CN109786494B - Ultraviolet detector with microcavity structure and preparation method thereof - Google Patents
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Abstract
The invention discloses a microcavity structure ultraviolet detector and a preparation method thereof, wherein the preparation process of the ultraviolet detector comprises the steps of substrate cleaning, seed crystal layer growth, micron line growth, preparation of metal films on the upper side and the lower side of a single wide bandgap semiconductor micron/nano line, preparation of metal nano particles and preparation of a detector metal electrode layer. The invention is characterized in that a high-performance and small-volume ultraviolet detector with a special structure is newly developed, the detection cut-off wavelength of the ultraviolet detector is less than 380nm, and the contradiction problem that the size reduction of the ultraviolet detector and the improvement of photoelectric conversion are difficult to realize simultaneously is solved. In addition, the ultraviolet detector with the microcavity structure has a simple structure, is easy to couple with a focal plane reading circuit, and is beneficial to the development of the next generation of high-density integrated photoelectric circuits.
Description
Technical Field
The invention belongs to the technical field of photoelectric detection, and particularly relates to a composite Fabry-Perot microcavity structure ultraviolet detector and a preparation method thereof.
Technical Field
The ultraviolet detection technology is another important civil and military photoelectric detector technology developed following the laser detection technology and the infrared detection technology. At present, the modern ultraviolet detection technology is a precise detection system integrating multiple disciplines such as an ultraviolet detector, optical design, micro-machining, an integrated circuit and the like, and has great effects in the fields of missile tail flame detection, ozone layer hole monitoring, medical detection, flame detection and the like due to the advantages of low background noise, good concealment and the like.
At present, along with the exponential improvement of the integration level of a semiconductor device in accordance with the law, the size of a photoelectric detector is also continuously reduced, but the reduction of the area of an active region can reduce the photoelectric conversion efficiency of the device, so that the detection of a weak signal and the design of a subsequent operation circuit and a reading circuit are not facilitated. Although the use of metal surface plasmon technology is an effective way to achieve high photoelectric conversion rate and small volume photodetectors (MRS ball. 2012,37, 728-738). However, due to the problems of energy matching of metal surface plasmon polariton and ultraviolet radiation, serious energy loss of an ultraviolet band and the like, the technology is mostly applied to visible and infrared bands at present.
Aiming at the technical problem, the invention provides the hybrid surface plasma microcavity structure ultraviolet detector, and the composite microcavity structure can integrate the dual advantages of interference modulation of an optical spatial layer on an electric field and forward scattering of surface plasmons, so that the extreme value of the main optical field intensity of ultraviolet radiation is distributed in an active region, and the contradiction that the size reduction of the ultraviolet detector and the improvement of the photoelectric conversion efficiency of a device are difficult to realize simultaneously is solved. In addition, the device has simple structure, is easy to couple with a focal plane reading circuit, and is beneficial to the development of the next generation of high-density integrated photoelectric circuit.
Disclosure of Invention
The invention aims to provide a hybrid surface plasma Fabry-Perot microcavity structure ultraviolet detector and a preparation method thereof, and finally the ultraviolet detector with the working wavelength less than 380nm, high performance and small volume is obtained.
The invention aims to provide a microcavity-structured ultraviolet detector as shown in the attached figure 1, which comprises the following components: the metal film comprises a metal film reflecting layer 1, a wide bandgap semiconductor micro/nano wire 2, a metal electrode layer 3 and metal nano particles 4.
The invention also aims to provide a preparation method of the ultraviolet detector with the microcavity structure.
The purpose of the invention is realized by the following technical scheme, as shown in the attached figure 2, the invention comprises the following steps:
before growing a seed crystal layer, adding sulfuric acid and hydrochloric acid in a volume ratio of 3: 1 for 5-30 minutes to remove inorganic substances attached to the surface of the substrate (the operation is not required for the substrate except sapphire), the substrate is sequentially placed into acetone, ethanol and deionized water for ultrasonic cleaning for 5-30 minutes to remove the organic substances attached to the surface of the substrate, the substrate is blown dry by nitrogen after being cleaned, and is placed into an oxygen plasma cleaning machine for treatment for 5 minutes, and the substrate is taken out for standby after the treatment is finished.
Preparing a seed crystal layer on the processed substrate.
And thirdly, fully mixing the high-purity wide-bandgap semiconductor powder with the mass ratio of 1:1 with graphite powder, and grinding for more than 2 hours. And placing the mixed powder in the middle of a ceramic boat, placing a substrate with a seed crystal layer right above the mixed powder, horizontally placing the ceramic boat into a quartz tube, and placing the quartz tube into a growth chamber of a horizontal high-temperature tube furnace to grow the quadrilateral wide-bandgap semiconductor micro/nanowire 2.
Fourthly, after the quadrilateral wide bandgap semiconductor micro/nanowire with the Fabry-Perot microcavity structure is grown, preparing the metal film 1 on the lower side of the single quadrilateral wide bandgap semiconductor micro/nanowire along the axial direction.
Preparing metal nano particles 4 with absorption peaks positioned in an ultraviolet band on the opposite side of the metal film material (namely the upper side of the quadrilateral wide bandgap semiconductor micro/nano wire), wherein the shape of the metal nano particles 4 comprises one of a sphere, an ellipsoid and a triangular prism and an irregular shape formed by the structures.
Finally, preparing metal electrode layers 3 at two ends of the single quadrilateral wide bandgap semiconductor micro/nanowire with the metal thin films and the metal nanoparticles on the upper side and the lower side.
The preparation of the wide bandgap semiconductor seed crystal layer in the second step can be realized by one or two methods of a chemical synthesis method and a magnetron sputtering method.
The growth environment of the quadrilateral wide bandgap semiconductor micro/nano-wire in the step ③ is normal pressure, carrier gas in the growth process is high-purity argon and high-purity oxygen, the geometric parameters of the single quadrilateral wide bandgap semiconductor micro/nano-wire can be adjusted by carrier gas flow, growth temperature and growth time, and finally the prepared wide bandgap semiconductor micro/nano-wire is MgO and Ga2O3、ZnO、SnO2、TiO2And one or more of NiO, a core-shell structure.
The preparation method of the metal film and the metal electrode in the step (iv) can be realized by methods such as vacuum thermal evaporation, magnetron sputtering, ion sputtering and the like.
The preparation method of the metal nanostructure of the fifth step can be realized by one or more processes of vacuum thermal evaporation, magnetron sputtering, ion sputtering, annealing, electron beam etching, ion beam etching and the like.
The metal material of the metal film and the metal nanoparticles in the fifth step is one or a mixed structure of Al, Ag, Pt, Ru, Rn, Pd and the like.
The metal electrode layer In the step (c) is a single-layer metal or metal composite layer In Ti, Al, Ni, Pt, Au, Ag and In.
Compared with the prior art, the invention has the following beneficial effects:
1. the microcavity detector prepared by the method is a brand-new ultraviolet photodetector structure (attached figure 1), and the structure can integrate hybrid metal surface plasmons and the photodetector together through a Fabry-Perot microcavity, so that the problem that the enhancement effect of the metal surface plasmon technology in an ultraviolet band is not good is solved, meanwhile, the structure can improve the quantum efficiency of the device while reducing the size of the device, is easy to couple a focal plane readout circuit, and is beneficial to the development of a next-generation high-density integrated photoelectric circuit. The working principle (figure 3) is briefly described as follows: when an external light field is incident on the upper surface of the hybrid surface plasma Fabry-Perot microcavity, the metal nano structure can overcome the optical diffraction limit to limit the ultraviolet radiation light field of the free space in the nano scale, and then the ultraviolet radiation of the free light field is limited in the wide-forbidden band semiconductor micro/nano wire in the form of hybrid surface plasma standing wave, namely the active region of the photoelectric detector, due to the reflection action of the Fabry-Perot microcavity and the metal film on the lower side, so that the generation and collection probability of photo-generated carriers is greatly increased.
2. The microcavity structure detector has good universality, and semiconductor materials such as MgO and Ga with different forbidden band widths pass through different active regions2O3、ZnO、SnO2、TiO2And NiO and the like are selected, the response cut-off wavelength range can cover UVA-UVC wave bands, and the application value of the method is wide in various fields.
Drawings
FIG. 1 is a schematic structural diagram of a hybrid surface plasma Fabry-Perot microcavity structure ultraviolet detector of the invention, wherein the reference numbers in the diagram are as follows: 1-metal reflecting layer, 2-wide bandgap semiconductor micro/nano wire, 3-metal electrode layer and 4-metal nano particle;
FIG. 2 is a flow chart of the preparation of the hybrid surface plasma Fabry-Perot microcavity structure ultraviolet detector of the invention, wherein: cleaning a substrate, preparing a seed crystal layer, preparing wide bandgap semiconductor micro/nano wires, preparing a metal film on the lower side of a single quadrilateral wide bandgap semiconductor micro/nano wire along the axis direction, preparing a metal nano structure on the upper side of the single quadrilateral wide bandgap semiconductor micro/nano wire along the axis direction, and preparing a metal electrode layer;
FIG. 3a is a schematic diagram of the operation of a hybrid surface plasma Fabry-Perot microcavity, wherein the reference numbers are as follows: 1-incident light, 2-metal nanostructure, 3-standing wave formed in Fabry-Perot microcavity, 4-wide band gap semiconductor micro/nanostructure, and 5-metal film reflecting layer; FIG. 3b is the result of optical field confinement in a hybrid surface plasmon Fabry-Perot microcavity simulated by using a finite difference time domain method.
Detailed Description
The technical solution of the present invention is further described with reference to fig. 2, but the present invention is not limited thereto, and any modification or equivalent replacement of the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention should be covered by the protection scope of the present invention.
Example 1
In this example, a hybrid surface plasma Fabry-Perot microcavity structure uv detector was prepared according to the following steps:
and (5) cleaning the substrate. Before growing the seed crystal layer, adding a solution of 3 volume ratio of sulfuric acid to hydrochloric acid: 1 for 5-30 minutes to remove inorganic substances attached to the surface of the substrate (the operation is not required for the substrate except sapphire), the substrate is sequentially placed into acetone, ethanol and deionized water for ultrasonic cleaning for 5-30 minutes to remove the organic substances attached to the surface of the substrate, the substrate is blown dry by nitrogen after being cleaned, and is placed into an oxygen plasma cleaning machine for treatment for 5 minutes, and the substrate is taken out for standby after the treatment is finished.
And preparing a ZnO seed crystal layer. Dissolving zinc acetate (99.99%) without crystal water in superior pure ethanol to prepare a zinc acetate ethanol solution with the concentration of 30 mg/ml; and then, spin-coating the zinc acetate ethanol solution on the surface of the treated substrate, then placing the substrate into a tube furnace, sintering the substrate for 15 minutes at 400 ℃ in an air atmosphere, and repeating the steps for 2-6 times to obtain ZnO nanocrystals on the surface of the substrate.
And growing the wide bandgap semiconductor micro/nanowire. And fully mixing high-purity ZnO powder and graphite powder in a mass ratio of 1:1, and grinding for more than 2 hours. Placing the mixed powder in the middle of a ceramic boat, placing a substrate with ZnO nanocrystalline right above the mixed powder, horizontally placing the ceramic boat into a quartz tube, placing the quartz tube into a growth chamber of a horizontal high-temperature tube furnace for growth, wherein the growth environment is normal pressure, carrier gas in the growth process is high-purity argon and high-purity oxygen, and the obtained single quadrilateral ZnO micro/nanowire has the cross section width of 10 nm-10 mu m, the cross section thickness of 10 nm-10 mu m and the length of 1mm-1 cm. The specific size can be determined by the comprehensive regulation and control of the growth temperature and the growth time.
And (4) preparing a metal film. After the quadrilateral wide bandgap semiconductor micro/nanowire with the Fabry-Perot microcavity structure is grown, a 5 nm-2 μm metal film is prepared on the lower side of the single quadrilateral wide bandgap semiconductor micro/nanowire by a magnetron sputtering method, the prepared metal film comprises various metals mentioned in claim 3, the selection is carried out according to different required conditions, and the thickness can be determined by sputtering time.
And (4) preparing a metal nano structure. Preparing a metal nano structure with an absorption peak positioned in an ultraviolet band on the opposite side (namely the upper side of the quadrilateral wide bandgap semiconductor micro/nano wire) of a metal thin film material by a vacuum thermal evaporation, magnetron sputtering or ion sputtering and annealing 2-step method, wherein the shape of the metal nano structure comprises one of a sphere, an ellipsoid and a triangular prism and an irregular shape formed by the structures, the prepared metal nano structure comprises various metals mentioned in claim 4, the metal nano structure is selected according to different required conditions, and the characteristic dimension of the metal nano structure can be determined by the sputtering current, the sputtering time and the annealing temperature.
And (4) preparing a metal electrode. Preparing metal electrodes at two ends of the single quadrilateral wide bandgap semiconductor micro/nanowire with the Al thin films and the Al nano particles at the upper side and the lower side by a magnetron sputtering method or a thermal evaporation method, wherein the prepared electrodes comprise various electrodes mentioned in claim 5, and the electrodes are selected according to different required contact conditions.
Example 2
This example is the same as example 1 except for the following features: step 2 in this example) With SnCl4·5H2Preparing a 0.1g/ml solution of O crystals (molecular weight of 350.6), and carrying out ultrasonic treatment for 2-3 minutes to uniformly mix the O crystals; using dropper to pick up SnCl just prepared4Dropping the solution on the washed silicon wafer until the silicon wafer is fully paved with SnCl4Drying the solution, and then putting the solution into a muffle furnace oven to anneal for 2 hours at 500 ℃ to obtain SnO2And (5) seed crystal. Meanwhile, high-purity SnO with the mass ratio of 1:12The powder and graphite powder are fully mixed and ground for more than 2 hours. Placing the mixed powder in the middle of a ceramic boat, and placing the ceramic boat with SnO2Putting a silicon substrate of the seed crystal right above the mixed powder, horizontally putting a ceramic boat into a quartz tube, putting the quartz tube into a growth chamber of a horizontal high-temperature tube furnace, growing at normal pressure in the growth environment, wherein carrier gas in the growth process is high-purity argon and high-purity oxygen, and obtaining single quadrilateral SnO2The width of the section of the micro/nano wire is 10 nm-10 mu m, the thickness of the section is 10 nm-10 mu m, and the length is 1mm-1 cm. The specific size can be determined by the comprehensive regulation and control of the growth temperature and the growth time.
Example 3
This example is the same as example 1 except for the following features: in this embodiment, step 2) puts the cleaned substrate into a growth chamber of a magnetron sputtering apparatus, the target material used for sputtering the seed crystal film is a ZnO ceramic target (99.999%), the power of the sputtering radio frequency source is adjusted to 130W, and oxygen (10SCCM) and argon (30SCCM) are continuously introduced into the growth chamber during sputtering. Keeping the vacuum degree of the growth chamber at 1Pa, rotating the substrate at 20 r/min, controlling the substrate temperature at 400 ℃ and the growth time at 0.5-1.5 hours to obtain the ZnO seed crystal. Meanwhile, the mass ratio of 1: 0.1: 1 high purity ZnO powder (99.999%), Ga2O3The powder (99.99%) and graphite powder are mixed thoroughly and ground for more than 2 hours. Placing the mixed powder in the middle of a ceramic boat, placing a substrate with ZnO seed crystals right above the mixed powder, horizontally placing the ceramic boat into a quartz tube, placing the quartz tube into a growth chamber of a horizontal high-temperature tube furnace, and growing at normal pressure in the growth environment of normal pressure, wherein carrier gas in the growth process is high-purity argon and high-purity oxygen, and the obtained ZnO-Ga2O3The section width of the single quadrilateral core-shell structure micro/nanowire is 10 nm-10 mu m, the section thickness is 10 nm-10 mu m, and the length is 1mm-1 cm. The specific size can be determined by the comprehensive regulation and control of the growth temperature and the growth time.
The above embodiments are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and all equivalent variations made according to the present invention are within the scope of the present invention.
Claims (9)
1. A microcavity structure uv detector, comprising: the device comprises a metal film, wide bandgap semiconductor micro/nano wires, metal nano particles and metal electrode layers at two ends of the device; adopting quadrilateral wide-bandgap semiconductor micro/nano wires to form a Fabry-Perot microcavity structure, forming metal nano-particles on the upper surface of the Fabry-Perot microcavity structure and forming a metal film on the lower surface of the Fabry-Perot microcavity structure, thereby forming a composite microcavity structure; the metal thin film is positioned at the bottom end of the quadrilateral wide bandgap semiconductor micro/nanowire, the metal nano particles are positioned at the top end of the quadrilateral wide bandgap semiconductor micro/nanowire, and the metal electrode layers are positioned at two sides of the top end of the quadrilateral wide bandgap semiconductor micro/nanowire and are not in contact with the metal nano particles; the thickness of the metal film is 5 nm-2 mu m, the section width of a single quadrilateral wide bandgap semiconductor micro/nanowire is 10 nm-10 mu m, the section thickness is 10 nm-10 mu m, the length of the quadrilateral wide bandgap semiconductor micro/nanowire is 1mm-1cm, the characteristic size range of the metal nanoparticles is 10-300 nm, the distance between adjacent metal nanoparticles is 5-100 nm, and the thickness of the metal electrode layer is 30-500 nm.
2. The microcavity-structured UV detector according to claim 1, wherein the wide-bandgap semiconductor micro/nano-wire is MgO, Ga2O3、ZnO、SnO2、TiO2And one or more core-shell structures in NiO.
3. The microcavity structure UV detector according to claim 1, wherein the metal thin film is made of a composite structure of one or more of Al, Ag, Pt, Ru, Rn, and Pd suitable for UV band.
4. The microcavity structure UV detector according to claim 1, wherein the metal nanoparticles are one or more composite asymmetric structures of Al, Ag, Pt, Ru, Rn, Pd materials with absorption peaks located in the UV band, and the shapes thereof include spheres, ellipsoids, triangular columns and regular and irregular shapes composed of the above structures.
5. The microcavity structure UV detector according to claim 1, wherein the metal electrode layer is a single-layer metal or a metal composite layer of Ti, Al, Ni, Pt, Au, Ag and In.
6. The microcavity structure ultraviolet detector according to claim 1, wherein a layer of Au with a thickness of 10-500 nm is deposited on the metal electrode layer.
7. The preparation method of the microcavity structure ultraviolet detector according to any one of claims 1 to 6, comprising the following steps:
cleaning a substrate, and before growing a seed crystal layer, mixing sulfuric acid and hydrochloric acid in a volume ratio of 3: 1 for 5-30 minutes to remove inorganic matters attached to the surface of the substrate, the sapphire outer substrate does not need the operation, the substrate is sequentially placed into acetone, ethanol and deionized water for ultrasonic cleaning for 5-30 minutes to remove the organic matters attached to the surface of the substrate, the substrate is blow-dried by nitrogen after being cleaned, and is placed into an oxygen plasma cleaning machine for treatment for 5 minutes, and the substrate is taken out for standby after the treatment is finished;
preparing a seed crystal layer, namely preparing the corresponding seed crystal layer by magnetron sputtering or a chemical synthesis method according to different selected materials;
the method comprises the following steps of (1) growing wide bandgap semiconductor micro/nano wires, fully mixing high-purity wide bandgap semiconductor powder with a mass ratio of 1:1 with graphite powder, grinding for more than 2 hours, placing the mixed powder in the middle of a ceramic boat, placing a substrate with a seed crystal layer right above the mixed powder, horizontally placing the ceramic boat into a quartz tube, placing the quartz tube into a growth chamber of a horizontal high-temperature tube furnace for growth, wherein the growth environment is normal pressure, and the carrier gas in the growth process is high-purity argon gas and high-purity oxygen gas;
preparing a metal film, namely preparing the metal film on the lower side of the single quadrilateral wide bandgap semiconductor micro/nanowire by a magnetron sputtering method after the quadrilateral wide bandgap semiconductor micro/nanowire with the Fabry-Perot microcavity structure is grown;
preparing metal nanoparticles, namely preparing the metal nanoparticles with absorption peaks positioned in an ultraviolet band on the opposite side of a metal film material, namely the upper side of the quadrilateral wide bandgap semiconductor micro/nanowire by a 2-step method of vacuum thermal evaporation, ion sputtering or magnetron sputtering and annealing, wherein the shape of the metal nanoparticles comprises one of a sphere, an ellipsoid and a triangular prism and an irregular shape formed by the structures;
preparing a metal electrode layer, namely preparing the metal electrode layer at two ends of the single quadrilateral wide bandgap semiconductor micro/nanowire with the metal thin films and the metal nanoparticles on the upper side and the lower side by a magnetron sputtering method or a thermal evaporation method.
8. The method for preparing a microcavity structure UV detector according to claim 7, wherein the substrate used for growing the seed layer in step ② is sapphire, quartz, diamond, mica, or SiO2a/Si or MgO hardness or flexible substrate.
9. The preparation method of the microcavity structure ultraviolet detector, according to claim 7, the third step is characterized in that the wide-bandgap semiconductor micro/nano-wire growth conditions are normal pressure, the growth temperature is 900-1300 ℃, the growth time is 20-60 minutes, and 100-150 SCCM argon and 0-25 SCCM oxygen are used as carrier gas in the growth process.
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