CN104952986A - Production method of GaN-based white LED epitaxial structure - Google Patents
Production method of GaN-based white LED epitaxial structure Download PDFInfo
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- CN104952986A CN104952986A CN201510305619.8A CN201510305619A CN104952986A CN 104952986 A CN104952986 A CN 104952986A CN 201510305619 A CN201510305619 A CN 201510305619A CN 104952986 A CN104952986 A CN 104952986A
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- 238000004519 manufacturing process Methods 0.000 title abstract description 7
- 239000000758 substrate Substances 0.000 claims abstract description 47
- 239000011248 coating agent Substances 0.000 claims abstract description 44
- 238000000576 coating method Methods 0.000 claims abstract description 44
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 18
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 16
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 14
- 229910002704 AlGaN Inorganic materials 0.000 claims abstract description 11
- 230000004888 barrier function Effects 0.000 claims abstract description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 80
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 48
- 229910021529 ammonia Inorganic materials 0.000 claims description 40
- 150000004678 hydrides Chemical class 0.000 claims description 30
- 229910052782 aluminium Inorganic materials 0.000 claims description 24
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 239000004411 aluminium Substances 0.000 claims description 22
- 239000012159 carrier gas Substances 0.000 claims description 20
- 239000001257 hydrogen Substances 0.000 claims description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims description 18
- 238000000407 epitaxy Methods 0.000 claims description 14
- 150000002431 hydrogen Chemical class 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 14
- 150000002910 rare earth metals Chemical class 0.000 claims description 14
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 11
- 230000003746 surface roughness Effects 0.000 claims description 10
- 229910052779 Neodymium Inorganic materials 0.000 claims description 8
- 229910052693 Europium Inorganic materials 0.000 claims description 7
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 6
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 6
- 230000008569 process Effects 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 4
- 238000005915 ammonolysis reaction Methods 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 19
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 abstract description 11
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000919 ceramic Substances 0.000 abstract description 6
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 abstract 2
- 235000012431 wafers Nutrition 0.000 abstract 2
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 abstract 2
- 230000010354 integration Effects 0.000 abstract 1
- 230000003287 optical effect Effects 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 25
- 229910017083 AlN Inorganic materials 0.000 description 10
- 238000004140 cleaning Methods 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 5
- 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
- 239000003292 glue Substances 0.000 description 3
- 238000004528 spin coating Methods 0.000 description 3
- 238000012536 packaging technology Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000004224 protection Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 241001025261 Neoraja caerulea Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 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
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002244 precipitate Substances 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
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying 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)
- Power Engineering (AREA)
- Computer Hardware Design (AREA)
- Manufacturing & Machinery (AREA)
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- Crystallography & Structural Chemistry (AREA)
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- Organic Chemistry (AREA)
- Led Devices (AREA)
Abstract
A production method of a GaN-based white LED epitaxial structure includes the steps of preparing a monocrystalline or polycrystalline aluminum nitride buffer layer on a rare earth element doped YAG (yttrium aluminum garnet) ceramic or monocrystalline substrate by means of hydride vapor phase epitaxy; growing a GaN-based LED epitaxial structure on the monocrystalline or polycrystalline aluminum nitride buffer layer by means of metal-organic chemical vapor deposition. The GaN-based LED epitaxial structure comprises a low-temperature GaN buffer layer, a high-temperature GaN layer, an N-type GaN layer, an InGaN/GaN multiple quantum well active area, an AlGaN electronic barrier layer, a P-type GaN layer and a high-doped P-type or N-type electrode contact layer sequentially from bottom to top. The GaN-based LED epitaxial structure has the advantages that optical and physical features of fluorescent material, such as doping, thickness and quality, can be accurately controlled, integration of the fluorescent material high in repeatability and uniformity is achieved, and the problem that in traditional phosphor coating, unavailable non-uniform phosphor content occurs to the different parts of a same wafer and the different wafers due to the production process is solved.
Description
Technical field:
The present invention relates to field of photoelectric technology, be specifically related to a kind of preparation method of GaN base white light LEDs epitaxial structure.
Background technology:
After Nakamura in 1991 etc. successfully develop GaN blue-ray LED, the GaN base LED with good characteristics such as high efficiency, small size, long-life, environmental protections obtains unprecedented development, has very wide application prospect.At present, white light LEDs adopts the mode of blue LED excited yellow fluorescent material to produce white light usually.Fluorescent powder coating technique mainly can be divided into 3 kinds: single packaged blue-light LED chip sprays (some glue) technique, before chip cutting on whole wafer spin coating proceeding and add the little plate technique of long-distance fluorescent powder in encapsulating structure.
In traditional spraying (some glue) technique, after fluorescent material mixes with colloid, be directly coated on LED chip.There is many defects being difficult to overcome in this packaging technology, such as, because fluorescent material is different from colloid proportion, in a glue process, fluorescent material can precipitate, even if thus cause the same batch of LED light source made also to have larger difference in the parameter such as colour temperature, color rendering index.Adopt spin coating proceeding can solve the problem of fluorescent material precipitation to a certain extent, but due to the restriction of spin coating proceeding itself, even if the thickness of same wafer zones of different fluorescent material, concentration also difference to some extent.The colour temperature that result between last white chip and chip there are differences, and reduces product yields.
Both traditional handicrafts above-mentioned in heat radiation also have problems.The heat that fluorescent material produces in photon frequency conversion process has to pass through chip and transmits a substrate, then by heat sink heat radiation.Total coefficient of heat conduction is subject to the thermal conduction characteristic impact each time between material and material.Heat transfer efficiency is not high, affects light efficiency and the life-span of white light LEDs.
The problems such as the fluorescent material precipitation that long-distance fluorescent powder technology (Remote Phosphor) can alleviate color shift, arogel proportion difference causes.Owing to being filled by the lower gas of thermal conductivity or colloid between fluorescent material and LED chip, in phosphor material powder, heat cannot leave by LED is heat sink effectively, also can cause that device color shift, light efficiency reduce, service life reduction.
Therefore, be badly in need of a kind of novel white-light LED manufacture craft, solve phosphor material powder uneven, by phenomenons such as heat deteriorations, simplify packaging technology simultaneously, improve yield, reduce production cost.
Summary of the invention:
The object of the invention is to solve the problems of the technologies described above, provide a kind of preparation method of GaN base white light LEDs epitaxial structure, a kind of GaN base white light LEDs epitaxial wafer that the YAG pottery or single crystalline substrate of novel rare-earth element doping grow, can obtain the White-light LED chip without the need to fluorescent powder coating technique by traditional die processing technology.
For achieving the above object, the present invention adopts following technical scheme to be achieved:
A preparation method for GaN base white light LEDs epitaxial structure, comprises the following steps:
Hydride gas-phase epitaxy is used to prepare monocrystalline or polycrystalline aluminum nitride resilient coating on rare earth doped YAG pottery or single crystalline substrate;
Use metal organic chemical vapor deposition growing GaN base LED epitaxial structure on described monocrystalline or polycrystalline aluminum nitride resilient coating, 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 region from bottom to top, AlGaN electronic barrier layer, P type GaN layer and highly dope p-type or highly doped contact electrode layer.
The present invention further improves and is, in described rare earth doped YAG pottery or single crystalline substrate, rare earth element comprises one or more in Ce, Eu, Nd, Yb, doping content is 0.05at% to 0.5at%, substrate thickness is 100 μm to 1000 μm, as substrate YAG pottery or single-crystal surface through meticulous polishing, its surface roughness is less than 0.5nm.
The present invention further improves and is, on rare earth doped YAG pottery or single crystalline substrate, prepare monocrystalline or polycrystalline aluminum nitride resilient coating by hydride gas-phase epitaxy, its concrete operations are:
First, rare earth doped YAG pottery or single crystalline substrate are toasted under hydrogen, passes into ammonia subsequently and carry out high-temperature ammonolysis process;
Finally, hydrogen chloride and ammonia are passed in aluminium source region and reative cell respectively, the rare earth doped YAG pottery after high-temperature ammonolysis process or single crystalline substrate are carried out the growth of monocrystalline or polycrystalline aluminum nitride resilient coating.
The present invention further improves and is, the temperature that rare earth doped YAG pottery or single crystalline substrate are 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, and the processing time is 3 to 60 minutes.
The present invention further improves and is, aluminium source region is aluminum shot, and the carrier gas of hydrogen chloride and ammonia is 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, and the flow of carrier gas is 500 to 2000Torr.
The present invention further improves and is, the temperature in aluminium source region is 450 DEG C to 600 DEG C, and growth temperature is 500 DEG C to 1500 DEG C.
The present invention further improves and is, the thickness of single-crystal aluminum nitride resilient coating is 5nm to 100nm.
The present invention further improves and is, uses metal organic chemical vapor deposition growing GaN base LED epitaxial structure on described monocrystalline or polycrystalline aluminum nitride resilient coating, comprising:
The low temperature GaN buffer of 50nm-300nm thickness is grown at temperature is 500 DEG C-700 DEG C;
The high temperature GaN resilient coating of 2-4um thickness is grown at temperature is 900 DEG C-1200 DEG C;
At temperature is 900 DEG C-1200 DEG C, grow the N-type GaN layer of 1um-3um, wherein, the Si doping content in N-type GaN layer is 1 × 10
17cm
-3-3 × 10
20cm
-3;
The InGaN/GaN multiple quantum well light emitting layer of 1-30 circulation is grown at temperature is 650 DEG C-850 DEG C;
At temperature is 800 DEG C-1150 DEG C, grow the P type GaN layer of 100nm-800nm, wherein, Mg doping content is 1 × 10
17cm
-3-3 × 10
20cm
-3;
At temperature is 800 DEG C-1200 DEG C, grow highly dope p-type or the N-type electrode contact layer of 5nm-50nm, wherein, Mg doping content is 1 × 10
18cm
-3-5 × 10
20cm
-3, Si doping content is 1 × 10
17cm
-3-5 × 10
20cm
-3.
The preparation method of a kind of GaN base white light LEDs of the present invention epitaxial structure, with rare earth doped YAG (Y
3al
5o
12) pottery or monocrystalline as substrate, substrate prepares monocrystalline or polycrystalline aluminum nitride (AlN) resilient coating by hydride gas-phase epitaxy (HVPE), then on aluminium nitride (AlN) resilient coating, grows white light LEDs epitaxial structure by metal organic chemical vapor deposition (MOVPE).Compared with prior art, can obtain high-quality aluminium nitride (AlN) epitaxial loayer by hydride gas-phase epitaxy (HVPE), the growth for GaN provides good nucleating condition.Adopt rare earth doped YAG (Y
3al
5o
12) ceramic or single crystalline substrate, directly can be excited by GaN base LED, directly produce white light emission by mixed light, decrease fluorescent material coating encapsulation link aborning, decrease cost; Meanwhile, adopt inverted structure to be conducive to chip heat pipe reason, fluorescent material that thermal effect causes lost efficacy to avoid using conventional fluorescent powder to eliminate, thus improved light efficiency and the life-span of white light LEDs.
To sum up, the present invention significantly can simplify manufacture craft, effectively reduces production cost.In addition owing to directly using fluorescent material to replace traditional sapphire as epitaxial substrate, the heat dissipation problem of phosphor material powder itself can be solved preferably, improve its stability under high-power driving, realize better colour temperature and control, the longer life-span.
Accompanying drawing illustrates:
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 to make the object, technical solutions and advantages of the present invention clearly understand, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in further detail.
Embodiment 1
Get a slice doping content 0.3at%, Ce:YAG single crystalline substrate that thickness 500 μm, surface roughness are less than 0.5nm, put into hydride gas-phase epitaxy (HVPE) equipment reaction chamber after cleaning.Pass into hydrogen (H
2) high-temperature baking 10 minutes, baking temperature 1200 DEG C, passes into ammonia (NH subsequently
3) carry out substrate surface nitrogen treatment at 1300 DEG C, 20 minutes time.
Keep reative cell ammonia (NH
3) with the passing into of carrier gas nitrogen, be that the hydrogen chloride (HCl) of 100sccm passes into aluminium source region by flow, reaction generates hydride source and also passes into reative cell, aluminium source region temperature 550 DEG C, the carrier gas of hydrogen chloride (HCl) is nitrogen, flow 2000sccm.In reative cell, hydride source and ammonia (NH
3) mixing, at Grown 100nm height (002) orientation polymorph A lN resilient coating.Wherein, reaction chamber temperature 1300 DEG C, growth pressure 200Torr, the flow of ammonia is 800sccm.
Substrate is put into metal organic chemical vapor deposition (MOVPE) equipment, growing GaN base LED epitaxial structure, is specially: at HVPE-AlN buffer-layer surface successively growing low temperature GaN resilient coating, GaN resilient coating, N-type GaN layer, InGaN/GaN multiple quantum well light emitting layer, AlGaN barrier layer, P type GaN layer and highly dope p-type GaN contact electrode layer.
Embodiment 2
Get the Eu:YAG ceramic substrate that a slice doping content is 0.5at%, thickness is 100 μm, surface roughness is less than 0.5nm, after cleaning, put into hydride gas-phase epitaxy (HVPE) equipment reaction chamber.Pass into hydrogen (H
2), toast 20 minutes at 800 DEG C of temperature, pass into ammonia (NH subsequently
3) carrying out 60 minutes substrate surface nitrogen treatment, nitriding temperature is 1300 DEG C.Keep reative cell ammonia (NH
3) with the passing into of carrier gas nitrogen, be that the hydrogen chloride (HCl) of 50sccm passes into aluminium source region by flow, reaction generates hydride source and also passes into reative cell, aluminium source region temperature 450 DEG C, and the carrier gas of hydrogen chloride (HCl) is nitrogen, flow 1000sccm.In reative cell, hydride source and ammonia (NH
3) mixing, at Grown 5nm (002) to single crystal AlN resilient coating.Wherein, reaction chamber temperature 1500 DEG C, growth pressure 100Torr, the flow of ammonia is 200sccm.Finally, the substrate that grown 5nm HVPE-AlN is put into metal organic chemical vapor deposition (MOVPE) equipment, growing GaN base LED epitaxial structure, is specially: at HVPE-AlN buffer-layer surface successively growing low temperature GaN resilient coating, GaN resilient coating, N-type GaN layer, InGaN/GaN multiple quantum well light emitting layer, AlGaN barrier layer, P type GaN layer and highly dope p-type GaN contact electrode layer.
Embodiment 3
Get the Nd:YAG ceramic substrate that a slice doping content is 0.05at%, thickness is 1000 μm, surface roughness is less than 0.5nm, after cleaning, put into hydride gas-phase epitaxy (HVPE) equipment reaction chamber.Pass into hydrogen (H
2), toast 5 minutes at 1400 DEG C of temperature, pass into ammonia (NH subsequently
3) carrying out 3 minutes substrate surface nitrogen treatment, nitriding temperature is 1500 DEG C.Keep reative cell ammonia (NH
3) with the passing into of carrier gas hydrogen, be that the hydrogen chloride (HCl) of 300sccm passes into aluminium source region by flow, reaction generates hydride source and also passes into reative cell, aluminium source region temperature 600 DEG C, the carrier gas of hydrogen chloride (HCl) is hydrogen, flow 2000sccm.In reative cell, hydride source and ammonia (NH
3) mixing, at Grown 20nm (002) orientation polymorph A lN resilient coating.Wherein, reaction chamber temperature 500 DEG C, growth pressure 760Torr, the flow of ammonia is 1000sccm.Finally, substrate is put into metal organic chemical vapor deposition (MOVPE) equipment, growing GaN base LED epitaxial structure, is specially: at HVPE-AlN buffer-layer surface successively growing low temperature GaN resilient coating, GaN resilient coating, N-type GaN layer, InGaN/GaN multiple quantum well light emitting layer, AlGaN barrier layer, P type GaN layer and highly dope p-type GaN contact electrode layer.
Embodiment 4
Get a slice doping content 0.4at%, Yb:YAG single crystalline substrate that thickness 400 μm, surface roughness are less than 0.5nm, put into hydride gas-phase epitaxy (HVPE) equipment reaction chamber after cleaning.Pass into hydrogen (H
2) high-temperature baking 10 minutes, baking temperature 1200 DEG C, passes into ammonia (NH subsequently
3) carry out substrate surface nitrogen treatment at 1300 DEG C, 20 minutes time.
Keep reative cell ammonia (NH
3) with the passing into of carrier gas nitrogen, be that the hydrogen chloride (HCl) of 100sccm passes into aluminium source region by flow, reaction generates hydride source and also passes into reative cell, aluminium source region temperature 550 DEG C, the carrier gas of hydrogen chloride (HCl) is nitrogen, flow 2000sccm.In reative cell, hydride source and ammonia (NH
3) mixing, at Grown 100nm height (002) orientation polymorph A lN resilient coating.Wherein, reaction chamber temperature 1300 DEG C, growth pressure 200Torr, the flow of ammonia is 800sccm.
Substrate is put into metal organic chemical vapor deposition (MOVPE) equipment, growing GaN base LED epitaxial structure, is specially: at HVPE-AlN buffer-layer surface successively growing low temperature GaN resilient coating, GaN resilient coating, N-type GaN layer, InGaN/GaN multiple quantum well light emitting layer, AlGaN barrier layer, P type GaN layer and highly dope p-type GaN contact electrode layer.
Embodiment 5
Get a slice thickness 500 μm, Ce, Nd:YAG single crystalline substrate that surface roughness is less than 0.5nm, wherein Ce doping content 0.2at%, Nd doping content 0.1at%, puts into hydride gas-phase epitaxy (HVPE) equipment reaction chamber after cleaning.Pass into hydrogen (H
2) high-temperature baking 10 minutes, baking temperature 1200 DEG C, passes into ammonia (NH subsequently
3) carry out substrate surface nitrogen treatment at 1300 DEG C, 20 minutes time.
Keep reative cell ammonia (NH
3) with the passing into of carrier gas nitrogen, be that the hydrogen chloride (HCl) of 100sccm passes into aluminium source region by flow, reaction generates hydride source and also passes into reative cell, aluminium source region temperature 550 DEG C, the carrier gas of hydrogen chloride (HCl) is nitrogen, flow 2000sccm.In reative cell, hydride source and ammonia (NH
3) mixing, at Grown 100nm height (002) orientation polymorph A lN resilient coating.Wherein, reaction chamber temperature 1300 DEG C, growth pressure 200Torr, the flow of ammonia is 800sccm.
Substrate is put into metal organic chemical vapor deposition (MOVPE) equipment, growing GaN base LED epitaxial structure, is specially: at HVPE-AlN buffer-layer surface successively growing low temperature GaN resilient coating, GaN resilient coating, N-type GaN layer, InGaN/GaN multiple quantum well light emitting layer, AlGaN barrier layer, P type GaN layer and highly dope p-type GaN contact electrode layer.
Embodiment 6
Get Eu, Yb:YAG ceramic substrate that a slice thickness is 200 μm, surface roughness is less than 0.5nm, wherein, Eu doping content is 0.3at%, Yb doping content is 0.2at%, puts into hydride gas-phase epitaxy (HVPE) equipment reaction chamber after cleaning.Pass into hydrogen (H
2), toast 20 minutes at 800 DEG C of temperature, pass into ammonia (NH subsequently
3) carrying out 60 minutes substrate surface nitrogen treatment, nitriding temperature is 1300 DEG C.Keep reative cell ammonia (NH
3) with the passing into of carrier gas nitrogen, be that the hydrogen chloride (HCl) of 50sccm passes into aluminium source region by flow, reaction generates hydride source and also passes into reative cell, aluminium source region temperature 450 DEG C, and the carrier gas of hydrogen chloride (HCl) is nitrogen, flow 1000sccm.In reative cell, hydride source and ammonia (NH
3) mixing, at Grown 5nm (002) to single crystal AlN resilient coating.Wherein, reaction chamber temperature 1500 DEG C, growth pressure 100Torr, the flow of ammonia is 200sccm.Finally, the substrate that grown 5nm HVPE-AlN is put into metal organic chemical vapor deposition (MOVPE) equipment, growing GaN base LED epitaxial structure, is specially: at HVPE-AlN buffer-layer surface successively growing low temperature GaN resilient coating, GaN resilient coating, N-type GaN layer, InGaN/GaN multiple quantum well light emitting layer, AlGaN barrier layer, P type GaN layer and highly dope p-type GaN contact electrode layer.
Embodiment 7
Get Ce, Eu, Nd:YAG ceramic substrate that a slice thickness is 800 μm, surface roughness is less than 0.5nm, wherein, Ce doping content is 0.05at%, Eu doping content is 0.05at%, Nd doping content is 0.05at%, puts into hydride gas-phase epitaxy (HVPE) equipment reaction chamber after cleaning.Pass into hydrogen (H
2), toast 5 minutes at 1400 DEG C of temperature, pass into ammonia (NH subsequently
3) carrying out 3 minutes substrate surface nitrogen treatment, nitriding temperature is 1500 DEG C.Keep reative cell ammonia (NH
3) with the passing into of carrier gas hydrogen, be that the hydrogen chloride (HCl) of 300sccm passes into aluminium source region by flow, reaction generates hydride source and also passes into reative cell, aluminium source region temperature 600 DEG C, the carrier gas of hydrogen chloride (HCl) is hydrogen, flow 2000sccm.In reative cell, hydride source and ammonia (NH
3) mixing, at Grown 20nm (002) orientation polymorph A lN resilient coating.Wherein, reaction chamber temperature 500 DEG C, growth pressure 760Torr, the flow of ammonia is 1000sccm.Finally, substrate is put into metal organic chemical vapor deposition (MOVPE) equipment, growing GaN base LED epitaxial structure, is specially: at HVPE-AlN buffer-layer surface successively growing low temperature GaN resilient coating, GaN resilient coating, N-type GaN layer, InGaN/GaN multiple quantum well light emitting layer, AlGaN barrier layer, P type GaN layer and highly dope p-type GaN contact electrode layer.
Embodiment 8
Get a slice thickness 400 μm, Ce, Eu, Nd, Yb:YAG single crystalline substrate that surface roughness is less than 0.5nm, wherein, Ce doping content 0.1at%, Eu doping content 0.1at%, Nd doping content 0.1at%, Yb doping content 0.1at%, puts into hydride gas-phase epitaxy (HVPE) equipment reaction chamber after cleaning.Pass into hydrogen (H
2) high-temperature baking 10 minutes, baking temperature 1200 DEG C, passes into ammonia (NH subsequently
3) carry out substrate surface nitrogen treatment at 1300 DEG C, 20 minutes time.
Keep reative cell ammonia (NH
3) with the passing into of carrier gas nitrogen, be that the hydrogen chloride (HCl) of 100sccm passes into aluminium source region by flow, reaction generates hydride source and also passes into reative cell, aluminium source region temperature 550 DEG C, the carrier gas of hydrogen chloride (HCl) is nitrogen, flow 2000sccm.In reative cell, hydride source and ammonia (NH
3) mixing, at Grown 100nm height (002) orientation polymorph A lN resilient coating.Wherein, reaction chamber temperature 1300 DEG C, growth pressure 200Torr, the flow of ammonia is 800sccm.
Substrate is put into metal organic chemical vapor deposition (MOVPE) equipment, growing GaN base LED epitaxial structure, is specially: at HVPE-AlN buffer-layer surface successively growing low temperature GaN resilient coating, GaN resilient coating, N-type GaN layer, InGaN/GaN multiple quantum well light emitting layer, AlGaN barrier layer, P type GaN layer and highly dope p-type GaN contact electrode layer.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. a preparation method for GaN base white light LEDs epitaxial structure, is characterized in that, comprises the following steps:
Hydride gas-phase epitaxy is used to prepare monocrystalline or polycrystalline aluminum nitride resilient coating on rare earth doped YAG pottery or single crystalline substrate;
Use metal organic chemical vapor deposition growing GaN base LED epitaxial structure on described monocrystalline or polycrystalline aluminum nitride resilient coating, 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 region from bottom to top, AlGaN electronic barrier layer, P type GaN layer and highly dope p-type or highly doped contact electrode layer.
2. preparation method according to claim 1, it is characterized in that, in described rare earth doped YAG pottery or single crystalline substrate, rare earth element comprises one or more in Ce, Eu, Nd, Yb, doping content is 0.05at% to 0.5at%, substrate thickness is 100 μm to 1000 μm, as substrate YAG pottery or single-crystal surface through meticulous polishing, its surface roughness is less than 0.5nm.
3. preparation method according to claim 1, is characterized in that, on rare earth doped YAG pottery or single crystalline substrate, prepare monocrystalline or polycrystalline aluminum nitride resilient coating by hydride gas-phase epitaxy, its concrete operations are:
First, rare earth doped YAG pottery or single crystalline substrate are toasted under hydrogen, passes into ammonia subsequently and carry out high-temperature ammonolysis process;
Finally, hydrogen chloride and ammonia are passed in aluminium source region and reative cell respectively, the rare earth doped YAG pottery after high-temperature ammonolysis process or single crystalline substrate are carried out the growth of monocrystalline or polycrystalline aluminum nitride resilient coating.
4. preparation method according to claim 3, is characterized in that, the temperature that rare earth doped YAG pottery or single crystalline substrate are 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, and the processing time is 3 to 60 minutes.
5. preparation method according to claim 3, is characterized in that, aluminium source region is aluminum shot, and the carrier gas of hydrogen chloride and ammonia is 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, and the flow of carrier gas is 500 to 2000Torr.
6. preparation method according to claim 3, is characterized in that, the temperature in aluminium source region is 450 DEG C to 600 DEG C, and growth temperature is 500 DEG C to 1500 DEG C.
7. the preparation method according to claim 1 or 3, is characterized in that, the thickness of single-crystal aluminum nitride resilient coating is 5nm to 100nm.
8. preparation method according to claim 1, is characterized in that, uses metal organic chemical vapor deposition growing GaN base LED epitaxial structure on described monocrystalline or polycrystalline aluminum nitride resilient coating, comprising:
The low temperature GaN buffer of 50nm-300nm thickness is grown at temperature is 500 DEG C-700 DEG C;
The high temperature GaN resilient coating of 2-4um thickness is grown at temperature is 900 DEG C-1200 DEG C;
At temperature is 900 DEG C-1200 DEG C, grow the N-type GaN layer of 1um-3um, wherein, the Si doping content in N-type GaN layer is 1 × 10
17cm
-3-3 × 10
20cm
-3;
The InGaN/GaN multiple quantum well light emitting layer of 1-30 circulation is grown at temperature is 650 DEG C-850 DEG C;
At temperature is 800 DEG C-1150 DEG C, grow the P type GaN layer of 100nm-800nm, wherein, Mg doping content is 1 × 10
17cm
-3-3 × 10
20cm
-3;
At temperature is 800 DEG C-1200 DEG C, grow highly dope p-type or the N-type electrode contact layer of 5nm-50nm, wherein, Mg doping content is 1 × 10
18cm
-3-5 × 10
20cm
-3, Si doping content is 1 × 10
17cm
-3-5 × 10
20cm
-3.
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