CN104952986B - A kind of preparation method of GaN base white light LEDs epitaxial structure - Google Patents
A kind of preparation method of GaN base white light LEDs epitaxial structure Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 45
- 150000004678 hydrides Chemical class 0.000 claims abstract description 29
- 239000000919 ceramic Substances 0.000 claims abstract description 21
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 18
- 238000000407 epitaxy Methods 0.000 claims abstract description 16
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 15
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 14
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 13
- 229910002704 AlGaN Inorganic materials 0.000 claims abstract description 11
- 230000004888 barrier function Effects 0.000 claims abstract description 11
- 238000012545 processing Methods 0.000 claims abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 104
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 46
- 229910021529 ammonia Inorganic materials 0.000 claims description 40
- 229910052757 nitrogen Inorganic materials 0.000 claims description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 21
- 239000001257 hydrogen Substances 0.000 claims description 21
- 229910052739 hydrogen Inorganic materials 0.000 claims description 21
- 229910052710 silicon Inorganic materials 0.000 claims description 21
- 239000010703 silicon Substances 0.000 claims description 21
- 239000012159 carrier gas Substances 0.000 claims description 20
- 150000002431 hydrogen Chemical class 0.000 claims description 14
- 230000003746 surface roughness Effects 0.000 claims description 10
- 229910052779 Neodymium Inorganic materials 0.000 claims description 7
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 7
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 7
- 229910052693 Europium Inorganic materials 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 238000005915 ammonolysis reaction Methods 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 2
- 230000001934 delay Effects 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 18
- 239000000843 powder Substances 0.000 abstract description 11
- 238000000034 method Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 abstract description 4
- 235000012431 wafers Nutrition 0.000 abstract 2
- 230000003252 repetitive effect Effects 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 27
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 24
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 20
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 description 10
- 229910017083 AlN Inorganic materials 0.000 description 9
- 238000004140 cleaning Methods 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 229910052769 Ytterbium Inorganic materials 0.000 description 4
- 238000005121 nitriding Methods 0.000 description 4
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- 238000004528 spin coating Methods 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- -1 hydrogen Compound Chemical class 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 241001025261 Neoraja caerulea Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012546 transfer Methods 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
- H01L33/005—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
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Microelectronics & Electronic Packaging (AREA)
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- Computer Hardware Design (AREA)
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- Crystallography & Structural Chemistry (AREA)
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- Led Devices (AREA)
Abstract
A kind of preparation method of GaN base white light LEDs epitaxial structure, comprises the following steps：Using hydride gas-phase epitaxy monocrystalline or polycrystalline aluminum nitride cushion are prepared on rare earth doped YAG ceramics or single crystalline substrate；GaN base LED epitaxial structure is grown on the monocrystalline or polycrystalline aluminum nitride cushion using metal organic chemical vapor deposition, wherein, GaN base LED epitaxial structure is followed successively by low temperature GaN buffer, high-temperature gan layer, N-type GaN layer, InGaN/GaN multi-quantum well active regions, AlGaN electronic barrier layers, p-type GaN layer and highly dope p-type or highly doped contact electrode layer from bottom to top.GaN base white light LEDs epitaxial structure prepared by the present invention can be controlled very precisely the optics such as doping, thickness and quality of fluorescent material special type and physical characteristic, realize that repetitive rate is very high, the extraordinary fluorescent material of the uniformity integrates, and solve the problems, such as in conventional fluorescent powder coating procedure on same wafer between diverse location and different wafers because inevitable fluorescence powder content caused by processing technology is uneven.
Description
Technical field：
The present invention relates to field of photoelectric technology, and in particular to a kind of preparation method of GaN base white light LEDs epitaxial structure.
Background technology：
After Nakamura in 1991 etc. successfully develops GaN blue-ray LEDs, have high efficiency, small size, the long-life,
The green GaN base LED for waiting good characteristic has obtained unprecedented development, has extremely wide application prospect.At present, white light
The mode of LED generally use blue LED excited yellow fluorescent material produces white light.Fluorescent powder coating technique can be divided mainly into 3 kinds：Envelope
(dispensing) technique is sprayed on the single blue-light LED chip installed, spin coating proceeding and is being sealed in whole wafer before chip cutting
The small plate technique of long-distance fluorescent powder is added in assembling structure.
In traditional spraying (dispensing) technique, after fluorescent material mixes with colloid, it is applied directly in LED chip.This envelope
Many the defects of being difficult to overcome be present in dress technique, for example, because fluorescent material is different from colloid proportion, the fluorescent material during dispensing
It can precipitate, so as to cause also have larger difference in the parameters such as colour temperature, colour rendering index even if the LED light source that same batch makes.
Can solve the problems, such as fluorescent material precipitation to a certain extent using spin coating proceeding, but the limitation due to spin coating proceeding in itself, i.e.,
Make the thickness of same wafer different zones fluorescent material, concentration also difference.It result between last white chip and chip
Colour temperature have differences, reduce product yield.
There is also problem for both above-mentioned traditional handicrafts in terms of radiating.Fluorescent material produces in photon frequency conversion process
Heat have to pass through chip and transmit substrate, then pass through heat sink radiating.Total coefficient of heat conduction by material each time and
Thermal conduction characteristic between material influences.Heat transfer efficiency is not high, influences light efficiency and the life-span of white light LEDs.
Long-distance fluorescent powder technology (Remote Phosphor) can alleviate fluorescence caused by color shift, arogel proportion difference
The problems such as powder precipitates.Due to being filled between fluorescent material and LED chip by the relatively low gas of thermal conductivity or colloid, in phosphor material powder
Heat effectively can not be dispersed by LED packaging heat sinks, will also result in device color shift, light efficiency reduces, service life reduction.
Therefore, it is badly in need of a kind of novel white-light LED manufacture crafts, solves phenomena such as phosphor material powder is uneven, by heat deterioration,
Simplify packaging technology simultaneously, improve yield, reduce production cost.
The content of the invention：
The invention aims to solve above-mentioned technical problem, there is provided a kind of system of GaN base white light LEDs epitaxial structure
A kind of Preparation Method, the GaN base white light LEDs epitaxial wafer grown on the YAG ceramics or single crystalline substrate of novel rare-earth element doping, leads to
White-light LED chip without fluorescent powder coating technique can be obtained by crossing traditional die processing technology.
To reach above-mentioned purpose, the present invention, which adopts the following technical scheme that, to be achieved：
A kind of preparation method of GaN base white light LEDs epitaxial structure, comprises the following steps：
Monocrystalline is prepared on rare earth doped YAG ceramics or single crystalline substrate or polycrystalline nitrogenizes using hydride gas-phase epitaxy
Aluminium cushion；
Grown using metal organic chemical vapor deposition on the monocrystalline or polycrystalline aluminum nitride cushion outside GaN base LED
Prolong structure, wherein, GaN base LED epitaxial structure be followed successively by from bottom to top low temperature GaN buffer, high-temperature gan layer, N-type GaN layer,
InGaN/GaN multi-quantum well active regions, AlGaN electronic barrier layers, p-type GaN layer and highly dope p-type or highly doped electrode
Contact layer.
Further improve of the invention is, in the rare earth doped YAG ceramics or single crystalline substrate, rare earth element bag
The one or more in Ce, Eu, Nd, Yb are included, doping concentration is 0.05at% to 0.5at%, and substrate thickness is 100 μm to 1000
μm, YAG ceramics or single-crystal surface as substrate are less than 0.5nm by fine polishing, its surface roughness.
Further improve of the invention is, by hydride gas-phase epitaxy in rare earth doped YAG ceramics or monocrystalline
Monocrystalline or polycrystalline aluminum nitride cushion are prepared on substrate, its concrete operations is：
First, rare earth doped YAG ceramics or single crystalline substrate are toasted under hydrogen, is subsequently passed ammonia and carries out high temperature
Nitrogen treatment；
Finally, hydrogen chloride and ammonia are each led into silicon source area and reative cell, the rare earth member after high-temperature ammonolysis processing
The growth of monocrystalline or polycrystalline aluminum nitride cushion is carried out on element doping YAG ceramics or single crystalline substrate.
Of the invention further improve be, the temperature that rare earth doped YAG ceramics or single crystalline substrate are toasted under hydrogen
Spend for 800 DEG C to 1400 DEG C, baking time 5 to 20 minutes；Nitrogen treatment temperature be 800 DEG C to 1500 DEG C, processing time be 3 to
60 minutes.
Further improve of the invention is that silicon source area is aluminum shot, and the carrier gas of hydrogen chloride and ammonia is hydrogen or nitrogen；It is raw
Long pressure is 100 to 760Torr, and the flow of hydrogen chloride is 50 to 300sccm, and the flow of ammonia is 200 to 1000sccm, carrier gas
Flow be 500 to 2000Torr.
Of the invention further improve is that the temperature in silicon source area is 450 DEG C to 600 DEG C, growth temperature be 500 DEG C extremely
1500℃。
Further improve of the invention is that the thickness of single-crystal aluminum nitride cushion is 5nm to 100nm.
Further improve of the invention is, using metal organic chemical vapor deposition in the monocrystalline or polycrystalline aluminum nitride
GaN base LED epitaxial structure is grown on cushion, including：
The low temperature GaN buffer of 50nm-300nm thickness is grown at being 500 DEG C -700 DEG C in temperature；
The high temperature GaN cushions of 2-4um thickness are grown at being 900 DEG C -1200 DEG C in temperature；
1um-3um N-type GaN layer is grown at being 900 DEG C -1200 DEG C in temperature, wherein, the Si doping in N-type GaN layer is dense
Spend for 1 × 1017cm-3-3×1020cm-3；
The InGaN/GaN multiple quantum well light emitting layers of 1-30 circulation of growth at being 650 DEG C -850 DEG C in temperature；
Temperature be 800 DEG C -1150 DEG C at grow 100nm-800nm p-type GaN layer, wherein, Mg doping concentrations be 1 ×
1017cm-3-3×1020cm-3；
5nm-50nm highly dope p-type or N-type electrode contact layer is grown at being 800 DEG C -1200 DEG C in temperature, wherein, Mg
Doping concentration is 1 × 1018cm-3-5×1020cm-3, Si doping concentrations are 1 × 1017cm-3-5×1020cm-3。
A kind of preparation method of GaN base white light LEDs epitaxial structure of the present invention, with rare earth doped YAG (Y3Al5O12) pottery
Porcelain or monocrystalline prepare monocrystalline by hydride gas-phase epitaxy (HVPE) on substrate or polycrystalline aluminum nitride (AlN) are slow as substrate
Layer is rushed, white light LEDs extension is then grown by metal organic chemical vapor deposition (MOVPE) on aluminium nitride (AlN) cushion
Structure.Compared with prior art, aluminium nitride (AlN) epitaxial layer of high quality can be obtained by hydride gas-phase epitaxy (HVPE),
Preferable nucleating condition is provided for GaN growth.Using rare earth doped YAG (Y3Al5O12) ceramic or single crystalline substrate, can be straight
Connect and excited by GaN base LED, white light emission is directly produced by mixed light, reduce fluorescent material coating encapsulation link in production, subtract
Cost is lacked；Meanwhile chip heat pipe reason is advantageous to using inverted structure, fuel factor can be eliminated using conventional fluorescent powder by, which avoiding, causes
Fluorescent material failure, so as to improve the light efficiency of white light LEDs and life-span.
To sum up, the present invention can significantly simplify manufacture craft, effectively reduce production cost.Additionally, due to directly using fluorescence
Material substitutes traditional sapphire preferably to solve the heat dissipation problem of phosphor material powder in itself as epitaxial substrate, improve
Its stability under high-power driving, realize more preferable colour temperature control, longer life-span.
Brief description of the drawings：
Fig. 1 is the schematic diagram of GaN base white light LEDs epitaxial structure prepared by preparation method of the present invention.
Embodiment：
In order that the object, technical solutions and advantages of the present invention are more clearly understood, below in conjunction with specific embodiment, and join
According to accompanying drawing, the present invention is described in further detail.
Embodiment 1
The Ce for taking a piece of doping concentration 0.3at%, 500 μm of thickness, surface roughness to be less than 0.5nm:YAG single crystalline substrates,
It is put into after cleaning in hydride gas-phase epitaxy (HVPE) equipment reaction chamber.It is passed through hydrogen (H2) high-temperature baking 10 minutes, baking temperature
1200 DEG C of degree, is subsequently passed ammonia (NH3) in 1300 DEG C of progress substrate surface nitrogen treatment, 20 minutes time.
Keep reative cell ammonia (NH3) be passed through with carrier gas nitrogen, the hydrogen chloride (HCl) that flow is 100sccm is passed through
Silicon source area, reaction generation hydride source are simultaneously passed through reative cell, and 550 DEG C of silicon source area temperature, the carrier gas of hydrogen chloride (HCl) is nitrogen,
Flow 2000sccm.In reative cell, hydride source and ammonia (NH3) mixing, in Grown 100nm height (002) orientation
Polymorph A lN cushions.Wherein, 1300 DEG C of reaction chamber temperature, growth pressure 200Torr, the flow of ammonia is 800sccm.
Place the substrate into metal organic chemical vapor deposition (MOVPE) equipment, grow GaN base LED epitaxial structure, specifically
For：In HVPE-AlN buffer-layer surfaces successively growing low temperature GaN cushions, GaN cushions, N-type GaN layer, InGaN/GaN volumes
Sub- trap luminescent layer, AlGaN barrier layers, p-type GaN layer and highly dope p-type GaN contact electrode layers.
Embodiment 2
It is 0.5at% to take a piece of doping concentration, thickness is 100 μm, Eu of the surface roughness less than 0.5nm:YAG ceramic liners
Bottom, it is put into after cleaning in hydride gas-phase epitaxy (HVPE) equipment reaction chamber.It is passed through hydrogen (H2), toasted at a temperature of 800 DEG C
20 minutes, it is subsequently passed ammonia (NH3) 60 minutes substrate surface nitrogen treatment are carried out, nitriding temperature is 1300 DEG C.Keep reaction
Room ammonia (NH3) be passed through with carrier gas nitrogen, the hydrogen chloride (HCl) that flow is 50sccm is passed through silicon source area, reaction generation hydrogen
Compound source is simultaneously passed through reative cell, 450 DEG C of silicon source area temperature, and the carrier gas of hydrogen chloride (HCl) is nitrogen, flow 1000sccm.Reaction
In room, hydride source and ammonia (NH3) mixing, in Grown 5nm (002) to single crystal AlN cushion.Wherein, reative cell
1500 DEG C, growth pressure 100Torr of temperature, the flow of ammonia is 200sccm.Finally, 5nm HVPE-AlN lining will be grown
Bottom is put into metal organic chemical vapor deposition (MOVPE) equipment, grows GaN base LED epitaxial structure, is specially：In HVPE-
AlN buffer-layer surfaces growing low temperature GaN cushions, GaN cushions, N-type GaN layer, InGaN/GaN multiple quantum well light emittings successively
Layer, AlGaN barrier layers, p-type GaN layer and highly dope p-type GaN contact electrode layers.
Embodiment 3
It is 0.05at% to take a piece of doping concentration, thickness is 1000 μm, Nd of the surface roughness less than 0.5nm:YAG ceramics
Substrate, it is put into after cleaning in hydride gas-phase epitaxy (HVPE) equipment reaction chamber.It is passed through hydrogen (H2), dried at a temperature of 1400 DEG C
It is roasting 5 minutes, it is subsequently passed ammonia (NH3) 3 minutes substrate surface nitrogen treatment are carried out, nitriding temperature is 1500 DEG C.Keep reaction
Room ammonia (NH3) be passed through with carrier gas hydrogen, the hydrogen chloride (HCl) that flow is 300sccm is passed through silicon source area, reaction generation hydrogen
Compound source is simultaneously passed through reative cell, 600 DEG C of silicon source area temperature, and the carrier gas of hydrogen chloride (HCl) is hydrogen, flow 2000sccm.Reaction
In room, hydride source and ammonia (NH3) mixing, it is orientated polymorph A lN cushions in Grown 20nm (002).Wherein, react
500 DEG C, growth pressure 760Torr of room temperature, the flow of ammonia is 1000sccm.Finally, Organometallic Chemistry is placed the substrate into
In (MOVPE) equipment that is vapor-deposited, GaN base LED epitaxial structure is grown, is specially：Given birth to successively in HVPE-AlN buffer-layer surfaces
Long low temperature GaN buffer, GaN cushions, N-type GaN layer, InGaN/GaN multiple quantum well light emittings layer, AlGaN barrier layers, p-type GaN
Layer and highly dope p-type GaN contact electrode layers.
Embodiment 4
The Yb for taking a piece of doping concentration 0.4at%, 400 μm of thickness, surface roughness to be less than 0.5nm:YAG single crystalline substrates,
It is put into after cleaning in hydride gas-phase epitaxy (HVPE) equipment reaction chamber.It is passed through hydrogen (H2) high-temperature baking 10 minutes, baking temperature
1200 DEG C of degree, is subsequently passed ammonia (NH3) in 1300 DEG C of progress substrate surface nitrogen treatment, 20 minutes time.
Keep reative cell ammonia (NH3) be passed through with carrier gas nitrogen, the hydrogen chloride (HCl) that flow is 100sccm is passed through
Silicon source area, reaction generation hydride source are simultaneously passed through reative cell, and 550 DEG C of silicon source area temperature, the carrier gas of hydrogen chloride (HCl) is nitrogen,
Flow 2000sccm.In reative cell, hydride source and ammonia (NH3) mixing, in Grown 100nm height (002) orientation
Polymorph A lN cushions.Wherein, 1300 DEG C of reaction chamber temperature, growth pressure 200Torr, the flow of ammonia is 800sccm.
Place the substrate into metal organic chemical vapor deposition (MOVPE) equipment, grow GaN base LED epitaxial structure, specifically
For：In HVPE-AlN buffer-layer surfaces successively growing low temperature GaN cushions, GaN cushions, N-type GaN layer, InGaN/GaN volumes
Sub- trap luminescent layer, AlGaN barrier layers, p-type GaN layer and highly dope p-type GaN contact electrode layers.
Embodiment 5
A piece of 500 μm of thickness, surface roughness is taken to be less than 0.5nm Ce, Nd:YAG single crystalline substrates, wherein Ce doping concentrations
0.2at%, Nd doping concentration 0.1at%, it is put into after cleaning in hydride gas-phase epitaxy (HVPE) equipment reaction chamber.It is passed through hydrogen
(H2) high-temperature baking 10 minutes, 1200 DEG C of baking temperature, it is subsequently passed ammonia (NH3) carried out at 1300 DEG C at substrate surface nitridation
Reason, 20 minutes time.
Keep reative cell ammonia (NH3) be passed through with carrier gas nitrogen, the hydrogen chloride (HCl) that flow is 100sccm is passed through
Silicon source area, reaction generation hydride source are simultaneously passed through reative cell, and 550 DEG C of silicon source area temperature, the carrier gas of hydrogen chloride (HCl) is nitrogen,
Flow 2000sccm.In reative cell, hydride source and ammonia (NH3) mixing, in Grown 100nm height (002) orientation
Polymorph A lN cushions.Wherein, 1300 DEG C of reaction chamber temperature, growth pressure 200Torr, the flow of ammonia is 800sccm.
Place the substrate into metal organic chemical vapor deposition (MOVPE) equipment, grow GaN base LED epitaxial structure, specifically
For：In HVPE-AlN buffer-layer surfaces successively growing low temperature GaN cushions, GaN cushions, N-type GaN layer, InGaN/GaN volumes
Sub- trap luminescent layer, AlGaN barrier layers, p-type GaN layer and highly dope p-type GaN contact electrode layers.
Embodiment 6
Eu, the Yb for taking a piece of thickness to be less than 0.5nm for 200 μm, surface roughness:YAG ceramic substrates, wherein, Eu doping
Concentration is 0.3at%, and Yb doping concentrations are 0.2at%, is put into after cleaning in hydride gas-phase epitaxy (HVPE) equipment reaction chamber.
It is passed through hydrogen (H2), toasted 20 minutes at a temperature of 800 DEG C, be subsequently passed ammonia (NH3) carry out at substrate surface nitridation in 60 minutes
Reason, nitriding temperature are 1300 DEG C.Keep reative cell ammonia (NH3) be passed through with carrier gas nitrogen, by the chlorination that flow is 50sccm
Hydrogen (HCl) is passed through silicon source area, and reaction generation hydride source is simultaneously passed through reative cell, 450 DEG C of silicon source area temperature, hydrogen chloride (HCl)
Carrier gas is nitrogen, flow 1000sccm.In reative cell, hydride source and ammonia (NH3) mixing, in Grown 5nm (002)
To single crystal AlN cushion.Wherein, 1500 DEG C of reaction chamber temperature, growth pressure 100Torr, the flow of ammonia is 200sccm.Most
Afterwards, the substrate that grown 5nm HVPE-AlN is put into metal organic chemical vapor deposition (MOVPE) equipment, grows GaN base
LED epitaxial structure, it is specially：In HVPE-AlN buffer-layer surfaces successively growing low temperature GaN cushions, GaN cushions, N-type GaN
Layer, InGaN/GaN multiple quantum well light emittings layer, AlGaN barrier layers, p-type GaN layer and highly dope p-type GaN contact electrode layers.
Embodiment 7
Ce, Eu, the Nd for taking a piece of thickness to be less than 0.5nm for 800 μm, surface roughness:YAG ceramic substrates, wherein, Ce mixes
Miscellaneous concentration is 0.05at%, and Eu doping concentrations are 0.05at%, and Nd doping concentrations are 0.05at%, and hydride gas is put into after cleaning
In phase epitaxy (HVPE) equipment reaction chamber.It is passed through hydrogen (H2), toasted 5 minutes at a temperature of 1400 DEG C, be subsequently passed ammonia
(NH3) 3 minutes substrate surface nitrogen treatment are carried out, nitriding temperature is 1500 DEG C.Keep reative cell ammonia (NH3) and carrier gas hydrogen
Be passed through, the hydrogen chloride (HCl) that flow is 300sccm is passed through silicon source area, reaction generation hydride source is simultaneously passed through reative cell, aluminium
600 DEG C of source region temperature, the carrier gas of hydrogen chloride (HCl) are hydrogen, flow 2000sccm.In reative cell, hydride source and ammonia
(NH3) mixing, it is orientated polymorph A lN cushions in Grown 20nm (002).Wherein, 500 DEG C of reaction chamber temperature, growth pressure
Strong 760Torr, the flow of ammonia is 1000sccm.Finally, metal organic chemical vapor deposition (MOVPE) equipment is placed the substrate into
In, GaN base LED epitaxial structure is grown, is specially：In HVPE-AlN buffer-layer surfaces successively growing low temperature GaN cushions, GaN
Cushion, N-type GaN layer, InGaN/GaN multiple quantum well light emittings layer, AlGaN barrier layers, p-type GaN layer and highly dope p-type GaN electricity
Pole contact layer.
Embodiment 8
A piece of 400 μm of thickness, surface roughness is taken to be less than 0.5nm Ce, Eu, Nd, Yb:YAG single crystalline substrates, wherein, Ce
Doping concentration 0.1at%, Eu doping concentration 0.1at%, Nd doping concentration 0.1at%, Yb doping concentration 0.1at%, after cleaning
It is put into hydride gas-phase epitaxy (HVPE) equipment reaction chamber.It is passed through hydrogen (H2) high-temperature baking 10 minutes, baking temperature 1200
DEG C, it is subsequently passed ammonia (NH3) in 1300 DEG C of progress substrate surface nitrogen treatment, 20 minutes time.
Keep reative cell ammonia (NH3) be passed through with carrier gas nitrogen, the hydrogen chloride (HCl) that flow is 100sccm is passed through
Silicon source area, reaction generation hydride source are simultaneously passed through reative cell, and 550 DEG C of silicon source area temperature, the carrier gas of hydrogen chloride (HCl) is nitrogen,
Flow 2000sccm.In reative cell, hydride source and ammonia (NH3) mixing, in Grown 100nm height (002) orientation
Polymorph A lN cushions.Wherein, 1300 DEG C of reaction chamber temperature, growth pressure 200Torr, the flow of ammonia is 800sccm.
Place the substrate into metal organic chemical vapor deposition (MOVPE) equipment, grow GaN base LED epitaxial structure, specifically
For：In HVPE-AlN buffer-layer surfaces successively growing low temperature GaN cushions, GaN cushions, N-type GaN layer, InGaN/GaN volumes
Sub- trap luminescent layer, AlGaN barrier layers, p-type GaN layer and highly dope p-type GaN contact electrode layers.
Particular embodiments described above, the purpose of the present invention, technical scheme and beneficial effect are carried out further in detail
Describe in detail bright, it should be understood that the foregoing is only the present invention specific embodiment, be not intended to limit the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvements done etc., the protection of the present invention should be included in
Within the scope of.
Claims (6)
1. a kind of preparation method of GaN base white light LEDs epitaxial structure, it is characterised in that comprise the following steps：
Monocrystalline is prepared on rare earth doped YAG ceramics or single crystalline substrate or polycrystalline aluminum nitride delays using hydride gas-phase epitaxy
Rush layer；
GaN base LED epitaxy junctions are grown on the monocrystalline or polycrystalline aluminum nitride cushion using metal organic chemical vapor deposition
Structure, wherein, GaN base LED epitaxial structure is followed successively by low temperature GaN buffer, high-temperature gan layer, N-type GaN layer, InGaN/ from bottom to top
GaN multi-quantum well active regions, AlGaN electronic barrier layers, p-type GaN layer and highly dope p-type or highly doped contact electrode layer；
In the rare earth doped YAG ceramics or single crystalline substrate, rare earth element includes one kind or several in Ce, Eu, Nd, Yb
Kind, doping concentration is 0.05at% to 0.5at%, and substrate thickness is 100 μm to 1000 μm, the YAG ceramics or single as substrate
Brilliant surface is less than 0.5nm by fine polishing, its surface roughness；
Monocrystalline is prepared on rare earth doped YAG ceramics or single crystalline substrate by hydride gas-phase epitaxy or polycrystalline aluminum nitride delays
Layer is rushed, its concrete operations is：
First, rare earth doped YAG ceramics or single crystalline substrate are toasted under hydrogen, is subsequently passed ammonia and carries out high-temperature ammonolysis
Processing；
Finally, hydrogen chloride and ammonia are each led into silicon source area and reative cell, the rare earth element after high-temperature ammonolysis processing is mixed
The growth of monocrystalline or polycrystalline aluminum nitride cushion is carried out on miscellaneous YAG ceramics or single crystalline substrate.
2. preparation method according to claim 1, it is characterised in that rare earth doped YAG ceramics or single crystalline substrate exist
The temperature toasted under hydrogen is 800 DEG C to 1400 DEG C, baking time 5 to 20 minutes；Nitrogen treatment temperature is 800 DEG C to 1500
DEG C, processing time is 3 to 60 minutes.
3. preparation method according to claim 1, it is characterised in that silicon source area is aluminum shot, the carrier gas of hydrogen chloride and ammonia
For hydrogen or nitrogen；Growth pressure is 100 to 760Torr, and the flow of hydrogen chloride is 50 to 300sccm, and the flow of ammonia is 200
To 1000sccm, the flow of carrier gas is 500 to 2000Torr.
4. preparation method according to claim 1, it is characterised in that the temperature in silicon source area is 450 DEG C to 600 DEG C, growth
Temperature is 500 DEG C to 1500 DEG C.
5. preparation method according to claim 1, it is characterised in that the thickness of single-crystal aluminum nitride cushion be 5nm extremely
100nm。
6. preparation method according to claim 1, it is characterised in that using metal organic chemical vapor deposition in the list
GaN base LED epitaxial structure is grown on brilliant or polycrystalline aluminum nitride cushion, including：
The low temperature GaN buffer of 50nm-300nm thickness is grown at being 500 DEG C -700 DEG C in temperature；
The high temperature GaN cushions of 2-4um thickness are grown at being 900 DEG C -1200 DEG C in temperature；
1um-3um N-type GaN layer is grown at being 900 DEG C -1200 DEG C in temperature, wherein, the Si doping concentrations in N-type GaN layer are
1×1017cm-3-3×1020cm-3；
The InGaN/GaN multiple quantum well light emitting layers of 1-30 circulation of growth at being 650 DEG C -850 DEG C in temperature；
Temperature be 800 DEG C -1150 DEG C at grow 100nm-800nm p-type GaN layer, wherein, Mg doping concentrations be 1 ×
1017cm-3-3×1020cm-3；
5nm-50nm highly dope p-type or N-type electrode contact layer is grown at being 800 DEG C -1200 DEG C in temperature, wherein, Mg doping
Concentration is 1 × 1018cm-3-5×1020cm-3, Si doping concentrations are 1 × 1017cm-3-5×1020cm-3。
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| CN106025008A (en) * | 2016-07-12 | 2016-10-12 | 河源市众拓光电科技有限公司 | LED epitaxial wafer growing on yttrium aluminum garnet substrate and manufacturing method |
| CN106098881A (en) * | 2016-07-12 | 2016-11-09 | 河源市众拓光电科技有限公司 | The InGaN/GaN MQW being grown on yttrium-aluminium-garnet substrate and preparation method |
| CN107681025B (en) * | 2017-09-12 | 2020-07-28 | 西安交通大学 | GaN-based white light L ED epitaxial structure and preparation method thereof |
| CN109244203B (en) * | 2018-09-12 | 2020-07-07 | 华灿光电(苏州）有限公司 | Epitaxial wafer of light emitting diode and preparation method thereof |
| CN111312867B (en) * | 2020-02-21 | 2023-12-15 | 湘能华磊光电股份有限公司 | Preparation method of single-chip white light LED |
| CN114292087A (en) * | 2021-12-28 | 2022-04-08 | 北京大学东莞光电研究院 | Preparation method of white light LED epitaxial material without packaging |
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