CN107452841A - LED epitaxial growth methods based on graphene - Google Patents
LED epitaxial growth methods based on graphene Download PDFInfo
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- CN107452841A CN107452841A CN201710787388.8A CN201710787388A CN107452841A CN 107452841 A CN107452841 A CN 107452841A CN 201710787388 A CN201710787388 A CN 201710787388A CN 107452841 A CN107452841 A CN 107452841A
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- 230000012010 growth Effects 0.000 title claims abstract description 80
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims abstract description 50
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 31
- 239000010980 sapphire Substances 0.000 claims abstract description 31
- 239000000758 substrate Substances 0.000 claims abstract description 30
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims abstract description 20
- 229910002704 AlGaN Inorganic materials 0.000 claims abstract description 16
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000000151 deposition Methods 0.000 claims abstract description 5
- 230000008021 deposition Effects 0.000 claims abstract description 5
- 238000005229 chemical vapour deposition Methods 0.000 claims description 8
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 230000007547 defect Effects 0.000 abstract description 11
- 239000013078 crystal Substances 0.000 abstract description 10
- 239000010408 film Substances 0.000 description 35
- 239000011777 magnesium Substances 0.000 description 20
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 20
- 239000000463 material Substances 0.000 description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- -1 graphite alkene Chemical class 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 description 5
- 238000007796 conventional method Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 241001269238 Data Species 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000000407 epitaxy Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- RGGPNXQUMRMPRA-UHFFFAOYSA-N triethylgallium Chemical compound CC[Ga](CC)CC RGGPNXQUMRMPRA-UHFFFAOYSA-N 0.000 description 2
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-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
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 238000001534 heteroepitaxy Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
- H01L33/0062—Processes for devices with an active region comprising only III-V compounds
- H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
- H01L33/007—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound comprising nitride compounds
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/183—Epitaxial-layer growth characterised by the substrate being provided with a buffer layer, e.g. a lattice matching layer
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02436—Intermediate layers between substrates and deposited layers
- H01L21/02439—Materials
- H01L21/02441—Group 14 semiconducting materials
- H01L21/02444—Carbon, e.g. diamond-like carbon
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- H01L21/02494—Structure
- H01L21/02496—Layer structure
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Abstract
This application discloses a kind of LED epitaxial growth methods based on graphene, include successively：Sapphire Substrate is placed in PECVD reaction chambers and grown successively：First graphene film layer and the second graphene film layer, after taking-up, are placed in MOCVD reaction chambers and grow successively：Adulterate Si N-type GaN layer, cyclical growth MQW active layers, p-type AlGaN layer, the p-type GaN layer for adulterating Mg, cooling down.The present invention is by the way that Sapphire Substrate is placed in PECVD reaction chambers, using the two uniform graphene films of step deposition growing as cushion, solve the defects of lattice mismatch induces caused heteroepitaxial growth problem, improve epitaxial crystal quality, lift LED photoelectric properties.
Description
Technical field
The application is related to LED growth technologies field, specifically, is related to a kind of LED extensions life based on graphene
Long method.
Background technology
LED (Light Emitting Diode, light emitting diode) is a kind of solid state lighting, is had：Small volume, power consumption
It is low, the features such as service life is long, brightness is high, environmentally friendly and sturdy and durable, deep to be approved by consumers in general, therefore, domestic production LED
Scale also progressively expanding.
Sapphire is the most frequently used backing materials of the LED of industrial production GaN at this stage, is limited by Sapphire Substrate and GaN
Between lattice mismatch, it is necessary to by growing all kinds of cushions, to reduce the lattice defect density in GaN LED component.
The growing method of traditional LED epitaxial layers is referring to Fig. 5 and Fig. 6：Handle substrate, low temperature growth buffer layer GaN, growth
3D GaN layer, the GaN layer for growing 2D, growth doping Si N-type GaN layer, cyclical growth have edge layer MQW, growing P-type AlGaN
Layer, growth mix Mg p-type GaN layer, cooling down.
In above-mentioned traditional epitaxy technology, in sapphire Al2O3Grown GaN material, due to Al2O3Material and GaN
There is larger lattice mismatch in material, cause the dislocation density of GaN material high, had a strong impact on the luminous efficiency of LED chip；Together
When Sapphire Substrate poor heat conductivity, extinction serious and difficult the shortcomings of peeling off also be present.The main method of control dislocation density is at present
One layer of GaN film of low-temperature epitaxy makees cushion, then grows 3D GaN layer 2D GaN layer on this basis, eventually forms and compare
Smooth GaN layer.
However, conventional buffer layer technology has become the further improving luminous efficiency of GaN material LED, reduction
Cost and the important technology bottleneck for realizing extensive innovation and application.
Therefore, in view of the above-mentioned problems, the present invention provides a kind of LED epitaxial growth methods based on graphene, in sapphire
The graphene of the uniform high quality of Grown is used as cushion, to solve the hetero-epitaxy of substrate lattice mismatch induced defect
Problem is grown, reduces fault in material, improves epitaxial crystal quality, lifts LED photoelectric properties.
The content of the invention
In view of this, technical problems to be solved in this application there is provided a kind of LED epitaxial growths based on graphene
Method, the graphene for growing uniform high quality on a sapphire substrate are used as cushion, to solve the induction of substrate lattice mismatch
The heteroepitaxial growth problem of defect, fault in material is reduced, improve epitaxial crystal quality, lift LED photoelectric properties.
In order to solve the above-mentioned technical problem, the application has following technical scheme：A kind of LED epitaxial growths based on graphene
Method, include successively：
Using plasma strengthens chemical vapour deposition technique PECVD, in 800 DEG C -950 DEG C of reaction chamber temperature, reaction chamber pressure
On the basis of power 850mtorr-1000mtorr and radio-frequency power are 50W-80W, it is 1000sccm-1500sccm's to be passed through flow
H2, 600sccm-900sccm CH4With 1000sccm-1200sccm Ar, the of 20nm-30nm is grown on a sapphire substrate
One graphene film layer；
Keep 800 DEG C -950 DEG C of reaction chamber temperature, reaction cavity pressure 850mtorr-1000mtorr and radio-frequency power 50W-
80W is constant, is passed through H2、CH4With 1000sccm-1200sccm Ar, 20nm-30nm the second graphene film layer is grown；Its
In, H2Flow is reduced to 800sccm-950sccm, CH by 1000sccm-1500sccm gradual changes4Flow is by 600sccm-900sccm
Gradual change increases to 950sccm-1100sccm；
The sapphire for having two layers of graphene film will be deposited from the taking-up of PECVD reaction chambers, using Metal Organic Chemical Vapor
Sedimentation MOCVD, is placed in reaction chamber, has in deposition and is grown successively on the sapphire of graphene film：
Adulterate Si N-type GaN layer；
Cyclical growth MQW active layers；
Growing P-type AlGaN layer；
Growth doping Mg p-type GaN layer；
700 DEG C -800 DEG C are cooled to, is passed through the N that flow is 100L/min-150L/min2, 20min-30min is incubated, is closed
Close heating system, furnace cooling.
Preferably, it is described growth doping Si N-type GaN layer, further for：
Reaction cavity pressure 150mbar-300mbar is kept, 1000 DEG C -1100 DEG C of keeping temperature, it is 40L/ to be passed through flow
Min-60L/min NH3, 200sccm-300sccm TMGa, 50L/min-90L/min H2And 20sccm-50sccm
SiH4, 2 μm of -4 μm of doping Si of continued propagation N-type GaN, wherein, Si doping concentrations 5E18atoms/cm3-1E19atoms/cm3。
Preferably, the cyclical growth MQW active layers, further for：
Reaction cavity pressure 300mbar-400mbar, 700 DEG C -750 DEG C of keeping temperature are kept, it is 40L/min- to be passed through flow
60L/min NH3, 10sccm-50sccm TMGa, 1000sccm-2000sccm TMIn and 50L/min-90L/min N2,
Growth doping In 3nm-4nm InxGa(1-x)N layers, wherein, x=0.15-0.25, In doping concentrations are 1E20atoms/cm3-
3E20atoms/cm3；
Temperature is raised to 800 DEG C -850 DEG C, keeps reaction cavity pressure 300mbar-400mbar, it is 40L/ to be passed through flow
Min-60L/min NH3, 10sccm-50sccm TMGa and 50L/min-90L/min N2, grow 10nm-15nm GaN
Layer；
Repeat alternating growth InxGa(1-x)N layers and GaN layer, MQW active layers are formed, wherein, InxGa(1-x)N layers and GaN layer
Alternating growth periodicity be 10-15.
Preferably, the growing P-type AlGaN layer, further for：
Reaction cavity pressure 200mbar-400mbar, 850 DEG C -950 DEG C of temperature are kept, it is 40L/min-60L/ to be passed through flow
Min NH3, 50sccm-100sccm TMGa and 50L/min-90L/min N2, continued propagation 50nm-100nm p-type
AlGaN layer, wherein, Al doping concentrations 1E20atoms/cm3-3E20atoms/cm3, Mg doping concentrations 5E18atoms/cm3-
1E19atoms/cm3。
Preferably, described grow mixes Mg p-type GaN layer, further for：
Reaction cavity pressure 200mbar-600mbar, 950 DEG C -1000 DEG C of temperature are kept, it is 40L/min-60L/ to be passed through flow
Min NH3, 50sccm-100sccm TMGa and 50L/min-90L/min N2, continued propagation 100nm-300nm's mixes Mg's
P-type GaN layer, wherein, Mg doping concentrations 1E19atoms/cm3-1E20atoms/cm3。
Compared with prior art, method described herein, following effect has been reached：
(1) the LED epitaxial growth methods of the invention based on graphene, by using plasma enhanced chemical vapor deposition
The graphene film that method (PECVD) grows uniform high quality on a sapphire substrate is used as cushion, due to graphenic surface
Without chemical dangling bonds, the defects of lattice mismatch being avoided to cause, the heterogeneous outer of substrate lattice mismatch induced defect can solve the problem that
Epitaxial growth problem, fault in material is reduced, epitaxial crystal quality is improved, so as to lift LED photoelectric properties.
(2) the LED epitaxial growth methods of the invention based on graphene, by using two step deposited graphite alkene films, and
Second step methane and hydrogen flowing quantity gradual change, graphene film can be made more uniform, improve the purity of graphene, reduce internal lack
The electric property for falling into, making graphene reaches optimal.In addition, the present invention instead of in conventional method using graphene buffer layers and grow
The technique of low temperature buffer layer GaN, 3D GaN layer and 2D GaN layer, the growth time of MOCVD reaction chambers is shortened, improves life
Produce efficiency.
By referring to the drawings to the present invention exemplary embodiment detailed description, further feature of the invention and its
Advantage will be made apparent from.
Brief description of the drawings
It is combined in the description and the accompanying drawing of a part for constitution instruction shows embodiments of the invention, and even
It is used for the principle for explaining the present invention together with its explanation.
Fig. 1 is the schematic flow sheet of the LED epitaxial growth methods based on graphene described in the embodiment of the present invention 1；
Fig. 2 is the structural representation of the LED epitaxial layers based on graphene described in the embodiment of the present invention 1；
Fig. 3 is the schematic flow sheet of the LED epitaxial growth methods based on graphene described in the embodiment of the present invention 2；
Fig. 4 is the structural representation of the LED epitaxial layers based on graphene described in the embodiment of the present invention 2；
Fig. 5 is the schematic flow sheet of conventional LED epitaxial growth methods；
Fig. 6 is the structural representation of conventional LED epitaxial layers.
Embodiment
The various exemplary embodiments of the present invention are described in detail now with reference to accompanying drawing.It should be noted that：Unless have in addition
Body illustrates that the unlimited system of part and the positioned opposite of step, numerical expression and the numerical value otherwise illustrated in these embodiments is originally
The scope of invention.
The description only actually at least one exemplary embodiment is illustrative to be never used as to the present invention below
And its application or any restrictions that use.
It may be not discussed in detail for technology, method and apparatus known to person of ordinary skill in the relevant, but suitable
In the case of, the technology, method and apparatus should be considered as part for specification.
In shown here and discussion all examples, any occurrence should be construed as merely exemplary, without
It is as limitation.Therefore, other examples of exemplary embodiment can have different values.
It should be noted that：Similar label and letter represents similar terms in following accompanying drawing, therefore, once a certain Xiang Yi
It is defined, then it need not be further discussed in subsequent accompanying drawing in individual accompanying drawing.
PECVD of the present invention first prepares graphene film on a sapphire substrate, then with MOCVD next life long high brightness GaN
Base LED epitaxial wafer.When growing high brightness GaN-based LED, using high-purity H2Or high-purity N2Or high-purity H2And high-purity N2It is mixed
Gas is closed as carrier gas, high-purity N H3As N sources, metal organic source trimethyl gallium (TMGa), metal organic source triethyl-gallium
(TEGa) gallium source is used as, trimethyl indium (TMIn) is used as indium source, and N type dopant is silane (SiH4), trimethyl aluminium (TMAl) is made
For silicon source, P-type dopant is two luxuriant magnesium (CP2Mg), substrate is (0001) surface sapphire.The present invention solves in the prior art
The heteroepitaxial growth problem of lattice mismatch induced defect present in LED epitaxial growths.High-purity gas of the present invention, its
Reinheitszahl is 99.999%.
Embodiment 1
As depicted in figs. 1 and 2, the LED epitaxial growth methods based on graphene described in the present embodiment, comprise the following steps：
Step 101, using plasma enhancing chemical vapour deposition technique PECVD, 800 DEG C -950 DEG C of reaction chamber temperature,
Cavity pressure 850mtorr-1000mtorr and radio-frequency power are reacted on the basis of 50W-80W, it is 1000sccm- to be passed through flow
1500sccm (sccm is that milliliter is per minute) H2, 600sccm-900sccm CH4With 1000sccm-1200sccm Ar,
Grown on Sapphire Substrates 20nm-30nm the first graphene film layer.
Step 102, keep 800 DEG C -950 DEG C of reaction chamber temperature, reaction cavity pressure 850mtorr-1000mtorr and radio frequency
Power 50W-80W is constant, is passed through H2、CH4With 1000sccm-1200sccm Ar, the second graphene for growing 20nm-30nm is thin
Film layer；Wherein, H2Flow is reduced to 800sccm-950sccm, CH by 1000sccm-1500sccm gradual changes4Flow is by 600sccm-
900sccm gradual changes increase to 950sccm-1100sccm.
Step 103, the sapphire for having two layers of graphene film will be deposited from the taking-up of PECVD reaction chambers, using organic metal
Chemical vapour deposition technique MOCVD, is placed in reaction chamber, has in deposition on the sapphire of graphene film, growth doping Si N-type
GaN layer.
Step 104, cyclical growth MQW active layers.
Step 105, growing P-type AlGaN layer.
The p-type GaN layer of step 106, growth doping Mg.
Step 107,700 DEG C -800 DEG C are cooled to, are passed through the N that flow is 100L/min-150L/min2, it is incubated 20min-
30min, close heating system, furnace cooling.
Uniform high quality is grown on a sapphire substrate by using plasma enhanced chemical vapor deposition method (PECVD)
Graphene film be used as cushion, because graphenic surface is free of chemical dangling bonds, can avoid caused by lattice mismatch lack
Fall into, can solve the problem that the heteroepitaxial growth problem of substrate lattice mismatch induced defect, reduce fault in material, improve epitaxial crystal matter
Amount, so as to lift LED photoelectric properties.By using two step deposited graphite alkene films, and second step methane and hydrogen flowing quantity
Gradual change, graphene film can be made more uniform, improve the purity of graphene, the electrical property for reducing internal flaw, making graphene
It can reach optimal.In addition, the present invention instead of low temperature growth buffer layer GaN, 3D in conventional method using graphene buffer layers
The technique of GaN layer and 2D GaN layer, the growth time of MOCVD reaction chambers is shortened, improves production efficiency.
As shown in Fig. 2 to be prepared using the LED epitaxial growth methods based on graphene described in the present embodiment
The structural representation of LED epitaxial layers, the LED include following structure：Substrate 11, the first graphene film layer 12, the first graphene
Film layer 13, to adulterate Si N-type GaN layer 14, MQW active layers 15 (wherein, including overlapping：InxGa(1-x)N layers 151 and GaN layer
152), p-type AlGaN layer 16 and doping Mg p-type GaN layer 17.
Embodiment 2
The particular content of overall growth LED epitaxial layers, as shown in Figure 3 and Figure 4, the present embodiment has been described in detail in the present embodiment
The LED epitaxial growth methods based on graphene, comprise the following steps：
Step 201, using plasma enhancing chemical vapour deposition technique PECVD, 800 DEG C -950 DEG C of reaction chamber temperature,
Cavity pressure 850mtorr-1000mtorr and radio-frequency power are reacted on the basis of 50W-80W, it is 1000sccm- to be passed through flow
1500sccm H2, 600sccm-900sccm CH4With 1000sccm-1200sccm Ar, grow on a sapphire substrate
20nm-30nm the first graphene film layer.
Step 202, keep 800 DEG C -950 DEG C of reaction chamber temperature, reaction cavity pressure 850mtorr-1000mtorr and radio frequency
Power 50W-80W is constant, is passed through H2、CH4With 1000sccm-1200sccm Ar, the second graphene for growing 20nm-30nm is thin
Film layer；Wherein, H2Flow is reduced to 800sccm-950sccm, CH by 1000sccm-1500sccm gradual changes4Flow is by 600sccm-
900sccm gradual changes increase to 950sccm-1100sccm.
Two layers of graphene film layer, and second step methane and hydrogen flowing quantity gradual change are grown on a sapphire substrate, can
Make graphene film more uniform, improve the purity of graphene, reduce internal flaw.
Step 203, the sapphire for having two layers of graphene film will be deposited from the taking-up of PECVD reaction chambers, using organic metal
Chemical vapour deposition technique MOCVD, is placed in reaction chamber, has in deposition on the sapphire of graphene film, growth doping Si N-type
GaN layer：Keeping reaction cavity pressure 150mbar-300mbar, (mbar is the barometric millimeter of mercury, 1mbar=0.75 × 103Mtorr), protect
1000 DEG C -1100 DEG C of temperature is held, is passed through the NH that flow is 40L/min-60L/min3, 200sccm-300sccm TMGa, 50L/
Min-90L/min H2And 20sccm-50sccm SiH4, 2 μm of -4 μm of doping Si of continued propagation N-type GaN, wherein, Si doping
Concentration 5E18atoms/cm3-1E19atoms/cm3(1E19 represents 10 19 powers, that is, 1019, 5E18 represents 5 × 1018,
atoms/cm3For concentration unit, following presentation mode is by that analogy).
Step 204, cyclical growth MQW active layers：Keep reaction cavity pressure 300mbar-400mbar, keeping temperature 700
DEG C -750 DEG C, it is passed through the NH that flow is 40L/min-60L/min3, 10sccm-50sccm TMGa, 1000sccm-2000sccm
TMIn and 50L/min-90L/min N2, growth doping In 3nm-4nm InxGa(1-x)N layers, wherein, x=0.15-
0.25, In doping concentration is 1E20atoms/cm3-3E20atoms/cm3。
Temperature is raised to 800 DEG C -850 DEG C, keeps reaction cavity pressure 300mbar-400mbar, it is 40L/ to be passed through flow
Min-60L/min NH3, 10sccm-50sccm TMGa and 50L/min-90L/min N2, grow 10nm-15nm GaN
Layer.
Repeat alternating growth InxGa(1-x)N layers and GaN layer, MQW active layers are formed, wherein, InxGa(1-x)N layers and GaN layer
Alternating growth periodicity be 10-15.
Step 205, growing P-type AlGaN layer：Reaction cavity pressure 200mbar-400mbar, 850 DEG C -950 DEG C of temperature are kept,
It is passed through the NH that flow is 40L/min-60L/min3, 50sccm-100sccm TMGa and 50L/min-90L/min N2, continue
50nm-100nm p-type AlGaN layer is grown, wherein, Al doping concentrations 1E20atoms/cm3-3E20atoms/cm3, Mg adulterates dense
Spend 5E18atoms/cm3-1E19atoms/cm3。
The p-type GaN layer of step 206, growth doping Mg：Holding reaction cavity pressure 200mbar-600mbar, 950 DEG C of temperature-
1000 DEG C, it is passed through the NH that flow is 40L/min-60L/min3, 50sccm-100sccm TMGa and 50L/min-90L/min
N2, the continued propagation 100nm-300nm p-type GaN layer for mixing Mg, wherein, Mg doping concentrations 1E19atoms/cm3-1E20atoms/
cm3。
Step 207,700 DEG C -800 DEG C are cooled to, are passed through the N that flow is 100L/min-150L/min2, it is incubated 20min-
30min, close heating system, furnace cooling.
As shown in figure 4, to be prepared using the LED epitaxial growth methods based on graphene described in the present embodiment
The structural representation of LED epitaxial layers, the LED include following structure：Substrate 21, the first graphene film layer 22, the first graphene
Film layer 23, to adulterate Si N-type GaN layer 24, MQW active layers 25 (wherein, including overlapping：InxGa(1-x)N layers 251 and GaN layer
252), p-type AlGaN layer 26 and doping Mg p-type GaN layer 27.
Uniform high quality is grown on a sapphire substrate by using plasma enhanced chemical vapor deposition method (PECVD)
Graphene film be used as cushion, because graphenic surface is free of chemical dangling bonds, can avoid caused by lattice mismatch lack
Fall into, can solve the problem that the heteroepitaxial growth problem of substrate lattice mismatch induced defect, reduce fault in material, improve epitaxial crystal matter
Amount, so as to lift LED photoelectric properties.By using two step deposited graphite alkene films, and second step methane and hydrogen flowing quantity
Gradual change, graphene film can be made more uniform, improve the purity of graphene, the electrical property for reducing internal flaw, making graphene
It can reach optimal.
Embodiment 3
A kind of comparative example of the conventional LED epitaxial growth methods presented below as the present invention.
As shown in Figure 5 and Figure 6, conventional LED epitaxial growth methods, comprise the following steps：
Step 301, processing Sapphire Substrate：To the reaction chamber for the metal organic chemical vapor deposition system for being placed with substrate
It is interior, in 900 DEG C -1100 DEG C of H2Under atmosphere, 50L/min-100L/min H is passed through2, keep reaction cavity pressure 100mbar-
200mbar, processing Sapphire Substrate 5min-10min.
Step 302, growth GaN low temperature buffer layers：500 DEG C -600 DEG C are cooled to, keeps reaction cavity pressure 300mbar-
600mbar, it is passed through the NH that flow is 40L/min-60L/min3, 50sccm-100sccm TMGa and 50L/min-90L/min
H2, growth thickness is 30nm-60nm GaN low temperature buffer layers on a sapphire substrate.
Step 303, the GaN layer for growing 3D：850 DEG C -1000 DEG C are warming up to, keeps reaction cavity pressure 300mbar-
600mbar, it is passed through the NH that flow is 40L/min-60L/min3, 200sccm-300sccm TMGa and 50L/min-90L/min
H2, the GaN layer for the 3D that 2 μm -3 μm of continued propagation.
Step 304, the GaN layer for growing 2D：1000 DEG C -1100 DEG C are warming up to, keeps reaction cavity pressure 300mbar-
600mbar, it is passed through the NH that flow is 40L/min-60L/min3, 300sccm-400sccm TMGa and 50L/min-90L/min
H2, the GaN layer for the 2D that 2 μm -3 μm of continued propagation.
The N-type GaN layer of step 305, growth doping Si：Keep reaction cavity pressure 150mbar-300mbar, keeping temperature
1000 DEG C -1100 DEG C, it is passed through the NH that flow is 40L/min-60L/min3, 200sccm-300sccm TMGa, 50L/min-
90L/min H2And 20sccm-50sccm SiH4, 2 μm of -4 μm of doping Si of continued propagation N-type GaN, wherein, Si doping concentrations
5E18atoms/cm3-1E19atoms/cm3。
Step 306, cyclical growth MQW active layers：Keep reaction cavity pressure 300mbar-400mbar, keeping temperature 700
DEG C -750 DEG C, it is passed through the NH that flow is 40L/min-60L/min3, 10sccm-50sccm TMGa, 1000sccm-2000sccm
TMIn and 50L/min-90L/min N2, growth doping In 3nm-4nm InxGa(1-x)N layers, wherein, x=0.15-
0.25, In doping concentration is 1E20atoms/cm3-3E20atoms/cm3。
Temperature is raised to 800 DEG C -850 DEG C, keeps reaction cavity pressure 300mbar-400mbar, it is 40L/ to be passed through flow
Min-60L/min NH3, 10sccm-50sccm TMGa and 50L/min-90L/min N2, grow 10nm-15nm GaN
Layer.
Repeat alternating growth InxGa(1-x)N layers and GaN layer, MQW active layers are formed, wherein, InxGa(1-x)N layers and GaN layer
Alternating growth periodicity be 10-15.
Step 307, growing P-type AlGaN layer：Reaction cavity pressure 200mbar-400mbar, 850 DEG C -950 DEG C of temperature are kept,
It is passed through the NH that flow is 40L/min-60L/min3, 50sccm-100sccm TMGa and 50L/min-90L/min N2, continue
50nm-100nm p-type AlGaN layer is grown, wherein, Al doping concentrations 1E20atoms/cm3-3E20atoms/cm3, Mg adulterates dense
Spend 5E18atoms/cm3-1E19atoms/cm3。
The p-type GaN layer of step 308, growth doping Mg：Holding reaction cavity pressure 200mbar-600mbar, 950 DEG C of temperature-
1000 DEG C, it is passed through the NH that flow is 40L/min-60L/min3, 50sccm-100sccm TMGa and 50L/min-90L/min
N2, the continued propagation 100nm-300nm p-type GaN layer for mixing Mg, wherein, Mg doping concentrations 1E19atoms/cm3-1E20atoms/
cm3。
Step 309,700 DEG C -800 DEG C are cooled to, are passed through the N that flow is 100L/min-150L/min2, it is incubated 20min-
30min, close heating system, furnace cooling obtains light emitting diode.
As shown in fig. 6, the LED epitaxial layers being prepared using routine techniques epitaxial growth method, are included such as from the bottom to top
Lower structure：Substrate 31, GaN low temperature buffer layers 32,3D GaN layer 33,2D GaN layer 34, the N-type GaN layer 35 for adulterating Si, MQW
Active layer 36 is (wherein, including overlapping：InxGa(1-x)N layers 361 and GaN layer 362), p-type AlGaN layer 37 and adulterate Mg p-type
GaN layer 38.
4 samples 1 are prepared according to the LED epitaxial growth methods (method of comparative example 3) of routine, retouched according to this patent
The method stated prepares 4 samples 2；The difference of sample 1 and the epitaxial growth method of sample 2 is：Sample 2 directly serves as a contrast sapphire
Bottom is placed in PECVD reaction two layers of graphene film layer of Intracavity, is then placed in the life that MOCVD reaction chambers carry out other film layers again
It is long；The whole growth that all film layers are carried out in MOCVD reaction chambers of sample 1.And the film layer amount of saying of sample 2 is compared with the film of sample 1
Layer number is few.Taking-up after sample 1 and sample 2 have grown, the faces of XRD 102 of epitaxial wafer are tested under the same conditions, test number
According to referring to table 1；
The sample 1 of table 1 and the extension XRD test datas of sample 2
Sample 1 and sample 2 plate about 1500 angstroms of ITO layer before identical under process conditions, plate Cr/Pt/ under the same conditions
About 2500 angstroms of Au electrodes, under the same conditions plating SiO2About 500 angstroms, then sample grinding is cut under the same conditions
The chip particle of 762 μm * 762 μm (30mil*30mil) is cut into, then sample 1 and sample 2 each select 100 in same position
Crystal grain, under identical packaging technology, is packaged into white light LEDs.Carry out photoelectric properties test：Exist in same LED point measurement machine
Test sample 1 and the photoelectric properties of sample 2 under the conditions of driving current 350mA.Table 2 below is sample 1 and the photoelectricity test number of sample 2
According to.
The sample 1 of table 2 and sample 2LED test machine opto-electronic test datas
It can be drawn by the data of table 1 to draw a conclusion：The sample XRD102 faces numerical value that the art of this patent makes diminishes, and shows this
The crystal mass for the sample epitaxial layer that patented technology makes substantially improves.
It can be drawn by the data of table 2 to draw a conclusion：The sample LED light electrical property that the art of this patent makes is more preferable, brightness height,
Voltage is low, electric leakage is small, and this has benefited from the art of this patent and reduces epitaxial layer dislocation, improves epitaxial layer crystal mass.
By various embodiments above, beneficial effect existing for the application is：
In LED epitaxial growth methods of the invention based on graphene, by using plasma enhanced chemical vapor deposition
The graphene film that method (PECVD) grows uniform high quality on a sapphire substrate is used as cushion, due to graphenic surface
Without chemical dangling bonds, the defects of lattice mismatch being avoided to cause, the heterogeneous outer of substrate lattice mismatch induced defect can solve the problem that
Epitaxial growth problem, fault in material is reduced, epitaxial crystal quality is improved, so as to lift LED photoelectric properties.Sunk by using two steps
Product graphene film, and second step methane and hydrogen flowing quantity gradual change, can make graphene film more uniform, improve graphene
Purity, reduce internal flaw, the electric property of graphene is reached optimal.In addition, the present invention is replaced using graphene buffer layers
The technique of the GaN layer of GaN layer and 2D for low temperature growth buffer layer GaN, 3D in conventional method, shortens MOCVD reaction chambers
Growth time, improve production efficiency.
Although some specific embodiments of the present invention are described in detail by example, the skill of this area
Art personnel it should be understood that example above merely to illustrating, the scope being not intended to be limiting of the invention.The skill of this area
Art personnel to above example it should be understood that can modify without departing from the scope and spirit of the present invention.This hair
Bright scope is defined by the following claims.
Claims (5)
1. a kind of LED epitaxial growth methods based on graphene, include successively：
Using plasma strengthens chemical vapour deposition technique PECVD, in 800 DEG C -950 DEG C of reaction chamber temperature, reaction cavity pressure
On the basis of 850mtorr-1000mtorr and radio-frequency power are 50W-80W, it is 1000sccm-1500sccm's to be passed through flow
H2, 600sccm-900sccm CH4With 1000sccm-1200sccm Ar, the of 20nm-30nm is grown on a sapphire substrate
One graphene film layer；
Keep 800 DEG C -950 DEG C of reaction chamber temperature, reaction cavity pressure 850mtorr-1000mtorr and radio-frequency power 50W-80W not
Become, be passed through H2、CH4With 1000sccm-1200sccm Ar, 20nm-30nm the second graphene film layer is grown；Wherein, H2Stream
Amount is reduced to 800sccm-950sccm, CH by 1000sccm-1500sccm gradual changes4Flow is increased by 600sccm-900sccm gradual changes
Add to 950sccm-1100sccm；
The sapphire for having two layers of graphene film will be deposited from the taking-up of PECVD reaction chambers, using Metalorganic chemical vapor deposition
Method MOCVD, is placed in reaction chamber, has in deposition and is grown successively on the sapphire of graphene film：
Adulterate Si N-type GaN layer；
Cyclical growth MQW active layers；
Growing P-type AlGaN layer；
Growth doping Mg p-type GaN layer；
700 DEG C -800 DEG C are cooled to, is passed through the N that flow is 100L/min-150L/min2, 20min-30min is incubated, closes heating
System, furnace cooling.
2. the LED epitaxial growth methods based on graphene according to claim 1, it is characterised in that the growth doping Si
N-type GaN layer, further for：
Reaction cavity pressure 150mbar-300mbar is kept, 1000 DEG C -1100 DEG C of keeping temperature, it is 40L/min- to be passed through flow
60L/min NH3, 200sccm-300sccm TMGa, 50L/min-90L/min H2And 20sccm-50sccm SiH4, hold
Continuous 2 μm of -4 μm of doping Si of growth N-type GaN, wherein, Si doping concentrations 5E18atoms/cm3-1E19atoms/cm3。
3. the LED epitaxial growth methods based on graphene according to claim 1, it is characterised in that the cyclical growth
MQW active layers, further for：
Reaction cavity pressure 300mbar-400mbar, 700 DEG C -750 DEG C of keeping temperature are kept, it is 40L/min-60L/ to be passed through flow
Min NH3, 10sccm-50sccm TMGa, 1000sccm-2000sccm TMIn and 50L/min-90L/min N2, growth
Adulterate In 3nm-4nm InxGa(1-x)N layers, wherein, x=0.15-0.25, In doping concentrations are 1E20atoms/cm3-
3E20atoms/cm3；
Temperature is raised to 800 DEG C -850 DEG C, keeps reaction cavity pressure 300mbar-400mbar, it is 40L/min- to be passed through flow
60L/min NH3, 10sccm-50sccm TMGa and 50L/min-90L/min N2, grow 10nm-15nm GaN layer；
Repeat alternating growth InxGa(1-x)N layers and GaN layer, MQW active layers are formed, wherein, InxGa(1-x)The friendship of N layers and GaN layer
It it is 10-15 for growth cycle number.
4. the LED epitaxial growth methods based on graphene according to claim 1, it is characterised in that the growing P-type
AlGaN layer, further for：
Reaction cavity pressure 200mbar-400mbar, 850 DEG C -950 DEG C of temperature are kept, it is 40L/min-60L/min's to be passed through flow
NH3, 50sccm-100sccm TMGa and 50L/min-90L/min N2, continued propagation 50nm-100nm p-type AlGaN layer,
Wherein, Al doping concentrations 1E20atoms/cm3-3E20atoms/cm3, Mg doping concentrations 5E18atoms/cm3-1E19atoms/
cm3。
5. the LED epitaxial growth methods based on graphene according to claim 1, it is characterised in that described to grow the P for mixing Mg
Type GaN layer, further for：
Reaction cavity pressure 200mbar-600mbar, 950 DEG C -1000 DEG C of temperature are kept, it is 40L/min-60L/min to be passed through flow
NH3, 50sccm-100sccm TMGa and 50L/min-90L/min N2, the continued propagation 100nm-300nm p-type for mixing Mg
GaN layer, wherein, Mg doping concentrations 1E19atoms/cm3-1E20atoms/cm3。
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