin oxide.
Optionally, the top electrode is made of metal or indium tin oxide.
Optionally, the graphene is chemical vapor deposition grown graphene or mechanically exfoliated graphene.
Optionally, the chemical vapor deposition method-grown graphene is attached to a metal substrate, and the step of transferring the prepared graphene onto the aluminum nitride crystal includes:
spin-coating a high polymer material on the surface of the graphene;
soaking the spin-coated graphene in an acid solution to remove the metal substrate;
transferring the graphene with the metal substrate removed to the surface of the aluminum nitride crystal in deionized water;
and sequentially soaking the aluminum nitride crystal with the graphene and the high polymer material attached to the surface in an organic solvent and deionized water, and removing the high polymer material on the surface of the graphene.
Optionally, after the step of removing the polymer material on the surface of the graphene, the method further includes:
and etching the graphene by a photoetching method so that the coverage area of the graphene and the aluminum nitride crystal is smaller than or equal to the surface area of the aluminum nitride crystal.
In addition, in order to achieve the above object, the present invention further provides a vacuum ultraviolet photodetector, which is prepared by using the preparation method of the vacuum ultraviolet photodetector described above; the vacuum ultraviolet photoelectric detector comprises a substrate, and a bottom electrode, an aluminum nitride crystal, graphene and a top electrode which are arranged on the surface of one side of the substrate.
The vacuum ultraviolet photoelectric detector is prepared by adopting the aluminum nitride crystal, the band gap of the energy band is wide, the vacuum ultraviolet selective detection is adapted, an optical filtering component is not needed, and compared with an epitaxial method for growing the aluminum nitride or aluminum gallium nitrogen film, the aluminum nitride crystal can be obtained without a gallium nitride substrate layer, the aluminum nitride crystal can be transferred to the substrate made of most materials and subjected to multi-surface processing, and the production cost is reduced.
Drawings
Fig. 1 is a schematic flow chart of a method for manufacturing a vacuum ultraviolet photodetector according to an embodiment of the present invention;
FIG. 2 is a Raman spectrum test chart of an aluminum nitride crystal prepared by a PVT method in an embodiment of the present invention;
FIG. 3 is a schematic view of the coverage of graphene and aluminum nitride crystals according to an embodiment of the present invention;
fig. 4 is a schematic structural diagram of a vacuum ultraviolet photodetector according to an embodiment of the present invention;
FIG. 5 is a graph of the spectrum selective characteristics of a vacuum ultraviolet photodetector according to an embodiment of the present invention;
FIG. 6 is a graph of current versus voltage for a vacuum ultraviolet photodetector with VUV illumination and off in accordance with an embodiment of the present invention;
FIG. 7 is a graph of current versus time for VUV light and when the vacuum UV photodetector is turned off in accordance with an embodiment of the present invention;
FIG. 8 is a graph showing the transient time response of a vacuum ultraviolet photodetector under 10 ns single pulse VUV light in accordance with an embodiment of the present invention.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that, if directional indications (such as up, down, left, right, front, and back 21398) are involved in the embodiment of the present invention, the directional indications are only used to explain the relative position relationship between the components, the motion situation, and the like in a specific posture (as shown in the drawing), and if the specific posture is changed, the directional indications are changed accordingly.
In addition, if there is a description of "first", "second", etc. in an embodiment of the present invention, the description of "first", "second", etc. is for descriptive purposes only and is not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of the feature. In addition, the expression "and/or" as used throughout is meant to encompass three juxtaposed aspects, exemplified by "A and/or B" and encompasses either A aspect, or B aspect, or both A and B aspects. Technical solutions between various embodiments may be combined with each other, but must be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
The embodiment of the invention provides a preparation method of a vacuum ultraviolet photoelectric detector, and with reference to fig. 1, the method comprises the following steps:
step S10, preparing an aluminum nitride crystal by adopting a physical vapor transport method;
the forbidden band width of aluminum nitride (AlN) can reach 6.2eV, and the AlN has the characteristics of high thermal conductivity and the like, has strong absorption on light with the wavelength of less than 200nm, and can be applied to vacuum ultraviolet detection. PVT (Physical Vapor Transport) is a method in which a material is sublimated in a high-temperature region, then transported to a condensation region to be saturated Vapor, and condensed and nucleated to grow crystals.
In the production of aluminum nitride crystals, it is necessary to undergo steps of raw material purification and crystal growth. In the purification of the raw material, an aluminum nitride powder having a purity of 99.7% was used as the raw material, and the raw material was placed in a resistance-heated tungsten growth furnace. Charging N with purity more than 99.999% into the growth furnace2And performing purification treatment for multiple times within the temperature gradient ranges of 1600-1750 ℃, 1750-2000 ℃ and 2000-2150 ℃ respectively to remove impurities such as C, O and the like in the aluminum nitride raw material, improve the purity of the aluminum nitride raw material and enable the aluminum nitride raw material to meet the purity requirement of crystal growth.
When crystal growth is carried out, the crystal growth is carried outPutting the purified aluminum nitride raw material into a growth chamber, and vacuumizing the growth chamber to 10 DEG- 4Less than Pa, and N with purity greater than 99.999%2Heating to 0.8-1.2 atm at 10-20 deg.c/min from room temperature to 1900-2300 deg.c, maintaining for 5 hr, and cooling naturally.
The aluminum nitride crystal prepared by the method of the embodiment comprises different sizes and shapes of nano-wires, micron-wires, nano-sheets, micron-sheets, bulk crystals and the like, and can be used for manufacturing vacuum ultraviolet photoelectric detectors.
FIG. 2 is a Raman (Raman) spectrum test chart of the aluminum nitride crystal prepared by the PVT method, and it can be seen from FIG. 2 that the Raman spectrum test result is identical to h-phase AlN, and the Raman phonon is relatively sharp, which shows that the crystal has good crystallization quality. Aluminum nitride is a tetrahedrally coordinated compound with a hexagonal wurtzite crystal structure, and due TO the fact that polar lattice vibration is accompanied by a macroscopic electric field, long-range electrostatic force generated by the compound causes polar optical modes A1 and E1 phonons with Raman activity TO split into a longitudinal phonon mode (LO) and a transverse phonon mode (TO), namely A1 (TO), A1 (LO), E1 (TO) and E1 (LO), respectively. E2 represents the nonpolar optical mode of Raman activity. The optical phonon mode corresponding to the Raman shift of the Raman scattering peak in fig. 2 can be expressed as: e2 (low) 252cm-1、A1(TO)614cm-1、E2(high)658cm-1、E1(TO)672cm-1、E1(LO)912cm-1. The intensity is expressed in a.u. (atomic units).
Step S20, preparing a substrate, and depositing and forming a bottom electrode on the surface of the substrate;
the substrate material can be selected from electronic glass substrate, sapphire (Al)2O3) At least one of silicon dioxide, plastic and quartz plate, the present embodiment uses an electronic glass substrate as a substrate. Alternative materials for the bottom electrode include metals, graphene or Indium Tin Oxide (ITO). The metal material for preparing the bottom electrode can be Au, cr, ag or Cu. The Cr-Au bottom electrode can be formed on the electronic glass substrate by thermal evaporation deposition.
Step S30, placing the aluminum nitride crystal on the bottom electrode;
and placing the aluminum nitride crystal prepared by the PVT method on the bottom electrode formed by deposition, wherein the aluminum nitride crystal covers part of the surface of the bottom electrode, and the uncovered part of the bottom electrode is used for circuit connection.
S40, transferring the prepared graphene to the aluminum nitride crystal;
graphene (Graphene) may be selected from single layer Graphene or multilayer Graphene. The prepared graphene may be chemical vapor deposition grown graphene or mechanically exfoliated graphene. Graphene grown by chemical vapor deposition may be attached to a metal substrate or a non-metal substrate. Graphene formed by CVD (Chemical Vapor Deposition) growth on a copper substrate may be selected, and specifically, graphene has a single-layer structure. The VUV transmittance of the graphene can reach 96%, and the light-sensitive window is large.
The copper-based single-layer graphene may be trimmed to a suitable size prior to transferring the copper-based single-layer graphene, such that the copper-based single-layer graphene may cover a majority of the aluminum nitride crystal. Specifically, copper-based single-layer graphene can be tailored to a size of 1cm by 1cm in area.
The graphene transfer can be performed by wet transfer, and the specific steps can include:
step a, spin-coating a high polymer material on the surface of graphene. Specifically, the polymer material is spin-coated on the surface of one side of the graphene. The polymer material used may be PMMA (polymethyl methacrylate). The spin coating speed is 2000r/min, and the spin coating time is 60s.
And b, soaking the spin-coated graphene in an acid solution, and removing the metal substrate. The heating table can be used for heating the copper-based single-layer graphene, wherein the heating temperature is 80 ℃, and the heating time is 2h. And soaking the heated copper-based single-layer graphene in an ammonium persulfate solution, and removing the copper substrate to obtain the single-layer graphene/PMMA, wherein the PMMA is positioned on one side of the single-layer graphene, which is far away from the copper substrate.
And c, transferring the graphene with the metal substrate removed to the surface of the aluminum nitride crystal in deionized water. Transferring the single-layer graphene/PMMA without the copper substrate to the surface of an aluminum nitride crystal in deionized water, fishing out the aluminum nitride crystal, heating the aluminum nitride crystal on a heating table at the temperature of 80 ℃ for 2 hours to obtain dry AlN crystal/single-layer graphene/PMMA, wherein the AlN crystal and the PMMA are respectively positioned on two sides of the single-layer graphene.
And d, sequentially soaking the aluminum nitride crystal with the graphene and the high polymer material attached to the surface in an organic solvent and deionized water, and removing the high polymer material on the surface of the graphene. PMMA is a high polymer material and is easy to dissolve in an organic solvent, and the organic solvent for dissolving PMMA can be one or more of toluene, anisole, dichloromethane, acetone and N-methyl pyrrolidone. The AlN crystal/single-layer graphene/PMMA can be soaked in acetone to dissolve PMMA, then absolute ethyl alcohol and deionized water are sequentially soaked, and the dissolved AlN crystal/single-layer graphene is cleaned. In dissolving PMMA, the soaking temperature does not exceed the boiling point of the organic solvent. And removing the PMMA on one side of the surface of the graphene to finally obtain the AlN crystal/single-layer graphene. PMMA adheres to the surface of graphene and can play a role in protecting the graphene in the transfer process. And after the transfer is finished, forming a bottom electrode-AlN crystal-graphene sandwich structure.
The graphene can also be etched by using a photoetching method, so that the coverage area of the graphene and the aluminum nitride crystal is smaller than or equal to the surface area of the aluminum nitride crystal. Fig. 3 is a schematic view of coverage of graphene and aluminum nitride crystal, and as shown in fig. 3, graphene may cover a part of the surface of the aluminum nitride crystal. During the photolithography etching process, an etching template may be used, and the graphene after etching has a specific shape corresponding to the etching template. The purpose of etching the graphene is to avoid contact between the graphene and the bottom electrode.
And S50, depositing and forming a top electrode in the upper area of the graphene.
The top electrode can be made of metal or indium tin oxide and other materials with high conductivity, the top electrode and the bottom electrode are used as two ends of a vacuum ultraviolet photoelectric detector access circuit, and the vacuum ultraviolet photoelectric detector can normally work after being accessed into the circuit. The top electrode may cover a partial region of a side of the graphene facing away from the AlN crystal. The metal material for preparing the top electrode can be Au, cr, ag or Cu. A gold electrode may be formed on the upper portion of the graphene by thermal evaporation deposition, the gold electrode having a thickness of about 50nm.
In some embodiments, graphene may also be used as a top electrode, i.e., the upper region of graphene does not need to be formed with an additional top electrode.
In this embodiment, adopt aluminium nitride crystal preparation vacuum ultraviolet photoelectric detector, the band gap of energy band is wide, adapts to vacuum ultraviolet's selectivity and surveys, does not need the optical filtering part, and compares in epitaxial growth aluminium nitride or aluminium gallium nitrogen film, does not need the gallium nitride substrate layer can obtain the aluminium nitride crystal, can transfer to the substrate of most material and carry out multiaspect processing, has reduced manufacturing cost.
The embodiment of the invention also provides a vacuum ultraviolet photodetector, as shown in fig. 4, the vacuum ultraviolet photodetector includes a substrate 1, and a bottom electrode 2, an aluminum nitride crystal 3, graphene 4 and a top electrode 5 which are sequentially stacked on a surface of one side of the substrate. As can be seen in fig. 3, the bottom electrode 2 covers a part of the surface of the substrate 1. The aluminum nitride crystal 3 covers a part of the surface of the bottom electrode 2. The graphene 4 covers a part of the surface of the aluminum nitride crystal. The top electrode 5 covers a part of the surface of the graphene 4. The size of the overlapping area between the graphene 4 and the aluminum nitride crystal 3 can be controlled by cutting the copper-based single-layer graphene and photoetching the graphene later, so that the copper-based single-layer graphene can cover most of the aluminum nitride crystal, the light receiving area of the vacuum ultraviolet photoelectric detector is enlarged, and the photocurrent is increased.
The aluminum nitride crystal for manufacturing the vacuum ultraviolet photoelectric detector is prepared by using a PVT method. In contrast, the aluminum nitride films obtained by epitaxy have a large majority of substrates made of gan due to lattice mismatch and thermal adaptation problems, and the expensive price of gan leads to increased cost and less selectivity to the substrate and device structure. The aluminum nitride crystal grown by the PVT method can be transferred to any substrate and subjected to multi-surface processing, so that the production and use cost is reduced, and the structural design of the device can be better carried out.
Fig. 5 is a graph of spectral selectivity characteristics of the vacuum ultraviolet photodetector, with the abscissa representing the wavelength of light in nanometers and the left ordinate representing the responsivity of the vacuum ultraviolet photodetector, corresponding to the hollow square point data in fig. 5; the right ordinate represents the optical absorption coefficient of the aluminum nitride crystal, corresponding to the solid line data in fig. 5. As shown in fig. 5, the vacuum ultraviolet photodetector prepared by the method of the present embodiment has a maximum responsivity at a wavelength of about 200nm, which is consistent with the absorption coefficient characteristics of AlN crystal, and at the upper limit of the VUV wavelength, it indicates that it can be excited by VUV light, has a good optical response, and does not respond to long waves other than VUV, has a strong spectral selectivity, and can be used for the photodetection of vacuum ultraviolet light.
Fig. 6 is a current-voltage graph of the vacuum ultraviolet detector under VUV illumination and off, the abscissa represents voltage (V) and the ordinate represents current (a), an ArF laser with a wavelength of 193nm is used for current-voltage characteristic test, the dark current of the detector under dark state (dark) is about 0.1nA, the detector has higher photocurrent under VUV illumination, and the +80V can reach about 50 nA.
Fig. 7 is a graph of current versus time for a vacuum ultraviolet photodetector with VUV illuminated and turned off, with time(s) on the abscissa and current (a) on the ordinate. The voltage of +30V is applied to two ends of the vacuum ultraviolet detector, and the VUV light is used for carrying out current-time characteristic test, so that the current response can be seen when the illumination is started, the current is rapidly reduced when the illumination is closed, and the response to the VUV illumination can be realized.
FIG. 8 is a graph of the instantaneous time response of a vacuum ultraviolet detector under 10 nanosecond single pulse VUV light, with time (seconds) on the abscissa and current (amps) on the ordinate. The response time may be expressed in terms of the time interval during which the photocurrent is shifted from 10% to 90%. The time interval during which the photocurrent was switched from 10% to 90% corresponds to the time interval during which the detector current rose from dark current to photocurrent after the laser was turned on. The time interval during which the photocurrent is shifted from 90% to 10% corresponds to the time interval during which the detector current drops from photocurrent to dark current after the laser is turned off. And when a voltage of +30V is applied to two ends of the vacuum ultraviolet detector, the response time of the photocurrent is changed from 10% to 90% to be 2ms, the ultra-fast response speed of the detector is shown, the response time is limited by the time constant of a test circuit, and the actual response time is shorter.
Compared with a vacuum tube device based on an external photoelectric effect, the vacuum tube device based on the external photoelectric effect is based on a solid material, and is small in size, low in energy consumption, impact-resistant and free of an optical filtering component. Compared with a photoelectric detector based on the photoelectric effect in a semiconductor, the aluminum nitride used in the embodiment has a wider band gap, is more suitable for selective detection of vacuum ultraviolet rays, and does not need an optical filtering component. On the basis of cost reduction, the extremely fast response speed brings wider application prospect for the application of the vacuum ultraviolet photoelectric detector.
The above-mentioned serial numbers of the embodiments of the present invention are only for description, and do not represent the advantages and disadvantages of the embodiments.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by using the contents of the present specification and the accompanying drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A preparation method of a vacuum ultraviolet photoelectric detector is characterized by comprising the following steps:
preparing an aluminum nitride crystal by adopting a physical vapor transport method;
preparing a substrate, and depositing and forming a bottom electrode on the surface of the substrate;
placing the aluminum nitride crystal on the bottom electrode;
transferring the prepared graphene onto the aluminum nitride crystal;
and depositing to form a top electrode on the upper area of the graphene.
2. The method of claim 1, wherein the aluminum nitride crystal is prepared at a temperature ranging from 1900 ℃ to 2300 ℃.
3. The method of claim 1, wherein the aluminum nitride crystal morphology comprises at least one of nanowire, microwire, nanosheet, and bulk crystal.
4. The method of claim 1, wherein the substrate is made of at least one of electronic glass substrate, sapphire, silica, plastic, and quartz plate.
5. The method of claim 1, wherein the bottom electrode is made of metal, graphene or indium tin oxide.
6. The method of claim 1, wherein the top electrode is made of metal or indium tin oxide.
7. The method of claim 1, wherein the graphene is a chemical vapor deposition grown graphene or a mechanically exfoliated graphene.
8. The method for manufacturing a vacuum ultraviolet photodetector according to claim 7, wherein the graphene grown by the chemical vapor deposition method is attached to a metal substrate, and the step of transferring the prepared graphene onto the aluminum nitride crystal comprises:
spin-coating a high polymer material on the surface of the graphene;
soaking the spin-coated graphene in an acid solution to remove the metal substrate;
transferring the graphene with the metal substrate removed to the surface of the aluminum nitride crystal in deionized water;
and sequentially soaking the aluminum nitride crystal with the graphene and the high polymer material attached to the surface in an organic solvent and deionized water, and removing the high polymer material on the surface of the graphene.
9. The method for manufacturing a vacuum ultraviolet photodetector according to claim 8, further comprising, after the step of removing the polymer material on the surface of the graphene:
and etching the graphene by a photoetching method so that the coverage area of the graphene and the aluminum nitride crystal is smaller than or equal to the surface area of the aluminum nitride crystal.
10. A vacuum ultraviolet photodetector manufactured by the method for manufacturing a vacuum ultraviolet photodetector according to any one of claims 1 to 9; the vacuum ultraviolet photoelectric detector comprises a substrate, and a bottom electrode, an aluminum nitride crystal, graphene and a top electrode which are arranged on the surface of one side of the substrate.
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