CN108063171B - ZnO nanorod array light-emitting diode and preparation method thereof - Google Patents
ZnO nanorod array light-emitting diode and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a ZnO nanorod array light-emitting diode, which comprises a p-GaN substrate, an n-ZnO nanorod array, an AlN thin film shell layer, Ag nano particles and a metal electrode, wherein the p-GaN substrate is provided with a GaN layer; the method comprises the following steps: growing an n-ZnO nanorod array on a p-GaN substrate; sputtering an AlN thin film shell layer on the n-ZnO nano rod; sputtering Ag nano particles on the ZnO-AlN core-shell nano rod; and preparing a metal electrode with ohmic contact at one end of the n-ZnO and the p-GaN to form the light-emitting diode. The surface of the AlN thin film passivates the nano rod, so that the surface state and the surface defects of ZnO are inhibited, the carrier injection efficiency of the nano rod is improved, and the stability of the light-emitting diode is improved; ag nano particles are sputtered on the nano rods, and through the mutual coupling effect of Ag surface plasmons and the electroluminescent intensity of the light-emitting diode, the electroluminescent performance is obviously improved, and meanwhile, defect luminescence is inhibited.
Description
Technical Field
The invention relates to the technical field of semiconductor optoelectronic devices, in particular to a ZnO nanorod array light-emitting diode and a preparation method thereof.
Background
Third generation wide bandgap semiconductor materials such as GaN, ZnO, etc. are widely used in light emitting diodes or detectors in blue and ultraviolet bands. In contrast to GaN, ZnO has an exciton confinement energy as high as 60meV, much higher than room temperature heat (26 meV). In addition, ZnO has the advantages of rich raw materials, good film forming property, good thermal stability and the like, and has important application prospect in the aspects of preparing room-temperature blue-violet light emitting diodes, ultraviolet detectors, ultraviolet semiconductor lasers and the like. However, the ZnO material has a large amount of zinc interstitial and oxygen vacancy defects, the background electron concentration is as high as 1018, the self-compensation effect of intrinsic point defects and the p-type doping of the ZnO material are extremely difficult, so that the luminous efficiency of the conventional ZnO-based light-emitting device is generally low.
A great deal of research work is carried out on improving the luminous efficiency of ZnO-based ultraviolet light-emitting devices, wherein single-crystal ZnO nanorods have excellent carrier transport characteristics and carrier confinement capacity, and the nano-scale heterostructure constructed by the ZnO nanorods shows good optical characteristics, can effectively improve the carrier injection efficiency and improve the stability of the devices. However, due to the high specific surface area of the one-dimensional ZnO nanorods, surface states and surface defects exist, thereby affecting the light emitting efficiency.
Disclosure of Invention
The purpose of the invention is as follows: in order to solve the problems of low luminous efficiency and obvious defect luminescence of the conventional ZnO light-emitting diode, the invention provides a ZnO nanorod array light-emitting diode and further provides a preparation method of the light-emitting diode.
The technical scheme is as follows: the invention relates to a preparation method of a ZnO nanorod array light-emitting diode, which comprises the following steps:
(1) growing an n-ZnO nanorod array on a p-GaN substrate to form a p-GaN-n-ZnO heterostructure;
(2) sputtering an AlN film on the n-ZnO nanorod array in the heterostructure obtained in the step (1) to form a p-GaN-n-ZnO-AlN composite system;
(3) sputtering Ag nano particles on the n-ZnO-AlN in the composite system obtained in the step (2) to form a p-GaN-n-ZnO-AlN-Ag composite system;
(4) and (4) respectively preparing metal electrodes at one end of the p-GaN and one end of the n-ZnO nanorod array in the composite system obtained in the step (3).
The growth method of the n-ZnO nanorod array in the step (1) is as follows:
(1) mixing ZnO powder and carbon powder according to the mass ratio of 1: 1-3 to obtain mixed powder, and placing the mixed powder at the bottom of a quartz tube with an opening at one end;
(2) dicing and cleaning a p-GaN substrate to be used as a growth substrate; wherein, a mask plate is used for covering a part of the upper part of the p-GaN substrate to prevent the n-ZnO nanorod array from growing at the part;
(3) and (3) putting the p-GaN substrate obtained in the step (2) into the quartz tube obtained in the step (1), horizontally pushing the quartz tube into a tube furnace, vacuumizing, introducing argon and oxygen to perform high-temperature reaction, and generating the n-ZnO nanorod array after the reaction is finished. The reaction temperature of the high-temperature reaction is 1000-1200 ℃, and the reaction time is 10-60 min; the argon flow is 130-180 sccm, and the oxygen flow is 13-18 sccm. Wherein, the purities of the ZnO powder and the carbon powder in the step (1) are 99.97-99.99%; the p-GaN substrate dicing and cleaning steps in the step (2) are as follows: cutting the p-GaN substrate into 1.5cm multiplied by 1cm, carrying out ultrasonic cleaning on acetone, absolute ethyl alcohol and deionized water in sequence, and drying the substrate by using nitrogen as a growth substrate, wherein one surface of the p-GaN surface, which is 0.5cm multiplied by 1cm, is covered by a mask plate; the quartz tube in the step (3) is a quartz tube with one end open, the length of the quartz tube is 30cm, and the diameter of the quartz tube is 3 cm; and placing the cleaned p-GaN substrate in a quartz tube at a position 5cm away from the tube opening.
Preferably, ZnO powder and carbon powder are mixed according to the mass ratio of 1:1 to obtain mixed powder; the reaction time of the high-temperature reaction is 10-45 min.
The equipment used in the sputtering in the step (2) is a magnetron sputtering instrument, wherein before sputtering, aluminum foil paper is used for covering a part of the upper part of the p-GaN substrate to prevent AIN from being sprayed on the substrate; the sputtering target is an AlN target with the specification of 60 multiplied by 3mm, the air pressure of the cavity is 1-4 Pa, the flow of argon is 30-50 sccm, the flow of nitrogen is 5-10 sccm, the sputtering power is 80-150W, and the sputtering time is 5-30 min; and (3) sputtering equipment is an ion sputtering instrument, the sputtering target material is an Ag target material, the specification is 50 multiplied by 3mm, the working gas is nitrogen, the air pressure of the cavity is 40-60 Pa, the sputtering power is 10-60W, and the sputtering time is 5-80 s.
Preferably, the sputtering time in the step (2) is 8-30 min, and the sputtering time in the step (3) is 5-45 s.
And (4) the method for preparing the metal electrode is a magnetron sputtering method or an electron beam evaporation method, and two layers of electrodes are respectively plated at one end of the p-GaN and one end of the n-ZnO nanorod to form the Ni/Au alloy electrode. The alloy electrode is an ohmic contact electrode.
The invention further aims to provide the ZnO nanorod array light-emitting diode prepared by the preparation method.
Wherein the thickness of the p-GaN substrate is 2-10 mu m, and the hole concentration is 1017～1019/cm3Hole mobility of 5-100 cm2/V·s。
Wherein the electron concentration of the n-ZnO nano rod is 1017～1019/cm3Electron mobility of 5-100 cm2/V·s。
Wherein the AlN thin film is 5-50 nm thick, and the Ag nanoparticles are 5-30 nm in particle size.
The metal electrode at one end of the n-ZnO nanorod array is a cathode, the metal electrode at one end of the p-GaN nanorod array is an anode, and the thickness of the metal electrode is 20-40 nm.
Has the advantages that: the invention inhibits the surface state and the surface defect by introducing the surface modification technology, further improves the efficiency of the nanoscale device: ZnO nanorods are passivated on the surface of the AlN thin film, so that the surface state and surface defects of ZnO are inhibited, the carrier injection efficiency of the ZnO nanorods is improved, and the stability of the light-emitting diode is improved; ag nano particles are sputtered on the ZnO-AlN nano rods, and through the mutual coupling effect of Ag surface plasmons and the electroluminescent intensity of the light-emitting diode, the electroluminescent performance of the light-emitting diode is obviously improved, and meanwhile, defect luminescence is inhibited.
Drawings
FIG. 1 is a schematic view of a scanning electron microscope of an n-ZnO nanorod array synthesized in example 1 of the present invention;
FIG. 2 is a schematic diagram of a transmission electron microscope of an Ag nanoparticle-modified n-ZnO/AlN nanorod synthesized in example 1 according to the present invention;
FIG. 3 is a schematic structural diagram of an Ag nanoparticle-modified n-ZnO/AlN nanorod array/p-GaN heterojunction light-emitting diode synthesized in example 1 of the present invention, in which 1 is a p-GaN substrate, 2 is an n-ZnO nanorod array, and 3 is an AlN thin film; 4 is Ag nano-particles; 5 is a gold-nickel alloy electrode;
FIG. 4 is an Electroluminescence (EL) spectrum of an Ag nanoparticle modified n-ZnO/AlN core-shell nanorod array/p-GaN heterojunction light-emitting diode synthesized in example 1 of the present invention.
Detailed Description
In the ZnO nanorod array light-emitting diode, the thickness of the p-GaN substrate is 2-10 mu m, and the hole concentration is 1017～1019/cm3Hole mobility of 5-100 cm2V.s; the electron concentration of the n-ZnO nano rod is 1017～1019/cm3Electron mobility of 5-100 cm2V.s; the AlN thin film is 5-50 nm thick, and the Ag nano particles are 5-30 nm in particle size; the metal electrode at one end of the n-ZnO is a cathode, the metal electrode at one end of the p-GaN is an anode, and the thickness of the metal electrode is 20-40 nm.
Example 1
The first step is as follows: mixing and grinding ZnO powder with the purity of 99.99% and carbon powder according to the mass ratio of 1:1, and filling the mixture into a ceramic boat; cutting the p-GaN substrate into 1.5cm multiplied by 1cm, carrying out ultrasonic cleaning on the p-GaN substrate by acetone, absolute ethyl alcohol and deionized water in sequence, drying the p-GaN substrate by using nitrogen to be used as a growth substrate, covering a part of the upper part of the p-GaN substrate by using a mask plate, then placing the p-GaN substrate into a quartz tube with an opening at one end, a length of 30cm and a diameter of 3cm at the closed end, and placing the cleaned p-GaN substrate into the quartz tube at a position 5cm away from a tube opening. The quartz tube was pushed into a horizontal tube furnace set at 1050 ℃ as a whole, the tube furnace was closed, evacuated, and argon flow of 150sccm and oxygen flow of 15sccm were introduced. After 30min reaction, the ZnO nano-rod array grows on the surface of the p-GaN, as shown in figure 1;
the second step is that: shielding one surface of the p-GaN by using aluminum foil paper, sputtering a layer of AlN thin film on a ZnO nanorod array by using a magnetron sputtering instrument, taking an AlN target as a sputtering source, wherein the specification is 60 multiplied by 3mm, the cavity air pressure is 2Pa, the argon flow is 50sccm, the nitrogen flow is 10sccm, the sputtering power is 100W, and the sputtering time is 8 min;
the third step: sputtering Ag nano particles on the ZnO-AlN core-shell nanorod by using a small ion sputtering instrument, wherein an Ag target material is used as a sputtering target material, the specification is 50 multiplied by 3mm, the working gas is nitrogen, the cavity air pressure is 40Pa, the sputtering power is 60W, and the sputtering time is 5s, so that the Ag modified ZnO/AlN core-shell nanorod is obtained, and the picture in figure 2 is shown;
the fourth step: plating two layers of electrodes on one ends of the n-ZnO-AlN core-shell nanorod array and the p-GaN by electron beam evaporation to form a Ni/Au electrode with the thickness of 30 nm; finally forming an Ag nano-particle modified n-ZnO-AlN core-shell nanorod array-p-GaN heterojunction light-emitting diode, wherein the thickness of the p-GaN substrate is 2 mu m, and the hole concentration is 8 multiplied by 1017/cm3Hole mobility of 81cm2V.s; the electron concentration of the n-ZnO nano-rod is 9 multiplied by 1018/cm3Electron mobility of 85cm2V.s; the AlN thin film is 8nm in thickness, and the Ag nano particles are 5-8 nm in particle size. See FIG. 3;
the fifth step: and (3) performing an electric pumping luminescence spectrum test on the light-emitting diode formed finally in the fourth step, as shown in figure 4, and obviously enhancing the electroluminescence of the device after the ZnO nanorod array is modified with the AlN thin film and the Ag nano particles are introduced in the device from an electroluminescence spectrum.
Example 2
The method is the same as example 1, except that the high temperature reaction time of the first step is 10min, the sputtering time of the second step is 15min, the sputtering time of the third step is 15s, and the electron concentration of the formed heterojunction light emitting diode n-ZnO nanorod is 6.4 × 1018A/cm 3 electron mobility of 64cm2V.s; the AlN thin film is 15nm in thickness, and the Ag nano particles are 6-9 nm in particle size.
Example 3
The method is the same as example 1, except that the high temperature reaction time of the first step is 15min, the sputtering time of the second step is 30min, and the sputtering time of the third step is 30s, wherein the electron concentration of the formed heterojunction light emitting diode n-ZnO nanorod is 7.2 × 1018/cm3Electron mobility of 56cm2V.s; the AlN thin film is 28nm in thickness, and the Ag nano particles are 12-15 nm in particle size.
Example 4
The method is the same as example 1, except that the high temperature reaction time of the first step is 45min, the sputtering time of the second step is 20min, and the sputtering time of the third step is 45s, wherein the electron concentration of the formed heterojunction light emitting diode n-ZnO nanorod is 9.2 × 1018/cm3Electron mobility of 87cm2V.s; the AlN thin film is 18nm in thickness, and the Ag nano particles are 15-20 nm in particle size.
Example 5
The method is the same as example 1, except that in the first step, ZnO powder and carbon powder are mixed according to the mass ratio of 1-3 to obtain mixed powder, the reaction temperature of the high-temperature reaction is 1000 ℃, and the reaction time is 60 min; the argon flow is 130sccm, and the oxygen flow is 13 sccm. In the second step, the pressure of the cavity is 1Pa, the flow of argon is 30sccm, the flow of nitrogen is 5sccm, the sputtering power is 150W, and the sputtering time is 30min during the sputtering of the magnetron sputtering instrument. In the third step, the sputtering power of the ion sputtering instrument is 10W, the air pressure of the cavity is 40Pa, and the sputtering time is 80 s.
Example 6
The method is the same as example 1, the reaction temperature of the high-temperature reaction in the first step is 1200 ℃, and the reaction time is 10 min; the argon flow is 180sccm and the oxygen flow is 18 sccm. In the second step, the cavity pressure is 4Pa, the argon flow is 50sccm, the nitrogen flow is 10sccm, the sputtering power is 80W, and the sputtering time is 5min during the magnetron sputtering. In the third step, the sputtering power of the ion sputtering instrument is 60W, the air pressure of the cavity is 60Pa, and the sputtering time is 5 s.
Comparative example 1
The method is the same as example 1, except that only the first step is needed, and an n-ZnO nanorod array/p-GaN heterojunction light-emitting diode is formed, and the electroluminescence spectrum is shown in figure 4.
Claims (10)
1. A preparation method of a ZnO nanorod array light-emitting diode is characterized by comprising the following steps:
(1) growing an n-ZnO nanorod array on a p-GaN substrate to form a p-GaN-n-ZnO heterostructure;
(2) sputtering an AlN film on the n-ZnO nanorod array in the heterostructure obtained in the step (1) to form a p-GaN-n-ZnO-AlN composite system;
(3) sputtering Ag nano particles on the n-ZnO-AlN in the composite system obtained in the step (2) to form a p-GaN-n-ZnO-AlN-Ag composite system;
(4) and (4) respectively preparing metal electrodes at one end of the p-GaN and one end of the n-ZnO nanorod array in the composite system obtained in the step (3).
2. The preparation method of claim 1, wherein the n-ZnO nanorod array of step (1) is grown by the following method:
(1) mixing ZnO powder and carbon powder according to the mass ratio of 1: 1-3 to obtain mixed powder, and placing the mixed powder at the bottom of a quartz tube with an opening at one end;
(2) dicing and cleaning a p-GaN substrate to be used as a growth substrate; wherein, a part of the upper part of the p-GaN substrate is shielded by a mask plate;
(3) and (3) putting the p-GaN substrate obtained in the step (2) into the quartz tube obtained in the step (1), horizontally pushing the quartz tube into a tube furnace, vacuumizing, introducing argon and oxygen to perform high-temperature reaction, and generating the n-ZnO nanorod array after the reaction is finished.
3. The preparation method according to claim 2, wherein the reaction temperature of the high-temperature reaction in the step (3) is 1000 to 1200 ℃, and the reaction time is 10 to 60 min; the argon flow is 130-180 sccm, and the oxygen flow is 13-18 sccm.
4. The method according to claim 1, wherein the sputtering in step (2) is performed using a magnetron sputtering apparatus in which a part of the upper part of the p-GaN substrate is masked with an aluminum foil paper before sputtering; the sputtering target is an AlN target with the specification of 60 multiplied by 3mm, the air pressure of the cavity is 1-4 Pa, the flow of argon is 30-50 sccm, the flow of nitrogen is 5-10 sccm, the sputtering power is 80-150W, and the sputtering time is 5-30 min; and (3) sputtering equipment is an ion sputtering instrument, the sputtering target material is an Ag target material, the specification is 50 multiplied by 3mm, the working gas is nitrogen, the air pressure of the cavity is 40-60 Pa, the sputtering power is 10-60W, and the sputtering time is 5-80 s.
5. The method for preparing the metal electrode according to claim 1, wherein the method for preparing the metal electrode in the step (4) is a magnetron sputtering method or an electron beam evaporation method, and two layers of electrodes are respectively plated at one end of the p-GaN and one end of the n-ZnO nanorod to form the Ni/Au alloy electrode.
6. The ZnO nanorod array light-emitting diode prepared by the preparation method of any one of claims 1-5.
7. The ZnO nanorod array light emitting diode of claim 6, wherein the p-GaN substrate is 2-10 μm thick and has a hole concentration of 1017～1019/cm3Hole mobility of 5-100 cm2/V·s。
8. The ZnO nanorod array of claim 6The column light-emitting diode is characterized in that the electron concentration of the n-ZnO nano-rod is 1017～1019/cm3Electron mobility of 5-100 cm2/V·s。
9. The ZnO nanorod array light-emitting diode of claim 6, wherein the AlN thin film has a thickness of 5-50 nm, and the Ag nanoparticles have a particle size of 5-30 nm.
10. The ZnO nanorod array light emitting diode of claim 6, wherein the metal electrode at one end of the n-ZnO nanorod array is a cathode, the metal electrode at one end of the p-GaN nanorod array is an anode, and the thickness of the metal electrode is 20-40 nm.
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| CN110323311B (en) * | 2019-06-12 | 2020-11-03 | 北京大学 | LED point light source based on graphene/ZnO nanowire/p-GaN film and preparation method thereof |
| CN110379897A (en) * | 2019-07-01 | 2019-10-25 | 东南大学 | III group-III nitride Quantum Well-metal-quantum dot mixed white light LED component |
| CN110808315A (en) * | 2019-09-29 | 2020-02-18 | 北京工业大学 | Method for increasing GaN Micro-LED color conversion efficiency |
| CN113540299B (en) * | 2021-06-30 | 2023-06-30 | 东南大学 | Based on p-GaN/CsPbBr 3 Light-emitting diode with n-ZnO heterojunction and preparation method thereof |
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