CN107452841B - LED epitaxial growth method based on graphene - Google Patents
LED epitaxial growth method based on graphene Download PDFInfo
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- CN107452841B CN107452841B CN201710787388.8A CN201710787388A CN107452841B CN 107452841 B CN107452841 B CN 107452841B CN 201710787388 A CN201710787388 A CN 201710787388A CN 107452841 B CN107452841 B CN 107452841B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000000758 substrate Substances 0.000 claims abstract description 33
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 31
- 239000010980 sapphire Substances 0.000 claims abstract description 31
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims abstract description 20
- 229910002704 AlGaN Inorganic materials 0.000 claims abstract description 15
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000005229 chemical vapour deposition Methods 0.000 claims description 7
- 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
- 238000000151 deposition Methods 0.000 abstract description 2
- 230000008021 deposition Effects 0.000 abstract 1
- 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
- 238000010586 diagram Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 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
- 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
- 239000013256 coordination polymer Substances 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
- 239000007787 solid Substances 0.000 description 1
- 230000017260 vegetative to reproductive phase transition of meristem Effects 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/0237—Materials
- H01L21/0242—Crystalline insulating materials
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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
- H01L21/02436—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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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02436—Intermediate layers between substrates and deposited layers
- H01L21/02494—Structure
- H01L21/02496—Layer structure
- H01L21/02502—Layer structure consisting of two layers
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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
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02538—Group 13/15 materials
- H01L21/0254—Nitrides
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- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
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- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
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- 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
This application discloses a kind of LED epitaxial growth method based on graphene, it successively include: that Sapphire Substrate is placed in PECVD reaction chamber successively to grow: the first graphene film layer and the second graphene film layer, after taking-up, it is placed in MOCVD reaction chamber and successively grows: adulterating N-type GaN layer, cyclical growth MQW active layer, the p-type AlGaN layer, the p-type GaN layer for adulterating Mg of Si, cooling down.The present invention is by the way that Sapphire Substrate to be placed in PECVD reaction chamber, using the two uniform graphene films of step deposition growing as buffer layer, heteroepitaxial growth problem caused by the defect that lattice mismatch induces is solved, epitaxial crystal quality is improved, promotes the photoelectric properties of LED.
Description
Technical field
This application involves LED growth technology fields, specifically, it is raw to be related to a kind of LED extension based on graphene
Long method.
Background technique
LED (Light Emitting Diode, light emitting diode) is a kind of solid state lighting, comprising: small in size, power consumption
It is the features such as low, long service life, high, environmentally friendly and sturdy and durable brightness, deep to be approved by the majority of consumers, therefore, domestic production LED
Scale also gradually expanding.
Sapphire is the most common substrate material of LED of industrial production GaN at this stage, is limited by Sapphire Substrate and GaN
Between lattice mismatch, need the lattice defect density in LED component by growing all kinds of buffer layers, to reduce GaN.
The growing method of traditional LED epitaxial layer is referring to figs. 5 and 6 are as follows: processing substrate, growing low temperature buffer layer GaN, growth
The GaN layer of 3D, the GaN layer for growing 2D, the N-type GaN layer of growth doping Si, cyclical growth have edge layer MQW, growing P-type AlGaN
Layer, growth mix p-type GaN layer, the cooling down of Mg.
In above-mentioned traditional epitaxy technology, in sapphire Al2O3Growth GaN material on substrate, due to Al2O3Material and GaN
There are biggish lattice mismatches for material, cause the dislocation density of GaN material high, have seriously affected the luminous efficiency of LED chip；Together
When Sapphire Substrate there is also poor heat conductivity, the disadvantages of extinction is serious and difficult removing.The main method of control dislocation density is at present
One layer of GaN film of low-temperature epitaxy makees buffer layer, then grows the GaN layer of the GaN layer 2D of 3D 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 light emitting device, 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 method based on graphene, in sapphire
The graphene of uniform high quality is grown on substrate as buffer layer, to solve the hetero-epitaxy of substrate lattice mismatch induced defect
Problem is grown, fault in material is reduced, epitaxial crystal quality is improved, promotes the photoelectric properties of LED.
Summary of the invention
In view of this, the technical problem to be solved by the application is to provide a kind of LED epitaxial growth based on graphene
Method grows the graphene of uniform high quality as buffer layer, to solve the induction of substrate lattice mismatch on a sapphire substrate
The heteroepitaxial growth problem of defect reduces fault in material, improves epitaxial crystal quality, promotes the photoelectric properties of LED.
In order to solve the above-mentioned technical problem, the application has following technical solution: a kind of LED epitaxial growth based on graphene
Method successively includes:
Using plasma enhances 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, being passed through flow is 1000sccm-1500sccm's
H2, 600sccm-900sccm CH4With the Ar of 1000sccm-1200sccm, 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 the Ar of 1000sccm-1200sccm, the second graphene film layer of 20nm-30nm is grown；Its
In, H2Flow is reduced by 1000sccm-1500sccm gradual change to 800sccm-950sccm, CH4Flow is by 600sccm-900sccm
Gradual change increases to 950sccm-1100sccm；
The sapphire for being deposited with two layers of graphene film is taken out from PECVD reaction chamber, using Metal Organic Chemical Vapor
Sedimentation MOCVD, is placed in reaction chamber, successively grows on the sapphire for be deposited with graphene film:
Adulterate the N-type GaN layer of Si；
Cyclical growth MQW active layer；
Growing P-type AlGaN layer；
The p-type GaN layer of growth doping Mg；
700 DEG C -800 DEG C are cooled to, the N that flow is 100L/min-150L/min is passed through2, 20min-30min is kept the temperature, is closed
Close heating system, furnace cooling.
Preferably, the N-type GaN layer of the growth doping Si, further are as follows:
Reaction cavity pressure 150mbar-300mbar is kept, is kept for 1000 DEG C -1100 DEG C of temperature, being passed through flow is 40L/
The NH of min-60L/min3, 200sccm-300sccm TMGa, 50L/min-90L/min H2And 20sccm-50sccm
SiH4, the N-type GaN of 2 μm of -4 μm of doping Si of continued propagation, wherein Si doping concentration 5E18atoms/cm3-1E19atoms/cm3。
Preferably, the cyclical growth MQW active layer, further are as follows:
It keeps reaction cavity pressure 300mbar-400mbar, kept for 700 DEG C -750 DEG C of temperature, being passed through flow is 40L/min-
The NH of 60L/min3, 10sccm-50sccm TMGa, 1000sccm-2000sccm TMIn and 50L/min-90L/min N2,
The In of the 3nm-4nm of growth doping InxGa(1-x)N layers, wherein x=0.15-0.25, In doping concentration are 1E20atoms/cm3-
3E20atoms/cm3；
Temperature is increased to 800 DEG C -850 DEG C, keeps reaction cavity pressure 300mbar-400mbar, being passed through flow is 40L/
The NH of min-60L/min3, 10sccm-50sccm TMGa and 50L/min-90L/min N2, grow the GaN of 10nm-15nm
Layer；
Repeat alternating growth InxGa(1-x)N layers and GaN layer form MQW active layer, wherein InxGa(1-x)N layers and GaN layer
Alternating growth periodicity be 10-15.
Preferably, the growing P-type AlGaN layer, further are as follows:
Reaction cavity pressure 200mbar-400mbar, 850 DEG C -950 DEG C of temperature are kept, being passed through flow is 40L/min-60L/
The NH of min3, 50sccm-100sccm TMGa and 50L/min-90L/min N2, the p-type of continued propagation 50nm-100nm
AlGaN layer, wherein Al doping concentration 1E20atoms/cm3-3E20atoms/cm3, Mg doping concentration 5E18atoms/cm3-
1E19atoms/cm3。
Preferably, described to grow the p-type GaN layer for mixing Mg, further are as follows:
Reaction cavity pressure 200mbar-600mbar, 950 DEG C -1000 DEG C of temperature are kept, being passed through flow is 40L/min-60L/
The NH of min3, 50sccm-100sccm TMGa and 50L/min-90L/min N2, continued propagation 100nm-300nm's mixes Mg's
P-type GaN layer, wherein Mg doping concentration 1E19atoms/cm3-1E20atoms/cm3。
Compared with prior art, method described herein achieving the following effects:
(1) the present invention is based on the LED epitaxial growth methods of graphene, by utilizing plasma enhanced chemical vapor deposition
Method (PECVD) grows the graphene film of uniform high quality as buffer layer, due to graphene surface on a sapphire substrate
Without chemical dangling bonds, defect caused by lattice mismatch can avoid, be able to solve the heterogeneous outer of substrate lattice mismatch induced defect
Prolong growth problem, reduce fault in material, epitaxial crystal quality is improved, to promote the photoelectric properties of LED.
(2) the present invention is based on the LED epitaxial growth methods of graphene, deposit graphene film by using two steps, and
Second step methane and hydrogen flowing quantity gradual change, can make graphene film more uniform, improve the purity of graphene, reduce internal lack
The electric property for falling into, making graphene reaches best.In addition, the present invention is using graphene buffer layers instead of growing in conventional method
The technique of the GaN layer of the GaN layer and 2D of low temperature buffer layer GaN, 3D, shortens the growth time of MOCVD reaction chamber, improves life
Produce efficiency.
By referring to the drawings to the detailed description of exemplary embodiment of the present invention, other feature of the invention and its
Advantage will become apparent.
Detailed description of the invention
It is combined in the description and the attached drawing for constituting part of specification shows the embodiment of the present invention, and even
With its explanation together principle for explaining the present invention.
Fig. 1 is the flow diagram of the LED epitaxial growth method based on graphene described in the embodiment of the present invention 1；
Fig. 2 is the structural schematic diagram of the LED epitaxial layer based on graphene described in the embodiment of the present invention 1；
Fig. 3 is the flow diagram of the LED epitaxial growth method based on graphene described in the embodiment of the present invention 2；
Fig. 4 is the structural schematic diagram of the LED epitaxial layer based on graphene described in the embodiment of the present invention 2；
Fig. 5 is the flow diagram of routine LED epitaxial growth method；
Fig. 6 is the structural schematic diagram of routine LED epitaxial layer.
Specific embodiment
Carry out the various exemplary embodiments of detailed description of the present invention now with reference to attached drawing.It should also be noted that unless in addition having
Body explanation, the unlimited system of component and the positioned opposite of step, numerical expression and the numerical value otherwise illustrated in these embodiments is originally
The range of invention.
Be to the description only actually of at least one exemplary embodiment below it is illustrative, never as to the present invention
And its application or any restrictions used.
Technology, method and apparatus known to person of ordinary skill in the relevant may be not discussed in detail, but suitable
In the case of, the technology, method and apparatus should be considered as part of specification.
It is shown here and discuss all examples in, any occurrence should be construed as merely illustratively, without
It is as limitation.Therefore, other examples of exemplary embodiment can have different values.
It should also be noted that similar label and letter indicate similar terms in following attached drawing, therefore, once a certain Xiang Yi
It is defined in a attached drawing, then in subsequent attached drawing does not need that it is further discussed.
PECVD of the present invention first prepares graphene film on a sapphire substrate, then high brightness GaN is grown with MOCVD
Base LED epitaxial wafer.When growing high brightness GaN-based LED epitaxial wafer, 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 the source N, metal organic source trimethyl gallium (TMGa), metal organic source triethyl-gallium
(TEGa) it is used as gallium source, 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 growth.High-purity gas of the present invention,
Reinheitszahl is 99.999%.
Embodiment 1
As depicted in figs. 1 and 2, the LED epitaxial growth method described in the present embodiment based on graphene, includes the following steps:
Step 101, using plasma enhance chemical vapour deposition technique PECVD, 800 DEG C -950 DEG C of reaction chamber temperature,
Reacting cavity pressure 850mtorr-1000mtorr and radio-frequency power on the basis of 50W-80W, to be passed through flow is 1000sccm-
The H of 1500sccm (sccm is that milliliter is per minute)2, 600sccm-900sccm CH4With the Ar of 1000sccm-1200sccm,
The first graphene film layer of Grown on Sapphire Substrates 20nm-30nm.
Step 102 keeps 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 the Ar of 1000sccm-1200sccm, the second graphene for growing 20nm-30nm is thin
Film layer；Wherein, H2Flow is reduced by 1000sccm-1500sccm gradual change to 800sccm-950sccm, CH4Flow is by 600sccm-
900sccm gradual change increases to 950sccm-1100sccm.
Step 103 takes out the sapphire for being deposited with two layers of graphene film from PECVD reaction chamber, using organic metal
Chemical vapour deposition technique MOCVD, is placed in reaction chamber, on the sapphire for being deposited with graphene film, the N-type of growth doping Si
GaN layer.
Step 104, cyclical growth MQW active layer.
Step 105, growing P-type AlGaN layer.
The p-type GaN layer of step 106, growth doping Mg.
Step 107 is cooled to 700 DEG C -800 DEG C, is passed through the N that flow is 100L/min-150L/min2, keep the temperature 20min-
30min closes heating system, furnace cooling.
By growing uniform high quality on a sapphire substrate using plasma enhanced chemical vapor deposition method (PECVD)
Graphene film as buffer layer, since graphene surface is free of chemical dangling bonds, can avoid lacking caused by lattice mismatch
It falls into, is able to solve the heteroepitaxial growth problem of substrate lattice mismatch induced defect, reduce fault in material, improve epitaxial crystal matter
Amount, to promote the photoelectric properties of LED.Graphene film, and second step methane and hydrogen flowing quantity are deposited by using two steps
Gradual change can make graphene film more uniform, the electrical property for improving the purity of graphene, reducing internal flaw, making graphene
It can reach best.In addition, the present invention is using graphene buffer layers instead of growing low temperature buffer layer GaN, 3D in conventional method
The technique of GaN layer and the GaN layer of 2D shortens the growth time of MOCVD reaction chamber, improves production efficiency.
As shown in Fig. 2, being to be prepared using the LED epitaxial growth method described in the present embodiment based on graphene
The structural schematic diagram of LED epitaxial layer, the LED are comprised the following structure: substrate 11, the first graphene film layer 12, the first graphene
Film layer 13 adulterates the N-type GaN layer 14 of Si, MQW active layer 15 (wherein, including overlapping: InxGa(1-x)N layer 151 and GaN layer
152), p-type AlGaN layer 16 and the p-type GaN layer 17 of doping Mg.
Embodiment 2
The particular content of whole growth LED epitaxial layer, as shown in Figure 3 and Figure 4, the present embodiment has been described in detail in the present embodiment
The LED epitaxial growth method based on graphene, includes the following steps:
Step 201, using plasma enhance chemical vapour deposition technique PECVD, 800 DEG C -950 DEG C of reaction chamber temperature,
Reacting cavity pressure 850mtorr-1000mtorr and radio-frequency power on the basis of 50W-80W, to be passed through flow is 1000sccm-
The H of 1500sccm2, 600sccm-900sccm CH4With the Ar of 1000sccm-1200sccm, grow on a sapphire substrate
The first graphene film layer of 20nm-30nm.
Step 202 keeps 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 the Ar of 1000sccm-1200sccm, the second graphene for growing 20nm-30nm is thin
Film layer；Wherein, H2Flow is reduced by 1000sccm-1500sccm gradual change to 800sccm-950sccm, CH4Flow is by 600sccm-
900sccm gradual change increases 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, it can
Keep graphene film more uniform, improves the purity of graphene, reduces internal flaw.
Step 203 takes out the sapphire for being deposited with two layers of graphene film from PECVD reaction chamber, using organic metal
Chemical vapour deposition technique MOCVD, is placed in reaction chamber, on the sapphire for being deposited with graphene film, the N-type of growth doping Si
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 are held, the NH that flow is 40L/min-60L/min is passed through3, 200sccm-300sccm TMGa, 50L/
The H of min-90L/min2And the SiH of 20sccm-50sccm4, the N-type GaN of 2 μm of -4 μm of doping Si of continued propagation, 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 and so on).
Step 204, cyclical growth MQW active layer: it keeps reaction cavity pressure 300mbar-400mbar, keep 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, the In of the 3nm-4nm of growth doping InxGa(1-x)N layers, wherein x=0.15-
0.25, In doping concentration is 1E20atoms/cm3-3E20atoms/cm3。
Temperature is increased to 800 DEG C -850 DEG C, keeps reaction cavity pressure 300mbar-400mbar, being passed through flow is 40L/
The NH of min-60L/min3, 10sccm-50sccm TMGa and 50L/min-90L/min N2, grow the GaN of 10nm-15nm
Layer.
Repeat alternating growth InxGa(1-x)N layers and GaN layer form MQW active layer, wherein InxGa(1-x)N layers and GaN layer
Alternating growth periodicity be 10-15.
Step 205, growing P-type AlGaN layer: keeping reaction cavity pressure 200mbar-400mbar, 850 DEG C -950 DEG C of temperature,
It is passed through the NH that flow is 40L/min-60L/min3, 50sccm-100sccm TMGa and 50L/min-90L/min N2, continue
Grow the p-type AlGaN layer of 50nm-100nm, wherein Al doping concentration 1E20atoms/cm3-3E20atoms/cm3, Mg adulterates dense
Spend 5E18atoms/cm3-1E19atoms/cm3。
The p-type GaN layer of step 206, growth doping Mg: reaction cavity pressure 200mbar-600mbar, 950 DEG C of temperature-are kept
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 p-type GaN layer for mixing Mg of continued propagation 100nm-300nm, wherein Mg doping concentration 1E19atoms/cm3-1E20atoms/
cm3。
Step 207 is cooled to 700 DEG C -800 DEG C, is passed through the N that flow is 100L/min-150L/min2, keep the temperature 20min-
30min closes heating system, furnace cooling.
As shown in figure 4, being to be prepared using the LED epitaxial growth method described in the present embodiment based on graphene
The structural schematic diagram of LED epitaxial layer, the LED are comprised the following structure: substrate 21, the first graphene film layer 22, the first graphene
Film layer 23 adulterates the N-type GaN layer 24 of Si, MQW active layer 25 (wherein, including overlapping: InxGa(1-x)N layer 251 and GaN layer
252), p-type AlGaN layer 26 and the p-type GaN layer 27 of doping Mg.
By growing uniform high quality on a sapphire substrate using plasma enhanced chemical vapor deposition method (PECVD)
Graphene film as buffer layer, since graphene surface is free of chemical dangling bonds, can avoid lacking caused by lattice mismatch
It falls into, is able to solve the heteroepitaxial growth problem of substrate lattice mismatch induced defect, reduce fault in material, improve epitaxial crystal matter
Amount, to promote the photoelectric properties of LED.Graphene film, and second step methane and hydrogen flowing quantity are deposited by using two steps
Gradual change can make graphene film more uniform, the electrical property for improving the purity of graphene, reducing internal flaw, making graphene
It can reach best.
Embodiment 3
A kind of routine LED epitaxial growth method presented below is as comparative example of the invention.
As shown in Figure 5 and Figure 6, conventional LED epitaxial growth method, includes the following steps:
Step 301, processing Sapphire Substrate: to the reaction chamber for the Metallo-Organic Chemical Vapor depositing system for being placed with substrate
It is interior, in 900 DEG C -1100 DEG C of H2Under atmosphere, it is passed through the H of 50L/min-100L/min2, keep reaction cavity pressure 100mbar-
200mbar handles Sapphire Substrate 5min-10min.
Step 302, growth GaN low temperature buffer layer: being cooled to 500 DEG C -600 DEG C, keeps reaction cavity pressure 300mbar-
600mbar is passed through the NH that flow is 40L/min-60L/min3, 50sccm-100sccm TMGa and 50L/min-90L/min
H2, growth thickness is the GaN low temperature buffer layer of 30nm-60nm on a sapphire substrate.
Step 303, the GaN layer for growing 3D: being warming up to 850 DEG C -1000 DEG C, keeps reaction cavity pressure 300mbar-
600mbar 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: being warming up to 1000 DEG C -1100 DEG C, keeps reaction cavity pressure 300mbar-
600mbar 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: reaction cavity pressure 150mbar-300mbar is kept, temperature is kept
1000 DEG C -1100 DEG C, it is passed through the NH that flow is 40L/min-60L/min3, 200sccm-300sccm TMGa, 50L/min-
The H of 90L/min2And the SiH of 20sccm-50sccm4, the N-type GaN of 2 μm of -4 μm of doping Si of continued propagation, wherein Si doping concentration
5E18atoms/cm3-1E19atoms/cm3。
Step 306, cyclical growth MQW active layer: it keeps reaction cavity pressure 300mbar-400mbar, keep 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, the In of the 3nm-4nm of growth doping InxGa(1-x)N layers, wherein x=0.15-
0.25, In doping concentration is 1E20atoms/cm3-3E20atoms/cm3。
Temperature is increased to 800 DEG C -850 DEG C, keeps reaction cavity pressure 300mbar-400mbar, being passed through flow is 40L/
The NH of min-60L/min3, 10sccm-50sccm TMGa and 50L/min-90L/min N2, grow the GaN of 10nm-15nm
Layer.
Repeat alternating growth InxGa(1-x)N layers and GaN layer form MQW active layer, wherein InxGa(1-x)N layers and GaN layer
Alternating growth periodicity be 10-15.
Step 307, growing P-type AlGaN layer: keeping reaction cavity pressure 200mbar-400mbar, 850 DEG C -950 DEG C of temperature,
It is passed through the NH that flow is 40L/min-60L/min3, 50sccm-100sccm TMGa and 50L/min-90L/min N2, continue
Grow the p-type AlGaN layer of 50nm-100nm, wherein Al doping concentration 1E20atoms/cm3-3E20atoms/cm3, Mg adulterates dense
Spend 5E18atoms/cm3-1E19atoms/cm3。
The p-type GaN layer of step 308, growth doping Mg: reaction cavity pressure 200mbar-600mbar, 950 DEG C of temperature-are kept
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 p-type GaN layer for mixing Mg of continued propagation 100nm-300nm, wherein Mg doping concentration 1E19atoms/cm3-1E20atoms/
cm3。
Step 309 is cooled to 700 DEG C -800 DEG C, is passed through the N that flow is 100L/min-150L/min2, keep the temperature 20min-
30min closes heating system, furnace cooling obtains light emitting diode.
As shown in fig. 6, the LED epitaxial layer being prepared using routine techniques epitaxial growth method, includes such as from the bottom to top
Flowering structure: substrate 31, GaN low temperature buffer layer 32, the GaN layer 33 of 3D, the GaN layer of 2D 34, the N-type GaN layer 35 for adulterating Si, MQW
Active layer 36 is (wherein, including overlapping: InxGa(1-x)N layer 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 conventional LED epitaxial growth method (method of comparative example 3), are retouched according to this patent
The method stated prepares 4 samples 2；The difference of 2 epitaxial growth method of sample 1 and sample 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 chamber carries out other film layers again
It is long；The whole growth that all film layers are carried out in MOCVD reaction chamber 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 been grown, tests 102 face XRD of epitaxial wafer at identical conditions, tests number
According to referring to table 1；
2 extension XRD test data of 1 sample 1 of table and sample
Sample 1 and sample 2 plate about 1500 angstroms of ITO layer under identical preceding process conditions, plate Cr/Pt/ under the same conditions
About 2500 angstroms of Au electrode, plating SiO under the same conditions2About 500 angstroms, then sample grinding is cut at identical conditions
It is cut into 762 μm * 762 μm (30mil*30mil) of chip particle, then sample 1 and sample 2 respectively select 100 in same position
Crystal grain is packaged into white light LEDs under identical packaging technology.It carries out photoelectric properties test: existing in same LED point measurement machine
The photoelectric properties of test sample 1 and sample 2 under the conditions of driving current 350mA.Following table 2 is 2 photoelectricity test number of sample 1 and sample
According to.
2 sample 1 of table and sample 2LED test machine opto-electronic test data
It can be concluded that the face the sample XRD102 numerical value of the art of this patent production becomes smaller by the data of table 1, show this
The crystal quality of the sample epitaxial layer of patented technology production obviously improves.
It can be concluded that the sample LED light electrical property of the art of this patent production is more preferable by the data of table 2, brightness height,
Voltage is low, electric leakage is small, this has benefited from the art of this patent and reduces epitaxial layer dislocation, improves epitaxial layer crystal quality.
As can be seen from the above embodiments beneficial effect existing for the application is:
The present invention is based in the LED epitaxial growth method of graphene, by utilizing plasma enhanced chemical vapor deposition
Method (PECVD) grows the graphene film of uniform high quality as buffer layer, due to graphene surface on a sapphire substrate
Without chemical dangling bonds, defect caused by lattice mismatch can avoid, be able to solve the heterogeneous outer of substrate lattice mismatch induced defect
Prolong growth problem, reduce fault in material, epitaxial crystal quality is improved, to promote the photoelectric properties of LED.It is heavy 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 made to reach best.In addition, the present invention is replaced using graphene buffer layers
The technique of the GaN layer of GaN layer and 2D for growing low temperature buffer layer GaN, 3D in conventional method, shortens MOCVD reaction chamber
Growth time, improve production efficiency.
Although some specific embodiments of the invention are described in detail by example, the skill of this field
Art personnel it should be understood that example above merely to being illustrated, the range being not intended to be limiting of the invention.The skill of this field
Art personnel are it should be understood that can without departing from the scope and spirit of the present invention modify to above embodiments.This hair
Bright range is defined by the following claims.
Claims (1)
1. a kind of LED epitaxial growth method based on graphene, successively includes:
Using plasma enhances 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, being passed through flow is 1000sccm-1500sccm's
H2, 600sccm-900sccm CH4With the Ar of 1000sccm-1200sccm, 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, is passed through H2、CH4With the Ar of 1000sccm-1200sccm, the second graphene film layer of 20nm-30nm is grown；Wherein, H2Stream
Amount is reduced by 1000sccm-1500sccm gradual change to 800sccm-950sccm, CH4Flow is increased by 600sccm-900sccm gradual change
Add to 950sccm-1100sccm；
The sapphire for being deposited with two layers of graphene film is taken out from PECVD reaction chamber, using Metalorganic chemical vapor deposition
Method MOCVD, is placed in reaction chamber, in the N-type GaN layer for the grown on sapphire doping Si for being deposited with graphene film: keeping anti-
Cavity pressure 150mbar-300mbar is answered, is kept for 1000 DEG C -1100 DEG C of temperature, is passed through the NH that flow is 40L/min-60L/min3、
The H of TMGa, 50L/min-90L/min of 200sccm-300sccm2And the SiH of 20sccm-50sccm4, 2 μm -4 μm of continued propagation
Adulterate the N-type GaN of Si, wherein Si doping concentration 5E18atoms/cm3-1E19atoms/cm3；
The cyclical growth MQW active layer in the N-type GaN layer of doping Si: it keeps reaction cavity pressure 300mbar-400mbar, protect
700 DEG C -750 DEG C of temperature are held, the NH that flow is 40L/min-60L/min is passed through3, 10sccm-50sccm TMGa,
The N of the TMIn and 50L/min-90L/min of 1000sccm-2000sccm2, the In of the 3nm-4nm of growth doping InxGa(1-x)N
Layer, wherein x=0.15-0.25, In doping concentration are 1E20 atoms/cm3-3E20 atoms/cm3；
Temperature is increased to 800 DEG C -850 DEG C, keeps reaction cavity pressure 300mbar-400mbar, being passed through flow is 40L/min-
The NH of 60L/min3, 10sccm-50sccm TMGa and 50L/min-90L/min N2, grow the GaN layer of 10nm-15nm；
Repeat alternating growth InxGa(1-x)N layers and GaN layer form MQW active layer, wherein InxGa(1-x)The friendship of N layers and GaN layer
It is 10-15 for growth cycle number；
Growing P-type AlGaN layer: reaction cavity pressure 200mbar-400mbar, 850 DEG C -950 DEG C of temperature are kept, being passed through flow is
The NH of 40L/min-60L/min3, 50sccm-100sccm TMGa and 50L/min-90L/min N2, continued propagation 50nm-
The p-type AlGaN layer of 100nm, wherein Al doping concentration 1E20atoms/cm3-3E20atoms/cm3, Mg doping concentration
5E18atoms/cm3-1E19atoms/cm3；
The p-type GaN layer of growth doping Mg: reaction cavity pressure 200mbar-600mbar, 950 DEG C -1000 DEG C of temperature are kept, is passed through
Flow is the NH of 40L/min-60L/min3, 50sccm-100sccm TMGa and 50L/min-90L/min N2, continued propagation
The p-type GaN layer for mixing Mg of 100nm-300nm, wherein Mg doping concentration 1E19atoms/cm3-1E20atoms/cm3；
700 DEG C -800 DEG C are cooled to, the N that flow is 100L/min-150L/min is passed through2, 20min-30min is kept the temperature, heating is closed
System, furnace cooling.
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| CN110010729A (en) * | 2019-03-28 | 2019-07-12 | 王晓靁 | Full-color InGaN base LED of RGB and preparation method thereof |
| CN110246943B (en) * | 2019-06-17 | 2021-12-07 | 湘能华磊光电股份有限公司 | Graphene-based LED epitaxial growth method |
| CN112795983A (en) * | 2020-12-28 | 2021-05-14 | 中国科学院半导体研究所 | Multi-cavity semiconductor film epitaxial device |
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Denomination of invention: LED epitaxial growth method based on graphene Granted publication date: 20190709 Pledgee: Huaxia Bank Co.,Ltd. Chenzhou Branch Pledgor: XIANGNENG HUALEI OPTOELECTRONIC Co.,Ltd. Registration number: Y2024980045783 |