CN106601884B - Zno-based nano rod/compound UV LED of Quantum Well and preparation method thereof - Google Patents
Zno-based nano rod/compound UV LED of Quantum Well and preparation method thereof Download PDFInfo
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- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 2
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- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 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
- H01L33/02—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
- H01L33/04—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 with a quantum effect structure or superlattice, e.g. tunnel junction
- H01L33/06—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 with a quantum effect structure or superlattice, e.g. tunnel junction within the light emitting region, e.g. quantum confinement structure or tunnel barrier
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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
- H01L33/12—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 with a stress relaxation structure, e.g. buffer layer
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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
- H01L33/14—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 with a carrier transport control structure, e.g. highly-doped semiconductor layer or current-blocking structure
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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 kind of zno-based nano rod/compound UV LED of Quantum Well and preparation method thereof, which includes substrate, is successively arranged N-shaped ZnO film layer, ZnO nano bar array, ZnO/Zn on substrate from the bottom up1‑xMgxO mqw active layer, p-type NiO film layer and first electrode；Second electrode and ZnO nano bar array are located at side by side on N-shaped ZnO film layer；ZnO/Zn1‑ xMgxO mqw active layer clading ZnO nano bar array, and 0.1≤x≤0.3.The light emitting diode electroluminescent peak wavelength is near 374nm, luminous peak width is about 17nm, the light emitting diode construction can give full play to the advantages such as the direct broad-band gap of ZnO material and high exciton bind energy, effectively weaken polarity effect, improves material and interface quality, increase active layer effective area, promote light extraction efficiency, improve spectrum monochromaticjty, and it can realize low temperature preparation, it is low in cost, it is easy to accomplish industrialization.
Description
Technical field
The present invention relates to opto-electronic devices, in particular to a kind of zno-based nano rod/compound UV LED of Quantum Well
And preparation method thereof.
Background technique
Light emitting diode (LED) is the light-emitting component made of semiconductor material, is a kind of solid-state electroluminescent cold light source.
Due to light emitting diode have low energy consumption and it is environmental-friendly the features such as, large-scale application can reduce the high-carbon energy such as coal oil
Source consumption, meets the theory of sustainable development requirement and low-carbon economy.Light emitting diode is low in energy consumption with its, the service life is long, light efficiency is high,
Numerous advantages such as radiationless, good portability, receive great favor, and correlative study and industry have obtained great support and hair
Exhibition.In LED research field, the realization and development of ultraviolet (Ultraviolet, the UV) LED of short wavelength is related fields scientific research people
One of the hot spot of member and industrial circle concern, it is considered to be the another of LED applies the New World after white light, and prospect is very happy
It sees.Although having some uses aluminum gallium nitride (AlGaN) and aluminium gallium nitrogen (InAlGaN) at present as active layer material prepares UV
The report of LED, but generally existing fault in material density is excessive, monochromaticjty is not good enough, luminous efficiency is relatively low, service life is too short, I
The problems such as state's core patented technology lacks, and UV LED is in optic communication, day-old chick detection, biological medicine, printing packaging, high density
Storage etc. fields huge applications demand make related scientific issues solution and product technology research and development it is extremely urgent.
ZnO is a kind of II-VI group direct band gap semiconductor material with wide forbidden band, and the forbidden bandwidth of ZnO is 3.37eV at room temperature,
Corresponding emission wavelength is near 370nm, in ultraviolet wavelength range.Lattice structure, cell parameter and the forbidden bandwidth of ZnO
It is similar to conventional photo functional material gallium nitride (GaN), but ZnO has fusing point more higher than GaN and bigger exciton confinement
Can, and have lower luminescence generated by light and stimulated radiation threshold and good electromechanical coupling characteristics, thermal stability and chemistry steady
Qualitative, material is easy to get, preparation cost is cheap, environmental-friendly.Thus, ZnO is considered as the ideal alternative materials of GaN, in shortwave
Application in terms of long light emitting diode, laser and related photoelectric device has huge potentiality.In addition, by carrying out magnesium to ZnO
(Mg) it adulterates, its forbidden bandwidth is adjusted, realize energy band engineering；And the lattice of low-doped magnesium zinc (ZnMgO) and ZnO lose
It is small with spending, it can be applied to ZnO/ZnMgO quantum well structure, expanded the application field of ZnO material.
At present there are also about using ZnO as the report of ultraviolet light emitting device material, such as: Chinese patent application
200810120346.X disclosing a kind of ZnO based LED of multiple quantum wells, the Zn provided1-xMgxO/Zn1-yCdyO volume
Sub- trap active layer is conventional planar structure, has compared with strong polarity effect, and active layer limited area, influences its luminous efficiency.It should
The Zinc oxide single crystal substrate that scheme provides is with high costs, and monocrystalline substrate then will lead to strong lattice mismatch, influence active
Layer material quality, the good high quality p-type ZnO of this external stability are still that current industry makes great efforts the important problem solved, and there is also move
The problems such as shifting rate, carrier concentration are relatively low and stability is poor.In addition, Liu Weizhen (ZnO nano-wire heterojunction ultraviolet light emitting
The device research Changchun [D]: Northeast Normal University, 2013.) use pulse laser deposition and hydro-thermal method to be prepared for MgZnO/ZnO core
Shell heterogeneous structural nano linear array, and luminescent device is constituted with p-type GaN.The ZnO nano-wire that the program prepares hydro-thermal method as
Light-emitting active layer, more defect and impurity will seriously affect luminous efficiency.
Generally speaking, the existing generally existing following problems of zno-based ultraviolet light emitting device: 1) lattice mismatch and polarity effect
It is lower that caused quantu m_confined Stark effect results in light emitting diode internal quantum efficiency；2) poor interface quality and material
Deep energy level caused by defect shines, and causes LED ultraviolet monochromatic poor；3) light extraction efficiency caused by traditional planar structure is inclined
It is low；4) preparation process is complicated, condition control is stringent, needs preparation cost caused by the factors such as high temperature preparation high.It is aforementioned these
Problem limits the application of zno-based ultra-violet light-emitting device.
Summary of the invention
Present invention aim to provide a kind of zno-based nano rod/compound UV LED of Quantum Well and its system
Preparation Method, the UV LED good luminous performance realize the pure ultraviolet electroluminescent hair that luminous peak position is located near 374nm
Light.
To achieve the above object, the technical solution adopted by the present invention is that: a kind of zno-based nano rod/Quantum Well is compound ultraviolet
Light emitting diode, including substrate are successively arranged N-shaped ZnO film layer, ZnO nano bar array, ZnO/ on the substrate from the bottom up
Zn1-xMgxO mqw active layer, p-type NiO film layer and first electrode；Second electrode and the ZnO nano bar array position arranged side by side
In on the N-shaped ZnO film layer；The ZnO/Zn1-xMgxO mqw active layer coats the ZnO nano bar array, and 0.1
≤x≤0.3。
Further, the ZnO/Zn1-xMgxO mqw active layer by 2~10 periods ZnO film and Zn1-xMgxO
Film alternating deposit forms.
Further, the first electrode is Au, Pt, Pt/Ni or Au/Ni.
Further, the second electrode is In, Al, Ga or Ag.
Further, the substrate is Sapphire Substrate.
A kind of preparation method of zno-based nano rod/compound UV LED of Quantum Well, comprising the following steps:
1) substrate is cleaned；
2) N-shaped ZnO film layer is sputtered using rf magnetron sputtering technique on substrate；
3) ZnO nano bar array is grown on N-shaped ZnO film layer using hydro-thermal method；
4) replace ZnO Thin Films Sputtered and Zn on the ZnO nano bar array using rf magnetron sputtering technique1-xMgxO
Film forms the ZnO/Zn being coated on the ZnO nano bar array1-xMgxO mqw active layer；
5) in the ZnO/Zn1-xMgxReactive sputtering p-type NiO film layer on O mqw active layer；
6) first electrode is plated in the p-type NiO thin-film surface using rf magnetron sputtering technique, and in the N-shaped
ZnO film layer edge plates second electrode.
Further, in the step 2), sputtering target material is ZnO:Al ceramic target, background air pressure≤10 when sputtering-3Pa, lining
Bottom temperature is 200~400 DEG C, and air pressure is 0.5~8Pa when deposition, and sputter gas Ar, sputtering power is 20~150W, sputtering
Time is 5~20min.
Further, in the step 3), hydro-thermal method prepare the presoma that the ZnO nano bar array uses for 0.01~
The zinc nitrate hexahydrate and hexa mixed solution of 0.1mol/L, hydrothermal temperature are 80~120 DEG C, the reaction time
For 1~3h.
Further, in the step 4), the sputtering target material of the ZnO film is ZnO ceramic target, the Zn1-xMgxO is thin
The sputtering target material of film is Mg and ZnO hybrid target, and the area ratio of Mg metallic target and ZnO ceramic target is 1:0.5~1.5；When sputtering
Background air pressure≤10-3Pa, underlayer temperature are 200~400 DEG C, and air pressure is 0.5~8Pa, relative partial pressure of oxygen O when deposition2/(O2+
It Ar) is 15~40%, sputtering power is 20~150W, the ZnO film and the Zn1-xMgxEvery layer of sputtering time of O film is 1
~3min.
Further, in the step 5), sputtering target material is Ni metallic target, relative partial pressure of oxygen O2/(O2+ Ar) be 50~
70%, cavity background air pressure≤10 before sputtering-3Pa, underlayer temperature are 150~250 DEG C, and sputtering pressure is 0.5~8Pa, sputtering
20~150W of power, sputtering time are 20~60min.
The present invention is acted on using quantum confinement possessed by ZnO quantum well structure, while it is exclusive to introduce ZnO nano material
Small-size effect and skin effect combine the quantum well structure (ZnO/ZnMgO) based on ZnO with ZnO 1-dimention nano bar, shape
At ZnO nano bar/Quantum Well core-shell structure as light-emitting active layer, the ZnO base LED based on the structure is constructed, it is real
Existing luminous peak position is located at the pure UV electroluminescence near 374nm and shows following advantage compared with prior art:
First, weakening polarity effect: the characteristics of utilizing ZnO nano bar material, in ZnO nano bar outgrowth Quantum Well knot
Structure, the isoepitaxial growth film on its lateral non-polar m face, can substantially weaken polarity effect；Nano material is big simultaneously
Specific surface area can preferably discharge inter-laminar stress, so that lattice mismatch big at heterogeneous interface is eased, further
The effect is reduced, to obtain device performance boost.
Second, improving material and interface quality: when ZnO is having certain lattice mismatched substrate surface heterogeneous medium nucleating growth
When, there is highest energy to cause its strong tendency in forming three-dimensional column structure in (0001) face, be formed in film a large amount of
Crystal boundary simultaneously accumulates a large amount of defect and impurity, it is difficult to and even curface is obtained, the application of quantum well structure is unfavorable for, and it is of the invention
It can get the ZnO film of low defect density and high-crystal quality and the high quality heterogeneous structure material that surface is smooth, interface is precipitous,
Improve radiative recombination rate.
Third, increasing active layer effective area: quantum well structure is prepared on the basis of One-Dimensional ZnO nano material substantially to be increased
Add the effective area of quantum well layer, it may be assumed that the region of light-emitting active layer is significantly increased, it is achieved that the exciton of higher efficiency radiates
Recombination luminescence.
Fourth, promoting light extraction efficiency: in view of the reflection of ZnO nano bar hexagonal column structure and upper and lower surface, passing through
Reasonable optical design can be such that its light extraction efficiency is improved to promote the luminescent properties of device entirety.
Fifth, being conducive to improve spectrum monochromaticjty: the optical waveguide effect of ZnO nano bar/Quantum Well core-shell structure
The lasing of Whispering-gallery-mode or Fabry-Perot modes can be caused to shine.Optical resonator is formed in material internal, and light is having
Lattice scattering occurs in active layer and forms optical circuit, population inversion can be achieved after reaching threshold value, compared to two pole of Conventional luminescent
Pipe, the design for not needing specific resonant cavity can substantially reduce luminous peak width, improve spectrum monochromaticjty.
Sixth, low temperature preparation can be realized: zno-based nano rod of the present invention/Quantum Well compound UV LED whole
The temperature of preparation link is can be controlled within 400 DEG C, substantially lower than 1000 DEG C of mainstream GaN base light emitting semiconductor device or more
Preparation temperature smoothly realizes low temperature preparation, is conducive to cost control and the application of associated materials.
Seventh, the N-shaped ZnO film using growth on a sapphire substrate, is both the good seed of ZnO nano bar growth
Layer and ZnO/Zn1-xMgxThe electron injecting layer of O mqw active layer, double action are beneficial to simplify preparation process, reduce life
Produce cost.
Eighth, forbidden bandwidth is bigger with respect to ZnO at room temperature using p-type NiO as hole injection layer, give full play to
The super injection advantage of hetero-junctions；Meanwhile there are Ni in NiO film2+Vacancy, so that natural hole is presented at room temperature and leads for film
Electricity, the influence so as to avoid excessive doping to crystal quality.
Ninth, the present invention prepares mqw active layer using rf magnetron sputtering system, organise relative to common metal
Object chemical gas-phase deposition system is closed, cost is greatly reduced, and is advantageously implemented industrialization production.
Detailed description of the invention
Fig. 1 is a kind of zno-based nano rod/Quantum Well compound UV LED structural schematic diagram.
Fig. 2 is zno-based nano rod/Quantum Well compound UV LED room temperature electroluminescent made from embodiment 1
Spectrogram.
Fig. 3 is zno-based nano rod/Quantum Well compound UV LED room temperature electroluminescent made from embodiment 2
Spectrogram.
Fig. 4 is zno-based nano rod/Quantum Well compound UV LED room temperature electroluminescent made from embodiment 3
Spectrogram.
Specific embodiment
The following further describes the present invention in detail with reference to the accompanying drawings and specific embodiments, convenient for more clearly understanding this
Invention, but they limiting the invention.
The zno-based nano rod as shown in Figure 1/compound UV LED of Quantum Well, including substrate 1, substrate 1 are blue precious
Stone lining bottom is successively arranged N-shaped ZnO film layer 2, ZnO nano bar array 3, ZnO/Zn on substrate 1 from the bottom up1-xMgxO Quantum Well
Active layer 4, p-type NiO film layer 5 and first electrode 6；Second electrode 7 and ZnO nano bar array 3 are located at N-shaped ZnO film side by side
On layer 2；ZnO/Zn1-xMgx4 clading ZnO nano bar array 3 of O mqw active layer, and 0.1≤x≤0.3, ZnO/Zn1-xMgxO amount
Sub- trap active layer 4 by 2~10 periods ZnO film and Zn1-xMgxO film alternating deposit forms.First electrode 6 be Au, Pt,
Pt/Ni or Au/Ni, second electrode 7 are In, Al, Ga or Ag.Zno-based nano rod/Quantum Well compound UV LED system
Standby process sees below Examples 1 to 3.
Embodiment 1
1) substrate cleans: using sapphire as substrate, be cut into 15mm × 15mm size, using acetone, alcohol and
Deionized water is cleaned by ultrasonic 3min respectively, finally uses N2Drying.
2) Sapphire Substrate after surface clean the preparation of N-shaped ZnO film layer: is put into the life of rf magnetron sputtering system
In long room, growth room is evacuated to background air pressure 5 × 10-4Pa, heating substrate to temperature are 200 DEG C.Select AZO ceramic target
The target of (ZnO:Al ceramic target) as depositing n-type ZnO film layer.Before plated film, pre-sputtering 10min is to remove target material surface
Impurity, then using radio frequency magnetron sputtering method depositing n-type ZnO film layer on a sapphire substrate.Deposition substrate temperature 200
DEG C, gas is argon gas, air pressure 0.5Pa, sputtering power 60W, sputtering time 20min when deposition.
3) preparation of ZnO nano bar array: the sample of N-shaped ZnO film layer is placed in Zn (NO sputtering3)2·6H2O and six
Methenamine concentration is that hydro-thermal reaction is carried out in the precursor solution of 0.01mol/L, and hydro-thermal reaction occurs closed anti-
It answers in kettle, reaction temperature is 100 DEG C, reaction time 2h, after reaction, sample is taken out and ultrasound 5s is residual to remove reaction
It stays, is then cleaned with a large amount of deionized waters, finally use N2Drying is placed in heating furnace, is annealed under the conditions of 400 DEG C in air
30min。
4)ZnO/Zn1-xMgxThe growth of O mqw active layer: the sample that grown ZnO nano bar array is put into
In the growth room of rf magnetron sputtering system, growth room is evacuated to background air pressure 5 × 10-4Pa, heating substrate to temperature are 200
DEG C, it selects ZnO ceramic target as the target of deposition ZnO potential well layer, selects the mixing target conduct of Mg metallic target and ZnO ceramic target
Deposit Zn1-xMgxThe target of O barrier layer, wherein the area ratio of Mg metallic target and ZnO ceramic target is 2:3, the preparation of this condition
Zn1-xMgxX=0.1 in O layers；Before plated film, then pre-sputtering 10min uses radio-frequency magnetic to remove the impurity of target material surface
Control the method sputtered alternating deposit ZnO film layer on the sample that successively growth has N-shaped ZnO film layer and ZnO nano bar array
And Zn0.9Mg0.1O film layer forms the ZnO/Zn in 10 periods0.9Mg0.1O mqw active layer, 200 DEG C of deposition substrate temperature,
Air pressure 0.5Pa when deposition, relative partial pressure of oxygen O2/(O2+ Ar) be 40%, sputtering power 60W, 1min/ layers of sputtering time.
5) preparation of p-type NiO: using the method for reactive sputtering in ZnO/Zn0.9Mg0.1Continue to sink on O mqw active layer
Product p-type NiO film, before plated film, for pre-sputtering 5min to remove the impurity of target material surface, target selects the W metal of high-purity
Target, background air pressure 5 × 10-4Pa, 150 DEG C of deposition substrate temperature, deposition pressure 0.5Pa, relative partial pressure of oxygen O2/(O2+ Ar) be
50%, sputtering power 120W, sputtering time 30min.
6) N-shaped ZnO film layer, ZnO nano bar array, ZnO/Zn will the preparation of electrode: be sequentially prepared0.9Mg0.1O quantum
The sample covering metal mask version of trap active layer, p-type NiO film, is put into the growth room of rf magnetron sputtering, growth room takes out true
Sky is to background air pressure 5 × 10-4Pa, heating substrate to temperature are 100 DEG C.Select Au metallic target as deposition first electrode (Au electricity
Pole) target.Before plated film, pre-sputtering 10s is to remove the impurity of target material surface.Then existed using radio frequency magnetron sputtering method
It is covered with deposition first electrode (Au electrode) on the p-type NiO film of metal mask version.100 DEG C of deposition substrate temperature；Gas when deposition
Body is Ar gas, air pressure 0.5Pa；Sputtering power 20W；Sputtering time 40s.Continue to plate In on the N-shaped ZnO of substrate surface as the
Two electrodes.
The electroluminescent hair of the nano rod of zno-based made from the present embodiment 1/compound UV LED of Quantum Well is measured at room temperature
Light spectrogram is as shown in Figure 2.
Embodiment 2
1) substrate cleans: using sapphire as substrate, being cut into 15mm × 15mm size, using acetone, alcohol is gone
Ionized water is cleaned by ultrasonic 3min respectively, finally uses N2Drying.
2) Sapphire Substrate after surface clean the preparation of N-shaped ZnO film layer: is put into the life of rf magnetron sputtering system
In long room, growth room is evacuated to background air pressure 1 × 10-4Pa, heating substrate to temperature are 400 DEG C.Select the conduct of AZO ceramic target
The target of depositing n-type ZnO film layer.Before plated film, pre-sputtering 10min is to remove the impurity of target material surface, then using penetrating
Frequency magnetically controlled sputter method depositing n-type ZnO film layer on a sapphire substrate；400 DEG C of deposition substrate temperature, gas is Ar when deposition
Gas, air pressure 5.0Pa, sputtering power 150W, sputtering time 5min.
3) sample that sputtering has N-shaped ZnO film the preparation of ZnO nano bar array: is placed in Zn (NO3)2·6H2O and six is sub-
Tetramine concentration is in the precursor solution of 0.1mol/L.The reaction temperature in closed reaction kettle occurs for hydro-thermal reaction
It is 80 DEG C, reaction time 3h.After, sample is taken out and ultrasound 5s is to remove reaction residual, then with a large amount of deionizations
Water cleaning, finally uses N2Drying is placed in heating furnace, and anneal under the conditions of 400 DEG C 30min in air.
4)ZnO/Zn1-xMgxThe growth of O mqw active layer: the sample that grown ZnO nano bar array is put into
In the growth room of rf magnetron sputtering system, growth room is evacuated to background air pressure 1 × 10-4Pa, heating substrate to temperature are 400
℃.It selects ZnO ceramic target as the target of deposition ZnO potential well layer, selects the mixing target conduct of Mg metallic target and ZnO ceramic target
Deposit Zn1-xMgxThe target of O barrier layer, wherein the area ratio of Mg metallic target and ZnO ceramic target is 1:1, the preparation of this condition
Zn1-xMgxX=0.18 in O layers.Before plated film, pre-sputtering 10min is to remove the impurity of target material surface.Then radio-frequency magnetic is used
Control the method sputtered alternating deposit ZnO film layer on the sample that successively growth has N-shaped ZnO film layer and ZnO nano bar array
And Zn0.82Mg0.18O film layer forms the ZnO/Zn in 2 periods0.82Mg0.18O mqw active layer.Deposition substrate temperature 400
℃；Air pressure 5.0Pa when deposition；Relative partial pressure of oxygen O2/(O2+ Ar) it is 15%；Sputtering power 150W；2min/ layers of sputtering time.
5) preparation of p-type NiO: using the method for reactive sputtering in ZnO/Zn0.82Mg0.18Continue to sink on O mqw active layer
Product p-type NiO film.Before plated film, pre-sputtering 5min is to remove the impurity of target material surface.The W metal of target selection high-purity
Target, background air pressure 1 × 10-4Pa, 200 DEG C of deposition substrate temperature；Deposition pressure 8.0Pa；Relative partial pressure of oxygen O2/(O2+ Ar) be
60%；Sputtering power 150W, sputtering time 20min.
6) N-shaped ZnO, ZnO nano bar array, ZnO/Zn will the preparation of electrode: be sequentially prepared0.82Mg0.18O Quantum Well has
Active layer, the sample covering metal mask version of p-type NiO film, are put into the growth room of rf magnetron sputtering, growth room is evacuated to
Background air pressure 1 × 10-4Pa, heating substrate to temperature are 100 DEG C.Select Pt metallic target as deposition first electrode (Pt electrode)
Target.Before plated film, pre-sputtering 10s is to remove the impurity of target material surface.Then it is being covered using radio frequency magnetron sputtering method
There is deposition first electrode (Pt electrode) on the p-type NiO film of metal mask version.100 DEG C of deposition substrate temperature；Gas is when deposition
Ar gas, air pressure 0.8Pa；Sputtering power 30W；Sputtering time 30s.Continue to plate Ga on the N-shaped ZnO of substrate surface as the second electricity
Pole.
The electroluminescent hair of the nano rod of zno-based made from the present embodiment 2/compound UV LED of Quantum Well is measured at room temperature
Light spectrogram is as shown in Figure 3.
Embodiment 3
1) substrate cleans: using sapphire as substrate, being cut into 15mm × 15mm size, using acetone, alcohol is gone
Ionized water is cleaned by ultrasonic 3min respectively, finally uses N2Drying.
2) Sapphire Substrate after surface clean the preparation of N-shaped ZnO film layer: is put into the life of rf magnetron sputtering system
In long room, growth room is evacuated to background air pressure 1 × 10-3Pa, heating substrate to temperature are 300 DEG C.Select the conduct of AZO ceramic target
The target of depositing n-type ZnO film layer.Before plated film, pre-sputtering 10min is to remove the impurity of target material surface.Then using penetrating
Frequency magnetically controlled sputter method depositing n-type ZnO film layer on a sapphire substrate.300 DEG C of deposition substrate temperature, gas is Ar when deposition
Gas, air pressure 8.0Pa, sputtering power 20W, sputtering time 15min.
3) sample that sputtering has N-shaped ZnO film the preparation of ZnO nano bar array: is placed in Zn (NO3)2·6H2O and six is sub-
Tetramine concentration is in the precursor solution of 0.05mol/L.The reaction temperature in closed reaction kettle occurs for hydro-thermal reaction
It is 120 DEG C, reaction time 1h.After, sample is taken out and ultrasound 5s is to remove reaction residual, then with a large amount of deionizations
Water cleaning, finally uses N2Drying is placed in heating furnace, and anneal under the conditions of 400 DEG C 30min in air.
4)ZnO/Zn1-xMgxThe growth of O mqw active layer: the sample that grown ZnO nano bar array is put into
In the growth room of rf magnetron sputtering system, growth room is evacuated to background air pressure 1 × 10-3Pa, heating substrate to temperature are 300
℃.It selects ZnO ceramic target as the target of deposition ZnO potential well layer, selects the mixing target conduct of Mg metallic target and ZnO ceramic target
Deposit Zn1-xMgxThe target of O barrier layer, wherein the area ratio of Mg metallic target and ZnO ceramic target is 2:1, the preparation of this condition
Zn1-xMgxX=0.3 in O layers.Before plated film, pre-sputtering 10min is to remove the impurity of target material surface.Then radio-frequency magnetic is used
Control the method sputtered alternating deposit ZnO film layer on the sample that successively growth has N-shaped ZnO film layer and ZnO nano bar array
And Zn0.7Mg0.3O film layer forms the ZnO/Zn in 8 periods0.7Mg0.3O mqw active layer.300 DEG C of deposition substrate temperature；It is heavy
Air pressure 8.0Pa when product；Relative partial pressure of oxygen O2/(O2+ Ar) it is 70%；Sputtering power 20W；3min/ layers of sputtering time.
5) preparation of p-type NiO: using the method for reactive sputtering in ZnO/Zn0.7Mg0.3Continue to sink on O mqw active layer
Product p-type NiO film.Before plated film, pre-sputtering 5min is to remove the impurity of target material surface.The W metal of target selection high-purity
Target, background air pressure 1 × 10-3Pa, 250 DEG C of deposition substrate temperature；Deposition pressure 5.0Pa；Relative partial pressure of oxygen O2/(O2+ Ar) be
60%；Sputtering power 20W, sputtering time 60min.
6) N-shaped ZnO, ZnO nano bar array, ZnO/Zn will the preparation of electrode: be sequentially prepared0.7Mg0.3O Quantum Well is active
The sample covering metal mask version of layer, p-type NiO film, is put into the growth room of rf magnetron sputtering, growth room is evacuated to this
Spirit pressure 1 × 10-3Pa, heating substrate to temperature are 100 DEG C.Select Ni metallic target and Pt metallic target as the first electricity of deposition respectively
The target of pole (Pt/Ni electrode).Before plated film, pre-sputtering 10s is to remove the impurity of target material surface.Then radio frequency magnetron is used
Sputtering method is sequentially depositing Ni film and Pt film as first electrode on the p-type NiO film for being covered with metal mask version
(Pt/Ni electrode).100 DEG C of deposition substrate temperature；Gas is Ar gas, air pressure 0.5Pa when deposition；Sputtering power 20W；Ni film and
The sputtering time of Pt film is respectively 20s and 40s.Continue to plate Ag on the N-shaped ZnO of substrate surface as second electrode.
The electroluminescent hair of the nano rod of zno-based made from the present embodiment 3/compound UV LED of Quantum Well is measured at room temperature
Light spectrogram is as shown in Figure 4.
From the embodiment of the present invention as can be seen that nano rod/Quantum Well composite construction ZnO UV LED of preparation
With preferable luminescent properties, the light emitting diode issue peak position be located at wavelength 374 (± 2) nm, the peak width that shines for 17 (±
8) UV electroluminescence of nm.
Claims (9)
1. a kind of zno-based nano rod/compound UV LED of Quantum Well, including substrate (1), it is characterised in that: the lining
N-shaped ZnO film layer (2), ZnO nano bar array (3), ZnO/Zn are successively arranged on bottom (1) from the bottom up1-xMgxO Quantum Well has
Active layer (4), p-type NiO film layer (5) and first electrode (6)；Second electrode (7) and the ZnO nano bar array (3) position arranged side by side
In on the N-shaped ZnO film layer (2)；The ZnO/Zn1-xMgxO mqw active layer (4) coats the ZnO nano bar array
And 0.1≤x≤0.3 (3),；
The zno-based nano rod/Quantum Well compound UV LED preparation method, comprising the following steps:
1) substrate is cleaned；
2) N-shaped ZnO film layer is sputtered using rf magnetron sputtering technique on substrate；
3) ZnO nano bar array is grown on N-shaped ZnO film layer using hydro-thermal method；
4) replace ZnO Thin Films Sputtered and Zn on the ZnO nano bar array using rf magnetron sputtering technique1-xMgxO film shape
At the ZnO/Zn being coated on the ZnO nano bar array1-xMgxO mqw active layer；
5) in the ZnO/Zn1-xMgxReactive sputtering p-type NiO film layer on O mqw active layer；
6) first electrode is plated in the p-type NiO thin-film surface using rf magnetron sputtering technique, and thin in the N-shaped ZnO
Film layer edge plates second electrode；
The ZnO/Zn1-xMgxO mqw active layer (4) by 2~10 periods ZnO film and Zn1-xMgxO film is alternately heavy
Product forms.
2. zno-based nano rod/compound UV LED of Quantum Well according to claim 1, it is characterised in that: described
One electrode (6) is Au, Pt, Pt/Ni or Au/Ni.
3. zno-based nano rod/compound UV LED of Quantum Well according to claim 1, it is characterised in that: described
Two electrodes (7) are In, Al, Ga or Ag.
4. zno-based nano rod/compound UV LED of Quantum Well according to claim 1, it is characterised in that: the lining
Bottom (1) is Sapphire Substrate.
5. a kind of zno-based nano rod/Quantum Well compound UV LED preparation method, comprising the following steps:
1) substrate is cleaned；
2) N-shaped ZnO film layer is sputtered using rf magnetron sputtering technique on substrate；
3) ZnO nano bar array is grown on N-shaped ZnO film layer using hydro-thermal method；
4) replace ZnO Thin Films Sputtered and Zn on the ZnO nano bar array using rf magnetron sputtering technique1-xMgxO film shape
At the ZnO/Zn being coated on the ZnO nano bar array1-xMgxO mqw active layer；
5) in the ZnO/Zn1-xMgxReactive sputtering p-type NiO film layer on O mqw active layer；
6) first electrode is plated in the p-type NiO thin-film surface using rf magnetron sputtering technique, and thin in the N-shaped ZnO
Film layer edge plates second electrode.
6. zno-based nano rod/Quantum Well compound UV LED preparation method according to claim 5, feature
Be: in the step 2), sputtering target material is ZnO:Al ceramic target, background air pressure≤10 when sputtering-3Pa, underlayer temperature 200
~400 DEG C, air pressure is 0.5~8Pa when deposition, sputter gas Ar, and sputtering power is 20~150W, sputtering time is 5~
20min。
7. special according to the zno-based nano rod of claim 5 or 6/Quantum Well compound UV LED preparation method
Sign is: in the step 3), hydro-thermal method prepares presoma that the ZnO nano bar array uses as 0.01~0.1mol/L's
Zinc nitrate hexahydrate and hexa mixed solution, hydrothermal temperature are 80~120 DEG C, and the reaction time is 1~3h.
8. special according to the zno-based nano rod of claim 5 or 6/Quantum Well compound UV LED preparation method
Sign is: in the step 4), the sputtering target material of the ZnO film is ZnO ceramic target, the Zn1-xMgxThe sputtering target of O film
Material is Mg and ZnO hybrid target, and the area ratio of Mg metallic target and ZnO ceramic target is 1:0.5~1.5；Background air pressure when sputtering≤
10-3Pa, underlayer temperature are 200~400 DEG C, and air pressure is 0.5~8Pa, relative partial pressure of oxygen O when deposition2/(O2+ Ar) be 15~
40%, sputtering power is 20~150W, the ZnO film and the Zn1-xMgxEvery layer of sputtering time of O film is 1~3min.
9. special according to the zno-based nano rod of claim 5 or 6/Quantum Well compound UV LED preparation method
Sign is: in the step 5), sputtering target material is Ni metallic target, relative partial pressure of oxygen O2/(O2+ Ar) it is 50~70%, before sputtering
Cavity background air pressure≤10-3Pa, underlayer temperature be 150~250 DEG C, sputtering pressure be 0.5~8Pa, 20~150W of sputtering power,
Sputtering time is 20~60min.
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