CN106531852A - LED epitaxial growth method for enhancing device antistatic capability - Google Patents
LED epitaxial growth method for enhancing device antistatic capability Download PDFInfo
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- 230000012010 growth Effects 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 23
- 230000002708 enhancing effect Effects 0.000 title abstract description 3
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 25
- 239000010980 sapphire Substances 0.000 claims abstract description 25
- 239000000758 substrate Substances 0.000 claims abstract description 24
- 239000013078 crystal Substances 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 229910002704 AlGaN Inorganic materials 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 80
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 78
- 229910021529 ammonia Inorganic materials 0.000 claims description 39
- 229910052757 nitrogen Inorganic materials 0.000 claims description 38
- 239000011777 magnesium Substances 0.000 claims description 22
- 230000000694 effects Effects 0.000 claims description 18
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 239000010409 thin film Substances 0.000 claims description 10
- 230000001965 increasing effect Effects 0.000 claims description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 7
- 229910052749 magnesium Inorganic materials 0.000 claims description 7
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 238000005546 reactive sputtering Methods 0.000 claims description 5
- 238000005728 strengthening Methods 0.000 claims description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims 2
- 229910052786 argon Inorganic materials 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000009413 insulation Methods 0.000 claims 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 14
- 229910052593 corundum Inorganic materials 0.000 abstract description 14
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 10
- 230000008901 benefit Effects 0.000 abstract description 7
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 30
- 238000012360 testing method Methods 0.000 description 10
- 229910052710 silicon Inorganic materials 0.000 description 9
- 150000002431 hydrogen Chemical class 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000001307 helium Substances 0.000 description 4
- 229910052734 helium Inorganic materials 0.000 description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 4
- 238000000407 epitaxy Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 241001269238 Data Species 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- -1 make as N sources Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-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
- H01L33/005—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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/0237—Materials
- H01L21/024—Group 12/16 materials
- H01L21/02403—Oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02436—Intermediate layers between substrates and deposited layers
- H01L21/02439—Materials
- H01L21/02455—Group 13/15 materials
- H01L21/02458—Nitrides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/20—Deposition of semiconductor materials on a substrate, e.g. epitaxial growth solid phase epitaxy
- H01L21/2003—Deposition of semiconductor materials on a substrate, e.g. epitaxial growth solid phase epitaxy characterised by the substrate
- H01L21/2011—Deposition of semiconductor materials on a substrate, e.g. epitaxial growth solid phase epitaxy characterised by the substrate the substrate being of crystalline insulating material, e.g. sapphire
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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
- H01L33/20—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 particular shape, e.g. curved or truncated substrate
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/26—Materials of the light emitting region
- H01L33/30—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table
- H01L33/32—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table containing nitrogen
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Abstract
The invention discloses an LED epitaxial growth method for enhancing a device antistatic capability. The method comprises the following steps: growing an AlN layer on a sapphire substrate; growing an InN layer on the AlN layer; continuously growing a Si-doped N-type GaN layer; periodically growing an active layer MQW; continuously growing a P-type AlGaN layer; continuously growing a P-type GaN layer; and performing cooling. According to the invention, by use of the advantage of small crystal lattice mismatch between AlN and the sapphire substrate Al2O3 and the advantage of small crystal lattice mismatch between an InN material and the AlN/GaN, through reducing dislocation generated by the crystal lattice mismatch, the dislocation density of an epitaxial layer is reduced, the crystal quality of the epitaxial layer is improved, the antistatic capability of an LED device is improved, at the same time, electric leakage of the LED device is reduced, and the quality of the LED product is improved.
Description
Technical field
The application is related to LED epitaxial scheme applied technical fields, specifically, is related to a kind of enhancing device antistatic effect
LED epitaxial growth methods.
Background technology
LED (Light Emitting Diode, light emitting diode) is a kind of solid state lighting, and small volume, power consumption are low to be made
With life-span length high brightness, environmental protection, it is sturdy and durable the advantages of approved by consumers in general, the scale of domestic production LED also by
Step expands.Country's MOCVD epitaxy growing technology covers the 70% or so of LED industry technology at present, how to grow more preferable extension
Piece is increasingly subject to pay attention to, and high-quality epitaxial wafer demand increasingly increases, because the raising of epitaxial layer crystal mass, LED component
Performance can be when being lifted, and the life-span of LED, ageing resistance, antistatic effect, stability can be with epitaxial layer crystal mass
Lifted and lifted, wherein antistatic effect is one important parameter of product, antistatic effect is strong, the price height of product, yield
Height, the remarkable in economical benefits of generation.
In sapphire Al in traditional epitaxy technology2O3Grown on substrates GaN material, because Al2O3Material and GaN material
About 14% lattice mismatch is there is, the impact for bringing is that GaN material dislocation density is up to 109/cm2, dislocation is controlled at present
The main method of density is that one layer of thin GaN of low-temperature epitaxy makees cushion, and the 3D growths and 2D for then carrying out GaN on this basis is given birth to
It is long, eventually form the smooth GaN layer of comparison.Because GaN material dislocation is close big, crystal mass is poor, there is provided the passage of electric leakage, LED
The antistatic effect of device is relatively weak, and particularly under high voltage, antistatic effect drastically weakens.
The content of the invention
To solve above-mentioned technical problem, the invention provides a kind of LED epitaxial growth sides for strengthening device antistatic effect
Method, including step：
Sapphire Al2O3 underlayer temperatures are heated to into 600 DEG C or so using DC magnetron reactive sputtering equipment, 70- is passed through
90sccm helium (Ar), 100-120sccm nitrogen (N2) and 2-3sccm oxygen (O2), with the bias impact aluminum of 2000-3000V
Target sputters the thick AlN thin film of 60-70nm on PSS surfaces；
The sapphire Al2O3 substrates for having sputtered AlN thin film are put into into MOCVD reaction chambers, high-temperature are risen to 900-
1000 DEG C, reaction cavity pressure maintains 400-500mbar, be passed through the nitrogen of 130-150L/min, the ammonia of 120-140L/min,
The InN layers of 7-9 μm of the TMIn sources continued propagation of 100-200sccm；
High-temperature is risen again to 1000-1100 DEG C, and reaction cavity pressure maintains 150-300mbar, is passed through 50-90L/min's
Hydrogen, the ammonia of 40-60L/min, the TMGa sources of 200-300sccm, the SiH of 20-50sccm4Source, the N of continued propagation doping Si
Type GaN, Si doping contents 5E+18atoms/cm3-1E+19atoms/cm3, gross thickness control is at 2-4 μm；
Cyclical growth has edge layer MQW, and reaction cavity pressure maintains 300-400mbar, temperature control at 700-750 DEG C,
It is passed through the nitrogen of 50-90L/min, the ammonia of 40-60L/min, the TMGa sources of 10-50sccm, the TMIn of 1000-2000sccm
Source, the 3-4nm In of growth doping InxGa(1-x)N (x=0.15-0.25) layer (1), In doping contents 1E+20atoms/cm3-3E
+20atoms/cm3, then 800-850 DEG C of intensification be passed through the nitrogen of 50-90L/min, the ammonia of 40-60L/min, 10-
The TMGa sources of 50sccm, growth 10-15nmGaN layers (2). then InxGa(1-x)N and GaN alternating growth in this way, cycle
Number is 10-15；
850-950 DEG C is increased the temperature to again, and reaction cavity pressure maintains 200-400mbar, is passed through the nitrogen of 50-90L/min
Gas, the ammonia of 40-60L/min, the TMGa sources of 50-100sccm, the p-type AlGaN layer of continued propagation 50-100nm, Al doping are dense
Degree 1E+20-3E+20atoms/cm3, Mg doping contents 5E+18atoms/cm3-1E+19atoms/cm3；
950-1000 DEG C is increased the temperature to, reaction cavity pressure maintains 200-600mbar, is passed through the nitrogen of 50-90L/min
Gas, the ammonia of 40-60L/min, the TMGa sources of 50-100sccm, the p-type GaN layer for mixing magnesium of continued propagation 100-300nm, Mg are mixed
Miscellaneous concentration 1E+19atoms/cm3-1E+20atoms/cm3；
700-800 DEG C is cooled to, the nitrogen of 100-150L/min is individually passed through, 20-30min is incubated, then cooling in stove.
Preferably, the InxGa(1-x)X spans in N shell are between 0.15-0.25.
The present invention replaces original low temperature GaN, 2D GaN, 3D GaN material using new AlN, InN material, obtains a kind of
New material and growth technique, because AlN and sapphire substrate Al2O3Mismatch about 2%, GaN and sapphire substrate
Al2O3Lattice mismatch 14%, using AlN and sapphire substrate Al2O3The little advantage of lattice mismatch, InN materials and AlN, GaN it is brilliant
The little advantage of lattice mismatch, by reducing the dislocation that lattice mismatch is produced, reduces epitaxial layer dislocation density, improves epitaxial layer crystal matter
Amount, dislocation density are little, and LED component exists>Under the electrostatic high-pressure of 2KV, there is provided leak channel is reduced, breakdown probability diminishes, and resists
Electrostatic capacity is lifted, so as to LED product quality gets a promotion.
Description of the drawings
Accompanying drawing described herein is used for providing a further understanding of the present invention, constitutes the part of the present invention, this
Bright schematic description and description does not constitute inappropriate limitation of the present invention for explaining the present invention.In the accompanying drawings：
LED junction compositions of the Fig. 1 for the method production of prior art；
Fig. 2 is the LED junction composition produced using the method for the present invention.
As in description and claim some vocabulary used in censuring specific components.Those skilled in the art should
It is understood that hardware manufacturer may call same component with different nouns.This specification and claims are not with name
The difference of title is used as the mode for distinguishing component, but the difference with component functionally is used as the criterion distinguished.Such as logical
The "comprising" of piece description and claim mentioned in is an open language, therefore should be construed to " include but do not limit
In "." substantially " refer in receivable range of error, those skilled in the art can solve described in the range of certain error
Technical problem, basically reaches the technique effect.Description subsequent descriptions are to implement the better embodiment of the present invention, so described
Description is, for the purpose of illustrating the rule of the present invention, to be not limited to the scope of the present invention.Protection scope of the present invention
When being defined depending on the defined person of claims.
Specific embodiment
The present invention is described in further detail below in conjunction with accompanying drawing, but it is not as a limitation of the invention.
Embodiment 1：
The present invention uses MOCVD next life long high brightness GaN-based LED.Using high-purity hydrogen or high pure nitrogen or height
The mixed gas of pure hydrogen and high pure nitrogen used as carrier gas, make as N sources, metal organic source trimethyl gallium (TMGa) by high-purity ammonia
For gallium source, used as indium source, N type dopant is silane (SiH to trimethyl indium (TMIn)4), trimethyl aluminium (TMAl) is used as silicon source, P
Type dopant is two luxuriant magnesium (CP2Mg), substrate is (0001) surface sapphire, and reaction pressure is between 100mbar to 800mbar.
Step 101：Using DC magnetron reactive sputtering equipment by sapphire Al2O31 temperature of substrate is heated to 600 DEG C, is passed through
70sccm helium (Ar), 100sccm nitrogen (N2) and 2sccm oxygen (O2), impact aluminum target in sapphire with the bias of 2000V
Al2O3The thick AlN thin film 6 of 60nm is sputtered on substrate 1；
Step 102：The sapphire Al2O3 substrates for having sputtered AlN thin film 6 are put into into MOCVD reaction chambers, high-temperature is risen
To 900 DEG C, reaction cavity pressure maintains 400mbar, is passed through the nitrogen of 130L/min, the ammonia of 120L/min, 100sccm
The InN layers 7 of 7 μm of TMIn sources continued propagation；
Step 103：High-temperature is risen again to 1000 DEG C, reaction cavity pressure maintain 150mbar, be passed through 50L/min hydrogen,
The ammonia of 40L/min, the TMGa sources of 200sccm, the SiH4 sources of 20sccm, N-type GaN 2 of continued propagation doping Si, Si doping
Concentration 5E+18atoms/cm3, gross thickness control is at 2 μm；
Step 104：Cyclical growth has edge layer MQW 3, and reaction cavity pressure maintains 300mbar, and temperature control is 700
DEG C, it is passed through the nitrogen of 50L/min, the ammonia of 40L/min, the TMGa sources of 10sccm, the TMIn sources of 1000sccm, growth doping In
3nm InxGa(1-x)N (x=0.15-0.25) layer 32, In doping contents 1E+20atoms/cm3, then heat up 800 DEG C, be passed through
The nitrogen of 50L/min, the ammonia of 40L/min, the TMGa sources of 10sccm, grow the then In of 10nmGaN layers 31.xGa(1-x)N and GaN
Alternating growth in this way, periodicity is 10；
Step 105：Increase the temperature to 850 DEG C again, reaction cavity pressure maintain 200mbar, be passed through 50L/min nitrogen,
The ammonia of 40L/min, the TMGa sources of 50sccm, the p-type AlGaN layer 4 of continued propagation 50nm, Al doping contents 1E+20atoms/
cm3, Mg doping contents 5E+18atoms/cm3；
Step 106：Increase the temperature to 950 DEG C, reaction cavity pressure maintain 200mbar, be passed through 50L/min nitrogen,
The ammonia of 40L/min, the TMGa sources of 50sccm, the p-type GaN layer 5 for mixing magnesium of continued propagation 100nm, Mg doping contents 1E+
19atoms/cm3；
Step 107：700 DEG C are cooled to, the nitrogen of 100L/min is individually passed through, 20min is incubated, then cooling in stove.
Embodiment 2：
Step 201：Using DC magnetron reactive sputtering equipment by sapphire Al2O31 temperature of substrate is heated to 600 DEG C, is passed through
80sccm helium (Ar), 110sccm nitrogen (N2) and 2.5sccm oxygen (O2), aluminum target is impacted in sapphire with the bias of 2600V
Al2O3The sputtering 66nm of substrate 1 thick AlN thin film 6；
Step 202：The sapphire Al of AlN thin film will have been sputtered2O3Substrate is put into MOCVD reaction chambers, rises high-temperature extremely
970 DEG C, reaction cavity pressure maintains 460mbar, is passed through the nitrogen of 140L/min, the ammonia of 125L/min, the TMIn of 160sccm
The InN layers 7 of 7.8 μm of source continued propagation；
Step 203：High-temperature is risen again to 1080 DEG C, reaction cavity pressure maintain 200mbar, be passed through 70L/min hydrogen,
The ammonia of 50L/min, the TMGa sources of 250sccm, the SiH of 40sccm4Source, N-type GaN 2 of continued propagation doping Si, Si doping
Concentration 8E+18atoms/cm3, gross thickness control is at 3 μm；
Step 204：Cyclical growth has edge layer MQW 3, and reaction cavity pressure maintains 370mbar, and temperature control is 730
DEG C, it is passed through the nitrogen of 60L/min, the ammonia of 50L/min, the TMGa sources of 40sccm, the TMIn sources of 1600sccm, growth doping In
3.4nm InxGa(1-x)N (x=0.15-0.25) layer 32, In doping contents 2E+20atoms/cm3, then heat up 830 DEG C, lead to
Enter the nitrogen of 70L/min, the ammonia of 48L/min, the TMGa sources of 38sccm, the then In of growth 13nmGaN layers 31.xGa(1-x)N and
GaN alternating growths in this way, periodicity is 13；
Step 205：Increase the temperature to 900 DEG C again, reaction cavity pressure maintain 300mbar, be passed through 60L/min nitrogen,
The ammonia of 52L/min, the TMGa sources of 85sccm, the p-type AlGaN layer 4 of continued propagation 80nm, Al doping contents 2E+20atoms/
cm3, Mg doping contents 7E+18atoms/cm3；
Step 206：Increase the temperature to 980 DEG C, reaction cavity pressure maintain 400mbar, be passed through 65L/min nitrogen,
The ammonia of 47L/min, the TMGa sources of 80sccm, the p-type GaN layer 5 for mixing magnesium of continued propagation 250nm, Mg doping contents 6E+
19atoms/cm3；
Step 207：760 DEG C are cooled to, the nitrogen of 120L/min is individually passed through, 26min is incubated, then cooling in stove.
Embodiment 3：
Step 301：1 temperature of sapphire Al2O3 substrates is heated to into 600 DEG C using DC magnetron reactive sputtering equipment, is led to
Enter 90sccm helium (Ar), 120sccm nitrogen (N2) and 3sccm oxygen (O2), aluminum target is impacted in sapphire with the bias of 3000V
Al2O3The sputtering 70nm of substrate 1 thick AlN thin film 6；
Step 302：The sapphire Al of AlN thin film will have been sputtered2O3Substrate is put into MOCVD reaction chambers, rises high-temperature extremely
1000 DEG C, reaction cavity pressure maintains 500mbar, is passed through the nitrogen of 150L/min, the ammonia of 140L/min, 200sccm
The InN layers 7 of 9 μm of TMIn sources continued propagation；
Step 303：High-temperature is risen again to 1100 DEG C, reaction cavity pressure maintain 300mbar, be passed through 90L/min hydrogen,
The ammonia of 60L/min, the TMGa sources of 300sccm, the SiH4 sources of 50sccm, N-type GaN 2 of continued propagation doping Si, Si doping
Concentration 1E+19atoms/cm3, gross thickness control is at 4 μm；
Step 304：Cyclical growth has edge layer MQW 3, and reaction cavity pressure maintains 400mbar, and temperature control is 750
DEG C, it is passed through the nitrogen of 90L/min, the ammonia of 60L/min, the TMGa sources of 50sccm, the TMIn sources of 2000sccm, growth doping In
4nm InxGa(1-x)N (x=0.15-0.25) layer 32, In doping contents 3E+20atoms/cm3, then heat up 850 DEG C, be passed through
The nitrogen of 90L/min, the ammonia of 60L/min, the TMGa sources of 50sccm, grow the then In of 15nmGaN layers 31.xGa(1-x)N and GaN
Alternating growth in this way, periodicity is 15；
Step 305：Increase the temperature to 950 DEG C again, reaction cavity pressure maintain 400mbar, be passed through 90L/min nitrogen,
The ammonia of 60L/min, the TMGa sources of 100sccm, the p-type AlGaN layer 4 of continued propagation 100nm, Al doping contents 3E+
20atoms/cm3, Mg doping contents 1E+19atoms/cm3；
Step 306：Increase the temperature to 1000 DEG C, reaction cavity pressure maintain 600mbar, be passed through 90L/min nitrogen,
The ammonia of 60L/min, the TMGa sources of 100sccm, the p-type GaN layer 5 for mixing magnesium of continued propagation 300nm, Mg doping contents 1E+
20atoms/cm3；
Step 307：800 DEG C are cooled to, the nitrogen of 150L/min is individually passed through, 230min is incubated, then cooling in stove.
Contrast experiment：
(1) at 900-1100 DEG C, react the hydrogen height for being passed through 50-100L/min that cavity pressure maintains 100-200mbar
Temperature processes Sapphire Substrate 1 in 5-10 minutes；
(2), at being cooled to 500-650 DEG C, reaction cavity pressure maintains 300-600mbar, is passed through the hydrogen of 50-90L/min
Gas, the ammonia of 40-60L/min, 50-100sccm TMGa sources on a sapphire substrate growth thickness for 30-60nm low temperature delay
Rush layer GaN 8；
(3), at increasing the temperature to 850-1000 DEG C, reaction cavity pressure maintains 300-600mbar, is passed through 50-90L/min
Hydrogen, the ammonia of 40-60L/min, the 3D GaN layers 9 of 1-2 μm of the TMGa sources continued propagation of 200-300sccm；
(4), at increasing the temperature to 1000-1100 DEG C, reaction cavity pressure maintains 300-600mbar, is passed through 50-90L/min
Hydrogen, the ammonia of 40-60L/min, the 2D GaN layers 10 of 2-3 μm of the TMGa sources continued propagation of 300-400sccm；
(5) and then keeping temperature is at 1000-1100 DEG C, reaction cavity pressure maintains 150-300mbar, is passed through 50-
The hydrogen of 90L/min, the ammonia of 40-60L/min, the TMGa sources of 200-300sccm, the SiH4 sources of 20-50sccm, continued propagation
The N-type GaN layer 2 of doping Si, Si doping contents 5E+18atoms/cm3-1E+19atoms/cm3, gross thickness control is at 2-4 μm；
(6) cyclical growth has edge layer MQW 3, and reaction cavity pressure maintains 300-400mbar, and temperature control is in 700-
750 DEG C, it is passed through the nitrogen of 50-90L/min, the ammonia of 40-60L/min, the TMGa sources of 10-50sccm, 1000-2000sccm
TMIn sources, the 3-4nm In of growth doping InxGa(1-x)N (x=0.15-0.25) layer 32, In doping contents 1E+20atoms/
cm3-3E+20atoms/cm3, then 800-850 DEG C of intensification be passed through the nitrogen of 50-90L/min, the ammonia of 40-60L/min, 10-
The TMGa sources of 50sccm, grow 10-15nmGaN layers 31, then InxGa(1-x)N shell 32 and GaN layer 31 are alternately given birth in this way
Long, periodicity is 10-15；
(7) 850-950 DEG C is increased the temperature to again, reaction cavity pressure maintains 200-400mbar, is passed through 50-90L/min's
Nitrogen, the ammonia of 40-60L/min, the TMGa sources of 50-100sccm, the p-type GaN layer 4 of continued propagation 50-100nm, Al doping are dense
Degree 1E+20-3E+20atoms/cm3, Mg doping contents 5E+18atoms/cm3-1E+19atoms/cm3；
(8) 950-1000 DEG C is increased the temperature to again, reaction cavity pressure maintains 200-600mbar, is passed through 50-90L/min
Nitrogen, the ammonia of 40-60L/min, the TMGa sources of 50-100sccm, the p-type GaN layer for mixing magnesium of continued propagation 100-300nm
5, Mg doping contents 1E+19atoms/cm3-1E+20atoms/cm3；
(9) 700-800 DEG C is finally cooled to, is individually passed through the nitrogen of 100-150L/min, be incubated 20-30min, then stove
Interior cooling.
Comparison of experiment results：
4 samples 1 are prepared according to the growing method of contrast experiment, 4 samples 2 are prepared according to the method for embodiment 3.Sample
1 is made using traditional growing method, and sample 2 provides growing method using this patent and makes.After sample 1 and sample 2 have grown
Take out, test the XRD102 faces (refer to table 1) of epitaxial wafer at identical conditions.Sample 1 and sample 2 technique before identical
Under the conditions of plate about 1500 angstroms of ITO layer, about 2500 angstroms of Cr/Pt/Au electrodes are plated under the conditions of identical, plating under the conditions of identical is protected
Sheath SiO2About 500 angstroms, then at identical conditions by sample grinding and cutting into 762 μm * 762 μm (30mi*30mil)
Chip granule, then sample 1 and sample 2 each select 100 crystal grain in same position, under identical packaging technology, encapsulation
Into white light LEDs.Carry out the test of following test (1) photoelectric properties：In same LED point measurement machine under the conditions of driving current 350mA
The photoelectric properties (2) of test sample 1 and sample 2 and antistatic effect：2KV is respectively adopted to sample in same LED point measurement machine
4KV 6KV 8KV pulses carry out antistatic test；It is shown in Table 2,3.
2 extension XRD test data of 1 sample 1 of table and sample
2 sample 1 of table and sample 2LED test machine opto-electronic test datas
3 sample 1 of table and sample 2LED test machine antistatic yield test datas
Data analysiss conclusion：(1) table 1 shows that the sample XRD102 faces numerical value of the art of this patent making diminishes and characterizes patent skill
The crystal mass of the sample epitaxial layer that art makes is more excellent, hence it is evident that improve；(2) table 2 shows the sample LED that the art of this patent makes
More preferably, brightness is high, voltage is low for photoelectric properties, and the sample LED component electric leakage that the art of this patent makes is significantly improved, and this obtains
Benefit the art of this patent and reduce epitaxial layer dislocation, reduce leak channel；(3) table 3 shows the sample LED that the art of this patent makes
Antistatic effect is preferable, with the increase of voltage, though antistatic effect has decline amplitude to diminish, it was demonstrated that the sample that this patent makes
Product antistatic effect has lifting.
Described above illustrates and describes some preferred embodiments of the present invention, but as previously mentioned, it should be understood that the present invention
Be not limited to form disclosed herein, be not to be taken as the exclusion to other embodiment, and can be used for various other combinations,
Modification and environment, and can be in invention contemplated scope described herein, by above-mentioned teaching or the technology or knowledge of association area
It is modified.And change that those skilled in the art are carried out and change be without departing from the spirit and scope of the present invention, then all should be at this
In the protection domain of bright claims.
Claims (6)
1. a kind of LED epitaxial growth methods for strengthening device antistatic effect, include successively：Growing AIN on a sapphire substrate
Layer；Grow above the AlN layers InN layers, the N-type GaN layer of growth doping Si, cyclical growth have edge layer, growing P-type AlGaN layer,
The p-type GaN layer of growth doping Mg, cooling down, it is characterised in that
The growing AIN layer on a sapphire substrate, further for：
Sapphire substrate temperature is heated to into 600 DEG C or so using DC magnetron reactive sputtering equipment, 70sccm-90sccm is passed through
Argon, the nitrogen of 80sccm-100sccm and 2sccm-3sccm oxygen, with the bias of 2000V-3000V impact aluminum target
The thick A1N thin film of 60nm-70nm is sputtered on patterned sapphire substrate surface；
It is described on AlN layers grow InN layers, further for：
The Sapphire Substrate for having sputtered AlN thin film is put into into MOCVD reaction chambers, high-temperature is risen at 900-1000 DEG C, reaction chamber
Pressure maintains 400-500mbar, is passed through the nitrogen of 130-150L/min, the ammonia of 120-140L/min, 100-200sccm
The InN layers of 7-9 μm of TMIn sources continued propagation.
2. the LED epitaxial growth methods of device antistatic effect are strengthened according to claim 1, it is characterised in that
It is described growth doping Si N-type GaN layer, further for：
At increasing the temperature to 1000-1100 DEG C, reaction cavity pressure maintain 150-300mbar, be passed through 50-90L/min hydrogen,
The ammonia of 40-60L/min, the TMGa sources of 200-300sccm, the SiH of 20-50sccm4Source, the N-type of continued propagation doping Si
GaN, Si doping content 5E+18atoms/cm3-1E+19atoms/cm3, gross thickness control is at 2-4 μm.
3. the LED epitaxial growth methods of device antistatic effect are strengthened according to claim 1, it is characterised in that
The cyclical growth has edge layer, further for：
Reaction cavity pressure maintains 300-400mbar, and temperature control is passed through nitrogen, the 40- of 50-90L/min at 700-750 DEG C
The ammonia of 60L/min, the TMGa sources of 10-50sccm, the TMIn sources of 1000-2000sccm, the 3-4nm of growth doping In
InxGa(1-x)N (x=0.15-0.25) layer (1), In doping contents 1E+20atoms/cm3-3E+20atoms/cm3, then heat up
800-850 DEG C, the nitrogen of 50-90L/min, the ammonia of 40-60L/min, the TMGa sources of 10-50sccm are passed through, grow 10-
15nmGaN layers (2). then InxGa(1-x)N and GaN alternating growth in this way, periodicity is 10-15.
4. the LED epitaxial growth methods of device antistatic effect are strengthened according to claim 1, it is characterised in that
The growing P-type AlGaN layer, further for：
850-950 DEG C is increased the temperature to, reaction cavity pressure maintains 200-400mbar, is passed through nitrogen, the 40- of 50-90L/min
The ammonia of 60L/min, the TMGa sources of 50-100sccm, the p-type AlGaN layer of continued propagation 50-100nm, Al doping contents 1E+
20atoms/cm3-3E+20atoms/cm3, Mg doping contents 5E+18atoms/cm3-1E+19atoms/cm3。
5. the LED epitaxial growth methods of device antistatic effect are strengthened according to claim 1, it is characterised in that
It is described growth doping Mg p-type GaN layer, further for：
950-1000 DEG C is increased the temperature to, reaction cavity pressure maintains 200-600mbar, is passed through nitrogen, the 40- of 50-90L/min
The ammonia of 60L/min, the TMGa sources of 50-100sccm, the p-type GaN layer for mixing magnesium of continued propagation 100-300nm, Mg doping contents
1E+19atoms/cm3-1E+20atoms/cm3。
6. according to claim 1-4 it is arbitrary described raising epitaxial crystal quality LED growing methods, it is characterised in that
The cooling down, further for：700 DEG C -800 DEG C are cooled to, the nitrogen of 100L/min-150L/min is individually passed through,
Insulation 20min-30min, furnace cooling.
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| CN105023976A (en) * | 2015-06-10 | 2015-11-04 | 湘能华磊光电股份有限公司 | An LED epitaxy growth method |
| CN105070653A (en) * | 2015-08-18 | 2015-11-18 | 湘能华磊光电股份有限公司 | LED epitaxial growth method for enhancing antistatic effect of device |
| CN105789388A (en) * | 2016-04-25 | 2016-07-20 | 湘能华磊光电股份有限公司 | LED growth method capable of improving quality of epitaxial crystal |
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| CN105023976A (en) * | 2015-06-10 | 2015-11-04 | 湘能华磊光电股份有限公司 | An LED epitaxy growth method |
| CN105070653A (en) * | 2015-08-18 | 2015-11-18 | 湘能华磊光电股份有限公司 | LED epitaxial growth method for enhancing antistatic effect of device |
| CN105789388A (en) * | 2016-04-25 | 2016-07-20 | 湘能华磊光电股份有限公司 | LED growth method capable of improving quality of epitaxial crystal |
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| CN116344684A (en) * | 2023-05-29 | 2023-06-27 | 江西兆驰半导体有限公司 | Light-emitting diode preparation method and diode |
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