CN105261683B - A kind of epitaxial growth method of raising LED epitaxial crystal quality - Google Patents
A kind of epitaxial growth method of raising LED epitaxial crystal quality Download PDFInfo
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- 230000012010 growth Effects 0.000 title claims abstract description 86
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000013078 crystal Substances 0.000 title claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 77
- 230000026267 regulation of growth Effects 0.000 claims abstract description 28
- 239000000758 substrate Substances 0.000 claims abstract description 16
- 229910002704 AlGaN Inorganic materials 0.000 claims abstract description 15
- 239000002019 doping agent Substances 0.000 claims abstract description 15
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 15
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 230000008859 change Effects 0.000 claims description 36
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 13
- 230000002045 lasting effect Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 4
- 230000007704 transition Effects 0.000 abstract description 2
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 54
- 239000011777 magnesium Substances 0.000 description 32
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 229910052594 sapphire Inorganic materials 0.000 description 5
- 239000010980 sapphire Substances 0.000 description 5
- 230000008878 coupling Effects 0.000 description 4
- 238000010168 coupling process Methods 0.000 description 4
- 238000005859 coupling reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 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
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
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- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
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- 229910000077 silane Inorganic materials 0.000 description 1
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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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- H—ELECTRICITY
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- 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
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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
- H01L33/0095—Post-treatment of devices, e.g. annealing, recrystallisation or short-circuit elimination
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- H—ELECTRICITY
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Abstract
This application discloses a kind of epitaxial growth method of raising LED epitaxial crystal quality, including step：AlN substrates are put into, the reaction 200mbar of cavity pressure 100 is kept, NH3,100 130L/min H2 that flow is 10000 20000sccm is passed through, reaction chamber temperature is increased to 900 1000 DEG C；The U-shaped gradient GaN of growth regulation one layer；The U-shaped gradient GaN of growth regulation two layer；Grow the N-type GaN layer for the Si that undopes；The doping of growth regulation one Si N-type GaN layer；The doping of growth regulation two Si N-type GaN layer；Grow luminescent layer；Growth doping Mg, Al p-type AlGaN layer；Grow high temperature dopant Mg p-type GaN layer；650 680 DEG C are finally cooled to, 20 30min is incubated, is then switched off heating system, closes and give gas system, furnace cooling.Present invention employs the growing method of AlN substrate high temperature gradient GaN, this method effectively solve AlN to the transition of GaN material, the GaN crystal quality of growth gets a promotion.
Description
Technical field
It is to be related to a kind of extension of LED epitaxial crystals quality specifically the present invention relates to technical field of semiconductor illumination
Growing method.
Background technology
Country's LED industry is just in vigorous growth at present, and LED product has the advantages that energy-saving and environmental protection, long lifespan；
LED extensions producer largely uses sapphire PSS substrate growth extensions at present, and PSS grows extension still in extension
There is the defect of very big density in layer, underlay substrate AlN templates of new generation have been developed, manufacture craft is original
One layer of AlN material is deposited by sputtering principle on sapphire PSS substrates, AlN materials replace original low temperature GaN so that extension
Growth is simplified, it is only necessary to high temperature GaN growth is directly realized in AlN template growths, it is not necessary to carry out original low temperature GaN and
Low temperature GaN is etched into island, then high growth temperature GaN steps；The LED epitaxial layer crystal mass of AlN template growths is carried
Rise, luminescent layer crystal mass gets a promotion, have the advantage that the LED light of AlN template growths epitaxial layer making is imitated, brightness
High, voltage is low, and backward voltage is high, antistatic effect is further strengthened, on the whole AlN templates with causing LED product product
A new step in matter.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of good epitaxial growth method so that AlN templates can be real
Existing mass production, and play advantage of the AlN templates in LED making.
In order to solve the above technical problems, the invention provides a kind of epitaxial growth method of raising LED epitaxial crystal quality,
Including step：
AlN substrates are put into, reaction cavity pressure 100-200mbar is kept, the NH that flow is 10000-20000sccm is passed through3、
100-130L/min H2, reaction chamber temperature is increased to 900-1000 DEG C；
The U-shaped gradient GaN of growth regulation one layer：It is passed through the NH that flow is 30000-40000sccm3, 100-130L/min H2,
Reaction chamber temperature is to 900-1000 DEG C of gradual change to 1000-1100 DEG C, and simultaneous reactions cavity pressure is from 100-150mbar gradual changes to 600-
700mbar, while TMGa is passed through from 50-70sccm gradual changes to 200-250sccm, pressure, temperature, TMGa gradual change simultaneously, and gradually
The time of change is 120-150s；
The U-shaped gradient GaN of growth regulation two layer：It is passed through the NH that flow is 30000-40000sccm3, 100-130L/min H2,
Reaction chamber temperature is to 1100-1200 DEG C of gradual change to 1200-1350 DEG C, and simultaneous reactions cavity pressure maintains stable 600-700mbar, together
When be passed through TMGa from 200-250sccm gradual changes to 300-400sccm, temperature, TMGa simultaneously gradual change, and gradual change time be 900-
1000s；
Grow the N-type GaN layer for the Si that undopes；
The doping of growth regulation one Si N-type GaN layer；
The doping of growth regulation two Si N-type GaN layer；
Grow luminescent layer；
Growth doping Mg, Al p-type AlGaN layer；
Grow high temperature dopant Mg p-type GaN layer；
650-680 DEG C is finally cooled to, 20-30min is incubated, is then switched off heating system, closes gas system of giving, it is cold with stove
But.
Preferably, described to fade to as linear gradient, gradual slope is equal to growth conditions difference before and after gradual change divided by gradually
The change time.
Preferably, the growth undopes Si N-type GaN layer, further for,
1200-1400 DEG C is increased the temperature to, reaction cavity pressure 300-600mbar is kept, flow is passed through for 30000-
40000sccm NH3, 200-400sccm TMGa, 100-130L/min H2, 2-4 μm of continued propagation the Si that undopes N-type
GaN layer.
Preferably, the growth regulation one adulterates Si N-type GaN layer, further for,
Growth doping Si N-type GaN layer：Reaction cavity pressure 300-600mbar, 1200-1400 DEG C of temperature are kept, stream is passed through
Measure the NH for 30000-60000sccm3, 200-400sccm TMGa, 100-130L/min H2, 20-50sccm SiH4, hold
Continuous 3-4 μm first doping Si of growth N-type GaN layer, Si doping concentrations 5 × 1018atoms/cm3-1×1019atoms/cm3。
Preferably, the growth regulation two adulterates Si N-type GaN layer, further for,
Reaction cavity pressure 300-600mbar, 1200-1400 DEG C of temperature are kept, it is 30000-60000sccm's to be passed through flow
NH3, 200-400sccm TMGa, 100-130L/min H2, 2-10sccm SiH4, continued propagation 200-400nm second mixes
Miscellaneous Si N-type GaN layer, Si doping concentrations 5 × 1017atoms/cm3-1×1018atoms/cm3。
Preferably, the growth luminescent layer, further for,
Reaction cavity pressure 300-400mbar, 700-750 DEG C of temperature are kept, it is 50000-70000sccm's to be passed through flow
NH3, 20-40sccm TMGa, 1500-2000sccm TMIn and 100-130L/min N2, growth 2.5-3.5nm doping In
N layers of InxGa (1-x), wherein x is between 0.20-0.25, emission wavelength 450-455nm；Then 750-850 DEG C of temperature is raised,
Keep reaction cavity pressure 300-400mbar, be passed through flow be 50000-70000sccm NH3,20-100sccm TMGa,
100-130L/min N2, grow 8-15nmGaN layers；Then N layers of repeated growth InxGa (1-x), repeated growth GaN layer, replace
InxGa (1-x) N/GaN luminescent layers are grown, controlling cycle number is 7-15.
Preferably, it is described growth doping Mg, Al p-type AlGaN layer, further for,
Reaction cavity pressure 200-400mbar, 900-950 DEG C of temperature are kept, it is 50000-70000sccm's to be passed through flow
NH3, 30-60sccm TMGa, 100-130L/min H2, 100-130sccm TMAl, 1000-1300sccm Cp2Mg, hold
Continuous growth 50-100nm doping Mg, Al p-type AlGaN layer, Al doping concentrations 1 × 1020atoms/cm3-3×1020atoms/
cm3, Mg doping concentrations 1 × 1019atoms/cm3-1×1020atoms/cm3。
Preferably, the p-type GaN layer of the growth high temperature dopant Mg, further for,
Reaction cavity pressure 400-900mbar, 950-1000 DEG C of temperature are kept, it is 50000-70000sccm's to be passed through flow
NH3, 20-100sccm TMGa, 100-130L/min H2, 1000-3000sccm Cp2Mg, continued propagation 50-100nm is high
Temperature doping Mg p-type GaN layer, Mg doping concentrations 1 × 1019atoms/cm3-1×1020atoms/cm3。
Compared with prior art, the epitaxial growth method of raising LED epitaxial crystal quality of the present invention, reached as
Lower effect：
Present invention employs the growing method of AlN substrate high temperature gradient GaN, this method effectively solve AlN to GaN
The transition of material, the GaN crystal quality of growth gets a promotion, and u-shaped GaN (GaN for the SI that undopes), n-type GaN growth
Angularity is improved, and warpage is growth course epitaxial layers BOW values, and benefit is the lifting of wavelength hit rate, the crystal of luminescent layer
Quality improves, and P layers of doping efficiency is improved, and crystal mass is improved, and the mobility lifting in hole, overall advantage is that LED is bright
Degree can increase, and the crystal mass of luminescent layer improves, and wavelength shoots straight, voltage can decline (pGaN hole mobility lifting),
Backward voltage rises (lifting of PN junction crystal mass), the lifting of antistatic effect (lifting of PN junction crystal mass).
Brief description of the drawings
Accompanying drawing described herein is used for providing a further understanding of the present invention, constitutes the part of the present invention, this hair
Bright schematic description and description is used to explain the present invention, does not constitute inappropriate limitation of the present invention.In the accompanying drawings：
Fig. 1 improves the flow chart of the epitaxial growth method of LED epitaxial crystal quality for the present invention；
Fig. 2 LED structures made from the epitaxial growth method of the present invention；
Fig. 3 is the LED structure that prior art epitaxial growth method is obtained.
Embodiment
Some vocabulary have such as been used to censure specific components among specification and claim.Those skilled in the art should
It is understood that hardware manufacturer may call same component with different nouns.This specification and claims are not with name
The difference of title is used as the mode for distinguishing component, but is used as the criterion of differentiation with the difference of component functionally.Such as logical
The "comprising" of piece specification and claim mentioned in is an open language, therefore should be construed to " include but do not limit
In "." substantially " refer in receivable error range, those skilled in the art can solve described in the range of certain error
Technical problem, basically reaches the technique effect.In addition, " coupling " one word is herein comprising any direct and indirect electric property coupling
Means.Therefore, if a first device is coupled to a second device described in text, representing the first device can directly electrical coupling
The second device is connected to, or the second device is electrically coupled to indirectly by other devices or coupling means.Specification
Subsequent descriptions for implement the present invention better embodiment, so it is described description be by illustrate the present invention rule for the purpose of,
It is not limited to the scope of the present invention.Protection scope of the present invention is worked as to be defined depending on the appended claims person of defining.
The present invention uses MOCVD next life long high brightness GaN-based LED.Using high-purity H2 or high-purity N2Or high-purity H2With
High-purity N2Mixed gas be used as carrier gas, high-purity N H3As N sources, metal organic source trimethyl gallium (TMGa) is used as gallium source, front three
Base indium (TMIn) is as indium source, and N type dopant is silane (SiH4), trimethyl aluminium (TMAl) is two as silicon source P-type dopant
Luxuriant magnesium (CP2Mg), substrate is the AlN template substrates in (0001) face, and reaction pressure is between 70mbar to 900mbar.
The present invention is described in further detail below in conjunction with accompanying drawing, but it is not as a limitation of the invention.
Embodiment 1：
With reference to Fig. 1 and Fig. 2, a kind of epitaxial growth method of raising LED epitaxial crystal quality is present embodiments provided, specifically
Step is as follows：
Step 101：AlN substrates 200 are put into, reaction cavity pressure 100mbar is kept, it is 10000sccm's to be passed through flow
NH3, 100L/min H2, reaction chamber temperature is increased to 900 DEG C；
Step 102：The U-shaped gradient GaN of growth regulation one layer 201：It is passed through the NH that flow is 30000sccm3, 100L/min H2,
Reaction chamber temperature is from 900 DEG C of gradual changes to 1000 DEG C, and simultaneous reactions cavity pressure is passed through simultaneously from 100mbar gradual changes to 600mbar
TMGa is from 50sccm gradual changes to 200sccm, and the time of pressure, temperature, TMGa gradual change simultaneously and gradual change is 120s；
Step 103：The U-shaped gradient GaN of growth regulation two layer 202：It is passed through the NH that flow is 30000sccm3, 100L/min H2,
Reaction chamber temperature is from 1100 DEG C of gradual changes to 1200 DEG C, and simultaneous reactions cavity pressure maintains stable 600mbar, at the same be passed through TMGa from
200sccm gradual changes are to 300sccm, temperature, TMGa while the time of gradual change and gradual change is 900s；
Gradual change in step 102 and step 103 refers to uniform gradual change, and gradual slope is equal to the growth conditions before and after gradual change
Difference divided by fade time, i.e., equal to x/b, wherein x is flow or pressure difference value, and b is the time, is linear gradient, gradual change here
Slope is certain.Cavity pressure is for example reacted in the present embodiment in step 102 from 100mbar gradual changes to 600mbar, the time of gradual change is
120s, so gradual slope is 500/120=4.1667mbar/s, the computational methods of the gradual change in other embodiments are therewith
It is identical, repeat no more.
Step 104：Grow the N-type GaN layer 203 for the Si that undopes：1200 DEG C are increased the temperature to, reaction cavity pressure is kept
300mbar, is passed through the NH that flow is 30000sccm3, 200sccm TMGa, 100L/min H2, 2 μm of continued propagation do not mix
Miscellaneous Si N-type GaN layer 203；
Step 105：The doping of growth regulation one Si N-type GaN layer 204：Keep reaction cavity pressure 300mbar, 1200 DEG C of temperature
It is constant, it is passed through the NH that flow is 30000sccm3, 200sccm TMGa, 100L/min H2, 20sccm SiH4, continued propagation
3 μm of first doping Si N-type GaN layer 204, Si doping concentrations 5 × 1018atoms/cm3；
Step 106：The doping of growth regulation two Si N-type GaN layer 205：Keep reaction cavity pressure 300mbar, 1200 DEG C of temperature
It is constant, it is passed through the NH that flow is 30000sccm3, 200sccm TMGa, 100L/min H2, 2sccm SiH4, continued propagation
200nm doping Si N-type GaN layer, Si doping concentrations 5 × 1017atoms/cm3；
Step 107：Grow luminescent layer 206：Reaction cavity pressure 300mbar, 700 DEG C of temperature are kept, being passed through flow is
50000sccm NH3, 20sccm TMGa, 1500sccm TMIn, 100L/min N2, growth 2.5nm doping In InxGa
(1-x) N layers 2061, wherein x=0.20, emission wavelength 450nm；Then 750 DEG C of temperature is raised, reaction cavity pressure is kept
300mbar, is passed through the NH that flow is 50000sccm3, 20sccm TMGa, 100L/min N2, growth 8nmGaN layers 2062；So
Repeated growth InxGa (1-x) N layers 2061, repeated growth GaN layer 2062, alternating growth InxGa (1-x) N/GaN luminescent layers afterwards
206, controlling cycle number is 7；
Step 108：Growth doping Mg, Al p-type AlGaN layer 207：Reaction cavity pressure 200mbar, 900 DEG C of temperature are kept,
It is passed through the NH that flow is 50000sccm3, 30sccm TMGa, 100L/min H2, 100sccm TMAl, 1000sccm
Cp2Mg, continued propagation 50nm doping Mg, Al p-type AlGaN layer 207, Al doping concentrations 1 × 1020atoms/cm3, Mg adulterates dense
Degree 1 × 1019atoms/cm3；
Step 109：Grow high temperature dopant Mg p-type GaN layer 208：Reaction cavity pressure 400mbar, 950 DEG C of temperature are kept,
It is passed through the NH that flow is 50000sccm3, 20sccm TMGa, 100L/min H2, 1000sccm Cp2Mg, continued propagation
50nm high temperature dopants Mg p-type GaN layer 208, Mg doping concentrations 1 × 1019atoms/cm3；
Step 110：650 DEG C are finally cooled to, 20min is incubated, is then switched off heating system, closes and give gas system, with stove
Cooling.
Embodiment 2：
A kind of epitaxial growth method of raising LED epitaxial crystal quality is present embodiments provided, is comprised the following steps that：
Step 201：AlN substrates 200 are put into, reaction cavity pressure 200mbar is kept, it is 20000sccm's to be passed through flow
NH3, 130L/min H2, reaction chamber temperature is increased to 1000 DEG C；
Step 202：The U-shaped gradient GaN of growth regulation one layer 201：It is passed through the NH that flow is 40000sccm3, 130L/min H2,
Reaction chamber temperature is from 1000 DEG C of gradual changes to 1100 DEG C, and simultaneous reactions cavity pressure is passed through simultaneously from 150mbar gradual changes to 700mbar
TMGa is from 70sccm gradual changes to 250sccm, pressure, temperature, TMGa gradual change simultaneously, and the time of gradual change is 150s；
Step 203：The U-shaped gradient GaN of growth regulation two layer 202：It is passed through the NH that flow is 40000sccm3, 130L/min H2,
Reaction chamber temperature is from 1200 DEG C of gradual changes to 1350 DEG C, and simultaneous reactions cavity pressure maintains stable 700mbar, at the same be passed through TMGa from
250sccm gradual changes to the time of 400sccm, temperature, TMGa gradual change simultaneously, and gradual change is 1000s；
Step 204：Grow the N-type GaN layer 203 for the Si that undopes：1400 DEG C are increased the temperature to, reaction cavity pressure is kept
600mbar, is passed through the NH that flow is 40000sccm3, 400sccm TMGa, 130L/min H2, 4 μm of continued propagation do not mix
Miscellaneous Si N-type GaN layer 203；
Step 205：The doping of growth regulation one Si N-type GaN layer 204：Keep reaction cavity pressure 600mbar, 1400 DEG C of temperature
It is constant, it is passed through the NH that flow is 60000sccm3, 400sccm TMGa, 130L/min H2, 50sccm SiH4, continued propagation
4 μm of the first doping Si N-type GaN, Si doping concentration 1 × 1019atoms/cm3；
Step 206：The doping of growth regulation two Si N-type GaN layer 205：Keep reaction cavity pressure 600mbar, 1400 DEG C of temperature
It is constant, it is passed through the NH that flow is 60000sccm3, 400sccm TMGa, 130L/min H2, 10sccm SiH4, continued propagation
The doping of 400nm second Si N-type GaN layer 205, Si doping concentrations 1 × 1018atoms/cm3；
Step 207：Grow luminescent layer 206：Reaction cavity pressure 400mbar, 750 DEG C of temperature are kept, being passed through flow is
70000sccm NH3, 40sccm TMGa, 2000sccm TMIn, 130L/min N2, growth 3.5nm doping In InxGa
(1-x) N layers 2061, wherein x=0.25, emission wavelength 455nm；Then 850 DEG C of temperature is raised, reaction cavity pressure is kept
400mbar is passed through the NH that flow is 70000sccm3, 100sccm TMGa, 130L/min N2, growth 15nmGaN layers 2062；
Then repeated growth InxGa (1-x) N layers 2061, repeated growth GaN layer 2062, alternating growth InxGa (1-x) N/GaN luminescent layers
206, controlling cycle number is 15；
Step 208：Growth doping Mg, Al p-type AlGaN layer 207：Reaction cavity pressure 400mbar, 950 DEG C of temperature are kept,
It is passed through the NH that flow is 70000sccm3, 60sccm TMGa, 130L/min H2, 130sccm TMAl, 1300sccm
Cp2Mg, continued propagation 100nm doping Mg, Al p-type AlGaN layer 207, Al doping concentrations 3 × 1020atoms/cm3, Mg doping
Concentration 1 × 1020atoms/cm3；
Step 209：Grow high temperature dopant Mg p-type GaN layer 208：Reaction cavity pressure 900mbar, 1000 DEG C of temperature are kept,
It is passed through the NH that flow is 70000sccm3, 100sccm TMGa, 130L/min H2, 3000sccm Cp2Mg, continued propagation
100nm high temperature dopants Mg p-type GaN layer 208, Mg doping concentrations 1 × 1020atoms/cm3；
Step 210：680 DEG C are finally cooled to, 30min is incubated, is then switched off heating system, closes and give gas system, with stove
Cooling.
Embodiment 3：
A kind of epitaxial growth method of raising LED epitaxial crystal quality is present embodiments provided, is comprised the following steps that：
Step 301：AlN substrates 200 are put into, reaction cavity pressure 150mbar is kept, it is 15000sccm's to be passed through flow
NH3, 115L/min H2, reaction chamber temperature is increased to 950 DEG C；
Step 302：The U-shaped gradient GaN of growth regulation one layer 201：It is passed through the NH that flow is 35000sccm3, 115L/min H2,
Reaction chamber temperature is from 950 DEG C of gradual changes to 1050 DEG C, and simultaneous reactions cavity pressure is passed through simultaneously from 125mbar gradual changes to 650mbar
TMGa is from 60sccm gradual changes to 225sccm, pressure, temperature, TMGa gradual change simultaneously, and the time of gradual change is 135s；
Step 303：The U-shaped gradient GaN of growth regulation two layer 202：It is passed through the NH that flow is 35000sccm3, 115L/min H2,
Reaction chamber temperature is from 1150 DEG C of gradual changes to 1275 DEG C, and simultaneous reactions cavity pressure maintains stable 650mbar, at the same be passed through TMGa from
225sccm gradual changes to the time of 350sccm, temperature, TMGa gradual change simultaneously, and gradual change is 950s；
Step 304：Grow the N-type GaN layer 203 for the Si that undopes：1300 DEG C are increased the temperature to, reaction cavity pressure is kept
450mbar, is passed through the NH that flow is 35000sccm3, 300sccm TMGa, 115L/min H2, 3 μm of continued propagation do not mix
Miscellaneous Si N-type GaN layer 203；
Step 305：The doping of growth regulation one Si N-type GaN layer 204：Keep reaction cavity pressure 450mbar, 1300 DEG C of temperature
It is constant, it is passed through the NH that flow is 45000sccm3, 300sccm TMGa, 115L/min H2, 35sccm SiH4, continued propagation
3.5 μm of first doping Si N-type GaN, Si doping concentration 7.5 × 1018atoms/cm3；
Step 306：The doping of growth regulation two Si N-type GaN layer 205：Keep reaction cavity pressure 450mbar, 130 DEG C of temperature not
Become, be passed through the NH that flow is 45000sccm3, 300sccm TMGa, 115L/min H2, 6sccm SiH4, continued propagation
The doping of 300nm second Si N-type GaN layer 205, Si doping concentrations 7.5 × 1017atoms/cm3；
Step 307：Grow luminescent layer 206：Reaction cavity pressure 350mbar, 725 DEG C of temperature are kept, being passed through flow is
60000sccm NH3, 30sccm TMGa, 1750sccm TMIn, 115L/min N2, growth 3nm doping In InxGa
(1-x) N layers 2061, wherein x=0.22, emission wavelength 452nm；Then 800 DEG C of temperature is raised, reaction cavity pressure is kept
350mbar is passed through the NH that flow is 60000sccm3, 60sccm TMGa, 115L/min N2, growth 12nmGaN layers 2062；So
Repeated growth InxGa (1-x) N layers 2061, repeated growth GaN layer 2062, alternating growth InxGa (1-x) N/GaN luminescent layers afterwards
206, controlling cycle number is 11；
Step 308：Growth doping Mg, Al p-type AlGaN layer 207：Reaction cavity pressure 300mbar, 925 DEG C of temperature are kept,
It is passed through the NH that flow is 60000sccm3, 45sccm TMGa, 115L/min H2, 115sccm TMAl, 1150sccm
Cp2Mg, continued propagation 75nm doping Mg, Al p-type AlGaN layer 207, Al doping concentrations 2 × 1020atoms/cm3, Mg adulterates dense
Degree 5 × 1019atoms/cm3；
Step 309：Grow high temperature dopant Mg p-type GaN layer 208：Reaction cavity pressure 650mbar, 975 DEG C of temperature are kept,
It is passed through the NH that flow is 60000sccm3, 60sccm TMGa, 115L/min H2, 2000sccm Cp2Mg, continued propagation
75nm high temperature dopants Mg p-type GaN layer 208, Mg doping concentrations 5 × 1019atoms/cm3；
Step 310：665 DEG C are finally cooled to, 25min is incubated, is then switched off heating system, closes and give gas system, with stove
Cooling.
Contrast experiment：
With reference to Fig. 3 there is provided a kind of epitaxial growth method of the prior art, comprise the following steps：
1st, Sapphire Substrate 301 is handled：Under 1000-1100 DEG C of hydrogen atmosphere, 100L/min-130L/min is passed through
H2, keep reaction cavity pressure 100-300mbar, processing Sapphire Substrate 3018-10 minutes；
2nd, low temperature growth buffer layer 302：It is cooled at 500-600 DEG C, keeps reaction cavity pressure 300-600mbar, be passed through
Flow is 10000-20000sccm NH3, 50-100sccm TMGa, 100L/min-130L/min H2, in Sapphire Substrate
Growth thickness is 20-40nm low temperature buffer layer 302 on 301；
3rd, low temperature buffer layer makes annealing treatment：1000-1200 DEG C is increased the temperature to, reaction cavity pressure 300-600mbar is kept,
It is passed through the NH that flow is 30000-40000sccm3, 100-130L/min H2Continue 300-500s so that low temperature buffer layer 302
Corrode as irregular GaN islands, this step is the annealing of low temperature buffer layer；
4th, the N-type GaN layer 303 for the Si that undopes is grown：1000-1200 DEG C is increased the temperature to, reaction cavity pressure 300- is kept
600mbar, is passed through the NH that flow is 30000-40000sccm3, 200-400sccm TMGa, 100-130L/min H2, continue
The Si that undopes of 2-4 μm of growth N-type GaN layer 303；
5th, the doping of growth regulation one Si N-type GaN layer 304：Keep reaction cavity pressure 300-600mbar, temperature 1000-1200
It is DEG C constant, it is passed through the NH that flow is 30000-60000sccm3, 200-400sccm TMGa, 100-130L/min H2、20-
50sccm 3-4 μm first doping Si of SiH4 continued propagations N-type GaN layer 304, Si doping concentrations 5 × 1018atoms/cm3-1
×1019atoms/cm3；
6th, the doping of growth regulation two Si N-type GaN layer 305：Keep reaction cavity pressure 300-600mbar, temperature 1000-1200
It is DEG C constant, it is passed through the NH that flow is 30000-60000sccm3, 200-400sccm TMGa, 100-130L/min H2、2-
10sccm SiH4The doping of continued propagation 200-400nm second Si N-type GaN layer 305, Si doping concentrations 5 × 1017atoms/
cm3-1×1018atoms/cm3；
7th, luminescent layer 306 is grown：Reaction cavity pressure 300-400mbar, 700-750 DEG C of temperature are kept, being passed through flow is
50000-70000sccm NH3, 20-40sccm TMGa, 1500-2000sccm TMIn, 100-130L/min N2, growth
Doping In 2.5-3.5nmInxGa (1-x) N layers 3061 (x=0.20-0.25), emission wavelength 450-455nm；Then temperature is raised
750-850 DEG C of degree, keeps reaction cavity pressure 300-400mbar, is passed through the NH that flow is 50000-70000sccm3、20-
100sccm TMGa, 100-130L/min N2, growth 8-15nmGaN layers 3062；Then N layers of repeated growth InxGa (1-x)
3061, then repeated growth GaN layer 3062, alternating growth InxGa (1-x) N/GaN luminescent layers 306, controlling cycle number is 7-15；
8th, growth doping Mg, Al p-type AlGaN layer 307：Keep reaction cavity pressure 200-400mbar, temperature 900-950
DEG C, it is passed through the NH that flow is 50000-70000sccm3, 30-60sccm TMGa, 100-130L/min H2、100-130sccm
TMAl, 1000-1300sccm Cp2Mg, continued propagation 50-100nm p-type AlGaN layer, Al doping concentrations 1 ×
1020atoms/cm3-3×1020Atoms/cm3, Mg doping concentration 1 × 1019atoms/cm3-1×1020atoms/cm3；
9th, growth high temperature dopant Mg p-type GaN layer 308：Keep reaction cavity pressure 400-900mbar, temperature 950-1000
DEG C, it is passed through the NH that flow is 50000-70000sccm3, 20-100sccm TMGa, 100-130L/min H2、1000-
3000sccm Cp2Mg, continued propagation 50-100nm high temperature dopant Mg p-type GaN layer 308, Mg doping concentrations 1 ×
1019atoms/cm3-1×1020atoms/cm3；
10th, 650-680 DEG C is finally cooled to, 20-30min is incubated, is then switched off heating system, closes and give gas system, with
Stove is cooled down.
The growing method of LED in contrast experiment prepares sample 1, and the method according to the invention prepares sample 2；Sample
Product 1 and the epitaxial growth method parameter difference of sample 2 be growing low temperature GaN, high temperature GaN growth conditions it is different：Growth
Other outer layer growth conditions are just the same (as shown in table 1)；Measurement obtains crystal in XRD equipment simultaneously for sample 1 and sample 2
Mass parameter, then sample 1 and sample 2 before identical under process conditions plate ITO layer about 150nm, Cr/ is plated under the same conditions
Pt/Au electrodes about 1500nm, plating SiO2 about 100nm, then under the same conditions grind sample under the same conditions
Mill cuts into the chip particle of 635 μm * 635 μm (25mil*25mil), and then sample 1 and sample 2 are each selected in same position
100 crystal grain, under identical packaging technology, are packaged into white light LEDs.Then using integrating sphere in driving current 350mA conditions
The photoelectric properties of lower test sample 1 and sample 2.U-shaped GaN refers to the N-type GaN layer for the Si that undopes.
The epitaxial growth method parameter comparison of table 1
The comparison of the sample 1 of table 2, the product electrical parameter of sample 2
The measure of the sample 1 of table 3,2 epitaxial wafer XRD parameters
Data analysis conclusion：The data that integrating sphere is obtained carry out analysis contrast, and such as table 2 and table 3 understand that the present invention is provided
The crystal mass of extension that obtains of growing method improve, item LED telecommunications parameters improve, experimental data shows side of the invention
Method can effectively lift LED product crystal mass.
Some preferred embodiments of the present invention have shown and described in described above, but as previously described, it should be understood that the present invention
Be not limited to form disclosed herein, be not to be taken as the exclusion to other embodiment, and available for various other combinations,
Modification and environment, and above-mentioned teaching or the technology or knowledge of association area can be passed through in invention contemplated scope described herein
It is modified., then all should be in this hair and the change and change that those skilled in the art are carried out do not depart from the spirit and scope of the present invention
In the protection domain of bright appended claims.
Claims (7)
1. a kind of epitaxial growth method of raising LED epitaxial crystal quality, it is characterised in that including step：
AlN substrates are put into, reaction cavity pressure 100-200mbar is kept, the NH that flow is 10000-20000sccm is passed through3、100-
130L/min H2, reaction chamber temperature is increased to 900-1000 DEG C；
The U-shaped gradient GaN of growth regulation one layer：It is passed through the NH that flow is 30000-40000sccm3, 100-130L/min H2, reaction
Chamber temperature is from 900-1000 DEG C of gradual change to 1000-1100 DEG C, and simultaneous reactions cavity pressure is from 100-150mbar, gradual change to 600-
700mbar, while TMGa is passed through from 50-70sccm gradual changes to 200-250sccm, pressure, temperature, TMGa gradual change simultaneously, and gradually
The time of change is 120-150s；
The U-shaped gradient GaN of growth regulation two layer：It is passed through the NH that flow is 30000-40000sccm3, 100-130L/min H2, reaction
Chamber temperature is from 1100-1200 DEG C, and gradual change is to 1200-1350 DEG C, and simultaneous reactions cavity pressure maintains stable 600-700mbar, simultaneously
TMGa is passed through from 200-250sccm gradual changes to 300-400sccm, temperature, TMGa gradual change simultaneously, and the time of gradual change is 900-
1000s；
Grow the N-type GaN layer for the Si that undopes；
The doping of growth regulation one Si N-type GaN layer；
The doping of growth regulation two Si N-type GaN layer；
Grow luminescent layer；
Growth doping Mg, Al p-type AlGaN layer；
Grow high temperature dopant Mg p-type GaN layer：Reaction cavity pressure 400-900mbar, 950-1000 DEG C of temperature are kept, stream is passed through
Measure TMGa, 100-130L/min of NH3,20-100sccm for 50000-70000sccm H2,1000-3000sccm
Cp2Mg, continued propagation 50-100nm high temperature dopants Mg p-type GaN layer, Mg doping concentrations 1 × 1019atoms/cm3-1×
1020atoms/cm3；
650-680 DEG C is finally cooled to, 20-30min is incubated, is then switched off heating system, closes and give gas system, furnace cooling.
2. the epitaxial growth method of raising LED epitaxial crystal quality according to claim 1, it is characterised in that it is described gradually
It is changed into linear gradient, gradual slope is equal to growth conditions difference divided by fade time before and after gradual change.
3. the epitaxial growth method of raising LED epitaxial crystal quality according to claim 1, it is characterised in that the life
The long Si that undopes N-type GaN layer, further for,
1200-1400 DEG C is increased the temperature to, reaction cavity pressure 300-600mbar is kept, flow is passed through for 30000-40000sccm
NH3, 200-400sccm TMGa, 100-130L/min H2, 2-4 μm of continued propagation the Si that undopes N-type GaN layer.
4. the epitaxial growth method of raising LED epitaxial crystal quality according to claim 1, it is characterised in that the life
The long first N-type GaN layer for adulterating Si, further for,
Growth doping Si N-type GaN layer：Reaction cavity pressure 300-600mbar, 1200-1400 DEG C of temperature are kept, being passed through flow is
30000-60000sccm NH3, 200-400sccm TMGa, 100-130L/min H2, 20-50sccm SiH4, it is lasting raw
Long 3-4 μm first doping Si N-type GaN layer, Si doping concentrations 5 × 1018atoms/cm3-1×1019atoms/cm3。
5. the epitaxial growth method of raising LED epitaxial crystal quality according to claim 1, it is characterised in that the life
The long second N-type GaN layer for adulterating Si, further for,
Reaction cavity pressure 300-600mbar, 1200-1400 DEG C of temperature are kept, the NH that flow is 30000-60000sccm is passed through3、
200-400sccm TMGa, 100-130L/min H2, 2-10sccm SiH4, the doping of continued propagation 200-400nm second Si
N-type GaN layer, Si doping concentrations 5 × 1017atoms/cm3-1×1018atoms/cm3。
6. the epitaxial growth method of raising LED epitaxial crystal quality according to claim 1, it is characterised in that the life
Long luminescent layer, further for,
Reaction cavity pressure 300-400mbar, 700-750 DEG C of temperature are kept, the NH that flow is 50000-70000sccm is passed through3、20-
40sccm TMGa, 1500-2000sccm TMIn and 100-130L/min N2, growth 2.5-3.5nm doping In InxGa
N layers of (1-x), wherein x is between 0.20-0.25, emission wavelength 450-455nm；Then 750-850 DEG C of temperature is raised, keeps anti-
Cavity pressure 300-400mbar is answered, the NH that flow is 50000-70000sccm is passed through3, 20-100sccm TMGa, 100-130L/
Min N2, grow 8-15nmGaN layers；Then N layers of repeated growth InxGa (1-x), repeated growth GaN layer, alternating growth InxGa
(1-x) N/GaN luminescent layers, controlling cycle number is 7-15.
7. the epitaxial growth method of raising LED epitaxial crystal quality according to claim 1, it is characterised in that the life
Long doping Mg, Al p-type AlGaN layer, further for,
Reaction cavity pressure 200-400mbar, 900-950 DEG C of temperature are kept, the NH that flow is 50000-70000sccm is passed through3、30-
60sccm TMGa, 100-130L/min H2, 100-130sccm TMAl, 1000-1300sccm Cp2Mg, continued propagation
50-100nm doping Mg, Al p-type AlGaN layer, Al doping concentrations 1 × 1020atoms/cm3-3×1020atoms/cm3, Mg mixes
Miscellaneous concentration 1 × 1019atoms/cm3-1×1020atoms/cm3。
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