CN109449268A - A kind of LED epitaxial structure and its growing method reducing p-type GaN layer resistivity - Google Patents
A kind of LED epitaxial structure and its growing method reducing p-type GaN layer resistivity Download PDFInfo
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- CN109449268A CN109449268A CN201811289199.9A CN201811289199A CN109449268A CN 109449268 A CN109449268 A CN 109449268A CN 201811289199 A CN201811289199 A CN 201811289199A CN 109449268 A CN109449268 A CN 109449268A
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- 238000000034 method Methods 0.000 title claims abstract description 29
- 230000012010 growth Effects 0.000 claims abstract description 48
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 18
- 239000010980 sapphire Substances 0.000 claims abstract description 18
- 229910002704 AlGaN Inorganic materials 0.000 claims abstract description 13
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical group [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 12
- 125000004433 nitrogen atom Chemical group N* 0.000 claims abstract description 10
- 238000000137 annealing Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 8
- 238000004020 luminiscence type Methods 0.000 claims abstract description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 10
- 230000004888 barrier function Effects 0.000 claims description 4
- 230000002045 lasting effect Effects 0.000 claims description 4
- 238000007781 pre-processing Methods 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 97
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 33
- 239000011777 magnesium Substances 0.000 description 22
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 7
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 description 7
- 239000007789 gas Substances 0.000 description 5
- 239000002019 doping agent Substances 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000013256 coordination polymer Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007773 growth pattern Effects 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/26—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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- 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
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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
- H01L33/04—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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/12—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a stress relaxation structure, e.g. buffer layer
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Abstract
The present invention provides a kind of growing method of LED epitaxial structure, including high-temperature process Sapphire Substrate, growing low temperature buffer gan layer, grows the GaN layer that undopes, the N-type GaN layer of growth doping Si, growth multi-quantum well luminescence layer, growing P-type AlGaN layer, growth P-type GaN layer and annealing cooling step；In growth P-type GaN layer, first in 900 DEG C of NH3, pre-processed under TMGa environment, then in NH3、TMGa、H2、Cp21000 DEG C are gradually heated to by 870 DEG C under Mg environment to be grown；The p-type GaN layer with a thickness of 50~200nm, the molar ratio control of institute's nitrogen atom and gallium atom is 1400:1, and the doping concentration of Mg is 1E19~1E20atoms/cm3.Present invention reduces the resistivity of p-type GaN layer, crystal quality and hole concentration are improved, and then improves the luminous intensity of LED.
Description
Technical field
The present invention relates to LED manufacturing fields, and in particular, to a kind of resistivity that can effectively reduce p-type GaN layer, in turn
The method for improving LED luminous intensity and improving LED epitaxial structure surface smoothness, and the LED being prepared by this method
Epitaxial structure.
Background technique
LED (Light Emitting Diode, light emitting diode) is a kind of solid state lighting electronic component, because it is with body
Product is small, power consumption is low, long service life, advantages of environment protection and the approval by the majority of consumers, wide market.?
In the epitaxial structure of LED, N layers for providing electronics and P layer are used to provide hole, electrons and holes are under the driving of constant current voltage
It meets in active layer and to generate electron hole pair compound, light-emitting function is realized by way of discharging photon.Current domestic and international LED
Although production scale gradually expanding, the product itself problem low there are still luminous efficiency, it is right in the market not to be able to satisfy
In the demand of LED luminance and light efficiency, the application range and energy-saving effect of LED are then influenced.
The reason of causing above-mentioned phenomenon is numerous, this provides a variety of path optimizings to this field researcher；It is wherein traditional
The resistivity of P-type layer (i.e. p-type GaN layer) in LED epitaxial structure is higher, and hole concentration is low, and crystal quality is not high, is to cause
Low one of the reason of LED chip luminous efficiency.
Summary of the invention
In order to overcome the above problem stated in the background, the present invention provides a kind of p-type GaN layer that can effectively reduce
The LED growing method of resistivity and the LED epitaxial structure being prepared by this method, and then reach and improve LED strong light
The purpose of degree.
A kind of growing method for the LED epitaxial structure reducing p-type GaN layer resistivity, successively includes high-temperature process sapphire
Substrate, growing low temperature buffer gan layer grow the GaN layer that undopes, the N-type GaN layer of growth doping Si, growth multiple quantum well light emitting
The step of layer, growing P-type AlGaN layer, growth P-type GaN layer and annealing cooling；Wherein the step of growth P-type GaN layer includes pre-
Treatment process and heating growth course.
Specific step is as follows for above-mentioned growth P-type GaN layer:
A, holding reaction cavity pressure is 500~600mbar, temperature is 850~900 DEG C, and being passed through flow is 80~100L/
The NH of min3, 15~20L/min TMGa pre-processed；
B, keeping reaction cavity pressure is 400~600mbar, is passed through the NH that flow is 50000~70000sccm3, 20~
The H of the TMGa of 100sccm, 100~130L/min2, 1000~3000sccm Cp2Mg is controlled in reaction chamber in growth course
Temperature is gradually heated to 1000 DEG C from 870 DEG C, and the molar ratio control of nitrogen-atoms and gallium atom is 1400:1~1500:1, lasting raw
The p-type GaN layer of long 50~200nm thickness, wherein the doping concentration of Mg is 1E19atoms/cm3~1E20atoms/cm3。
Preferably, it controls reaction chamber temperature and is gradually heated to 1000 DEG C from 870 DEG C with 0.5~1 DEG C of speed per second.
Preferably, the step of high-temperature process Sapphire Substrate are as follows: keep reaction cavity pressure be 100~300mbar,
Temperature is 1000~1100 DEG C, is passed through the H that flow is 100~130L/min2, it is heat-treated Sapphire Substrate 8~10 minutes.
Preferably, the step of annealing cools down are as follows: reaction cavity temperature is down to 650~680 DEG C, keeps the temperature 20~30min,
Close heating and to gas system, LED epitaxial structure furnace cooling obtained.
Preferably, the step of growing low temperature buffer gan layer are as follows:
Keep reaction cavity pressure be 300~600mbar, temperature is 500~600 DEG C, be passed through flow be 10000~
The NH of 20000sccm3, the TMGa of 50~100sccm, 100~130L/min H2, growth thickness is 20 on a sapphire substrate
The low temperature buffer layer GaN of~40nm；
Keep reaction cavity pressure be 300~600mbar, temperature is 1000~1100 DEG C, be passed through flow be 30000~
The NH of 40000sccm3And the H of 100~130L/min2, keep temperature constant, the low temperature buffer layer GaN grown moved back
300~500s of fire processing.
It is preferably, described to grow the step of undoping GaN layer are as follows:
Keep reaction cavity pressure be 300~600mbar, temperature is 1000~1200 DEG C, be passed through flow be 30000~
The NH of 40000sccm3, the TMGa of 200~400sccm, 100~130L/min H2, the continued propagation in low temperature buffer GaN layer
With a thickness of 2~4 μm of the GaN layer that undopes.
Preferably, the step of N-type GaN layer of the growth doping Si are as follows:
Keep reaction cavity pressure be 300~600mbar, temperature is 1000~1200 DEG C, be passed through flow be 30000~
The NH of 60000sccm3, the TMGa of 200~400sccm, 100~130L/min H2, 20~50sccm SiH4, undoping
Continued propagation is in GaN layer with a thickness of the N-type GaN layer of 3~4 μm of doping Si, and wherein the doping concentration of Si is 5E19atoms/cm3
~1E20atoms/cm3；
It keeps the pressure and temperature in reaction chamber constant, is passed through the NH that flow is 30000~60000sccm3, 200~
The H of the TMGa of 400sccm, 100~130L/min2, 2~10sccm SiH4, continued growth with a thickness of 200~400nm doping
The N-type GaN layer of Si, wherein the doping concentration 5E18atoms/cm of Si3~1E19atoms/cm3；
It keeps the pressure and temperature in reaction chamber constant, is passed through the NH that flow is 30000~60000sccm3, 200~
The H of the TMGa of 400sccm, 100~130L/min2, 1~2sccm SiH4, continued growth with a thickness of 200~400nm doping
The N-type GaN layer of Si, wherein the doping concentration 5E17atoms/cm of Si3~1E18atoms/cm3。
Preferably, the step of growth multi-quantum well luminescence layer are as follows:
Keep reaction cavity pressure be 300~400mbar, temperature is 700~750 DEG C, be passed through flow be 50000~
The NH of 70000sccm3, the TMGa of 20~40sccm, the TMIn of 1500~2000sccm, 100~130L/min N2, lasting raw
The In of the long doping In with a thickness of 2.5~3.5nmXGa(1-X)N well layer, wherein X=0.20~0.25, emission wavelength is 450~
455nm；
Keep reaction cavity pressure be 300~400mbar, temperature is 750~850 DEG C, be passed through flow be 50000~
The NH of 70000sccm3, the TMGa of 20~100sccm, 100~130L/min N2, continued propagation with a thickness of 8~15nm GaN
Barrier layer；
Periodical alternating growth InXGa(1-X)N well layer and GaN build layer, and total periodicity is 7~15.
Preferably, the step of growing P-type AlGaN layer are as follows:
Keep reaction cavity pressure be 200~400mbar, temperature is 900~950 DEG C, be passed through flow be 50000~
The NH of 70000sccm3, the TMGa of 30~60sccm, 100~130L/min H2, 100~130sccm TMAl, 1000~
The Cp of 1300sccm2Mg, continued propagation is with a thickness of the p-type AlGaN layer of 50~100nm, the wherein doping concentration of Al
1E20atoms/cm3~3E20atoms/cm3, the doping concentration of Mg is 1E19atoms/cm3~1E20atoms/cm3。
The present invention also provides a kind of LED epitaxial structures for reducing p-type GaN layer resistivity, including are set in sequence from the bottom to top
Sapphire Substrate, low temperature buffer GaN layer, the GaN layer that undopes, adulterate Si N-type GaN layer, multi-quantum well luminescence layer, p-type
AlGaN layer and p-type GaN layer；The p-type GaN layer was grown by first 900 DEG C of pretreatments and rear 870~1000 DEG C of heating
Journey is prepared.
Preferably, the p-type GaN layer with a thickness of 50~200nm, in p-type GaN layer, nitrogen-atoms rubs with gallium atom
, than being 1400:1~1500:1, the doping concentration of Mg is 1E19atoms/cm for you3~1E20atoms/cm3。
The flux unit sccm being related in the present invention is that standard milliliters are per minute.
Technical solution provided by the invention has the following beneficial effects:
1, the present invention is conducive to excite nitrogen-atoms and gallium former by being pre-processed before the p-type GaN layer that Mg is mixed in growth
The activity of son simultaneously makes nitrogen-atoms and the distribution of gallium atom more uniform, while reducing nitrogen vacancy and improving NH3Injection efficiency,
The compensation for inhibiting acceptor (magnesium elements), greatly improves the activation rate of acceptor, to reduce P layers of resistivity, improve P-type layer
Hole concentration achievees the purpose that the luminous efficiency for improving LED.
2, the present invention advantageously reduces material by introducing temperature change mechanism in the growth course for the p-type GaN layer for mixing Mg
Expect internal flaw, and then improves the activation rate of incorporation Mg and the electric conductivity of P-type layer, and by avoiding under high temperature in P-type layer
Mg is spread to active layer, reduces the generation of non-radiative recombination center, at the same can also reduce during growth P-type GaN layer because
InGaN caused by temperature is excessively high is decomposed and segregation is injured caused by Quantum well active district, and makes the distribution of rich In quantum dot be in
Small and more situation, and then promote the luminous efficiency of Quantum Well.
3, the present invention is realized by the molar ratio of control nitrogen-atoms and gallium atom to nitrogen-atoms and gallium atom two-dimensional growth mistake
The control of journey, so that epi-layer surface be made to become smooth.
4, for the present invention when growing N-type GaN layer, the change of gradient that Si doping is arranged to gradually decrease from the bottom to top is dense
Degree, can effectively reduce dislocation defects present in epitaxial process, and defect is blocked to upwardly extend, and improve epitaxial crystal matter
Amount.
Specific embodiment
Below in conjunction with the embodiment in the present invention, technical solution in the embodiment of the present invention is carried out clearly and completely
Description, it is clear that the described embodiments are merely a part of the embodiments of the present invention, instead of all the embodiments.Based on this hair
Embodiment in bright, all other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, shall fall within the protection scope of the present invention.
Comparative example 1
High brightness GaN-based LED epitaxial wafer is grown in the present embodiment with MOCVD, using high-purity H2Or high-purity N2Or it is high-purity
H2And high-purity N2Mixed gas as carrier gas, high-purity N H3As the source N, trimethyl gallium (TMGa) is used as gallium source, trimethyl indium
(TMIn) indium source, silane (SiH are used as4) it is used as N type dopant, trimethyl aluminium (TMAl) is used as silicon source, two luxuriant magnesium (CP2Mg) make
For P-type dopant, substrate is (0001) surface sapphire.Specific growth pattern is as follows:
1, Sapphire Substrate is handled
Holding reaction cavity pressure is 200mbar, temperature is 1100 DEG C, is passed through the H that flow is 100L/min2, heat treatment
Sapphire Substrate 10 minutes.
2, growing low temperature buffer layer
2.1 holding reaction cavity pressures are 500mbar, temperature is 500 DEG C, are passed through the NH that flow is 15000sccm3、
The H of TMGa, 100L/min of 100sccm2, growth thickness is the low temperature buffer layer GaN of 30nm on a sapphire substrate；
2.2 holding reaction cavity pressures are 500mbar, temperature is 1100 DEG C, are passed through the NH that flow is 35000sccm3With
And the H of 100L/min2, keep temperature constant, annealing 500s carried out to the low temperature buffer layer GaN grown.
3, the GaN layer that undopes is grown
Holding reaction cavity pressure is 500mbar, temperature is 1100 DEG C, is passed through the NH that flow is 35000sccm3、
The H of TMGa, 100L/min of 300sccm2, continued propagation is in low temperature buffer GaN layer with a thickness of 3 μm of the GaN layer that undopes.
4, the N-type GaN layer of growth doping Si
4.1 holding reaction cavity pressures are 500mbar, temperature is 1100 DEG C, are passed through the NH that flow is 50000sccm3、
The H of TMGa, 100L/min of 300sccm2, 40sccm SiH4, in the doping of continued propagation in GaN layer with a thickness of 4 μm that undopes
The N-type GaN layer of Si, wherein the doping concentration of Si is 5E19atoms/cm3~1E20atoms/cm3；
4.2 keep the pressure and temperature in reaction chamber constant, are passed through the NH that flow is 50000sccm3, 300sccm
The H of TMGa, 100L/min2, 4sccm SiH4, continued growth is with a thickness of the N-type GaN layer of the doping Si of 400nm, and wherein Si mixes
Miscellaneous concentration 5E18atoms/cm3~1E19atoms/cm3；
4.3 keep the pressure and temperature in reaction chamber constant, are passed through the NH that flow is 50000sccm3, 300sccm
The H of TMGa, 100L/min2, 1sccm SiH4, continued growth is with a thickness of the N-type GaN layer of the doping Si of 400nm, and wherein Si mixes
Miscellaneous concentration 5E17atoms/cm3~1E18atoms/cm3。
5, multi-quantum well luminescence layer is grown
5.1 holding reaction cavity pressures are 400mbar, temperature is 750 DEG C, are passed through the NH that flow is 60000sccm3、
The N of TMIn, 100L/min of TMGa, 1800sccm of 40sccm2, continued propagation with a thickness of 3nm doping In InXGa(1-X)N
Well layer, wherein X=0.20~0.25, emission wavelength are 450~455nm；
5.2 holding reaction cavity pressures are 400mbar, temperature is 750 DEG C, are passed through the NH that flow is 60000sccm3、
The N of TMGa, 100L/min of 50sccm2, continued propagation with a thickness of 12nm GaN barrier layer；
5.3 periodical alternating growth InXGa(1-X)N well layer and GaN build layer, and total periodicity is 15.
6, growing P-type AlGaN layer
Holding reaction cavity pressure is 400mbar, temperature is 950 DEG C, is passed through the NH that flow is 60000sccm3、60sccm
TMGa, 100L/min H2, 100sccm TMAl, 1200sccm Cp2Mg, continued propagation with a thickness of 100nm p-type
AlGaN layer, wherein the doping concentration 1E20atoms/cm of Al3~3E20atoms/cm3, the doping concentration of Mg is 1E19atoms/
cm3~1E20atoms/cm3。
7, growth P-type GaN layer
Holding reaction cavity pressure is 550mbar, temperature is 1000 DEG C, is passed through the NH that flow is 60000sccm3、
The H of TMGa, 100L/min of 50sccm2, 2000sccm Cp2The p-type GaN layer of Mg, continued propagation 150nm, the wherein doping of Mg
Concentration is 1E19atoms/cm3~1E20atoms/cm3。
8, annealing cooling
Reaction cavity temperature is down to 650~680 DEG C, keeps the temperature 30min, closes heating and to gas system, LED extension obtained
Sample 1 is obtained after structure furnace cooling.
Embodiment 1 (uses growing method of the invention)
High brightness GaN-based LED epitaxial wafer is grown in the present embodiment with MOCVD, using high-purity H2Or high-purity N2Or it is high-purity
H2And high-purity N2Mixed gas as carrier gas, high-purity N H3As the source N, trimethyl gallium (TMGa) is used as gallium source, trimethyl indium
(TMIn) indium source, silane (SiH are used as4) it is used as N type dopant, trimethyl aluminium (TMAl) is used as silicon source, two luxuriant magnesium (CP2Mg) make
For P-type dopant, substrate is (0001) surface sapphire.Specific growth pattern is as follows:
1, Sapphire Substrate is handled
Holding reaction cavity pressure is 200mbar, temperature is 1100 DEG C, is passed through the H that flow is 100L/min2, heat treatment
Sapphire Substrate 10 minutes.
2, growing low temperature buffer layer
2.1 holding reaction cavity pressures are 500mbar, temperature is 500 DEG C, are passed through the NH that flow is 15000sccm3、
The H of TMGa, 100L/min of 100sccm2, growth thickness is the low temperature buffer layer GaN of 30nm on a sapphire substrate；
2.2 holding reaction cavity pressures are 500mbar, temperature is 1100 DEG C, are passed through the NH that flow is 35000sccm3With
And the H of 100L/min2, keep temperature constant, annealing 500s carried out to the low temperature buffer layer GaN grown.
3, the GaN layer that undopes is grown
Holding reaction cavity pressure is 500mbar, temperature is 1100 DEG C, is passed through the NH that flow is 35000sccm3、
The H of TMGa, 100L/min of 300sccm2, continued propagation is in low temperature buffer GaN layer with a thickness of 3 μm of the GaN layer that undopes.
4, the N-type GaN layer of growth doping Si
4.1 holding reaction cavity pressures are 500mbar, temperature is 1100 DEG C, are passed through the NH that flow is 50000sccm3、
The H of TMGa, 100L/min of 300sccm2, 40sccm SiH4, in the doping of continued propagation in GaN layer with a thickness of 4 μm that undopes
The N-type GaN layer of Si, wherein the doping concentration of Si is 5E19atoms/cm3~1E20atoms/cm3；
4.2 keep the pressure and temperature in reaction chamber constant, are passed through the NH that flow is 50000sccm3, 300sccm
The H of TMGa, 100L/min2, 4sccm SiH4, continued growth is with a thickness of the N-type GaN layer of the doping Si of 400nm, and wherein Si mixes
Miscellaneous concentration 5E18atoms/cm3~1E19atoms/cm3；
4.3 keep the pressure and temperature in reaction chamber constant, are passed through the NH that flow is 50000sccm3, 300sccm
The H of TMGa, 100L/min2, 1sccm SiH4, continued growth is with a thickness of the N-type GaN layer of the doping Si of 400nm, and wherein Si mixes
Miscellaneous concentration 5E17atoms/cm3~1E18atoms/cm3。
5, multi-quantum well luminescence layer is grown
5.1 holding reaction cavity pressures are 400mbar, temperature is 750 DEG C, are passed through the NH that flow is 60000sccm3、
The N of TMIn, 100L/min of TMGa, 1800sccm of 40sccm2, continued propagation with a thickness of 3nm doping In InXGa(1-X)N
Well layer, wherein X=0.20~0.25, emission wavelength are 450~455nm；
5.2 holding reaction cavity pressures are 400mbar, temperature is 750 DEG C, are passed through the NH that flow is 60000sccm3、
The N of TMGa, 100L/min of 50sccm2, continued propagation with a thickness of 12nm GaN barrier layer；
5.3 periodical alternating growth InXGa(1-X)N well layer and GaN build layer, and total periodicity is 15.
6, growing P-type AlGaN layer
Holding reaction cavity pressure is 400mbar, temperature is 950 DEG C, is passed through the NH that flow is 60000sccm3、60sccm
TMGa, 100L/min H2, 100sccm TMAl, 1200sccm Cp2Mg, continued propagation with a thickness of 100nm p-type
AlGaN layer, wherein the doping concentration 1E20atoms/cm of Al3~3E20atoms/cm3, the doping concentration of Mg is 1E19atoms/
cm3~1E20atoms/cm3。
7, growth P-type GaN layer
7.1 holding reaction cavity pressures are 550mbar, temperature is 900 DEG C, are passed through the NH that flow is 100L/min3、20L/
The TMGa of min carries out the pretreatment of 15s；
7.2 keep reaction cavity pressure for 550mbar, are passed through the NH that flow is 60000sccm3, 50sccm TMGa,
The H of 100L/min2, 2000sccm Cp2Mg controls the temperature in reaction chamber in growth course from 870 DEG C with 1 DEG C of speed per second
Degree is gradually heated to 1000 DEG C, and the molar ratio control of nitrogen-atoms and gallium atom is 1400:1, the p-type of continued propagation 150nm thickness
GaN layer, wherein the doping concentration of Mg is 1E19atoms/cm3~1E20atoms/cm3。
8, annealing cooling
Reaction cavity temperature is down to 650~680 DEG C, keeps the temperature 30min, closes heating and to gas system, LED extension obtained
Sample 2 is obtained after structure furnace cooling.
Under identical preceding process conditions, sample 1 and sample 2 are respectively plated to the Cr/Pt/ of the ITO layer of 150nm, 1500nm
The SiO of Au electrode and 100nm2Then two samples are ground respectively at identical conditions and are cut into 635 μ by protective layer
M*635 μm (25mil*25mil) of chip particle, is then tested for the property.100 samples are respectively selected at same position
Crystal grain is packaged into white light LEDs under identical packaging technology.
Using the photoelectric properties of integrating sphere test sample 1 and sample 2 under conditions of driving current 350mA, the data obtained
(average value of 100 sample crystal grain) is referring to following table.
Table 1
As shown in Table 1, improved LED product, brightness have been increased to 615.32mw from 550.05mw, forward voltage from
3.16V is reduced to 3.00V, and backward voltage is increased to 39.90V from 35.33V, and antistatic yield is increased to from 90.75%
92.07%.It therefore follows that draw a conclusion:
Growing method provided by the invention is substantially better than traditional growing method, and the LED being prepared through the invention is produced
Product are improved on light efficiency and antistatic yield, while forward voltage declines, and illustrates that LED component is more energy saving, and reversed electricity
Pressure increases, and illustrates the longer life expectancy of LED component.Above-mentioned experimental data proves that the technical solution in the present invention is improving LED really
There is feasibility in terms of epitaxial crystal quality.
The above description is only a preferred embodiment of the present invention, is not intended to limit scope of patent protection of the invention, for
For those skilled in the art, the invention may be variously modified and varied.Within the spirit and principles in the present invention, all
Using any improvement or equivalent replacement made by present specification, it is directly or indirectly used in other relevant technology necks
Domain should all be included within the scope of the present invention.
Claims (10)
1. a kind of growing method for the LED epitaxial structure for reducing p-type GaN layer resistivity, which is characterized in that successively include at high temperature
Reason Sapphire Substrate, growing low temperature buffer gan layer grow the GaN layer that undopes, the N-type GaN layer of growth doping Si, growth volume
The step of sub- trap luminescent layer, growing P-type AlGaN layer, growth P-type GaN layer and annealing cooling；The wherein step of growth P-type GaN layer
It suddenly include preprocessing process and heating growth course.
2. the growing method of LED epitaxial structure according to claim 1, which is characterized in that the specific step of growth P-type GaN layer
It is rapid as follows:
A, holding reaction cavity pressure is 500~600mbar, temperature is 850~900 DEG C, and being passed through flow is 80~100L/min
NH3, 15~20L/min TMGa pre-processed；
B, keeping reaction cavity pressure is 400~600mbar, is passed through the NH that flow is 50000~70000sccm3, 20~
The H of the TMGa of 100sccm, 100~130L/min2, 1000~3000sccm Cp2Mg is controlled in reaction chamber in growth course
Temperature is gradually heated to 1000 DEG C from 870 DEG C, and the molar ratio control of nitrogen-atoms and gallium atom is 1400:1~1500:1, lasting raw
The p-type GaN layer of long 50~200nm thickness, wherein the doping concentration of Mg is 1E19atoms/cm3~1E20atoms/cm3。
3. the growing method of LED epitaxial structure according to claim 2, which is characterized in that
The step of high-temperature process Sapphire Substrate are as follows: keep reaction cavity pressure be 100~300mbar, temperature 1000
~1100 DEG C, it is passed through the H that flow is 100~130L/min2, it is heat-treated Sapphire Substrate 8~10 minutes；
The step of annealing cools down are as follows: reaction cavity temperature is down to 650~680 DEG C, keeps the temperature 20~30min, close heating and
Give gas system, LED epitaxial structure furnace cooling obtained.
4. the growing method of LED epitaxial structure according to claim 2, which is characterized in that the growing low temperature buffer gan layer
The step of are as follows:
Keep reaction cavity pressure be 300~600mbar, temperature is 500~600 DEG C, be passed through flow be 10000~
The NH of 20000sccm3, the TMGa of 50~100sccm, 100~130L/min H2, growth thickness is 20 on a sapphire substrate
The low temperature buffer layer GaN of~40nm；
Keep reaction cavity pressure be 300~600mbar, temperature is 1000~1100 DEG C, be passed through flow be 30000~
The NH of 40000sccm3And the H of 100~130L/min2, keep temperature constant, the low temperature buffer layer GaN grown moved back
300~500s of fire processing.
5. the growing method of LED epitaxial structure according to claim 2, which is characterized in that described to grow the GaN layer that undopes
Step are as follows:
Keep reaction cavity pressure be 300~600mbar, temperature is 1000~1200 DEG C, be passed through flow be 30000~
The NH of 40000sccm3, the TMGa of 200~400sccm, 100~130L/min H2, the continued propagation in low temperature buffer GaN layer
With a thickness of 2~4 μm of the GaN layer that undopes.
6. the growing method of LED epitaxial structure according to claim 2, which is characterized in that the N-type of the growth doping Si
The step of GaN layer are as follows:
Keep reaction cavity pressure be 300~600mbar, temperature is 1000~1200 DEG C, be passed through flow be 30000~
The NH of 60000sccm3, the TMGa of 200~400sccm, 100~130L/min H2, 20~50sccm SiH4, undoping
Continued propagation is in GaN layer with a thickness of the N-type GaN layer of 3~4 μm of doping Si, and wherein the doping concentration of Si is 5E19atoms/cm3
~1E20atoms/cm3；
It keeps the pressure and temperature in reaction chamber constant, is passed through the NH that flow is 30000~60000sccm3, 200~400sccm
TMGa, 100~130L/min H2, 2~10sccm SiH4, continued growth with a thickness of 200~400nm doping Si N-type
GaN layer, wherein the doping concentration 5E18atoms/cm of Si3~1E19atoms/cm3；
It keeps the pressure and temperature in reaction chamber constant, is passed through the NH that flow is 30000~60000sccm3, 200~400sccm
TMGa, 100~130L/min H2, 1~2sccm SiH4, continued growth with a thickness of 200~400nm doping Si N-type
GaN layer, wherein the doping concentration 5E17atoms/cm of Si3~1E18atoms/cm3。
7. the growing method of LED epitaxial structure according to claim 2, which is characterized in that the growth multiple quantum well light emitting
The step of layer are as follows:
Keep reaction cavity pressure be 300~400mbar, temperature is 700~750 DEG C, be passed through flow be 50000~
The NH of 70000sccm3, the TMGa of 20~40sccm, the TMIn of 1500~2000sccm, 100~130L/min N2, lasting raw
The In of the long doping In with a thickness of 2.5~3.5nmXGa(1-X)N well layer, wherein X=0.20~0.25, emission wavelength is 450~
455nm；
Keep reaction cavity pressure be 300~400mbar, temperature is 750~850 DEG C, be passed through flow be 50000~
The NH of 70000sccm3, the TMGa of 20~100sccm, 100~130L/min N2, continued propagation with a thickness of 8~15nm GaN
Barrier layer；
Periodical alternating growth InXGa(1-X)N well layer and GaN build layer, and total periodicity is 7~15.
8. the growing method of LED epitaxial structure according to claim 2, which is characterized in that the growing P-type AlGaN layer
Step are as follows:
Keep reaction cavity pressure be 200~400mbar, temperature is 900~950 DEG C, be passed through flow be 50000~
The NH of 70000sccm3, the TMGa of 30~60sccm, 100~130L/min H2, 100~130sccm TMAl, 1000~
The Cp of 1300sccm2Mg, continued propagation is with a thickness of the p-type AlGaN layer of 50~100nm, the wherein doping concentration of Al
1E20atoms/cm3~3E20atoms/cm3, the doping concentration of Mg is 1E19atoms/cm3~1E20atoms/cm3。
9. outside a kind of LED for the reduction p-type GaN layer resistivity being prepared such as any one of claim 2~8 the method
Prolong structure, which is characterized in that including be set in sequence from the bottom to top Sapphire Substrate, low temperature buffer GaN layer, the GaN layer that undopes,
Adulterate N-type GaN layer, multi-quantum well luminescence layer, p-type AlGaN layer and the p-type GaN layer of Si；The p-type GaN layer passes through first 900
DEG C pretreatment and latter 870~1000 DEG C of heating growth course are prepared.
10. LED epitaxial structure according to claim 9, which is characterized in that the p-type GaN layer with a thickness of 50~200nm,
In p-type GaN layer, the molar ratio of nitrogen-atoms and gallium atom is 1400:1~1500:1, and the doping concentration of Mg is 1E19atoms/
cm3~1E20atoms/cm3。
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