CN111180558A - ZnO micron line heterojunction ultraviolet light-emitting diode and preparation method thereof - Google Patents
ZnO micron line heterojunction ultraviolet light-emitting diode and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000002131 composite material Substances 0.000 claims abstract description 27
- 239000002042 Silver nanowire Substances 0.000 claims abstract description 16
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 13
- 239000000956 alloy Substances 0.000 claims abstract description 13
- 239000002923 metal particle Substances 0.000 claims abstract description 12
- 239000011521 glass Substances 0.000 claims abstract description 10
- 238000003825 pressing Methods 0.000 claims abstract description 7
- 239000002070 nanowire Substances 0.000 claims description 17
- 238000004528 spin coating Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000005566 electron beam evaporation Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 83
- 239000011787 zinc oxide Substances 0.000 description 53
- 239000000463 material Substances 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
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- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
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- 229910001020 Au alloy Inorganic materials 0.000 description 2
- 229910000990 Ni alloy Inorganic materials 0.000 description 2
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- 230000005540 biological transmission Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
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- 238000000576 coating method Methods 0.000 description 1
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- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
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- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/0004—Devices characterised by their operation
- H01L33/002—Devices characterised by their operation having heterojunctions or graded gap
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
- H01L33/0083—Processes for devices with an active region comprising only II-VI compounds
- H01L33/0087—Processes for devices with an active region comprising only II-VI compounds with a substrate not being a II-VI compound
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/26—Materials of the light emitting region
- H01L33/28—Materials of the light emitting region containing only elements of Group II and Group VI of the Periodic Table
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Abstract
The invention discloses a ZnO micron line heterojunction ultraviolet light-emitting diode and a preparation method thereof, wherein the diode comprises a p-GaN substrate, n-ZnO, Ga @ AgNWs composite micron line, ITO conductive glass and a gasket, wherein the n-ZnO, Ga @ AgNWs composite micron line is tightly attached to the p-GaN substrate and the gasket, one end of the n-ZnO, Ga @ AgNWs composite micron line is attached to the p-GaN substrate and the gasket, a metal particle electrode is attached to one end of the n-ZnO, Ga @ AgNWs composite micron line is coated on the p-GaN substrate, and the ITO conductive glass is pressed on the n-ZnO, Ga @ AgNWs composite micron line on the p-GaN; the preparation method of the diode comprises the following steps: (S1) preparing n-ZnO: Ga @ AgNWs composite micron line; (S2) preparing a p-GaN/n-ZnO: Ga @ AgNWs heterostructure; (S3) preparing an alloy electrode on the p-GaN substrate; (S4) preparing a metal particle electrode on the n-ZnO: Ga @ AgNWs micron line; (S5) pressing ITO conductive glass on the surface of a p-GaN/n-ZnO Ga @ AgNWs heterostructure to obtain the ZnO micron line heterojunction ultraviolet light-emitting diode. The diode utilizes AgNWs to modify n-ZnO and Ga micron wires, improves the ultraviolet luminous efficiency, enables the ultraviolet light to emit stably, and is a micron-sized photoelectric device which is convenient to use and prepare.
Description
Technical Field
The invention relates to a light emitting diode and a preparation method thereof, in particular to a ZnO microwire heterojunction ultraviolet light emitting diode and a preparation method thereof.
Background
The ultraviolet light emitting diode has very wide application prospect in the fields of information storage, medical treatment and health, environmental purification, microelectronic device assembly and the like due to the advantages of long service life, good environmental compatibility, low heat radiation and the like. As a representative of a third-generation wide-bandgap direct band-gap semiconductor material, a zinc oxide (ZnO) semiconductor material is an ideal material for preparing an ultraviolet band photoelectronic device, and in addition, a ZnO-based micro-nano structure also has high crystallization quality, excellent optical and electrical characteristics and a natural optical resonant cavity structure, and is an ideal material structure for constructing small units and micro-miniature high-efficiency ultraviolet photoelectric devices. However, due to the inherent properties of the ZnO material, p-type doping is difficult to realize, and the effective injection rate of carriers is low; meanwhile, the stable and reliable p-n homogeneous structure prepared by the ZnO material is difficult to realize. p-GaN is used as an inorganic semiconductor material, is resistant to high temperature and is not easy to be broken down by electrons, and has an energy level structure matched with ZnO, so that p-GaN and ZnO are commonly used to form a p-n junction at present to manufacture a ZnO heterojunction light-emitting diode. However, when p-GaN and ZnO form a p-n junction, ZnO is often a nanowire or nanowire array, which is difficult to be mass-produced and applied to practical diodes, and a p-n junction device formed by a pure ZnO nanowire or nanowire array has low light emitting efficiency and performance which is difficult to be expected, whereas for an unmodified single nanowire heterojunction diode, a relatively serious interface emission exists, which is difficult to realize ultraviolet emission dominated by ZnO near-band edge emission, and the re-injection of ZnO nanowire carriers is affected due to the low carrier transmission efficiency caused by the presence of ZnO surface defects, so that the high-efficiency light emission is difficult to realize, the invention patent with the application number of 201910337989.8 discloses a single ZnO-Ga nanowire heterojunction base point light source device and a preparation method thereof, wherein an Ag nanoparticle layer is manufactured on the surface of a single ZnO-Ga nanowire to form a composite structure of Ag-wrapped ZnO-Ga nanowire, the Ag nano particles are chemically synthesized on the surface of the micron line by sputtering or spin coating, but the technical scheme is that the energy is limited to one point by utilizing the extremely strong field limiting property of the surface plasmon polariton of the Ag nano particles, the carrier recombination region is regulated and controlled, and the point light-emitting diode device is realized, so that the efficient light emission in a large range cannot be realized.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a ZnO micron line heterojunction ultraviolet light-emitting diode which has high ultraviolet light-emitting efficiency and stable light emission, takes near-band edge emission as a main factor and is convenient to use, and the invention also aims to provide a preparation method of the diode.
The technical scheme is as follows: the invention discloses a ZnO micron line heterojunction ultraviolet light-emitting diode which comprises a p-GaN substrate, n-ZnO Ga @ AgNWs composite micron line, ITO conductive glass and a gasket, wherein the gasket is equal to the p-GaN substrate in thickness and is arranged side by side, the n-ZnO Ga @ AgNWs composite micron line is tightly attached to the p-GaN substrate and the gasket, a metal particle electrode is attached to one end of the gasket, an alloy electrode is plated on one end of the p-GaN substrate, which is not in contact with the n-ZnO Ga @ AgNWs composite micron line, and the ITO conductive glass is pressed on the n-ZnO Ga @ AgNWs composite micron line on the p-GaN substrate.
Wherein the thickness of the p-GaN substrate is 2-10 μm, and the hole concentration is 1017～1019/cm3Hole mobility of 5-100 cm2the/V.s, n-ZnO: Ga @ AgNWs composite micron line is prepared by covering AgNWs on the surface of the n-ZnO: Ga micron line, the length of the n-ZnO: Ga micron line is 0.5-0.8 cm, and the electron concentration is 1017～1019/cm3Electron mobility of 5-100 cm2The concentration of AgNWs is 0.02mg/mL, and the doping concentration of Ga is less than 1%; the length of AgNWs is 3-100 um, and the diameter is 30-130 nm; the metal particle electrode is a cathode, the alloy electrode is an anode, the metal particle electrode is an In particle electrode, and the alloy electrode is a Ni/Au electrode.
The preparation method of the ZnO micron line heterojunction ultraviolet light-emitting diode comprises the following steps:
(S1) spin-coating Ag nano wires on the surface of the n-ZnO: Ga micron wire to form n-ZnO: Ga @ AgNWs composite micron wire;
(S2) pressing the n-ZnO: Ga @ AgNWs composite micron line on a p-GaN substrate and a gasket to form a p-GaN/n-ZnO: Ga @ AgNWs heterostructure;
(S3) preparing an alloy electrode at a position where the p-GaN substrate does not contact the n-ZnO: Ga @ AgNWs composite microwire in the p-GaN/n-ZnO: Ga @ AgNWs heterostructure;
(S4) preparing a metal particle electrode at one end of the n-ZnO: Ga @ AgNWs micron line positioned on the gasket in the p-GaN/n-ZnO: Ga @ AgNWs heterostructure;
(S5) pressing a layer of ITO conductive glass on the surface of the p-GaN/n-ZnO: Ga @ AgNWs heterostructure of the prepared electrode to obtain the ZnO microwire heterojunction ultraviolet light-emitting diode.
Wherein, the AgNWs spin coating rate in the step S1 is 0.03-0.05 mm/min, the AgNWs spin coating is dried in the air at 90-100 ℃ for 1-2 h, and the alloy electrode (3) is prepared by an electron beam evaporation method in the step S3, and the thickness is 20-40 nm.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: 1. ga micron line, namely n-ZnO is modified by AgNWs, so that intrinsic emission of the Ga micron line is enhanced, and the ultraviolet light emitting efficiency of the ZnO micron line heterojunction ultraviolet light emitting diode is improved; 2. by utilizing the unique field locality and field enhancement characteristics of AgNWs surface plasmons, the ZnO microwire heterojunction ultraviolet light-emitting diode has stable ultraviolet light emission and a large light-emitting range; 3. the ZnO micron line heterojunction ultraviolet light-emitting diode is a micron-sized high-efficiency ultraviolet light-emitting diode which takes ZnO near-band edge emission as a main factor, and is convenient to use and prepare.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a graph of the I-V characteristic of the present invention;
FIG. 3 is a graph of the luminescence spectrum of the present invention;
fig. 4 is a diagram of the luminous effect of the present invention.
Detailed Description
Putting the quartz glass sheet into a trichloroethylene solution, ultrasonically cleaning for 15-20min by using an ultrasonic instrument, then sequentially transferring the quartz glass sheet into acetone, ethanol and deionized water for cleaning for 15min respectively, and then drying the quartz glass sheet in nitrogen for later use; placing n-ZnO-Ga micron wire on quartz glass sheet, compacting two ends with indium particles, and coating with spin coaterWrapping AgNWs on the surface of a ZnO Ga micron wire in a spin coating mode, wherein the spin coating time is 30min, the pulling speed is 0.03mm/min, the concentration of an AgNWs solution is 0.02mg/mL, the average length of the AgNWs is 35 mu m, the average diameter is 60nm, placing a sample in a vacuum drying box for drying treatment after spin coating, setting the temperature to be 90 ℃ and the time to be 2h, taking down the micron wire, and removing indium particles on the surface to obtain an n-ZnO Ga @ AgNWs composite micron wire 2, wherein the length of the n-ZnO Ga micron wire is 0.6cm, and the electron concentration is 1019/cm3Electron mobility of 50cm2V.s, the Ga doping concentration is less than 1 percent;
putting the p-GaN substrate 1 in a high-temperature tube furnace for annealing treatment at 900 ℃ for 2h, after the annealing is finished, putting the p-GaN substrate 1 and the gasket 6 in trichloroethylene solution, ultrasonically cleaning the p-GaN substrate 1 and the gasket 6 in an ultrasonic instrument for 15 minutes, sequentially putting the p-GaN substrate in acetone, ethanol and deionized water for ultrasonic cleaning for 15 minutes, and then blowing the p-GaN substrate in nitrogen for later use, wherein the size of the p-GaN substrate is 3.0cm multiplied by 2.0cm, the thickness of the p-GaN substrate is 2.5 mu m, and the hole concentration of the p-GaN substrate is 1019/cm3Hole mobility of 50cm2V.s, the gasket 6 is a sapphire substrate and has the thickness of 2.5 mu m; placing one surface of the n-ZnO: Ga @ AgNWs composite micron line 2 on the surfaces of a p-GaN substrate 1 and a gasket 6 tightly on a micro-operation platform to obtain a p-GaN/n-ZnO: Ga @ AgNWs heterojunction; using a mask to shield the n-ZnO, Ga @ AgNWs composite microwire 2, and using an electron beam evaporation method to evaporate an ohmic contact alloy electrode 3 on the exposed end of the p-GaN substrate 1, wherein the alloy electrode 3 is a Ni/Au alloy electrode with the thickness of 30nm, the Ni electrode is 20nm, and the Au electrode is 10 nm; pressing indium particles at one end of the n-ZnO: Ga @ AgNWs micron line, which is positioned on the gasket 6, as a metal particle electrode 4, wherein the metal particle electrode 4 is a cathode, and a Ni/Au alloy electrode positioned at one end of the p-GaN substrate is an anode; placing ITO conductive glass 5 with the size of 1.0cm multiplied by 2.5cm in trichloroethylene, acetone, ethanol and deionized water for ultrasonic cleaning in sequence, drying in nitrogen, placing in a vacuum drying oven for drying treatment for 2 hours at the temperature of 160 ℃, taking out and cooling, and then pressing in a p-GaN/n-ZnO constant force clamp to obtain the ZnO micron line heterojunction ultraviolet light-emitting diode with the structure as follows, wherein the Ga @ AgNWs heterojunction is positioned on the surface of n-ZnO on the p-GaN substrate 1, and the Ga @ AgNWs composite micron line 2As shown in fig. 1.
An electrical test is carried out on the ZnO micron-line heterojunction ultraviolet light-emitting diode, the I-V characteristic curve of the ZnO micron-line heterojunction ultraviolet light-emitting diode is shown in figure 2, the starting voltage of the ZnO micron-line heterojunction ultraviolet light-emitting diode is 1.25V, and the ZnO micron-line heterojunction ultraviolet light-emitting diode is excellent in conductivity. The diode is subjected to photoelectric performance test, an electroluminescence spectrum is shown in figure 3, an ultraviolet emission peak is positioned at 375nm and is dominant to ZnO near-band edge emission, and the full width at half maximum is extremely narrow and is only 10 nm. As can be seen from fig. 4, as the injection current increases, the heterojunction appears as a glaring light emission with a strong halo effect. The diode does not need protective gas encapsulation, and can stably and efficiently emit light in the air at room temperature.
Claims (10)
1. A ZnO micron line heterojunction ultraviolet light-emitting diode is characterized by comprising a p-GaN substrate (1), n-ZnO Ga @ AgNWs composite micron lines (2), ITO conductive glass (5) and a gasket (6), wherein the gasket (6) and the p-GaN substrate (1) are equal in thickness and are arranged side by side, the n-ZnO Ga @ AgNWs composite micron lines (2) are tightly attached to the p-GaN substrate (1) and the gasket (6), a metal particle electrode (4) is attached to one end of the gasket (6), an alloy electrode (3) is plated on one end, which is not in contact with the n-ZnO Ga AgNWs composite micron lines (2), of the p-GaN substrate (1), and the ITO conductive glass (5) is pressed on the n-ZnO Ga @ AgNWs composite micron lines (2) on the p-GaN substrate (1).
2. The ZnO microwire heterojunction ultraviolet light-emitting diode of claim 1, wherein the thickness of the p-GaN substrate is 2-10 μm, and the hole concentration is 1017～1019/cm3Hole mobility of 5-100 cm2/V·s。
3. The ZnO nanowire heterojunction ultraviolet light-emitting diode of claim 1, wherein the n-ZnO: Ga @ AgNWs composite nanowire (2) is made of n-ZnO: Ga nanowire surface covered with AgNWs.
4. The ZnO nanowire heterojunction ultraviolet light-emitting diode of claim 3, wherein the n-ZnO Ga nanowire has a length of 0.5-0.8 cm and is electrically connected with a power supplyA sub-concentration of 1017～1019/cm3Electron mobility of 5-100 cm2The Ga doping concentration is less than 1 percent.
5. The ZnO microwire heterojunction ultraviolet light-emitting diode of claim 3, wherein the AgNWs concentration is 0.02mg/mL, the AgNWs length is 3-100 um, and the diameter is 30-130 nm.
6. The ZnO microwire heterojunction ultraviolet light-emitting diode of claim 1, wherein the metal particle electrode (4) is a cathode and the alloy electrode (3) is an anode.
7. The ZnO nanowire heterojunction UV-LED according to claim 1, wherein the metal particle electrode (4) is an In particle electrode and the alloy electrode (3) is a Ni/Au electrode.
8. The preparation method of the ZnO microwire heterojunction ultraviolet light-emitting diode of claim 1, characterized by comprising the following steps:
(S1) spin-coating Ag nano wires on the surface of the n-ZnO: Ga micron wire to form an n-ZnO: Ga @ AgNWs composite micron wire (2);
(S2) pressing the n-ZnO: Ga @ AgNWs composite micron line (2) on the p-GaN substrate (1) and the gasket (6) to form a p-GaN/n-ZnO: Ga @ AgNWs heterostructure;
(S3) preparing an alloy electrode (3) at a position where the p-GaN substrate (1) does not contact the n-ZnO: Ga @ AgNWs composite micron line (2) in the p-GaN/n-ZnO: Ga @ AgNWs heterostructure;
(S4) preparing a metal particle electrode (4) at one end of the n-ZnO: Ga @ AgNWs micron line (2) positioned on the gasket (6) in the p-GaN/n-ZnO: Ga @ AgNWs heterostructure;
(S5) pressing a layer of ITO conductive glass on the surface of the p-GaN/n-ZnO: Ga @ AgNWs heterostructure of the prepared electrode to obtain the ZnO microwire heterojunction ultraviolet light-emitting diode.
9. The ZnO nanowire heterojunction ultraviolet light-emitting diode of claim 8, wherein AgNWs spin-coating rate in the step S1 is 0.03-0.05 mm/min, and drying is carried out in air at 90-100 ℃ for 1-2 h after spin-coating.
10. The ZnO nanowire heterojunction ultraviolet light-emitting diode of claim 8, wherein the alloy electrode (3) is prepared by an electron beam evaporation method in step S3, and the thickness is 20-40 nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112108168A (en) * | 2020-10-15 | 2020-12-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method, product and application of zinc oxide modified gallium nitride silver-loaded nanorod heterojunction photocatalyst |
| CN112234127A (en) * | 2020-10-16 | 2021-01-15 | 南京工程学院 | Single Rh @ ZnO micron line heterojunction ultraviolet-enhanced light-emitting diode and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106848007A (en) * | 2017-01-12 | 2017-06-13 | 东南大学 | One kind enhancing zinc oxide electroluminescent method of gallium nitride heterojunction structure |
| CN110137315A (en) * | 2019-04-25 | 2019-08-16 | 南京航空航天大学 | Single ZnO:Ga micro wire hetero-junctions substantial point source device and preparation method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106848007A (en) * | 2017-01-12 | 2017-06-13 | 东南大学 | One kind enhancing zinc oxide electroluminescent method of gallium nitride heterojunction structure |
| CN110137315A (en) * | 2019-04-25 | 2019-08-16 | 南京航空航天大学 | Single ZnO:Ga micro wire hetero-junctions substantial point source device and preparation method |
Non-Patent Citations (1)
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| MINGMING JIANG 等: ""Wavelength‐Tunable Electroluminescent Light Sources from Individual Ga‐Doped ZnO Microwires"", 《SMALL》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112108168A (en) * | 2020-10-15 | 2020-12-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method, product and application of zinc oxide modified gallium nitride silver-loaded nanorod heterojunction photocatalyst |
| CN112108168B (en) * | 2020-10-15 | 2023-02-14 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method, product and application of zinc oxide modified gallium nitride silver-loaded nanorod heterojunction photocatalyst |
| CN112234127A (en) * | 2020-10-16 | 2021-01-15 | 南京工程学院 | Single Rh @ ZnO micron line heterojunction ultraviolet-enhanced light-emitting diode and preparation method and application thereof |
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Application publication date: 20200519 |