CN109300855A - Improve the LED epitaxial growth method of growth quality - Google Patents
Improve the LED epitaxial growth method of growth quality Download PDFInfo
- Publication number
- CN109300855A CN109300855A CN201811210449.5A CN201811210449A CN109300855A CN 109300855 A CN109300855 A CN 109300855A CN 201811210449 A CN201811210449 A CN 201811210449A CN 109300855 A CN109300855 A CN 109300855A
- Authority
- CN
- China
- Prior art keywords
- growth
- flow
- layers
- temperature
- layer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 45
- 239000000758 substrate Substances 0.000 claims abstract description 42
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 41
- 239000010980 sapphire Substances 0.000 claims abstract description 41
- 229910002704 AlGaN Inorganic materials 0.000 claims abstract description 22
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 239000011777 magnesium Substances 0.000 claims description 29
- 238000000137 annealing Methods 0.000 claims description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052749 magnesium Inorganic materials 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000013078 crystal Substances 0.000 abstract description 22
- 230000000694 effects Effects 0.000 abstract description 14
- 230000007547 defect Effects 0.000 abstract description 9
- 238000002955 isolation Methods 0.000 abstract description 8
- 238000012360 testing method Methods 0.000 abstract description 6
- 230000000903 blocking effect Effects 0.000 abstract description 4
- 230000002950 deficient Effects 0.000 abstract description 4
- 230000001186 cumulative effect Effects 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 19
- 239000000463 material Substances 0.000 description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000000407 epitaxy Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 3
- 238000012797 qualification Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- JRVCPDVOFCWKAG-UHFFFAOYSA-N Amosulalol hydrochloride Chemical compound Cl.COC1=CC=CC=C1OCCNCC(O)C1=CC=C(C)C(S(N)(=O)=O)=C1 JRVCPDVOFCWKAG-UHFFFAOYSA-N 0.000 description 1
- 241001025261 Neoraja caerulea Species 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000007771 core particle Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 230000009643 growth defect Effects 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
Classifications
-
- 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
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/77—Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in, or on, a common substrate
- H01L21/78—Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in, or on, a common substrate with subsequent division of the substrate into plural individual devices
- H01L21/82—Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in, or on, a common substrate with subsequent division of the substrate into plural individual devices to produce devices, e.g. integrated circuits, each consisting of a plurality of components
- H01L21/84—Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in, or on, a common substrate with subsequent division of the substrate into plural individual devices to produce devices, e.g. integrated circuits, each consisting of a plurality of components the substrate being other than a semiconductor body, e.g. being an insulating body
- H01L21/86—Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in, or on, a common substrate with subsequent division of the substrate into plural individual devices to produce devices, e.g. integrated circuits, each consisting of a plurality of components the substrate being other than a semiconductor body, e.g. being an insulating body the insulating body being sapphire, e.g. silicon on sapphire structure, i.e. SOS
-
- 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
- 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
- H01L33/0075—Processes for devices with an active region comprising only III-V compounds comprising nitride compounds
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/04—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction
- H01L33/06—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction within the light emitting region, e.g. quantum confinement structure or tunnel barrier
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/12—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a stress relaxation structure, e.g. buffer layer
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Led Devices (AREA)
Abstract
This application discloses a kind of LED epitaxial growth method for improving growth quality, method includes the Sapphire Substrate for handling surface and having AlN film, sequentially grows Al in the Sapphire Substrate0.8Ga0.2N layers, growth Al0.5Ga0.5N layers and growth Al0.2Ga0.8N layers, grow the GaN layer that undopes, the N-type GaN layer of growth doping Si, cyclical growth active layer MQW, growing P-type AlGaN layer, the p-type GaN layer and cooling down of growth doping Mg.The blocking and isolation mech isolation test of defect when the method for the present invention increases epitaxial crystal growth improve Lattice Matching, reduce dislocation density, reduce defective proportion, crystal quality is improved, to improve LED luminous efficiency, improve antistatic effect, and improves epitaxial wafer appearance situation.Be conducive to eliminate Sapphire Substrate simultaneously to the cumulative stress effect of GaN film, reduce epitaxial wafer warpage, improve product yield.
Description
Technical field
The present invention relates to LED epitaxial wafer growing technology fields, specifically, being related to outside a kind of LED of raising growth quality
Prolong growing method.
Background technique
The GaN growth method generallyd use at present is to be patterned on a sapphire substrate.Sapphire crystal is third
Best one of substrate material is grown for semiconductor material GaN epitaxial layer, single crystal preparation technique is mature.GaN is blue-ray LED system
Make substrate.The wherein substrate material SiC of GaN epitaxial layer, it is small with GaN lattice mismatch, only 3.4%, but its thermal expansion system
Number is larger with GaN difference, easily leads to GaN epitaxial layer fracture, and manufacturing cost is high, is sapphire 10 times；Substrate material Si
It is at low cost, it is big with GaN lattice mismatch, reach 17%, growth GaN is more difficult, and luminous efficiency is too low compared with sapphire；Substrate
Material sapphire crystal structure is identical (the symmetrical wurtzite crystal structure of six sides), big by 13% with GaN lattice mismatch, easily leads to
GaN epitaxial layer high dislocation density can drop for this purpose, AlN or low temperature GaN epitaxial layer or SiO2 layers etc. are added on a sapphire substrate
Low GaN epitaxial layer dislocation density.
There are biggish lattice mismatch (13-16%) and thermal mismatchings between sapphire and GaN, so that the mistake in GaN epitaxial layer
Density of misfit dislocations is higher by (~1010cm-2), influence GaN epitaxial layer quality, thus influence device quality (luminous efficiency, drain electrode,
Service life etc.).
Traditional way is using low temperature buffer layer, by adjusting the nitridation of Sapphire Substrate, the growth of low temperature buffer layer
Temperature, thickness of buffer layer etc., to improve the crystal quality of GaN epitaxial layer.But due to low temperature buffer layer still fall within it is heterogeneous
Extension, the crystal quality promoted are limited.In addition, since there are biggish lattice mismatches between each epitaxial thin-film layer, so that outside
Prolong the effect that crystal film is constantly subjected to stress during the growth process, causes epitaxial wafer to bend, warpage.Conventional cryogenic buffering
For layer method when carrying out epitaxial crystal growth on large-size sapphire substrate, epitaxial wafer warpage is big, leads to subsequent chip manufacturing mistake
Fragment rate height is ground in journey, product yield is low.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of LED epitaxial growth method for improving growth quality, feature exists
In, comprising steps of
Handle the Sapphire Substrate that surface has AlN film；
Al is sequentially grown in the Sapphire Substrate0.8Ga0.2N layers, growth Al0.5Ga0.5N layers and growth Al0.2Ga0.8N
Layer, wherein
The growth Al0.8Ga0.2N layers include: the reaction cavity pressure for controlling 400-600mbar, are passed through flow to reaction chamber
Q1 is the NH of 60-70L/min3, it is passed through the N that flow is 90-95L/min2, 100-110sccm TMGa, 230-250sccm
The source TMAl increases 0.4 DEG C with each second in growth course and growth temperature is increased to 900 DEG C from 800 DEG C of gradual changes, described blue precious
Growth thickness D1 is the Al of 8-10nm on stone lining bottom0.8Ga0.2N layers；
It keeps reaction cavity pressure and growth temperature constant, controls N2Flow is 150-160L/min, to the Al0.8Ga0.2N
Layer carries out the annealing of 8-10s；
The growth Al0.5Ga0.5N layers include: growth temperature maintain 900 DEG C it is constant, keep reaction cavity pressure and TMGa,
TMAl is passed through that flow is constant, is passed through the NH that flow Q2 is 72-84L/min to reaction chamber3, be passed through flow be 90-95L/min N2,
In the Al0.8Ga0.2Growth thickness D2 is the Al of 8-10nm on N layer0.5Ga0.5N layers, D2=D1, Q2=1.2Q1；
It keeps reaction cavity pressure and growth temperature constant, controls N2Flow is 150-160L/min, to the Al0.5Ga0.5N
Layer carries out the annealing of 8-10s；
The growth Al0.2Ga0.8N layers include: to keep reaction cavity pressure constant, and growth temperature is increased to 1100 from 900 DEG C
DEG C, keeping TMGa, TMAl to be passed through, flow is constant, is passed through the NH that flow Q3 is 60-84L/min to reaction chamber3, be passed through flow and be
The N of 90-95L/min2, control growth temperature reduces by 0.5 DEG C with each second and reduces from 1100 DEG C of gradual changes to 1000 in growth course
DEG C, in the Al0.5Ga0.5Growth thickness D3 is the Al of 8-10nm on N layer0.2Ga0.8N layers, D3=D2, Q1 < Q3 < Q2；
It keeps reaction cavity pressure and growth temperature constant, controls N2Flow is 150-160L/min, to the Al0.2Ga0.8N
Layer carries out the annealing of 8-10s；
Grow the GaN layer that undopes；
The N-type GaN layer of growth doping Si；
Cyclical growth active layer MQW；
Growing P-type AlGaN layer；
The p-type GaN layer of growth doping Mg；
And cooling down.
Preferably, at 1000-1200 DEG C, reaction cavity pressure maintains high-temperature process under the hydrogen atmosphere of 100-150mbar
There are Sapphire Substrate 5-10 minutes of AlN film on surface.
Preferably, the growth undopes GaN layer, further to increase the temperature to 1000-1200 DEG C, react cavity pressure
150-300mbar is maintained, the NH that flow is 30000-40000sccm is passed through3, 200-400sccm TMGa, 100-130L/
The H of min2, on the low temperature buffer layer 2-4 μm of continued propagation of the GaN layer that undopes.
Preferably, the N-type GaN layer of the growth doping Si, further for, keep reaction cavity pressure in 150-300mbar,
It is kept for 1000-1100 DEG C of temperature, is passed through the NH that flow is 40-60L/min3, 200-300sccm TMGa, 50-90L/min H2
And the SiH of 20-50sccm4, the N-type GaN layer of 2-4 μm of continued propagation doping Si, Si doping concentration in the GaN layer that undopes
5E+18-1E+19atoms/cm3。
Preferably, the cyclical growth active layer MQW, further for,
Reaction cavity pressure maintains 300-400mbar, 700-750 DEG C of low temperature, is passed through the NH of 50000-60000sccm3、
The flow of the TEGa and TMIn of 100-150sccm, TMIn are gradually increased with increase 25-52sccm per second from 150-170sccm
To 1500-1700sccm, the In of 30-50s is growny1Ga(1-y1)N, growth thickness D4, In doping concentration is with increase 4E+ per second
17-7E+17atoms/cm3From 1E+19atoms/cm3Fade to 3E+19atoms/cm3；
Maintain growth conditions constant, the flow for stablizing TMIn is 1500-1700sccm, grows 100-150s's
Iny2Ga(1-y2)N, growth thickness D5, In doping concentration 1E+20-3E+20atoms/cm3, the range of D4+D5 is 3-3.5nm,
The range of y1 and y2 is 0.015-0.25, and wherein y1 and y2 are unequal；
Increase temperature to 800-850 DEG C, pressure maintains 300-400mbar, be passed through 50000-60000sccm NH3,
The TEGa of 400-500sccm grows the GaN layer of 10nm, Iny1Ga(1-y1)N/Iny2Ga(1-y2)N/GaN periodicity is 10-15.
Preferably, the growing P-type AlGaN layer, further to increase the temperature to 900-1000 DEG C, reaction cavity pressure dimension
It holds in 200-400mbar, the p-type AlGaN layer of continued propagation 20-50nm on the active layer MQW, Al doping concentration 1E+20-
3E+20atoms/cm3, Mg doping concentration 5E+18-1E+19atoms/cm3。
Preferably, the p-type GaN layer of the growth doping Mg, further to increase the temperature to 930-950 DEG C, reaction chamber pressure
Power maintains 200-600mbar, and the p-type GaN layer for mixing magnesium of continued propagation 100-300nm, Mg mix in the p-type AlGaN layer
Miscellaneous concentration 1E+19-1E+20atoms/cm3。
Preferably, the cooling down, further for, be cooled to 700-800 DEG C, keep the temperature 20-30min, it is then cold in furnace
But.
Compared with prior art, the LED epitaxial growth method provided by the invention for improving growth quality reaches following beneficial
Effect:
The first, pass through the Grown on Sapphire Substrates Al in AlN film0.8Ga0.2N layers, and increased by growth temperature gradual change
Al doping efficiency improves in Calais, reduces the lattice mismatch with substrate.
The second, in Al0.8Ga0.2Al is grown on N layers0.5Ga0.5N layers, growth temperature gradual change increase can promote epitaxial layer atom
Releasing piece internal stress is conducive to that lattice mismatch early period is stopped to generate upwardly extending for defect, reduces dislocation density, improves crystal matter
Amount.
Third, in Al0.5Ga0.5Al is grown on N layers0.2Ga0.8N layers, pass through growth temperature gradual change and the control of ammonia flow
It is uniformly upward that the filling of epitaxial layer atom is presented in system, improves uniformity in piece, and improve Al0.2Ga0.8N layers with the crystalline substance of GaN layer
Lattice matching degree, epitaxial layer of the continued growth containing GaN material, GaN material reach the state of complete relaxation on this basis, to disappear
In addition to lattice mismatch bring stress during LED epitaxial material growth, the window of epitaxial film material stress control is significantly increased
Mouthful, so as to reduce epitaxial wafer warpage, be conducive to improve GaN epitaxy piece qualification rate, and improve LED luminous efficiency and
Antistatic effect.
4th, respectively to Al0.8Ga0.2N layers, Al0.5Ga0.5N layers and Al0.2Ga0.8N layers are made annealing treatment, so that
Al0.8Ga0.2N layers, Al0.5Ga0.5N layers and Al0.2Ga0.8N layers of each layer crystal lattice all obtain new regularly arranged under heat effect, obtain
Surface neatly is obtained, is conducive to next layer of growth, and keep entire epi-layer surface more smooth, surface hexagonal defect and concave hole are more
Few, entire appearance is more preferable.
5th, the blocking and isolation mech isolation test of defect when the method for the present invention increases epitaxial crystal growth improve Lattice Matching,
Dislocation density is reduced, defective proportion is reduced, improves crystal quality, thus improve LED luminous efficiency, improve antistatic effect, and
And improve epitaxial wafer appearance situation.Be conducive to eliminate Sapphire Substrate simultaneously to the cumulative stress effect of GaN film, reduce
Epitaxial wafer warpage improves product yield.
Detailed description of the invention
The drawings described herein are used to provide a further understanding of the present application, constitutes part of this application, this Shen
Illustrative embodiments and their description please are not constituted an undue limitation on the present application for explaining the application.In the accompanying drawings:
Fig. 1 is the flow chart that the LED epitaxial growth method of growth quality is improved in the embodiment of the present invention 1.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description.It should be noted that described embodiment only actually is a part of the embodiment of the present invention, rather than whole realities
Example is applied, and is actually merely illustrative, never as to the present invention and its application or any restrictions used.The guarantor of the application
Protect range as defined by the appended claims.
Embodiment 1:
Specific embodiment shown in Figure 1 for the herein described LED epitaxial growth method for improving growth quality, the party
Method includes:
Step 101, processing surface have the Sapphire Substrate of AlN film, specifically, at 1000 DEG C, reaction cavity pressure dimension
It holds Sapphire Substrate 5 minutes that there is AlN film on the high-temperature process surface under the hydrogen atmosphere of 100mbar.
Step 102 sequentially grows Al in the Sapphire Substrate0.8Ga0.2N layers, growth Al0.5Ga0.5N layers and growth
Al0.2Ga0.8N layers:
The growth Al0.8Ga0.2N layers include: the reaction cavity pressure for controlling 400mbar, and being passed through flow Q1 to reaction chamber is
The NH of 60L/min3, it is passed through the N that flow is 90L/min2, 100sccm TMGa, 230sccm the source TMAl, in growth course with
Each second increases 0.4 DEG C and growth temperature is increased to 900 DEG C from 800 DEG C of gradual changes, in the Grown on Sapphire Substrates thickness D1
For the Al of 8nm0.8Ga0.2N layers；
It keeps reaction cavity pressure and growth temperature constant, controls N2Flow is 150L/min, to the Al0.8Ga0.2N layers into
The annealing of row 8s；
The growth Al0.5Ga0.5N layers include: growth temperature maintain 900 DEG C it is constant, keep reaction cavity pressure and TMGa,
TMAl is passed through that flow is constant, is passed through the NH that flow Q2 is 72L/min to reaction chamber3, be passed through flow be 90L/min N2, described
Al0.8Ga0.2Growth thickness D2 is the Al of 8nm on N layer0.5Ga0.5N layers；
It keeps reaction cavity pressure and growth temperature constant, controls N2Flow is 150L/min, to the Al0.5Ga0.5N layers into
The annealing of row 8s；
The growth Al0.2Ga0.8N layers include: to keep reaction cavity pressure constant, and growth temperature is increased to 1100 from 900 DEG C
DEG C, keeping TMGa, TMAl to be passed through, flow is constant, is passed through the NH that flow Q3 is 60L/min to reaction chamber3, be passed through flow be 90L/
The N of min2, control growth temperature reduces by 0.5 DEG C with each second and reduces from 1100 DEG C of gradual changes to 1000 DEG C, in institute in growth course
State Al0.5Ga0.5Growth thickness D3 is the Al of 8nm on N layer0.2Ga0.8N layers；
It keeps reaction cavity pressure and growth temperature constant, controls N2Flow is 150L/min, to the Al0.2Ga0.8N layers into
The annealing of row 8s.
Step 103 grows the GaN layer that undopes: increasing the temperature to 1000 DEG C, reaction cavity pressure maintains 150mbar, is passed through
Flow is the NH of 30000sccm3, 200sccm TMGa, 100L/min H2, on the low temperature buffer layer 2 μm of continued propagation
The GaN layer that undopes.
The N-type GaN layer of step 104, growth doping Si: keeping reaction cavity pressure in 150mbar, kept for 1000 DEG C of temperature,
It is passed through the NH that flow is 40L/min3, 200sccm TMGa, 50L/min H2And the SiH of 20sccm4, in the GaN that undopes
The N-type GaN layer of 2 μm of continued propagation doping Si on layer, Si doping concentration are 5E+18atoms/cm3。
Step 105, cyclical growth active layer MQW:
Reaction cavity pressure maintains 300mbar, 700 DEG C of low temperature, is passed through the NH of 50000sccm3, 100sccm TEGa, with
And the flow of TMIn, TMIn progressively increase to 1500sccm from 150sccm with increase 45sccm per second, grow 30s's
In0.015Ga0.985N, growth thickness 1nm, In doping concentration is with increase 6.7E+17atoms/cm per second3From 1E+19atoms/
cm3Fade to 3E+19atoms/cm3；
Maintain growth conditions constant, the flow for stablizing TMIn is 1500sccm, grows the In of 100s0.25Ga0.75N, growth are thick
Degree is 2nm, and In doping concentration is 1E+20atoms/cm3；
Temperature is increased to 800 DEG C, pressure maintains 300mbar, is passed through the TEGa of NH3,400sccm of 50000sccm, raw
The GaN layer of long 10nm, In0.015Ga0.985N/In0.25Ga0.75N/GaN periodicity is 10.
Step 106, growing P-type AlGaN layer: 900 DEG C are increased the temperature to, reaction cavity pressure maintains 200mbar, described
The p-type AlGaN layer of continued propagation 20nm on active layer MQW, Al doping concentration are 1E+20atoms/cm3, Mg doping concentration is 5E
+18atoms/cm3。
The p-type GaN layer of step 107, growth doping Mg: increasing the temperature to 930 DEG C, and reaction cavity pressure maintains 200mbar,
The p-type GaN layer for mixing magnesium of continued propagation 100nm in the p-type AlGaN layer, Mg doping concentration are 1E+19atoms/cm3。
Step 108, cooling down: being cooled to 700 DEG C, keeps the temperature 20min, then cooling in furnace.
Embodiment 2:
The LED epitaxial growth method for improving growth quality is present embodiments provided, this method comprises:
Step 201, processing surface have the Sapphire Substrate of AlN film, specifically, at 1200 DEG C, reaction cavity pressure dimension
It holds Sapphire Substrate 10 minutes that there is AlN film on the high-temperature process surface under the hydrogen atmosphere of 150mbar.
Step 202 sequentially grows Al in the Sapphire Substrate0.8Ga0.2N layers, growth Al0.5Ga0.5N layers and growth
Al0.2Ga0.8N layers:
The growth Al0.8Ga0.2N layers include: the reaction cavity pressure for controlling 600mbar, and being passed through flow Q1 to reaction chamber is
The NH of 70L/min3, it is passed through the N that flow is 95L/min2, 110sccm TMGa, 250sccm the source TMAl, in growth course with
Each second increases 0.4 DEG C and growth temperature is increased to 900 DEG C from 800 DEG C of gradual changes, in the Grown on Sapphire Substrates thickness D1
For the Al of 10nm0.8Ga0.2N layers；
It keeps reaction cavity pressure and growth temperature constant, controls N2Flow is 160L/min, to the Al0.8Ga0.2N layers into
The annealing of row 10s；
The growth Al0.5Ga0.5N layers include: growth temperature maintain 900 DEG C it is constant, keep reaction cavity pressure and TMGa,
TMAl is passed through that flow is constant, is passed through the NH that flow Q2 is 84L/min to reaction chamber3, be passed through flow be 95L/min N2, described
Al0.8Ga0.2Growth thickness D2 is the Al of 10nm on N layer0.5Ga0.5N layers；
It keeps reaction cavity pressure and growth temperature constant, controls N2Flow is 160L/min, to the Al0.5Ga0.5N layers into
The annealing of row 10s；
The growth Al0.2Ga0.8N layers include: to keep reaction cavity pressure constant, and growth temperature is increased to 1100 from 900 DEG C
DEG C, keeping TMGa, TMAl to be passed through, flow is constant, is passed through the NH that flow Q3 is 84L/min to reaction chamber3, be passed through flow be 95L/
The N of min2, control growth temperature reduces by 0.5 DEG C with each second and reduces from 1100 DEG C of gradual changes to 1000 DEG C, in institute in growth course
State Al0.5Ga0.5Growth thickness D3 is the Al of 10nm on N layer0.2Ga0.8N layers；
It keeps reaction cavity pressure and growth temperature constant, controls N2Flow is 160L/min, to the Al0.2Ga0.8N layers into
The annealing of row 10s.
Step 203 grows the GaN layer that undopes: increasing the temperature to 1200 DEG C, reaction cavity pressure maintains 300mbar, is passed through
Flow is the NH of 40000sccm3, 400sccm TMGa, 130L/min H2, on the low temperature buffer layer 4 μm of continued propagation
The GaN layer that undopes.
The N-type GaN layer of step 204, growth doping Si: keeping reaction cavity pressure in 300mbar, kept for 1100 DEG C of temperature,
It is passed through the NH that flow is 60L/min3, 300sccm TMGa, 90L/min H2And the SiH of 50sccm4, in the GaN that undopes
The N-type GaN layer of 4 μm of continued propagation doping Si on layer, Si doping concentration are 1E+19atoms/cm3。
Step 205, cyclical growth active layer MQW:
Reaction cavity pressure maintains 400mbar, 750 DEG C of low temperature, is passed through the NH of 60000sccm3, 150sccm TEGa, with
And the flow of TMIn, TMIn progressively increase to 1700sccm from 170sccm with increase 30.6sccm per second, grow 50s's
In0.010Ga0.990N, growth thickness 1.5nm, In doping concentration is with increase 4E+17atoms/cm per second3From 1E+19atoms/
cm3Fade to 3E+19atoms/cm3；
Maintain growth conditions constant, the flow for stablizing TMIn is 1700sccm, grows the In of 150s0.2Ga0.8N, growth are thick
Degree is 2nm, In doping concentration 3E+20atoms/cm3；
Temperature is increased to 850 DEG C, pressure maintains 400mbar, is passed through the TEGa of NH3,500sccm of 60000sccm, raw
The GaN layer of long 10nm, In0.010Ga0.990N/In0.2Ga0.8N/GaN periodicity is 15.
Step 206, growing P-type AlGaN layer: 1000 DEG C are increased the temperature to, reaction cavity pressure maintains 400mbar, in institute
The p-type AlGaN layer of continued propagation 50nm on active layer MQW is stated, Al doping concentration is 3E+20atoms/cm3, Mg doping concentration is
1E+19atoms/cm3。
The p-type GaN layer of step 207, growth doping Mg: increasing the temperature to 950 DEG C, and reaction cavity pressure maintains 600mbar,
The p-type GaN layer for mixing magnesium of continued propagation 300nm in the p-type AlGaN layer, Mg doping concentration are 1E+20atoms/cm3。
Step 208, cooling down: being cooled to 800 DEG C, keeps the temperature 30min, then cooling in furnace.
Embodiment 3
Step 301, processing surface have the Sapphire Substrate of AlN film, specifically, at 1100 DEG C, reaction cavity pressure dimension
It holds Sapphire Substrate 7 minutes that there is AlN film on the high-temperature process surface under the hydrogen atmosphere of 125mbar.
Step 302 sequentially grows Al in the Sapphire Substrate0.8Ga0.2N layers, growth Al0.5Ga0.5N layers and growth
Al0.2Ga0.8N layers:
The growth Al0.8Ga0.2N layers include: the reaction cavity pressure for controlling 500mbar, and being passed through flow Q1 to reaction chamber is
The NH of 65L/min3, it is passed through the N that flow is 92.5L/min2, 105sccm TMGa, 240sccm the source TMAl, in growth course
0.4 DEG C is increased with each second, growth temperature is increased to 900 DEG C from 800 DEG C of gradual changes, in the Grown on Sapphire Substrates thickness
D1 is the Al of 9nm0.8Ga0.2N layers；
It keeps reaction cavity pressure and growth temperature constant, controls N2Flow is 155L/min, to the Al0.8Ga0.2N layers into
The annealing of row 9s；
The growth Al0.5Ga0.5N layers include: growth temperature maintain 900 DEG C it is constant, keep reaction cavity pressure and TMGa,
TMAl is passed through that flow is constant, is passed through the NH that flow Q2 is 78L/min to reaction chamber3, be passed through flow be 92.5L/min N2, institute
State Al0.8Ga0.2Growth thickness D2 is the Al of 9nm on N layer0.5Ga0.5N layers；
It keeps reaction cavity pressure and growth temperature constant, controls N2Flow is 155L/min, to the Al0.5Ga0.5N layers into
The annealing of row 9s；
The growth Al0.2Ga0.8N layers include: to keep reaction cavity pressure constant, and growth temperature is increased to 1100 from 900 DEG C
DEG C, keeping TMGa, TMAl to be passed through, flow is constant, is passed through the NH that flow Q3 is 71.5L/min to reaction chamber3, be passed through flow and be
92.5L/min N2, control growth temperature reduces by 0.5 DEG C with each second and reduces from 1100 DEG C of gradual changes to 1000 in growth course
DEG C, in the Al0.5Ga0.5Growth thickness D3 is the Al of 9nm on N layer0.2Ga0.8N layers；
It keeps reaction cavity pressure and growth temperature constant, controls N2Flow is 155L/min, to the Al0.2Ga0.8N layers into
The annealing of row 9s.
Step 303 grows the GaN layer that undopes: increasing the temperature to 1100 DEG C, reaction cavity pressure maintains 225mbar, is passed through
Flow is the NH of 35000sccm3, 300sccm TMGa, 115L/min H2, on the low temperature buffer layer 3 μm of continued propagation
The GaN layer that undopes.
The N-type GaN layer of step 304, growth doping Si: keeping reaction cavity pressure in 225mbar, kept for 1050 DEG C of temperature,
It is passed through the NH that flow is 50L/min3, 250sccm TMGa, 70L/min H2And the SiH of 35sccm4, in the GaN that undopes
The N-type GaN layer of 3 μm of continued propagation doping Si, Si doping concentration 7E+18atoms/cm on layer3。
Step 305, cyclical growth active layer MQW:
Reaction cavity pressure maintains 350mbar, 725 DEG C of low temperature, is passed through the NH of 55000sccm3, 125sccm TEGa, with
And the flow of TMIn, TMIn progressively increase to 1600sccm from 160sccm with increase 36sccm per second, grow 40s's
In0.1Ga0.9N, growth thickness 1.15nm, In doping concentration is with increase 5E+17atoms/cm per second3From 1E+19atoms/cm3
Fade to 3E+19atoms/cm3；
Maintain growth conditions constant, the flow for stablizing TMIn is 1600sccm, grows the In of 125s0.15Ga0.85N, growth are thick
Degree is 2.1nm, and In doping concentration is 2E+20atoms/cm3；
Temperature is increased to 825 DEG C, pressure maintains 350mbar, is passed through the TEGa of NH3,450sccm of 55000sccm, raw
The GaN layer of long 10nm, In0.1Ga0.9N/In0.15Ga0.85N/GaN periodicity is 13.
Step 306, growing P-type AlGaN layer: 950 DEG C are increased the temperature to, reaction cavity pressure maintains 300mbar, described
The p-type AlGaN layer of continued propagation 35nm on active layer MQW, Al doping concentration are 2E+20atoms/cm3, Mg doping concentration is
7.5E+18atoms/cm3。
The p-type GaN layer of step 307, growth doping Mg: increasing the temperature to 940 DEG C, and reaction cavity pressure maintains 400mbar,
The p-type GaN layer for mixing magnesium of continued propagation 200nm in the p-type AlGaN layer, Mg doping concentration are 5E+19atoms/cm3。
Step 308, cooling down: being cooled to 750 DEG C, keeps the temperature 25min, then cooling in furnace.
Embodiment 4
Step 401, processing surface have the Sapphire Substrate of AlN film, specifically, at 1050 DEG C, reaction cavity pressure dimension
It holds Sapphire Substrate 6 minutes that there is AlN film on the high-temperature process surface under the hydrogen atmosphere of 110mbar.
Step 402 sequentially grows Al in the Sapphire Substrate0.8Ga0.2N layers, growth Al0.5Ga0.5N layers and growth
Al0.2Ga0.8N layers:
The growth Al0.8Ga0.2N layers include: the reaction cavity pressure for controlling 450mbar, and being passed through flow Q1 to reaction chamber is
The NH of 62L/min3, it is passed through the N that flow is 91L/min2, 102sccm TMGa, 235sccm the source TMAl, in growth course with
Each second increases 0.4 DEG C and growth temperature is increased to 900 DEG C from 800 DEG C of gradual changes, in the Grown on Sapphire Substrates thickness D1
For the Al of 8.5nm0.8Ga0.2N layers；
It keeps reaction cavity pressure and growth temperature constant, controls N2Flow is 152L/min, to the Al0.8Ga0.2N layers into
The annealing of row 9s；
The growth Al0.5Ga0.5N layers include: growth temperature maintain 900 DEG C it is constant, keep reaction cavity pressure and TMGa,
TMAl is passed through that flow is constant, is passed through the NH that flow Q2 is 74.4L/min to reaction chamber3, be passed through flow be 91L/min N2, institute
State Al0.8Ga0.2Growth thickness D2 is the Al of 8.5nm on N layer0.5Ga0.5N layers；
It keeps reaction cavity pressure and growth temperature constant, controls N2Flow is 152L/min, to the Al0.5Ga0.5N layers into
The annealing of row 9s；
The growth Al0.2Ga0.8N layers include: to keep reaction cavity pressure constant, and growth temperature is increased to 1100 from 900 DEG C
DEG C, keeping TMGa, TMAl to be passed through, flow is constant, is passed through the NH that flow Q3 is 68L/min to reaction chamber3, be passed through flow be 91L/
The N of min2, control growth temperature reduces by 0.5 DEG C with each second and reduces from 1100 DEG C of gradual changes to 1000 DEG C, in institute in growth course
State Al0.5Ga0.5Growth thickness D3 is the Al of 8.5nm on N layer0.2Ga0.8N layers；
It keeps reaction cavity pressure and growth temperature constant, controls N2Flow is 152L/min, to the Al0.2Ga0.8N layers into
The annealing of row 9s.
Step 403 grows the GaN layer that undopes: increasing the temperature to 1050 DEG C, reaction cavity pressure maintains 180mbar, is passed through
Flow is the NH of 33000sccm3, 250sccm TMGa, 110L/min H2, on the low temperature buffer layer 2.5 μ of continued propagation
The GaN layer that undopes of m.
The N-type GaN layer of step 404, growth doping Si: keeping reaction cavity pressure in 190mbar, kept for 1010 DEG C of temperature,
It is passed through the NH that flow is 45L/min3, 220sccm TMGa, 60L/min H2And the SiH of 25sccm4, in the GaN that undopes
The N-type GaN layer of 2.5 μm of continued propagation doping Si, Si doping concentration 6E+18atoms/cm on layer3。
Step 405, cyclical growth active layer MQW:
Reaction cavity pressure maintains 330mbar, 710 DEG C of low temperature, is passed through the NH of 53000sccm3, 110sccm TEGa, with
And the flow of TMIn, TMIn progressively increase to 1550sccm from 155sccm with increase 39.8sccm per second, grow 35s's
In0.2Ga0.8N, growth thickness 1.2nm, In doping concentration is with increase 5.7E+17atoms/cm per second3From 1E+19atoms/cm3
Fade to 3E+19atoms/cm3；
Maintain growth conditions constant, the flow for stablizing TMIn is 1550sccm, grows the In of 110s0.22Ga0.78N, growth are thick
Degree is 2.15nm, and In doping concentration is 1.5E+20atoms/cm3；
Temperature is increased to 810 DEG C, pressure maintains 330mbar, is passed through the TEGa of NH3,430sccm of 53000sccm, raw
The GaN layer of long 10nm, In0.2Ga0.8N/In0.22Ga0.78N/GaN periodicity is 11.
Step 406, growing P-type AlGaN layer: 930 DEG C are increased the temperature to, reaction cavity pressure maintains 250mbar, described
The p-type AlGaN layer of continued propagation 25nm on active layer MQW, Al doping concentration are 1.5E+20atoms/cm3, Mg doping concentration is
6E+18atoms/cm3。
The p-type GaN layer of step 407, growth doping Mg: increasing the temperature to 910 DEG C, and reaction cavity pressure maintains 300mbar,
The p-type GaN layer for mixing magnesium of continued propagation 150nm in the p-type AlGaN layer, Mg doping concentration are 3E+19atoms/cm3。
Step 408, cooling down: being cooled to 720 DEG C, keeps the temperature 22min, then cooling in furnace.
Comparative experiments:
It is a kind of traditional handicraft LED structure epitaxial growth method, specific steps below are as follows:
1, at 1000-1200 DEG C, reaction cavity pressure, which maintains high-temperature process surface under the hydrogen atmosphere of 100-150mbar, to be had
The Sapphire Substrate of AlN film 5-10 minutes.
2, it is cooled at 550-650 DEG C, reaction cavity pressure maintains 400-600mbar, and being passed through flow is 10000-
20000sccm NH3, 50-100sccm TMGa, 100-130L/min H2, growth thickness is 20- on a sapphire substrate
The low temperature buffer layer GaN of 50nm.
3,1000-1200 DEG C is increased the temperature to, reaction cavity pressure maintains 150-300mbar, and being passed through flow is 30000-
The NH of 40000sccm3, 200sccm-400sccm TMGa, 100L/min-130L/min H2, 2-4 μm of continued propagation do not mix
Miscellaneous GaN；
4, N-type GaN, the Si doping concentration 5E+18-1E+19atoms/cm of continued propagation doping Si3, overall thickness, which controls, to exist
2-4μm。
5, cyclical growth active layer MQW, including step,
Reaction cavity pressure maintains 300-400mbar, 700-750 DEG C of low temperature, is passed through the NH of 50000-60000sccm3、
The flow of the TEGa and TMIn of 100-150sccm, TMIn progressively increase to 1500-1700sccm from 150-170sccm, raw
The In of long 30-50sy1Ga(1-y1)N, growth thickness D6, In doping concentration is from 1E+19atoms/cm3Fade to 3E+19atoms/
cm3；
Maintain growth conditions constant, the flow for stablizing TMIn is 1500-1700sccm, grows 100-150s's
Iny2Ga(1-y2)N, growth thickness D7, In doping concentration 1E+20-3E+20atoms/cm3, the range of D6+D7 is 3-3.5nm,
The range of y1 and y2 is 0.015-0.25, and wherein y1 and y2 are unequal；
Increase temperature to 800-850 DEG C, pressure maintains 300-400mbar, be passed through 50000-60000sccm NH3,
The TEGa of 400-500sccm grows the GaN layer of 10nm, Iny1Ga(1-y1)N/Iny2Ga(1-y2)N/GaN periodicity is 10-15.
6,900-1000 DEG C is increased the temperature to again, and reaction cavity pressure maintains 200-400mbar, continued propagation 20-50nm
P-type AlGaN layer, Al doping concentration 1E+20-3E+20atoms/cm3, Mg doping concentration 5E+18-1E+19atoms/cm3。
7,930-950 DEG C is increased the temperature to again, and reaction cavity pressure maintains 200-600mbar, continued propagation 100-300nm
The p-type GaN layer for mixing magnesium, Mg doping concentration 1E+19-1E+20atoms/cm3。
8, it is finally cooled to 700-800 DEG C, keeps the temperature 20-30min, it is then cooling in furnace.
It grown one group of epitaxial wafer sample W1 using growing method provided by the invention, use the growing method of traditional handicraft
It grown one group of epitaxial wafer sample W2.Epitaxial wafer sample W1 is fabricated to according to standard technology on production line having a size of 254 μ ms
Epitaxial wafer sample W2 is fabricated to according to standard technology on production line having a size of 686 μm of 254 μ m by 686 μm of chip sample C1
Chip sample C2.
Crystallization using the high-resolution X-ray diffractometer (HRXRD) of model D8Discover to GaN epitaxy piece sample
Quality is characterized, and tests chip sample using the semi-integral ball full-automatic wafer point measurement machine of model LEDA-8F P7202
Photoelectric characteristic, as shown in table 1:
The FWHM (halfwidth) and dislocation density of the XRD rocking curve of 1 sample W1W2 of table
It is available such as to draw a conclusion by analytical table 1: compared with sample W2, the threading dislocation density and edge dislocation of sample W1
Density all decreased significantly, and halfwidth is smaller, illustrate that the method for the present invention can effectively improve the crystal quality of epitaxial film.
In addition, the appearance yield to sample W1, W2 counts, the ratio that surface is cheated there are hexagonal defect and concave in W2 sample is
Surface is 0.25% there are the ratio that hexagonal defect and concave are cheated in 0.75%, W1 sample, this illustrates that the method for the present invention can be bright
The aobvious state of appearance for improving epitaxial wafer surface.
The angularity BOW Value Data (um) of epitaxial wafer sample W1, W2 are counted, W1 sample angularity average value is
5.5um, W2 sample angularity average value are 6.5um, and the angularity of the LED epitaxial wafer sample of the method for the present invention production is obviously wanted
Small, this illustrates that the method for the present invention can significantly reduce epitaxial wafer warpage, improves product qualification rate.
LED component photoelectricity is joined in order to illustrate the crystal quality of the GaN epitaxy piece of the method for the present invention and conventional method growth
Sample W1 and sample W2 are fabricated to chip by several influences respectively.Specifically, sample W1 is fabricated to chip, obtain having a size of
The chip sample C1 of 254 686 μm of μ ms；Sample W2 is fabricated to chip, obtains the chip sample having a size of 686 μm of 254 μ m
C2；Luminous power (LOP) is tested at positive 150mA using point measurement machine, leakage current (IR) is tested at reversed -5V, in human body
Antistatic effect (ESD percent of pass) is tested under mode (HBM) 2000V and 4000V, acquires being averaged for all core particles photoelectric parameters
Value, as shown in table 2:
The main photoelectric parameter testing value of table 2 chip sample C1 and C2
Available such as to draw a conclusion by analytical table 2: the chip sample of growing method production provided by the invention shines
Power is high, and electric leakage obviously wants small, and antistatic yield is high.Wherein, the master that luminous power is high, electric leakage is small, antistatic effect is strong
Want the reason is that when the method for the present invention increases epitaxial crystal growth defect blocking and isolation mech isolation test, successively reduce dislocation uplink,
Step up Lattice Matching, reduce dislocation density, reduce defective proportion, improve crystal quality, thus improve LED luminous efficiency,
Improve antistatic effect.
As can be seen from the above embodiments beneficial effect existing for the application is:
The first, pass through the Grown on Sapphire Substrates Al in AlN film0.8Ga0.2N layers, and increased by growth temperature gradual change
Al doping efficiency improves in Calais, reduces the lattice mismatch with substrate.
The second, in Al0.8Ga0.2Al is grown on N layers0.5Ga0.5N layers, growth temperature gradual change increase can promote epitaxial layer atom
Releasing piece internal stress is conducive to that lattice mismatch early period is stopped to generate upwardly extending for defect, reduces dislocation density, improves crystal matter
Amount.
Third, in Al0.5Ga0.5Al is grown on N layers0.2Ga0.8N layers, pass through growth temperature gradual change and the control of ammonia flow
It is uniformly upward that the filling of epitaxial layer atom is presented in system, improves uniformity in piece, and improve Al0.2Ga0.8N layers with the crystalline substance of GaN layer
Lattice matching degree, epitaxial layer of the continued growth containing GaN material, GaN material reach the state of complete relaxation on this basis, to disappear
In addition to lattice mismatch bring stress during LED epitaxial material growth, the window of epitaxial film material stress control is significantly increased
Mouthful, so as to reduce epitaxial wafer warpage, be conducive to improve GaN epitaxy piece qualification rate, and improve LED luminous efficiency and
Antistatic effect.
4th, respectively to Al0.8Ga0.2N layers, Al0.5Ga0.5N layers and Al0.2Ga0.8N layers are made annealing treatment, so that
Al0.8Ga0.2N layers, Al0.5Ga0.5N layers and Al0.2Ga0.8N layers of each layer crystal lattice all obtain new regularly arranged under heat effect, obtain
Surface neatly is obtained, is conducive to next layer of growth, and keep entire epi-layer surface more smooth, surface hexagonal defect and concave hole are more
Few, entire appearance is more preferable.
5th, the blocking and isolation mech isolation test of defect when the method for the present invention increases epitaxial crystal growth improve Lattice Matching,
Dislocation density is reduced, defective proportion is reduced, improves crystal quality, thus improve LED luminous efficiency, improve antistatic effect, and
And improve epitaxial wafer appearance situation.Be conducive to eliminate Sapphire Substrate simultaneously to the cumulative stress effect of GaN film, reduce
Epitaxial wafer warpage improves product yield.
Although some specific embodiments of the invention are described in detail by example, the skill of this field
Art personnel it should be understood that example above merely to being illustrated, the range being not intended to be limiting of the invention.Although referring to before
Stating embodiment, invention is explained in detail, for those skilled in the art, still can be to aforementioned reality
Technical solution documented by example is applied to modify or equivalent replacement of some of the technical features.It is all of the invention
Within spirit and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
The scope of the present invention is defined by the appended claims.
Claims (8)
1. a kind of LED epitaxial growth method for improving growth quality, which is characterized in that comprising steps of
Handle the Sapphire Substrate that surface has AlN film；
Al is sequentially grown in the Sapphire Substrate0.8Ga0.2N layers, growth Al0.5Ga0.5N layers and growth Al0.2Ga0.8N layers,
In,
The growth Al0.8Ga0.2N layers include: the reaction cavity pressure for controlling 400-600mbar, and being passed through flow Q1 to reaction chamber is
The NH of 60-70L/min3, it is passed through the N that flow is 90-95L/min2, 100-110sccm TMGa, 230-250sccm TMAl
Source increases 0.4 DEG C with each second in growth course and growth temperature is increased to 900 DEG C from 800 DEG C of gradual changes, serves as a contrast in the sapphire
Growth thickness D1 is the Al of 8-10nm on bottom0.8Ga0.2N layers；
It keeps reaction cavity pressure and growth temperature constant, controls N2Flow is 150-160L/min, to the Al0.8Ga0.2N layers into
The annealing of row 8-10s；
The growth Al0.5Ga0.5N layers include: that growth temperature maintains 900 DEG C of constant, holding reaction cavity pressure and TMGa, TMAl
It is passed through that flow is constant, is passed through the NH that flow Q2 is 72-84L/min to reaction chamber3, be passed through flow be 90-95L/min N2, institute
State Al0.8Ga0.2Growth thickness D2 is the Al of 8-10nm on N layer0.5Ga0.5N layers, D2=D1, Q2=1.2Q1；
It keeps reaction cavity pressure and growth temperature constant, controls N2Flow is 150-160L/min, to the Al0.5Ga0.5N layers into
The annealing of row 8-10s；
The growth Al0.2Ga0.8N layers include: to keep reaction cavity pressure constant, and growth temperature is increased to 1100 DEG C from 900 DEG C, protects
It holds TMGa, TMAl and is passed through that flow is constant, be passed through the NH that flow Q3 is 60-84L/min to reaction chamber3, be passed through flow be 90-95L/
The N of min2, control growth temperature reduces by 0.5 DEG C with each second and reduces from 1100 DEG C of gradual changes to 1000 DEG C, in institute in growth course
State Al0.5Ga0.5Growth thickness D3 is the Al of 8-10nm on N layer0.2Ga0.8N layers, D3=D2, Q1 < Q3 < Q2；
It keeps reaction cavity pressure and growth temperature constant, controls N2Flow is 150-160L/min, to the Al0.2Ga0.8N layers into
The annealing of row 8-10s；
Grow the GaN layer that undopes；
The N-type GaN layer of growth doping Si；
Cyclical growth active layer MQW；
Growing P-type AlGaN layer；
The p-type GaN layer of growth doping Mg；
And cooling down.
2. the LED epitaxial growth method according to claim 1 for improving growth quality, which is characterized in that in 1000-1200
DEG C, reaction cavity pressure maintains the Sapphire Substrate 5- that there is AlN film on high-temperature process surface under the hydrogen atmosphere of 100-150mbar
10 minutes.
3. the LED epitaxial growth method according to claim 1 for improving growth quality, which is characterized in that the growth is not
Doped gan layer, further to increase the temperature to 1000-1200 DEG C, reaction cavity pressure maintains 150-300mbar, is passed through flow
For the NH of 30000-40000sccm3, 200-400sccm TMGa, 100-130L/min H2, hold on the low temperature buffer layer
The GaN layer that undopes of continuous 2-4 μm of growth.
4. the LED epitaxial growth method according to claim 1 for improving growth quality, which is characterized in that the growth is mixed
The N-type GaN layer of miscellaneous Si, further for holding reaction cavity pressure is kept for 1000-1100 DEG C of temperature, be passed through in 150-300mbar
Flow is the NH of 40-60L/min3, 200-300sccm TMGa, 50-90L/min H2And the SiH of 20-50sccm4, described
The N-type GaN layer of 2-4 μm of continued propagation doping Si, Si doping concentration 5E+18-1E+19atoms/cm in the GaN layer that undopes3。
5. the LED epitaxial growth method according to claim 1 for improving growth quality, which is characterized in that the periodicity
Grow active layer MQW, further for,
Reaction cavity pressure maintains 300-400mbar, 700-750 DEG C of low temperature, is passed through the NH of 50000-60000sccm3、100-
The flow of the TEGa and TMIn of 150sccm, TMIn are progressively increased to increase 25-52sccm per second from 150-170sccm
1500-1700sccm grows the In of 30-50sy1Ga(1-y1)N, growth thickness D4, In doping concentration is with increase 4E+17- per second
7E+17atoms/cm3From 1E+19atoms/cm3Fade to 3E+19atoms/cm3；
Maintain growth conditions constant, the flow for stablizing TMIn is 1500-1700sccm, grows the In of 100-150sy2Ga(1-y2)N,
Growth thickness is D5, In doping concentration 1E+20-3E+20atoms/cm3, the range of D4+D5 is the range of 3-3.5nm, y1 and y2
For 0.015-0.25, wherein y1 and y2 are unequal；
Temperature is increased to 800-850 DEG C, pressure maintains 300-400mbar, is passed through NH3,400- of 50000-60000sccm
The TEGa of 500sccm grows the GaN layer of 10nm, Iny1Ga(1-y1)N/Iny2Ga(1-y2)N/GaN periodicity is 10-15.
6. the LED epitaxial growth method according to claim 1 for improving growth quality, which is characterized in that the growing P-type
AlGaN layer, further to increase the temperature to 900-1000 DEG C, reaction cavity pressure maintains 200-400mbar, described active
The p-type AlGaN layer of continued propagation 20-50nm, Al doping concentration 1E+20-3E+20atoms/cm on layer MQW3, Mg doping concentration
5E+18-1E+19atoms/cm3。
7. the LED epitaxial growth method according to claim 1 for improving growth quality, which is characterized in that the growth is mixed
The p-type GaN layer of miscellaneous Mg, further to increase the temperature to 930-950 DEG C, reaction cavity pressure maintains 200-600mbar, in institute
State the p-type GaN layer for mixing magnesium of continued propagation 100-300nm in p-type AlGaN layer, Mg doping concentration 1E+19-1E+20atoms/
cm3。
8. the LED epitaxial growth method according to claim 1 for improving growth quality, which is characterized in that the cooling is cold
But, further for, be cooled to 700-800 DEG C, keep the temperature 20-30min, it is then cooling in furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811210449.5A CN109300855A (en) | 2018-10-17 | 2018-10-17 | Improve the LED epitaxial growth method of growth quality |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811210449.5A CN109300855A (en) | 2018-10-17 | 2018-10-17 | Improve the LED epitaxial growth method of growth quality |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109300855A true CN109300855A (en) | 2019-02-01 |
Family
ID=65163095
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811210449.5A Pending CN109300855A (en) | 2018-10-17 | 2018-10-17 | Improve the LED epitaxial growth method of growth quality |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109300855A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112349821A (en) * | 2020-10-22 | 2021-02-09 | 武汉大学 | Method for reducing dislocation and stress by using stacking faults, LED epitaxial wafer and application |
| CN113643962A (en) * | 2021-10-19 | 2021-11-12 | 江苏第三代半导体研究院有限公司 | Preparation method of gallium nitride epitaxial layer and gallium nitride epitaxial wafer structure |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103367421A (en) * | 2012-03-26 | 2013-10-23 | 富士通株式会社 | Semiconductor device, nitride semiconductor crystal, method for manufacturing semiconductor device, and method for manufacturing nitride semiconductor crystal |
| CN103715248A (en) * | 2012-09-28 | 2014-04-09 | 富士通株式会社 | Semiconductor device and method for manufacturing a semiconductor device |
| CN103715245A (en) * | 2012-09-28 | 2014-04-09 | 富士通株式会社 | Semiconductor apparatus |
| CN106887485A (en) * | 2017-03-01 | 2017-06-23 | 湘能华磊光电股份有限公司 | A kind of LED epitaxial growing method and light emitting diode |
-
2018
- 2018-10-17 CN CN201811210449.5A patent/CN109300855A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103367421A (en) * | 2012-03-26 | 2013-10-23 | 富士通株式会社 | Semiconductor device, nitride semiconductor crystal, method for manufacturing semiconductor device, and method for manufacturing nitride semiconductor crystal |
| CN103715248A (en) * | 2012-09-28 | 2014-04-09 | 富士通株式会社 | Semiconductor device and method for manufacturing a semiconductor device |
| CN103715245A (en) * | 2012-09-28 | 2014-04-09 | 富士通株式会社 | Semiconductor apparatus |
| CN106887485A (en) * | 2017-03-01 | 2017-06-23 | 湘能华磊光电股份有限公司 | A kind of LED epitaxial growing method and light emitting diode |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112349821A (en) * | 2020-10-22 | 2021-02-09 | 武汉大学 | Method for reducing dislocation and stress by using stacking faults, LED epitaxial wafer and application |
| CN113643962A (en) * | 2021-10-19 | 2021-11-12 | 江苏第三代半导体研究院有限公司 | Preparation method of gallium nitride epitaxial layer and gallium nitride epitaxial wafer structure |
| CN113643962B (en) * | 2021-10-19 | 2021-12-10 | 江苏第三代半导体研究院有限公司 | Preparation method of gallium nitride epitaxial layer and gallium nitride epitaxial wafer structure |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104037287A (en) | LED epitaxial wafer grown on Si substrate and preparation method thereof | |
| CN103337573B (en) | The epitaxial wafer of semiconductor light-emitting-diode and manufacture method thereof | |
| CN109300854A (en) | LED epitaxial wafer growing method | |
| CN106816499B (en) | Preparation method of light-emitting diode epitaxial wafer | |
| CN106711295B (en) | Growth method of GaN-based light emitting diode epitaxial wafer | |
| CN105702817A (en) | Light emitting diode and preparation method of light emitting diode | |
| CN108878609B (en) | The ALN buffer layer and its epitaxial growth method of LED | |
| CN104103721B (en) | P-type LED epitaxial structure, growing method | |
| WO2021062799A1 (en) | Epitaxial structure and preparation method therefor, and led | |
| CN111180564A (en) | High-luminous-efficiency green light LED epitaxial wafer and manufacturing method thereof | |
| CN109300855A (en) | Improve the LED epitaxial growth method of growth quality | |
| CN109378377A (en) | Improve the LED epitaxial growth method of crystal quality | |
| CN105895753B (en) | Improve the epitaxial growth method of LED luminous efficiency | |
| CN106384764A (en) | LED epitaxial structure and growing method thereof | |
| CN116364825A (en) | Composite buffer layer, preparation method thereof, epitaxial wafer and light-emitting diode | |
| CN109004073B (en) | Epitaxial growth method for improving luminous efficiency of GaN-based LED chip | |
| CN108511322B (en) | Method for preparing GaN film on two-dimensional graphite substrate | |
| CN107799631B (en) | High-brightness LED preparation process | |
| CN109888071A (en) | A kind of novel GaN base LED epitaxial layer structure and preparation method thereof | |
| CN106328780A (en) | Method for substrate epitaxial growth of luminous diode based on AlN template | |
| CN107180896B (en) | Epitaxial wafer of light emitting diode and preparation method thereof | |
| CN109378371A (en) | LED epitaxial wafer growing method | |
| CN117410402A (en) | Light-emitting diode epitaxial wafer, preparation method thereof and Micro-LED chip | |
| CN104966767B (en) | A kind of growing method of GaN base light emitting epitaxial wafer | |
| CN109300856A (en) | LED epitaxial growth method suitable for AlN substrate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190201 |