CN108493309A - A kind of nano-pillar ultraviolet LED and the preparation method and application thereof - Google Patents
A kind of nano-pillar ultraviolet LED and the preparation method and application thereof Download PDFInfo
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- 239000002061 nanopillar Substances 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 69
- 229910002704 AlGaN Inorganic materials 0.000 claims abstract description 54
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 34
- 239000000758 substrate Substances 0.000 claims abstract description 24
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 18
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims description 51
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 28
- 230000004888 barrier function Effects 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 24
- RGGPNXQUMRMPRA-UHFFFAOYSA-N triethylgallium Chemical compound CC[Ga](CC)CC RGGPNXQUMRMPRA-UHFFFAOYSA-N 0.000 claims description 22
- 229910052681 coesite Inorganic materials 0.000 claims description 20
- 229910052906 cristobalite Inorganic materials 0.000 claims description 20
- 229910052682 stishovite Inorganic materials 0.000 claims description 20
- 229910052905 tridymite Inorganic materials 0.000 claims description 20
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 15
- 238000005530 etching Methods 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 12
- 239000010439 graphite Substances 0.000 claims description 12
- 230000012010 growth Effects 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 11
- 239000013256 coordination polymer Substances 0.000 claims description 8
- 239000005543 nano-size silicon particle Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229910015844 BCl3 Inorganic materials 0.000 claims description 6
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 4
- 238000010168 coupling process Methods 0.000 claims description 4
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- JOTBHEPHROWQDJ-UHFFFAOYSA-N methylgallium Chemical compound [Ga]C JOTBHEPHROWQDJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004528 spin coating Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000002242 deionisation method Methods 0.000 claims 1
- 230000005701 quantum confined stark effect Effects 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 16
- 239000000463 material Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 4
- 239000000084 colloidal system Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 230000003698 anagen phase Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000012826 global research Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000011856 silicon-based particle Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- H01L33/0062—Processes for devices with an active region comprising only III-V compounds
- H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
- H01L33/007—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound comprising nitride compounds
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- Engineering & Computer Science (AREA)
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- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
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- Condensed Matter Physics & Semiconductors (AREA)
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- Led Devices (AREA)
Abstract
The invention belongs to the technical field of semiconductor, a kind of nano-pillar ultraviolet LED and the preparation method and application thereof is disclosed.The preparation method is that one layer of nanometer silicon dioxide particle is arranged on the surface of ultraviolet LED epitaxial wafer to etch a nanometer rod structure on ultraviolet LED epitaxial wafer then using nanometer silicon dioxide particle as mask, to obtain nano-pillar ultraviolet LED.The nano-pillar ultraviolet LED includes successively from the bottom to top substrate, overlay Al layers, AlN layers, AlGaN layer, u GaN layers, n GaN layers, Quantum Well nano-pillar and p GaN nano-pillars.The nano-pillar ultraviolet LED of the present invention discharges the stress of LED Quantum Well, weakens quantum confined stark effect, enhances LED component performance.In addition, preparation method is simple by the present invention, the complex steps and cost for making mask are avoided, and can be by using the SiO of varying particle size2To adjust the size of nano-pillar.
Description
Technical field
The invention belongs to the technical fields of semiconductor, and in particular to a kind of nano-pillar UV LED (LED) and its
Preparation method and application.The nano-pillar LED of the present invention is for fields such as LED, LD, photodetector, solar cells.
Background technology
With the rapid development of LED technology, the luminescence band of LED has all been widely applied to quotient from green light to ultraviolet light
On industry product, in recent years, the wide application prospect of ultraviolet LED (UV-LED) is constantly excavated by people, has attracted many people that will grind
Study carefully emphasis to shift to it, also becomes the new hot spot of global research and investment of the same trade.Ultraviolet LED is due to small, knot
The features such as structure is simple, high speed, and Wavelength tunable, energy are high and service life is long, energy saving, environmentally protective, in white solid state photograph
The fields such as bright, optical storage, ink printing, water and air purification, biomedicine, environmental protection are widely used.And ultraviolet LED
There is lot of advantages compared with ultraviolet mercury lamp, get a good chance of that existing mercury lamp is replaced to become follow-on ultraviolet source, have huge
Big society and economic value.
But compared to the LED of bluish-green optical band, UV-LED quantum efficiencies and power are all universal relatively low, become it and move towards production
The bottleneck of industry.The reason of this is mainly due to two aspects, ultraviolet LED generally uses AlGaN to shine as active area first
Layer, but high quality AlGaN material is prepared with great difficulty, on the one hand it is that there are more serious for material in epitaxial process
Lattice mismatch, occur reaction it is more complex and uncontrollable, be on the other hand AlGaN material greater band gap, exist doping and
The all relatively low equal physical problems of activation efficiency.In addition, problem drops in a kind of also efficiency of generally existing suddenly in the led, when LED operation exists
When under low current, efficiency will soon become to be saturated with the increase of electric current, further increase Injection Current, luminous efficiency meeting
Drastically decline, the problem of dropping is commonly referred to as quantum confined Stark phenomenon suddenly for the efficiency of this LED, this phenomenon mainly due to
Caused by piezoelectric polarization in Quantum Well, and the piezoelectric polarization effect in AlGaN Quantum Well is stronger, it limits ultra-violet light-emitting
The luminous power of diode restricts ultraviolet LED in various applications.Therefore, the critical issue of ultraviolet LED application is pushed just
It is the quantum efficiency and power of ultraviolet LED to be improved.
Invention content
It is an object of the invention to overcome the defect of the above-mentioned prior art, a kind of nano-pillar ultraviolet LED and its preparation are provided
Method.The present invention passes through SiO2It is coated with technology and prepares nano-pillar ultraviolet LED.The nano-pillar ultraviolet LED of the present invention discharges LED amounts
The stress of sub- trap enhances LED component performance to weaken quantum confined stark effect.
Another object of the present invention is to provide the applications of above-mentioned nano-pillar ultraviolet LED.The nano-pillar ultraviolet LED application
In fields such as LED, LD, photodetector, solar cells.
To achieve the above object, the present invention adopts the following technical scheme that：
The present invention nano-pillar ultraviolet LED, from the bottom to top successively include substrate, overlay Al layers, AlN layers, AlGaN layer, u-
GaN layer, n-GaN layers, Quantum Well nano-pillar and p-GaN nano-pillars；The Quantum Well nano-pillar is InGaN/GaN-1/
AlGaN/GaN-2 Quantum Well nano-pillars, GaN-1 and GaN-2 are barrier layer, and InGaN is well layer, and the periodicity of Quantum Well is 5-10
A, the first layer of Quantum Well and last layer are GaN barrier layer.What GaN-1 was indicated is GaN layer, and what GaN-2 was indicated is GaN layer.
The thickness for overlaying Al layers is 1-5nm, and AlN layers of thickness is 100-300nm, and the thickness of AlGaN layer is 300-
900nm, u-GaN layers of thickness is 500-1000nm, and n-GaN layers of thickness is 1000-3000nm；Quantum well layer nano-pillar is
The thickness of InGaN/GaN-1/AlGaN/GaN-2 Quantum Well nano-pillars, wherein GaN-1 and GaN-2 are 3-7nm, and AlGaN thickness is
1-3nm, InGaN thickness are 2-5nm, and period of Quantum Well is 5-10 period, the first layer of Quantum Well nano-pillar and last
Layer is GaN barrier layer；The thickness of p-GaN nano-pillars is 200-400nm.
The preparation method of the nano-pillar ultraviolet LED is that one layer of nanometer titanium dioxide is arranged on the surface of ultraviolet LED epitaxial wafer
Silicon particle etches a nanometer rod structure then using nanometer silicon dioxide particle as mask on ultraviolet LED epitaxial wafer, to obtain
Obtain nano-pillar ultraviolet LED.
The preparation method of the nano-pillar ultraviolet LED, specifically includes following steps：
(1) on substrate successively growth overlay Al layers (Al layers), AlN layers, AlGaN layer, u-GaN layers, n-GaN layers, quantum
Well layer and p-GaN layer obtain ultraviolet LED film, that is, ultraviolet LED epitaxial wafer；
(2) in p-GaN layer one layer of nano silicon dioxide of spin coating colloidal solution, remove solvent, formed in p-GaN layer
One layer of nanometer silicon dioxide particle layer；It uses sense coupling method and is circle with nanometer silicon dioxide particle layer
The mask of column figure, successively performs etching p-GaN layer and quantum well layer, after Quantum Well etching is complete, obtains Quantum Well and receives
Rice column and p-GaN nano-pillars；Nanometer silicon dioxide particle layer is removed, nano-pillar ultraviolet LED is obtained.
The thickness for overlaying Al layers is 1-5nm, and AlN layers of thickness is 100-300nm, and the thickness of AlGaN layer is 300-
The thickness of 900nm, undoped GaN layer (u-GaN layers) are 500-1000nm, and N-shaped adulterates the thickness of GaN film layer (n-GaN layers)
For 1000-3000nm；Quantum well layer is InGaN/GaN-1/AlGaN/GaN-2 Quantum Well, the thickness of wherein GaN-1 and GaN-2
For 3-7nm, AlGaN thickness is 1-3nm, and InGaN thickness is 2-5nm, is built the well layer 5-10 period of repeated growth, first layer and most
Later layer is GaN barrier layer；The thickness of p-type doped gan layer (p-GaN layer) is 200-400nm.
It is room temperature, vacuum drying or heat drying that solvent is removed described in step (2)；
The grain size of nano silicon dioxide is 500-1000nm in the colloidal solution of nano silicon dioxide, and solvent is water or second
Alcohol, SiO2Mass fraction in the solution is 2-15wt%.
It refers to being put into the ultraviolet LED after the completion of etching to remove nanometer silicon dioxide particle layer described in step (2)
It is cleaned by ultrasonic in ionized water, removes SiO2。
The etching gas etched in step (2) is Cl2/BCl3。
Each film layer is prepared using the method for MOCVD in step (1).Substrate described in step (1) is Si substrates.
The specific preparation method of ultraviolet LED film, includes the following steps in step (1)：
(a) substrate is positioned in MOCVD, extension a layer thickness overlays Al layers for 1-5nm on substrate：Underlayer temperature
It it is 700-100 DEG C, chamber pressure 40-100Torr, graphite disk rotating speed is 600-1200r/min, trimethyl aluminium (TMAl)
Flow is 200-300sccm；
(b) the AlN nucleation film layers that a layer thickness is grown on Al layers for 100-300nm are overlay what step (a) obtained
(AlN layers)：Underlayer temperature is 900-1200 DEG C, chamber pressure 40-100Torr, and graphite disk rotating speed is 1000-1200r/
The flow of min, TMAl are 200-400sccm, ammonia (NH3) flow be 5-20slm；
(c) 300-900nm AlGaN film layers are grown on the AlN layers that step (b) obtains：Underlayer temperature is 1000-
1200 DEG C, chamber pressure 40-100Torr, graphite disk rotating speed is 1000-1200r/min, and the flow of TMAl is 200-
The flow of 400sccm, trimethyl gallium (TMGa) are 50-200sccm, NH3Flow be 5-20slm；
(d) the undoped GaN layers of 500-1000nm (u-GaN layers), technique item are grown in the AlGaN layer that step (c) obtains
Part is：Underlayer temperature is 1000-1200 DEG C, and the flow of chamber pressure 100-200Torr, TMGa are 200-500sccm,
NH3Flow be 10-30slm；
(e) 1000-3000nm N-shapeds doping GaN film layer (n-GaN is grown on the undoped GaN that step (d) obtains
Layer), process conditions are：Underlayer temperature is 1000-1200 DEG C, and chamber pressure 100-200Torr is passed through TMGa, NH3、
SiH4, the flow of TMGa is 200-500sccm, SiH4Flow be 100-300sccm, NH3Flow be 10-30slm；Doping
Electron concentration 5.0 × 1018-5.0×1019cm-3；
(f) InGaN/GaN-1/AlGaN/GaN-2 Quantum Well is grown in the N-shaped doping GaN film that step (e) obtains,
Process conditions are：GaN-1 and GaN-2 is barrier layer, GaN-1 and GaN-2 when preparing the condition of each barrier layer be：Underlayer temperature is 800-
850 DEG C, chamber pressure 100-200Torr, it is passed through triethyl-gallium (TEGa) and NH3, the flow of TEGa is 200-
600sccm, NH3Flow be 10-30slm, thickness 3-7nm；AlGaN barrier layer, underlayer temperature are 800-850 DEG C, reative cell
Pressure is 100-200Torr, is passed through TMAl, TEGa and NH3, the flow of TMAl is 1-50sccm, and the flow of TEGa is 200-
600sccm, NH3Flow be 10-30slm, thickness 1-3nm；InGaN well layer, underlayer temperature are 750-850 DEG C, reative cell
Pressure is 100-200Torr, is passed through TEGa, TMIn and NH3, the flow of TEGa is 200-500sccm, and the flow of TMIn is 100-
500sccm, NH3Flow be 30-100slm, thickness 2-5nm；Build well layer 5-10 period of repeated growth, first layer and most
Later layer is GaN barrier layer；
(g) the p-type doping of the InGaN/GaN-1/AlGaN/GaN-2 quantum trap growths 200-400nm obtained in step (f)
GaN film, process conditions are：Underlayer temperature be 900-1200 DEG C, chamber pressure 100-200Torr, be passed through TMGa,
CP2Mg and NH3, the flow of TMGa is 100-300sccm, CP2The flow of Mg is 300-900sccm, NH3Flow be 20-
80slm；Adulterate hole concentration 2.0 × 1016-8.0×1018cm-3。
Nano-pillar ultraviolet LED prepared by the present invention can improve the quantum efficiency and power of ultraviolet LED.The luminous effect of LED
Rate includes light extraction efficiency and internal quantum efficiency, and the principal element for influencing light extraction efficiency of LED is to be happened inside GaN material
Internal reflection, nanometer rod structure LED materially increases the sidewall area of material, to increase photon escape angle,
Effectively reduce the luminous energy loss brought by total reflection；In addition, nanometer rod structure has been also equipped with the guiding role to light path,
The light extraction efficiency of luminescent material can further be promoted.Secondly, nanostructure because have passed through multi-quantum well active region to
So that the surface volume of active area increases, the part stress inside Quantum Well is effectively released, is reduced caused by stress
Piezoelectric field reduces quantum confined stark effect, to improve the internal quantum efficiency of ultraviolet LED.
The present invention need not prepare the mask of nano-scale, cost directly using nanometer silicon dioxide particle as mask
It is low, it is easy to accomplish industrialization, and nanometer rod structure is uniform in ultraviolet LED, effect is good.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention uses SiO2It is coated with technology, with the SiO of dispersion2Nano particle is as mask, using inductive couple plasma
Body lithographic technique prepares nano-pillar ultraviolet LED.Preparation method is simple, avoid make mask complex steps and at
This, and can be by using the SiO of varying particle size2To adjust the size of nano-pillar.Prepared nanometer rod structure
Ultraviolet LED materially increases the sidewall area of material, simultaneously effective releases the part stress inside Quantum Well,
To improve the internal quantum efficiency and luminous power of ultraviolet LED.
Description of the drawings
Fig. 1 is the nano-pillar ultraviolet LED epitaxial structure schematic diagram of the present invention；Wherein, substrate -1, overlay Al layers -2, AlN
Layer -3, AlGaN layer -4, u-GaN layers -5, n-GaN layers -6, Quantum Well -7, p-GaN-8；
Fig. 2 is to be coated with SiO on LED epitaxial films in embodiment 12Then the technique that etching prepares nano-pillar ultraviolet LED
Flow chart；
Fig. 3 is the luminescence generated by light collection of illustrative plates of nano-pillar ultraviolet LED epitaxial wafer prepared by embodiment 1；
Fig. 4 is the internal quantum efficiency figure of nano-pillar ultraviolet LED epitaxial wafer prepared by embodiment 1.
Specific implementation mode
With reference to specific embodiments and the drawings, the present invention is described in further detail, but the embodiment party of the present invention
Formula is without being limited thereto.
The structural schematic diagram of the nano-pillar ultraviolet LED (epitaxial wafer) of the present invention is as shown in Figure 1, include lining successively from the bottom to top
Bottom 1 overlays Al layers 2, AlN layers 3, AlGaN layer 4, u-GaN layers 5, n-GaN layers 6, Quantum Well nano-pillar 7 and p-GaN nano-pillars
8。
The Quantum Well nano-pillar 7 is InGaN/GaN-1/AlGaN/GaN-2 Quantum Well nano-pillars, and GaN-1 and GaN-2 are
Barrier layer, InGaN are well layer, and the periodicity of Quantum Well is 5-10, and the first layer of Quantum Well and last layer are GaN barrier layer.
What GaN-1 was indicated is GaN layer, and what GaN-2 was indicated is GaN layer.
The thickness for overlaying Al layers is 1-5nm, and AlN layers of thickness is 100-300nm, and the thickness of AlGaN layer is 300-
The thickness of 900nm, undoped GaN layer (u-GaN layers) are 500-1000nm, and N-shaped adulterates the thickness of GaN film layer (n-GaN layers)
For 1000-3000nm；Quantum well layer nano-pillar be InGaN/GaN-1/AlGaN/GaN-2 Quantum Well nano-pillars, wherein GaN-1 and
The thickness of GaN-2 is 3-7nm, and AlGaN thickness is 1-3nm, and InGaN thickness is 2-5nm, builds 5-10 week of well layer repeated growth
Phase, first layer and last layer are GaN barrier layer；The thickness of p-GaN nano-pillars is 200-400nm.
Embodiment 1
Include successively from the bottom to top Si substrates 1 as shown in Figure 1, the nano-pillar ultraviolet LED of the present embodiment, overlay Al layers 2,
AlN layers 3, AlGaN layer 4, u-GaN layers 5, n-GaN layers 6, Quantum Well 7, p-GaN8.
The preparation method of the nano-pillar ultraviolet LED, includes the following steps：
1) Si substrates are placed into MOCVD, extension a layer thickness overlays Al layers for 3nm on substrate：Underlayer temperature
It it is 900 DEG C, chamber pressure 50Torr, graphite disk rotating speed is 1200r/min, and the flow of TMAl is 300sccm；
2) the AlN nucleating layers (AlN layers) that a layer thickness is grown on Al layers for 300nm are overlay what step (1) obtained：Substrate
Temperature is 1200 DEG C, chamber pressure 60Torr, and graphite disk rotating speed is 1200r/min, and the flow of TMAl is 350sccm, NH3
Flow be 15slm；
3) 600nm AlGaN film layers (AlGaN layer) are grown on the AlN films (AlN layers) that step (2) obtains：Substrate
Temperature is 1200 DEG C, chamber pressure 100Torr, and graphite disk rotating speed is 1200r/min, and the flow of TMAl is 400sccm, three
The flow of methyl gallium (TMGa) is 60sccm, NH3Flow be 15slm；
4) the undoped GaN layers of 1000nm (u-GaN layers) are grown on the AlGaN that step (3) obtains, process conditions are：Lining
Bottom temperature is 1100 DEG C, and the flow of chamber pressure 200Torr, TMGa are 300sccm, NH3Flow be 20slm；
5) 3000nm N-shapeds doping GaN film (n- is grown in the undoped GaN layer (u-GaN layers) that step (4) obtains
GaN layer), process conditions are：Underlayer temperature is 1100 DEG C, and chamber pressure 200Torr is passed through TMGa, NH3、SiH4, TMGa
Flow be 350sccm, SiH4Flow be 300sccm, NH3Flow be 15slm；Adulterate electron concentration 2.0 × 1019cm-3；
6) the grown quantum trap film (InGaN/GaN-1/ in the N-shaped doping GaN film (n-GaN layers) that step (5) obtains
AlGaN/GaN-2 Quantum Well), process conditions are：The condition of GaN-1 and GaN-2 barrier layer, GaN-1 and GaN-2 each barrier layer when preparing
For：Underlayer temperature is 850 DEG C, chamber pressure 200Torr, is passed through triethyl-gallium (TEGa) and NH3, the flow of TEGa is
400sccm, NH3Flow be 30slm, thickness 6nm；AlGaN barrier layer, underlayer temperature are 850 DEG C, and chamber pressure is
200Torr is passed through TMAl, TEGa and NH3, the flow of TMAl is 20sccm, and the flow of TEGa is 400sccm, NH3Flow be
30slm, thickness 2nm；InGaN well layer, underlayer temperature be 800 DEG C, chamber pressure 200Torr, be passed through TEGa, TMIn with
NH3, the flow of TEGa is 400sccm, and the flow of TMIn is 200sccm, NH3Flow be 60slm, thickness 3nm；Build well layer
In 9 periods of repeated growth, first layer and last layer are GaN barrier layer；
(7) p-type of the InGaN/GaN-1/AlGaN/GaN-2 quantum trap growths 400nm obtained in step (6) adulterates GaN
Film (p-GaN film layers), process conditions are：Underlayer temperature is 900 DEG C, and chamber pressure 200Torr is passed through TMGa, CP2Mg
With NH3, the flow of TMGa is 300sccm, CP2The flow of Mg is 600sccm, NH3Flow be 50slm；Adulterate hole concentration
5.0×1018cm-3；LED epitaxial films are obtained at this time；
(8) the LED epitaxial films that step (7) obtains are placed in sol evenning machine, 10ml is coated in p-GaN film surfaces
SiO2Film surface is completely covered in colloidal solution, solution；Sol evenning machine rotary speed is 1000r/min, and rotational time is
30s；SiO will have been coated2The film of colloidal solution waits for solvent to volatilize completely in room temperature 6h；Used SiO2Colloid is molten
Liquid SiO2Grain diameter is 500nm, etoh solvent, SiO2Mass fraction in the solution is 5wt%；
(9) film that step (8) obtains is placed in sense coupling equipment, needs to etch before etching
Cavity is evacuated to 10-5Pa, etching gas Cl2And BCl3, Cl2Throughput is 80sccm, BCl3Throughput is 10sccm, is carved
It is 20 minutes to lose the time, and quantum well segment is run through, Quantum Well nano-pillar and p-GaN nano-pillars are obtained；It, will be outer after having etched
Prolong piece and be put into deionized water and clean 6min with ultrasonic machine, removes SiO2。
The present invention is with SiO2Particle can be used as mask layer to protect surface, and SiO2The gap of particle can then be etched, thus meeting
Nano-pillar is etched, scale depends on SiO2Grain size.
The preparation of embodiment 1 is coated with SiO on LED epitaxial films2Then etching prepares the technological process of nano-pillar ultraviolet LED
Figure is as shown in Figure 2.
The luminescence generated by light collection of illustrative plates of nano-pillar ultraviolet LED epitaxial wafer prepared by embodiment 1 is as shown in Figure 3.
The internal quantum efficiency figure of nano-pillar ultraviolet LED epitaxial wafer prepared by embodiment 1 is as shown in Figure 4.
Embodiment 2
The nano-pillar ultraviolet LED of the present embodiment includes successively from the bottom to top Si substrates, overlays Al layers, AlN layers, AlGaN
Layer, u-GaN layers, n-GaN layers, Quantum Well, p-GaN.
The preparation method of the nano-pillar ultraviolet LED, includes the following steps：
1) Si substrates are placed into MOCVD, extension a layer thickness overlays Al layers for 3nm on substrate：Underlayer temperature
It it is 900 DEG C, chamber pressure 50Torr, graphite disk rotating speed is 1200r/min, and the flow of TMAl is 300sccm；
2) the AlN nucleating layers (AlN layers) that a layer thickness is grown on Al layers for 300nm are overlay what step (1) obtained：Substrate
Temperature is 1200 DEG C, chamber pressure 60Torr, and graphite disk rotating speed is 1200r/min, and the flow of TMAl is 350sccm, NH3
Flow be 15slm；
3) 600nm AlGaN film layers (AlGaN layer) are grown on the AlN films (AlN layers) that step (2) obtains：Substrate
Temperature is 1200 DEG C, chamber pressure 100Torr, and graphite disk rotating speed is 1200r/min, and the flow of TMAl is 400sccm, three
The flow of methyl gallium (TMGa) is 60sccm, NH3Flow be 15slm；
4) the undoped GaN layers of 1000nm (u-GaN layers), technique are grown on the AlGaN (AlGaN layer) that step (3) obtains
Condition is：Underlayer temperature is 1100 DEG C, and the flow of chamber pressure 200Torr, TMGa are 300sccm, NH3Flow be
20slm；
5) 3000nm N-shapeds doping GaN film (n-GaN is grown on the undoped GaN (u-GaN layers) that step (4) obtains
Layer), process conditions are：Underlayer temperature is 1100 DEG C, and chamber pressure 200Torr is passed through TMGa, NH3、SiH4, the stream of TMGa
Amount is 350sccm, SiH4Flow be 300sccm, NH3Flow be 15slm.Adulterate electron concentration 2.0 × 1019cm-3；
6) InGaN/GaN-1/AlGaN/GaN-2 is grown in the N-shaped doping GaN film (n-GaN layers) that step (5) obtains
Quantum Well, process conditions are：The condition of each barrier layer is when GaN-1 and GaN-2 barrier layer, GaN-1 and GaN-2 preparations：Underlayer temperature
It is 850 DEG C, chamber pressure 200Torr, is passed through triethyl-gallium (TEGa) and NH3, the flow of TEGa is 400sccm, NH3's
Flow is 30slm, thickness 5nm；AlGaN barrier layer, underlayer temperature be 850 DEG C, chamber pressure 200Torr, be passed through TMAl,
TEGa and NH3, the flow of TMAl is 20sccm, and the flow of TEGa is 400sccm, NH3Flow be 30slm, thickness 2nm；Trap
Layer, underlayer temperature are 800 DEG C, and chamber pressure 200Torr is passed through TEGa, TMIn and NH3, the flow of TEGa is
The flow of 400sccm, TMIn are 150sccm, NH3Flow be 60slm, thickness 3nm.Well layer 5 periods of repeated growth are built,
First layer and last layer are GaN barrier layer；
(7) p-type of the InGaN/GaN-1/AlGaN/GaN-2 quantum trap growths 400nm obtained in step (6) adulterates GaN
Film (p-GaN film layers), process conditions are：Underlayer temperature is 900 DEG C, and chamber pressure 200Torr is passed through TMGa, CP2Mg
With NH3, the flow of TMGa is 300sccm, CP2The flow of Mg is 600sccm, NH3Flow be 50slm；Adulterate hole concentration
5.0×1018cm-3；
(8) the LED epitaxial films that step (7) obtains are placed in sol evenning machine, 10ml is coated in p-GaN film surfaces
SiO2Film surface is completely covered in colloidal solution, solution；Sol evenning machine rotary speed is 1000r/min, and rotational time is
30s；SiO will have been coated2The film of colloidal solution waits for solvent to volatilize completely in room temperature 6h；Used SiO2Colloid is molten
Liquid SiO2Grain diameter is 900nm, etoh solvent, SiO2Mass fraction in the solution is 5wt%；
(9) film that step (8) obtains is placed in sense coupling equipment, needs to etch before etching
Cavity is evacuated to 10-5Pa, etching gas Cl2And BCl3, Cl2Throughput is 80sccm, BCl3Throughput is 10sccm, is carved
It is 20 minutes to lose the time, and quantum well segment is run through, Quantum Well nano-pillar and p-GaN nano-pillars are obtained；It, will be outer after having etched
Prolong piece and be put into deionized water and clean 6min with ultrasonic machine, removes SiO2.The performance of nano-pillar ultraviolet LED manufactured in the present embodiment
It is similar to Example 1.
The grain size of nano silicon dioxide is 500-1000nm in the colloidal solution of nano silicon dioxide in the present invention, and solvent is
Water or ethyl alcohol, SiO2Mass fraction in the solution is 2-15wt%.Spin coating SiO of the present invention2Colloidal solution, solution are completely covered
Film surface.Sol evenning machine rotary speed is 200-5000r/min, rotational time 10-100s.SiO will have been coated2Colloid
The film of solution waits for solvent to volatilize completely in 5~12h of room temperature, or vacuum drying, 1~2h of heating, drying.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by the embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of nano-pillar ultraviolet LED, it is characterised in that：Include successively from the bottom to top substrate, overlay Al layers, AlN layers, AlGaN
Layer, u-GaN layers, n-GaN layers, Quantum Well nano-pillar and p-GaN nano-pillars；The Quantum Well nano-pillar is InGaN/GaN-1/
AlGaN/GaN-2 Quantum Well nano-pillars, GaN-1 and GaN-2 are barrier layer, and InGaN is well layer, and GaN-1 and GaN-2 are GaN layers.
2. nano-pillar ultraviolet LED according to claim 1, it is characterised in that：The thickness for overlaying Al layers is 1-5nm, AlN layers
Thickness is 100-300nm, and the thickness of AlGaN layer is 300-900nm, and u-GaN layers of thickness is 500-1000nm, n-GaN layers
Thickness is 1000-3000nm；Quantum well layer nano-pillar is InGaN/GaN-1/AlGaN/GaN-2 Quantum Well nano-pillars, wherein
The thickness of GaN-1 and GaN-2 is 3-7nm, and AlGaN thickness is 1-3nm, and InGaN thickness is 2-5nm, and the period of Quantum Well is 5-
In 10 periods, the first layer of Quantum Well nano-pillar and last layer are GaN barrier layer；The thickness of p-GaN nano-pillars is 200-
400nm。
3. the preparation method of nano-pillar ultraviolet LED according to claim 1 or claim 2, it is characterised in that：It is in ultraviolet LED extension
One layer of nanometer silicon dioxide particle is arranged in the surface of piece, then using nanometer silicon dioxide particle as mask, in ultraviolet LED epitaxial wafer
On etch a nanometer rod structure, to obtain nano-pillar ultraviolet LED.
4. the preparation method of nano-pillar ultraviolet LED according to claim 3, it is characterised in that：Include the following steps：
(1) on substrate successively growth overlay Al layers, AlN layers, AlGaN layer, u-GaN layers, n-GaN layers, quantum well layer and p-
GaN layer obtains ultraviolet LED film, that is, ultraviolet LED epitaxial wafer；
(2) in p-GaN layer one layer of nano silicon dioxide of spin coating colloidal solution, remove solvent, in p-GaN layer formed one layer
Nanometer silicon dioxide particle layer；Use sense coupling method and using nanometer silicon dioxide particle layer as cylinder
The mask of shape, successively performs etching p-GaN layer and quantum well layer, after Quantum Well etching is complete, obtains Quantum Well nano-pillar
And p-GaN nano-pillars；Nanometer silicon dioxide particle layer is removed, nano-pillar ultraviolet LED is obtained.
5. the preparation method of nano-pillar ultraviolet LED according to claim 4, it is characterised in that：
The thickness that Al layers are overlay in step (1) is 1-5nm, and AlN layers of thickness is 100-300nm, and the thickness of AlGaN layer is 300-
900nm, u-GaN layers of thickness is 500-1000nm, and n-GaN layers of thickness is 1000-3000nm；Quantum well layer is InGaN/
The thickness of GaN-1/AlGaN/GaN-2 Quantum Well, wherein GaN-1 and GaN-2 is 3-7nm, and AlGaN thickness is 1-3nm, InGaN
Thickness is 2-5nm, and the period of Quantum Well is 5-10 period, and the first layer of Quantum Well and last layer are GaN barrier layer；p-
The thickness of GaN layer is 200-400nm.
6. the preparation method of nano-pillar ultraviolet LED according to claim 4, it is characterised in that：Removal described in step (2) is molten
Agent is room temperature, vacuum drying or heat drying；
The grain size of nano silicon dioxide is 500-1000nm in the colloidal solution of nano silicon dioxide, and solvent is water or ethyl alcohol, SiO2
Mass fraction in the solution is 2-15wt%；
It refers to that the ultraviolet LED after the completion of etching is put into deionization to remove nanometer silicon dioxide particle layer described in step (2)
It is cleaned by ultrasonic in water, removes SiO2；
The etching gas etched in step (2) is Cl2/BCl3。
7. the preparation method of nano-pillar ultraviolet LED according to claim 4, it is characterised in that：Each film layer uses in step (1)
It is prepared by the method for MOCVD；
Substrate described in step (1) is Si substrates.
8. the preparation method of nano-pillar ultraviolet LED according to claim 4, it is characterised in that：Ultraviolet LED is thin in step (1)
The specific preparation method of film, includes the following steps：
(a) substrate is positioned in MOCVD, extension a layer thickness overlays Al layers for 1-5nm on substrate：Underlayer temperature is
700-100 DEG C, chamber pressure 40-100Torr, graphite disk rotating speed is 600-1200r/min, and the flow of trimethyl aluminium is
200-300sccm；
(b) the AlN layers that a layer thickness is grown on Al layers for 100-300nm are overlay what step (a) obtained：Underlayer temperature is 900-
1200 DEG C, chamber pressure 40-100Torr, graphite disk rotating speed is 1000-1200r/min, and the flow of TMAl is 200-
The flow of 400sccm, ammonia are 5-20slm；
(c) 300-900nm AlGaN film layers are grown on the AlN layers that step (b) obtains：Underlayer temperature is 1000-1200 DEG C,
Chamber pressure is 40-100Torr, and graphite disk rotating speed is 1000-1200r/min, and the flow of TMAl is 200-400sccm, three
The flow of methyl gallium is 50-200sccm, NH3Flow be 5-20slm；
(d) the undoped GaN layers of 500-1000nm are grown in the AlGaN layer that step (c) obtains, process conditions are：Underlayer temperature
It it is 1000-1200 DEG C, the flow of chamber pressure 100-200Torr, TMGa are 200-500sccm, NH3Flow be 10-
30slm；
(e) n-GaN layers of 1000-3000nm is grown on the undoped GaN that step (d) obtains, process conditions are：Underlayer temperature
It it is 1000-1200 DEG C, chamber pressure 100-200Torr is passed through TMGa, NH3、SiH4, the flow of TMGa is 200-
500sccm, SiH4Flow be 100-300sccm, NH3Flow be 10-30slm；Adulterate electron concentration 5.0 × 1018-5.0
×1019cm-3；
(f) InGaN/GaN-1/AlGaN/GaN-2 Quantum Well, technique are grown in the N-shaped doping GaN film that step (e) obtains
Condition is：The condition of each barrier layer is when GaN-1 and GaN-2 barrier layer, GaN-1 and GaN-2 preparations：Underlayer temperature is 800-850 DEG C,
Chamber pressure is 100-200Torr, is passed through triethyl-gallium and NH3, the flow of TEGa is 200-600sccm, NH3Flow be
10-30slm, thickness 3-7nm；AlGaN barrier layer, underlayer temperature are 800-850 DEG C, chamber pressure 100-200Torr, are led to
Enter TMAl, TEGa and NH3, the flow of TMAl is 1-50sccm, and the flow of TEGa is 200-600sccm, NH3Flow be 10-
30slm, thickness 1-3nm；InGaN well layer, underlayer temperature are 750-850 DEG C, and chamber pressure 100-200Torr is passed through
TEGa, TMIn and NH3, the flow of TEGa is 200-500sccm, and the flow of TMIn is 100-500sccm, NH3Flow be 30-
100slm, thickness 2-5nm；It builds the well layer 5-10 period of repeated growth, first layer and last layer are GaN barrier layer；
(g) p-type of the InGaN/GaN-1/AlGaN/GaN-2 quantum trap growths 200-400nm obtained in step (f) adulterates GaN
Film, process conditions are：Underlayer temperature is 900-1200 DEG C, and chamber pressure 100-200Torr is passed through TMGa, CP2Mg with
NH3, the flow of TMGa is 100-300sccm, CP2The flow of Mg is 300-900sccm, NH3Flow be 20-80slm；Doping
Hole concentration 2.0 × 1016-8.0×1018cm-3。
9. the preparation method of nano-pillar ultraviolet LED according to claim 3, it is characterised in that：Prepare nano-pillar ultraviolet LED
Method is used to prepare LED, LD, photodetector and/or solar cell with nanometer rod structure.
10. the application of nano-pillar ultraviolet LED according to claim 1 or claim 2, it is characterised in that：The nano-pillar ultraviolet LED is used
In LED, LD, photodetector and/or area of solar cell.
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