CN109698278B - Organic-inorganic composite structure self-driven solar blind ultraviolet detector and preparation method thereof - Google Patents
Organic-inorganic composite structure self-driven solar blind ultraviolet detector and preparation method thereof Download PDFInfo
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- CN109698278B CN109698278B CN201811546508.6A CN201811546508A CN109698278B CN 109698278 B CN109698278 B CN 109698278B CN 201811546508 A CN201811546508 A CN 201811546508A CN 109698278 B CN109698278 B CN 109698278B
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Abstract
The invention belongs to the technical field of photoelectric detectors, and particularly relates to a p-n junction self-driven solar blind ultraviolet detector based on an organic-inorganic composite structure and a preparation method thereof. The device structure of the invention comprises: the semiconductor device comprises a substrate, n-type gallium oxide micro-wires, a p-type organic conductive polymer nano-film and metal contact electrodes prepared on p-type and n-type layers. The invention is characterized in that the p-type organic conductive polymer and the n-type gallium oxide micron line form a core-shell structure, so that the core-shell structure has good photoelectric property and deep ultraviolet selectivity when working under zero bias, and the device solves the problem that the p-type material in the traditional p-n structure inorganic semiconductor deep ultraviolet photoelectric detector cannot be prepared controllably. The detector disclosed by the invention is simple in preparation process and has a great application prospect in the field of solar blind ultraviolet detection.
Description
Technical Field
The invention relates to the field of semiconductor photoelectric devices, in particular to a self-driven solar blind ultraviolet detector with an organic-inorganic composite structure and a preparation method thereof.
Background
Solar radiation is known as solar blind ultraviolet because ultraviolet radiation in the wavelength range of 200-280nm is strongly absorbed by the presence of the ozone layer when passing through the atmosphere, and solar ultraviolet radiation in this band is almost absent from the ground. Thus, a detector operating in this band is called a solar blind ultraviolet detector. Since there is little background radiation interference from the sun in the solar blind band at the earth's surface, it can achieve higher detection rates for target objects. Can be widely applied to military and civil fields such as missile early warning, ultraviolet communication, environment monitoring, fire disaster early warning and the like.
In recent years, along with the development of military and industry and agriculture and the continuous progress of technology, some high-efficiency energy-saving ultraviolet detectors with special functions and applicable to special environments gradually become hot spots for research in the field of photoelectric detectors. Of these, a self-driven ultraviolet detector (one that can be used without an externally applied bias) is a typical representation. The self-driven ultraviolet detector has the following three advantages compared with the traditional photoelectric detector: in the first aspect, a power supply fitting part in a traditional detector structure can be omitted, so that the size of the device is effectively reduced; on the other hand, the detector can be used for reducing huge energy consumption caused by long-term operation of the detector for ultraviolet detection, medical detection and fire monitoring of sewage treatment; the third aspect can be applied to ultraviolet monitoring in some harsh or dangerous environments such as outer space, seabed and the like.
Currently, alloy materials such as GaAlN and ZnMgO are applied to solar blind ultraviolet detection. The alloy material can change the bandwidth by adjusting the components, so as to realize detection of different wavelengths. Component tuning, however, can cause a change in the lattice structure and thus a significant number of lattice defects to form within the material, resulting in reduced device function. In contrast, the gallium oxide material used as the non-alloy material has a forbidden bandwidth of 4.9eV, can realize the detection of solar blind ultraviolet without alloying corresponding to 253nm wavelength, has high growth temperature, good crystallization quality and high thermal stability and chemical stability, and is very suitable for being used as a material for solar blind ultraviolet detection. In the current research, the p-type doping and high-quality Schottky contact of the gallium oxide material are difficult to realize, so that the high-performance self-driven photoelectric detector based on the gallium oxide material is difficult to prepare.
Disclosure of Invention
In view of the above-mentioned shortcomings, the present invention aims to provide a self-driven solar blind ultraviolet detector with an organic-inorganic composite structure and a preparation method thereof, and the present invention provides a self-driven deep ultraviolet photoelectric detector with high responsivity. The adopted organic-inorganic core-shell structure can effectively separate the photon-generated carriers, wherein the p-type organic conductive polymer nano film only plays a role in hole transmission, has no optical response to light of any wave band, and can ensure that the corresponding cut-off edge of the p-type organic conductive polymer nano film is positioned in a solar blind wave band. Therefore, the structure is beneficial to improving the responsivity of the detector to solar blind ultraviolet signals, reducing the power consumption and lowering the preparation cost.
The aim of the invention is achieved by the following technical scheme:
the solar blind ultraviolet detector with the organic-inorganic composite structure is characterized by comprising a substrate, n-type gallium oxide micro-wires, a p-type organic conductive polymer nano-film and metal contact electrodes prepared on p-type layers and n-type layers; wherein the cross section width of the single quadrilateral gallium oxide micro-wire is 1-10 mu m, the cross section thickness is 1-10 mu m, the length of the micro-wire is 1mm-1cm, and the thickness of the organic conductive polymer nano-film is 20-500nm.
Preferably, the substrate is a rigid or flexible substrate, the rigid substrate is made of materials such as sapphire, quartz, silicon wafers and the like, and the flexible substrate is made of materials such as polyimide, polyethylene terephthalate and the like.
Preferably, the contact metal electrode is selected from a single layer metal or metal composite layer of titanium, aluminum, indium, nickel, platinum, gold, silver, molybdenum, tantalum, cobalt and tungsten.
The invention also provides a preparation method of the solar blind ultraviolet detector with the organic-inorganic composite structure, which comprises the following steps:
1) Preparing a micrometer wire: high-purity gallium oxide powder and carbon powder with the mass ratio of 1:1 are measured and mixed, and are fully ground to be uniformly mixed.
Placing the mixed powder in the middle of a corundum boat, placing a substrate right above the mixed powder, placing the corundum boat in a quartz tube, then 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 introducing high-purity argon as carrier gas in the growth process. And naturally cooling after the growth is finished, and obtaining the gallium oxide micro-wire.
2) Preparation of a core-shell structure: firstly, preparing inorganic acid with a certain concentration for dissolution, taking an equal amount of inorganic acid solution into two clean beakers, respectively adding conductive polymer monomers and oxidizing agents, and fully stirring to dissolve the conductive polymer monomers and the oxidizing agents. Placing a single gallium oxide micrometer wire on a substrate, fixing one end of the single gallium oxide micrometer wire, placing the single gallium oxide micrometer wire into a clean beaker, pouring the inorganic acid solution containing the conductive polymer monomer and the oxidant, which is prepared in the step 2), into the beaker to submerge the substrate and the micrometer wire, stirring, and standing for a period of time at a certain temperature to react to obtain the core-shell structure.
3) Preparation of a metal electrode: and taking out the sample from the solution, washing the sample for a plurality of times by using deionized water and ethanol, and then drying the sample to prepare metal electrodes at a gallium oxide end and an organic conductive polymer end respectively, thereby obtaining the solar blind ultraviolet detector with the organic-inorganic composite structure.
Preferably, the mineral acid of step 2) is H 2 SO 4 HCl and HClO 4 The concentration of the acid solution is 0.1-1.0mol/L.
Preferably, the conductive polymer monomer in the step 2) is one of aniline, pyrrole and 3, 4-ethylenedioxythiophene.
Preferably, the oxidant of step 2) is (NH) 4 ) 2 SO 8 、K 2 Cr 2 O 7 、KIO 3 、FeCl 3 、FeCl 4 、H 2 O 2 、 Ce(SO 4 ) 2 、MO 2 And one of BPO.
Preferably, the molar ratio of the conductive polymer monomer and the oxidant in the step 2) is 1 (1-2.5).
Preferably, the reaction temperature in the step 3) is between-20 and 60 ℃ and the reaction time is between 5 and 300 minutes.
The invention has the following beneficial effects:
1. compared with a photoconductive photoelectric detector, the self-driven solar blind ultraviolet detector with the organic-inorganic composite structure has better detection performance, zero bias is applied under the irradiation of an external light source, an n-type gallium oxide nuclear layer in the device absorbs photons to generate electrons and hole pairs, the electrons and the hole pairs are rapidly separated under the action of a built-in electric field, a p-type conductive polymer does not respond to light of any wave band, high-efficiency transmission of holes can be realized, and obvious photo-generated current can be detected at two ends of the device under the condition of no external bias.
2. The conductive polymer used for the self-driven solar blind ultraviolet detector with the organic-inorganic composite structure, which is prepared by the invention, belongs to an organic semiconductor material, the doping concentration can be regulated by changing the reaction condition, the electrical property of the conductive polymer is changed, the material cost is low, and the preparation process is simple.
3. The solar blind ultraviolet detector with the organic-inorganic composite structure prepared by the invention can normally work without an external power supply, realizes solar blind wave band self-driven detection of devices, has higher detection rate, and can be widely applied to special environments such as space seabed and the like.
Drawings
FIG. 1 is a schematic diagram of a self-driven solar blind ultraviolet detector with an organic-inorganic composite structure, wherein the structure is a 1-substrate, a 2-n-type gallium oxide microwire, a 3-p-type conductive polymer film, a 4-first metal contact electrode and a 5-second metal contact electrode.
FIG. 2 is a flow chart of the preparation of the self-driven solar blind ultraviolet detector with the organic-inorganic composite structure.
FIG. 3a is an I-V diagram of the gallium oxide nanowire prepared in example 1 of the present invention, FIG. 3b is an I-V diagram of polyaniline, and FIG. 3c is an I-V diagram of the gallium oxide/polyaniline p-n junction.
FIG. 4 is a graph showing the spectral response of a plurality of organic-inorganic composite structure self-driven solar blind UV detectors at 0V bias prepared in example 1 of the present invention.
Detailed Description
The following describes in further detail the embodiments of the present invention with reference to the drawings and examples.
Example 1:
the embodiment prepares the self-driven solar blind ultraviolet detector with the organic-inorganic composite structure according to the following steps:
and (3) preparing the microwires. High-purity gallium oxide powder and carbon powder with the mass ratio of 1:1 are measured and mixed, and the mixture is ground for more than 2 hours. Placing the mixed powder in the middle of a corundum boat, placing a substrate right above the mixed powder, placing the corundum boat in a quartz tube, then 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 introducing high-purity argon as carrier gas in the growth process. And naturally cooling after the growth is finished, and obtaining the gallium oxide micro-wire. The size of the micro-wire can be comprehensively regulated and controlled by the growth temperature and the growth time.
And (3) preparing a reaction solution. Firstly preparing a dilute sulfuric acid solution with the concentration of 0.1mol/L, and then taking two clean beakers, and adding 10ml of the dilute sulfuric acid solution respectively. 10. Mu.L of aniline solution and 22.82mg of ammonium persulfate ((NH) were measured out 4 ) 2 S 2 O 8 ) Added to each of the two beakers and stirred to dissolve completely.
And (3) preparing an organic-inorganic core-shell structure. The single gallium oxide micron line is clamped by forceps and placed on a quartz glass substrate, and one end of the single gallium oxide micron line is fixed by indium grains and then placed in a clean beaker. Pouring the aniline solution and the ammonium persulfate solution prepared in the second step into a beaker, immersing the substrate and the micrometer wire in the liquid level, stirring, and then placing the mixture at 0 ℃ to react for 5 hours.
And (3) preparing a metal electrode. And taking out the sample from the solution, washing the sample for multiple times by using deionized water and ethanol, drying the sample at 60 ℃ for 2 hours, and preparing indium electrodes on the gallium oxide side and the polymer side respectively to obtain the gallium oxide/polyaniline core-shell micron line solar blind ultraviolet detector.
Example 2:
this example is identical to example 1 except for the following features: step 2) in this example 7.6. Mu.L of pyrrole was taken and dissolved in dilute sulfuric acid.
Example 3:
this example is identical to example 1 except for the following features: step 2) in this example, 11.7. Mu.L of 3, 4-ethylenedioxythiophene was taken and dissolved in a dilute sulfuric acid solution.
The mineral acid may also be HCl or HClO under other conditions 4 The oxidant may also be K 2 Cr 2 O 7 、KIO 3 、FeCl 3 、FeCl 4 、H 2 O 2 、Ce(SO 4 ) 2 、MO 2 Or BPO.
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 changes made according to the present invention are all the scope of the present invention.
Claims (9)
1. An organic-inorganic composite structure self-driven solar blind ultraviolet detector, which is characterized by comprising: the metal contact electrode is prepared on the n-type gallium oxide micron line and the p-type organic conductive polymer nano film; wherein the width of the quadrilateral cross section of the single n-type gallium oxide micrometer wire is 1-10 mu m, the thickness of the cross section is 1-10 mu m, the length of the n-type gallium oxide micrometer wire is 1mm-1cm, and the thickness of the p-type organic conductive polymer nano film is 20-500nm.
2. The organic-inorganic composite structure self-driven solar blind ultraviolet detector according to claim 1, wherein the substrate is a rigid or flexible substrate, the rigid substrate is made of sapphire, quartz or silicon wafer materials, and the flexible substrate is made of polyimide or polyethylene terephthalate materials.
3. The organic-inorganic composite structure self-driven solar blind ultraviolet detector according to claim 1, wherein the n-type gallium oxide micro-wires and the p-type organic conductive polymer nano-film are contacted with a metal electrode selected from a single-layer metal or a metal composite layer of titanium, aluminum, indium, nickel, platinum, gold, silver, molybdenum, tantalum, cobalt and tungsten.
4. The method for preparing the self-driven solar blind ultraviolet detector with the organic-inorganic composite structure according to claim 1, which is characterized by comprising the following steps:
1) Preparing n-type gallium oxide micro-wires: preparing n-type gallium oxide micro-wires by using a chemical vapor deposition method; weighing high-purity gallium oxide powder and carbon powder with the mass ratio of 1:1, mixing, and fully grinding to uniformly mix the gallium oxide powder and the carbon powder; placing the mixed powder of the gallium oxide powder and the carbon powder in the middle of a corundum boat, placing a substrate right above the mixed powder, placing the corundum boat into a quartz tube, then placing the quartz tube into a growth chamber of a horizontal high-temperature tube furnace for growth, wherein the growth environment is normal pressure, the growth temperature is 900-1200 ℃, and high-purity argon is introduced as carrier gas in the growth process; naturally cooling after the growth is finished to obtain n-type gallium oxide micro-wires; the length of the gallium oxide micron line is 0.1-1cm, the width is 2-10 mu m, and the thickness is 2-10 mu m;
2) Preparation of a core-shell structure: firstly, preparing an inorganic acid solution with a certain concentration, taking an equal amount of the inorganic acid solution into two clean beakers, respectively adding a conductive polymer monomer and an oxidant, and fully stirring to dissolve the conductive polymer monomer acid solution and the oxidant acid solution; placing a single n-type gallium oxide micron line on another substrate, fixing one end of the single n-type gallium oxide micron line, pouring the prepared inorganic acid solution containing the conductive polymer monomer and the oxidant into a beaker, immersing the substrate fixed with the n-type gallium oxide micron line and the n-type gallium oxide micron line at one side of the fixed position into the mixed inorganic acid solution at the same time, exposing the n-type gallium oxide micron line at the other side of the fixed position into air, stirring, and standing to enable the polymer monomer, the oxidant and the inorganic acid to perform polymerization reaction on the surface of the n-type gallium oxide micron line immersed in the solution, thus obtaining a n-type gallium oxide micron line/p-type organic conductive polymer nano film sample;
3) Preparing a metal electrode: taking out an n-type gallium oxide nanowire/p-type organic conductive polymer nano film sample from an inorganic acid solution dissolved with a polymer monomer and an oxidant, washing the sample for a plurality of times by deionized water and ethanol, drying the sample, and preparing a metal electrode at a gallium oxide end and one end of a gallium oxide/polymer core-shell structure micron wire of which the p-type organic conductive polymer is coated with gallium oxide by a magnetron sputtering and vapor deposition method respectively to obtain the self-driven solar blind ultraviolet detector of the organic-inorganic composite structure.
5. The process according to claim 4, wherein the mineral acid in step 2) is H 2 SO 4 HCl and HClO 4 The concentration of the acid solution is 0.1-2.0mol/L.
6. The method according to claim 4, wherein the conductive polymer monomer in the step 2) is one of aniline, pyrrole and 3, 4-ethylenedioxythiophene.
7. The method according to claim 4, wherein the oxidizing agent is (NH) 4 ) 2 SO 8 、K 2 Cr 2 O 7 、KIO 3 、FeCl 3 、FeCl 4 、H 2 O 2 、Ce(SO 4 ) 2 、MO 2 And one of BPO.
8. The method of claim 4, wherein the molar ratio of the conductive polymer monomer to the oxidizing agent in step 2) is 1 (1-2.5).
9. The method according to claim 4, wherein the polymerization temperature after the conductive polymer monomer acid solution and the oxidizer acid solution are mixed together in step 2) is-20 to 60 ℃ and the reaction time is 5 to 300min.
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| CN112614943B (en) * | 2020-12-09 | 2024-01-19 | 华南师范大学 | Micron-sized core-shell heterojunction self-driven ultraviolet detector and preparation method thereof |
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