CN110148663A - A kind of LED epitaxial wafer and preparation method thereof - Google Patents
A kind of LED epitaxial wafer and preparation method thereof Download PDFInfo
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- CN110148663A CN110148663A CN201910405944.XA CN201910405944A CN110148663A CN 110148663 A CN110148663 A CN 110148663A CN 201910405944 A CN201910405944 A CN 201910405944A CN 110148663 A CN110148663 A CN 110148663A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 63
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 60
- 239000000758 substrate Substances 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000002390 adhesive tape Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000004381 surface treatment Methods 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 56
- 229910017083 AlN Inorganic materials 0.000 description 55
- 239000010408 film Substances 0.000 description 27
- 230000012010 growth Effects 0.000 description 26
- 229910052594 sapphire Inorganic materials 0.000 description 18
- 239000010980 sapphire Substances 0.000 description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 239000012159 carrier gas Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 238000000151 deposition Methods 0.000 description 7
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 6
- 229910000077 silane Inorganic materials 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 4
- 150000004767 nitrides Chemical class 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000001505 atmospheric-pressure chemical vapour deposition Methods 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 238000004630 atomic force microscopy Methods 0.000 description 2
- 238000000407 epitaxy Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 2
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- GMACPFCYCYJHOC-UHFFFAOYSA-N [C].C Chemical compound [C].C GMACPFCYCYJHOC-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 150000004678 hydrides Chemical group 0.000 description 1
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- H01L33/0093—Wafer bonding; Removal of the growth substrate
-
- 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
- H01L33/48—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 body packages
- H01L33/64—Heat extraction or cooling elements
- H01L33/641—Heat extraction or cooling elements characterized by the materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0033—Processes relating to semiconductor body packages
- H01L2933/0075—Processes relating to semiconductor body packages relating to heat extraction or cooling elements
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Led Devices (AREA)
Abstract
An embodiment of the present invention provides a kind of LED epitaxial wafer and preparation method thereof, which includes: that graphene layer is arranged in substrate；AlN layers are arranged on the graphene layer；Described AlN layers is removed from the substrate；And LED epitaxial layer is set on the AlN layer.The preparation method of an embodiment of the present invention is acted on based on the extraordinary thermal conductivity of multi-layer graphene and stress release, two one-step film forming methods in traditional industry is changed into one-step method, significantly reduce the production time；And by AlN layers of removing, convenient for production flexible LED device, while the normal luminous of device is not influenced.
Description
Technical field
The present invention relates to LED epitaxial wafer, specially a kind of based on LED epitaxial wafer made from graphene and preparation method thereof.
Background technique
Third generation semiconductor based on III group nitride materials such as aluminium nitride (AlN), GaN has a extensive future, but common
Sapphire Substrate weak heat-dissipating and there are problems that biggish lattice mismatch and thermal mismatching with AlN and GaN, this all limits third
For the popularization and application of semiconductor lighting devices.
AlN is a kind of III-V semiconductor with direct band gap, has high mechanical strength, Radiation hardness, high stability
Etc. properties, had broad application prospects in high-power photoelectric device field.In addition, the important set of AlN or uv-LED device
At part.
At present industrially using preparing uv-LED device in sapphire substrates, and it is thin using two-step method growing AIN
Then film grows u-GaN layers, n-GaN layers, Al0.5Ga0.5N/AlyGa1-yN active layer p-GaN layer, then depositing electrode layer is carried out,
Finally processing and packaging.Lattice mismatch is larger with thermal mismatching in this method, and device light emitting efficiency is relatively low；And two-step method is raw
Time-consuming for long AlN film, and cost is big.
Summary of the invention
A primary object of the present invention is to provide a kind of preparation method of LED epitaxial wafer, comprising: is arranged in substrate
Graphene layer；AlN layers are arranged on the graphene layer；Described AlN layers is removed from the substrate；And in the AlN
LED epitaxial layer is set on layer.
According to an embodiment of the present invention, the LED epitaxial layer include u-GaN layers, n-GaN layers, active layer and p-GaN
Layer.
According to an embodiment of the present invention, described AlN layers is removed from the basal layer using adhesive tape.
According to an embodiment of the present invention, the method includes formed it is described before AlN layers to the graphene layer into
Row plasma surface treatment.
According to an embodiment of the present invention, the plasma surface treatment includes using oxygen plasma, Nitrogen ion body
At least one of with argon plasma, handled 30 seconds under conditions of 100W.
According to an embodiment of the present invention, the graphene layer includes multi-layer graphene, and the substrate is sapphire.
An embodiment of the present invention additionally provides a kind of LED epitaxial wafer, comprising:
AlN layers；And
LED epitaxial layer is set on the AlN layer.
According to an embodiment of the present invention, the LED epitaxial layer include the u-GaN layer set gradually, n-GaN layers, it is active
Layer and p-GaN layer.
According to an embodiment of the present invention, described AlN layers with a thickness of 0.5~2 μm；Described u-GaN layers with a thickness of 1~
3μm；Described n-GaN layers with a thickness of 0.5~5 μm；The active layer includes multiple Al0.5Ga0.5N layers and multiple AlyGa1-yN
Layer, 0.2≤y≤0.7, the Al0.5Ga0.5N layers and the AlyGa1-yN layers are arranged alternately；The p-GaN layer with a thickness of 50
~200nm.
An embodiment of the present invention further provides a kind of preparation method of AlN film, comprising:
Graphene layer is set in substrate；
AlN layers are arranged on the graphene layer；And
Described AlN layers is removed from the graphene layer using adhesive tape.
The preparation method of an embodiment of the present invention is made based on the extraordinary thermal conductivity of multi-layer graphene and stress release
With two one-step film forming methods in traditional industry are changed into one-step method, significantly reduce the production time；And by AlN layers of removing,
Convenient for making flexible LED device, while the normal luminous of device is not influenced.
Detailed description of the invention
Consider following the following detailed description of the embodiment of the present invention in conjunction with the accompanying drawings, various targets of the invention,
Feature and advantage will become apparent.Attached drawing is only exemplary diagram of the invention, is not necessarily drawn to scale.
In the accompanying drawings, same appended drawing reference always shows same or similar component.
Fig. 1 is the structural schematic diagram of the LED epitaxial wafer of an embodiment of the present invention；
Fig. 2 is the structural schematic diagram for removing AlN film from substrate of an embodiment of the present invention；
Fig. 3 a is the scanning electron microscope diagram for the AlN film of the embodiment of the present invention 1 grown on multi-layer graphene；
Fig. 3 b is the atomic force microscopy diagram for the AlN film of the embodiment of the present invention 1 grown on multi-layer graphene；
Fig. 3 c is (0002) the XRD rocking curve for the AlN film of the embodiment of the present invention 1 grown on multi-layer graphene；
Fig. 3 d is (10-12) the XRD rocking curve for the AlN film of the embodiment of the present invention 1 grown on multi-layer graphene；
Fig. 4 is the embodiment of the present invention 1 in the AlN film being located in sapphire substrates and the AlN removed from substrate
The Raman spectrogram of film；
Fig. 5 is the electric property figure of the resulting LED epitaxial wafer of the embodiment of the present invention 1.
Specific embodiment
The exemplary embodiment for embodying feature of present invention and advantage will describe in detail in the following description.It should be understood that
The present invention can have various variations in different embodiments, neither depart from the scope of the present invention, and theory therein
Bright and diagram inherently is illustrated as being used, rather than to limit the present invention.
Referring to Fig. 1,2, the preparation method of the LED epitaxial wafer of an embodiment of the present invention, comprising: be arranged in substrate 110
Graphene layer 111；AlN layer 120 (aln layer) is set on graphene layer 111；AlN layer 120 is removed from substrate 110；
And LED epitaxial layer is set on AlN layer 120.
The present invention removes AlN layers from substrate, obtains the LED epitaxial wafer comprising AlN layers, and obtained LED is normally sent out
Light, flexible for production and high heat dispersion LED manufacture are of great significance.And two traditional one-step film forming methods are changed into one
Footwork significantly reduces the production time.
Graphene is the two-dimensional layer material being only made of carbon atom, has excellent calorifics, electrology characteristic.In the present invention
In one embodiment, it is tight with what is spent can to reduce lattice in conventional epitaxial as buffer layer for directly growth graphene on sapphire
Lattice requirement, then III group-III nitride film of epitaxial growth high quality and is removed in graphene-Sapphire Substrate, finally
It is made into light emitting diode.Graphene has extraordinary thermal conductivity, electric conductivity to can solve the problems in device, this makes graphene
There is huge applications prospect in the fields such as photoelectric material and device.
In an embodiment, graphene layer 111 includes multi-layer graphene.
In an embodiment, as shown in Fig. 2, adhesive tape 200 can be used to remove AlN layer 120 from substrate 110.
In an embodiment, AlN layer 120 includes first surface and the second surface being oppositely arranged with first surface, AlN
Layer 120 is set to graphene layer 111 by first surface, and adhesive tape 200 is pasted on the second surface of AlN layer 120.In adhesive tape 200
Under the action of, multiple graphene layers 111 separate, and part graphene layer 111 stays in substrate 110, another part graphene
Layer 111 is still set to the first surface of AlN layer 120.
In an embodiment, substrate 110 can be sapphire substrates, such as plate sapphire substrates.
In an embodiment, graphene layer 111 can pass through chemical vapor deposition, plasma enhanced chemical vapor deposition
Etc. modes be made.For example, graphene layer 111 can be used, methane is the aumospheric pressure cvd of carbon source, ethyl alcohol is the low of carbon source
Pressure chemical vapor deposition or low temperature plasma enhancing chemical vapor deposition are prepared.
In an embodiment, graphene layer 111 deposited in substrate 110 after by plasma surface treatment, with suitable
Epitaxial growth for nitride film.
In an embodiment, plasma surface treatment includes: to utilize oxygen plasma, Nitrogen ion body and argon plasma
At least one of body handles 30s under conditions of 100W, obtains the multi-layer graphene suitable for epitaxial growth of nitride films
Layer.
In an embodiment, AlN layer 120 can be formed by Metallo-Organic Chemical Vapor depositing operation at high temperature.
In the preparation of the AlN layer 120 of an embodiment, growth temperature is directly risen to 1100 DEG C~1400 DEG C, such as
It is 1200 DEG C, 1300 DEG C etc., without 800 DEG C of low-temperature epitaxy process.
In the preparation of the AlN layer 120 of an embodiment, the source Al is provided using TMAl (trimethyl aluminium), flow can be
50~120sccm, such as 50sccm, 70sccm, 100sccm etc..
In the preparation of the AlN layer 120 of an embodiment, using NH3The source N is provided, flow can for 200~
20000sccm, such as 500sccm, 700sccm, 1000sccm, 5000sccm, 10000sccm etc..
In the preparation of the AlN layer 120 of an embodiment, growth chamber pressure can be 30~200torr, such as
50torr, 70torr, 100torr, 150torr etc.；Use N2As carrier gas, flow can be 12000sccm, and hydrogen flowing quantity can
Think 0~20000sccm, such as 1000sccm, 5000sccm, 10000sccm, 15400sccm etc..
In an embodiment, the AlN layer 120 that is grown in multi-layer graphene-sapphire substrates with a thickness of 0.5~2 μ
M, such as 0.7 μm, 1.0 μm, 1.5 μm etc..
In an embodiment, LED epitaxial layer includes u-GaN layer 130, n-GaN layer 140, active layer and p-GaN layer 160.
In an embodiment, the thickness of u-GaN layer 130 can be 1~3 μm, such as 1 μm, 1.5 μm, 2 μm, 2.5 μm
Deng.
In an embodiment, u-GaN layer 130 can be formed by Metallo-Organic Chemical Vapor depositing operation at high temperature.
In an embodiment, after AlN layer 120 is grown, temperature-resistant, NH is kept3Flow is raw for 6000sccm
Long u-GaN layer 130.
In the preparation of the u-GaN layer 130 of an embodiment, growth chamber pressure is 80torr.
In the preparation of the u-GaN layer 130 of an embodiment, it is passed through TMGa (trimethyl gallium) and the source Ga is provided, flow can be with
For 20~500sccm, such as 50sccm, 80sccm, 100sccm, 200sccm, 400sccm etc..
In the preparation of the u-GaN layer 130 of an embodiment, N is used2As carrier gas, hydrogen flowing quantity 15400sccm,
U-GaN layer 130 is grown on AlN layer 120.
In an embodiment, the thickness of n-GaN layer 140 can be 0.5~5 μm, such as 1 μm, 2 μm, 2.5 μm, 3 μm, 4
μm etc..
In an embodiment, n-GaN layer 140 can be formed by Metallo-Organic Chemical Vapor depositing operation at high temperature.
In an embodiment, after u-GaN layer 130 is grown, keeping temperature-resistant, TMGa flow is 80sccm,
It is passed through silane thereto, is adulterated for n.
In the preparation of the n-GaN layer 140 of an embodiment, silane flow rate 2.5sccm, NH3Flow is 6000sccm,
Growth chamber pressure is 50torr, uses N2As carrier gas, hydrogen flowing quantity 15400sccm grows n-GaN on u-GaN layers of lattice
Layer 140.
In an embodiment, active layer Al0.5Ga0.5N/AlyGa1-yN multiple quantum well active layer 150, wherein 0.2≤
Y≤0.7, such as y can be 0.4,0.6 etc..
In an embodiment, Al0.5Ga0.5N/AlyGa1-yN multiple quantum well active layer 150 is alternately to arrange in certain sequence
The Al of column0.5Ga0.5N layers and AlyGa1-yN layers of laminated construction, such as may include 3~10 couples of Al0.5Ga0.5N/Al0.4Ga0.6N amount
Sub- trap composite layer.
In an embodiment, Al0.5Ga0.5N/AlyGa1-yN multiple quantum well active layer 150 has 5 couples of Al0.5Ga0.5N/
AlyGa1-yN Quantum Well composite layer specifically includes the first Al being sequentially stacked0.5Ga0.5N layers, the first AlyGa1-yN layers, second
Al0.5Ga0.5N layers, the 2nd AlyGa1-yN layers, the 3rd Al0.5Ga0.5N layers, the 3rd AlyGa1-yN layers, the 4th Al0.5Ga0.5N layers, the 4th
AlyGa1-yN layers, the 5th Al0.5Ga0.5N layers, the 5th AlyGa1-yN layers.
In an embodiment, every Al0.5Ga0.5N/AlyGa1-yThe thickness of N Quantum Well composite layer can be 18nm, tool
For body, each Al0.5Ga0.5N layers of thickness can be 3nm, each AlyGa1-yThe thickness of N can be 15nm.
In an embodiment, Al0.5Ga0.5N/AlyGa1-yN quantum well layer can pass through Organometallic Chemistry gas at high temperature
Phase depositing operation is formed.
In an embodiment, Al0.5Ga0.5N/AlyGa1-yThe preparation method of N multiple quantum well active layer 150 includes: in n-
After GaN layer 140 is grown, terminating silane and be passed through, TMAl flow is switched to 25sccm, TMGa flow is switched to 25sccm,
It keeps other growth conditions constant, grows 3~10 couples of 3nm Al0.5Ga0.5N/15nm AlyGa1-yN quantum well layer, wherein y can
Think 0.4.
In an embodiment, the thickness of p-GaN layer 160 can be 50~200nm, for example, 70nm, 100nm, 120nm,
150nm etc..
In an embodiment, p-GaN layer 160 can be formed by Metallo-Organic Chemical Vapor depositing operation at high temperature.
In the preparation of the p-GaN layer 160 of an embodiment, in Al0.5Ga0.5N/AlyGa1-yN multiple quantum well active layer
After 150 growths, underlayer temperature can be 950~1100 DEG C, such as 1000 DEG C, 1050 DEG C etc.；TMGa flow can be 50
~120sccm, such as 70sccm, 90sccm, 100sccm etc.；The flow-rate ratio for being passed through two luxuriant magnesium and TMGa thereto be (0.1~
1.0): 1, it is adulterated for p, which such as can be 0.2:1,0.5:1,0.8:1；NH3Flow is 500sccm, growth
Chamber pressure is 50torr, uses N2As carrier gas, hydrogen flowing quantity 15400sccm.
The preparation method of an embodiment of the present invention is made based on the extraordinary thermal conductivity of multi-layer graphene and stress release
With two one-step film forming methods in traditional industry are changed into one-step method, significantly reduce the production time.
As shown in Figure 1, LED epitaxial wafer structure made from an embodiment of the present invention includes graphene layer 111, it is set to stone
AlN layer 120 on black alkene layer 111, the u-GaN layer 130 being set on AlN layer 120, the n-GaN being set on u-GaN layer 130
Layer 140, the Al being set on n-GaN layer 1400.5Ga0.5N/AlyGa1-yN multiple quantum well active layer 150, and be set to
Al0.5Ga0.5N/AlyGa1-yP-GaN layer 160 in N multiple quantum well active layer 150.
Hereinafter, being described further by specific embodiment to the preparation of the LED epitaxial wafer of an embodiment of the present invention.
Embodiment 1
1) multi-layer graphene film is grown: clean single sapphire substrates of throwing being put into APCVD cavity, by Ar and H2Gas
Flowmeter body is respectively set as 300sccm and 100sccm, after gas washing, furnace body is warming up to 1050 DEG C, in temperature-rise period
Keep Ar and H2Flow velocity is constant.After furnace temperature rises to 1050 DEG C, after stablizing 15min, by CH4Flow meter settings are 20sccm, growth
Time is 6h, and growth finishes, Temperature fall, obtains the sapphire substrates of multi-layer graphene covering.
2) under Room-temperature low-pressure, after carrying out nitrogen plasma to the sapphire substrates that surface is covered with multi-layer graphene
Reason, wherein nitrogen flow is 100sccm, and power setting 100w, the processing time is 30s, pressure 500Pa, multi-layer graphene
Cavity is got, multi-layer graphene sapphire substrates are obtained.
3) multi-layer graphene sapphire substrates obtained in step 2) are put into mocvd growth chamber, heat substrate, substrate temperature
1200 DEG C of degree, TMAl flow are 50sccm, NH3Flow is 500sccm, and growth chamber pressure is 50torr, uses N2As carrier gas,
Hydrogen flowing quantity is 15400sccm, obtains the preferable AlN film of quality, in graphene sapphire substrates with a thickness of 1.5 μm.
AlN film is removed according to mode shown in Fig. 2 from substrate, the AlN film grown on multi-layer graphene is carried out
Relevant characterization, wherein Fig. 3 a is the scanning electron microscope diagram of AlN film；Fig. 3 b is the atomic force microscopy diagram of AlN film, from
In it can be seen that AlN film surface realizes atomically flating, surface is flawless；Fig. 3 c is that (0002) XRD of AlN film waves song
Line；Fig. 3 d is (10-12) XRD rocking curve of AlN film；Fig. 4 is the Raman spectrum of AlN film.
Continued growth LED epitaxial layer on the AlN layer grown on multi-layer graphene.
4) u-GaN layers of growth: kept for 1200 DEG C of temperature, NH3Flow is 6000sccm, and growth chamber pressure is 80torr,
It is passed through TMGa (trimethyl gallium) and the source Ga is provided, flow 80sccm uses N2As carrier gas, hydrogen flowing quantity 15400sccm,
2.0 μm of u-GaN layer is grown on AlN layer.
5) n-GaN layers of growth: after the growth of the u-GaN of step 4) layer, kept for 1200 DEG C of temperature, TMGa flow is
80sccm is passed through silane thereto, adulterates for n, silane flow rate 2.5sccm, NH3Flow is 6000sccm, grows chamber pressure
It is by force 50torr, uses N2As carrier gas, hydrogen flowing quantity 15400sccm, growth thickness is 2.0 μm on u-GaN layers of lattice
N-GaN layers.
6)Al0.5Ga0.5N/AlyGa1-yThe growth of N multi-quantum well active region: n-Al0.55Ga0.45After N thin film is grown,
It terminates silane to be passed through, TMAl flow is switched to 25sccm, TMGa flow is 25sccm, keeps other growth conditions of step 5)
It is constant, grow 5 couples of 3nm Al0.5Ga0.5N/15nmAl0.4Ga0.6N quantum well layer.
7) growth of p-GaN layer: in step 6) 3nm Al0.5Ga0.5N/15nmAl0.4Ga0.6The growth of N multi-quantum well active region
After complete, being kept for 950 DEG C of temperature, TMGa flow is 50sccm, and being passed through two luxuriant magnesium flows thereto is 50sccm, it is adulterated for p,
NH3Flow is 500sccm, and growth chamber pressure is 50torr, uses N2As carrier gas, hydrogen flowing quantity 15400sccm obtains thickness
The p-GaN film that degree is 1.5 μm, obtains the LED base epitaxial wafer for being used to prepare LED chip device.
8) electrode evaporation, scribing conventionally are carried out to LED base epitaxial wafer obtained by step 7), encapsulation obtains LED device
Part.
Fig. 5 is the photoelectric properties figure of 1 gained LED base epitaxial wafer of embodiment.It can be seen that raw in multi-layer graphene sapphire substrates
Long strippable AlN layers continue to make LED component, device normal luminous.
Embodiment 2
The step of according to embodiment 1, MOCVD only is replaced with hydride gas-phase epitaxy, it is ultraviolet to be similarly obtained multi-layer graphene
LED。
Embodiment 3
The step of according to embodiment 1, MOCVD only is replaced with molecular beam epitaxy system, it is ultraviolet to be similarly obtained multi-layer graphene
LED。
Embodiment 4
The step of according to embodiment 1, MOCVD only is replaced with impulse laser deposition system, is similarly obtained multi-layer graphene purple
Outer LED.
Embodiment 5
The step of according to embodiment 1, MOCVD only is replaced with sputtering method, is similarly obtained multi-layer graphene ultraviolet LED.
Embodiment 6
The step of according to embodiment 1, plane sapphire substrate only is replaced with graphic sapphire substrate, is similarly obtained multilayer
Graphene ultraviolet LED.
Embodiment 7
The step of according to embodiment 1, the APCVD of methane carbon source is only replaced with the LPCVD of ethyl alcohol carbon source, is similarly obtained multilayer
Graphene ultraviolet LED.
Embodiment 8
It the step of according to embodiment 1, is only replaced in APCVD with PECVD, is similarly obtained multi-layer graphene ultraviolet LED.
Embodiment 9
The step of according to embodiment 1, nitrogen plasma only is replaced with oxygen plasma, it is ultraviolet to be similarly obtained multi-layer graphene
LED。
Unless limited otherwise, term used herein is the normally understood meaning of those skilled in the art.
Embodiment described in the invention is merely for exemplary purpose, the protection scope being not intended to limit the invention,
Those skilled in the art can be made within the scope of the invention various other replacements, changes and improvements, thus, the present invention is not limited to
Above embodiment, and be only defined by the claims.
Claims (10)
1. a kind of preparation method of LED epitaxial wafer, comprising:
Graphene layer is set in substrate；
AlN layers are arranged on the graphene layer；
Described AlN layers is removed from the substrate；And
LED epitaxial layer is set on the AlN layer.
2. according to the method described in claim 1, wherein, the LED epitaxial layer includes u-GaN layers, n-GaN layers, active layer and
P-GaN layer.
3. according to the method described in claim 1, wherein, described AlN layers is removed from the substrate using adhesive tape.
4. according to the method described in claim 1, wherein, being included in front of forming described AlN layers and being carried out to the graphene layer
Plasma surface treatment.
5. according to the method described in claim 4, wherein, the plasma surface treatment includes using oxygen plasma, nitrogen
At least one of gas ions and argon plasma are handled 30 seconds under conditions of 100W.
6. the substrate is blue precious according to the method described in claim 1, wherein, the graphene layer includes multi-layer graphene
Stone.
7. a kind of LED epitaxial wafer, comprising:
AlN layers；And
LED epitaxial layer is set on the AlN layer.
8. LED epitaxial wafer according to claim 7, wherein the LED epitaxial layer includes u-GaN layer, the n- set gradually
GaN layer, active layer and p-GaN layer.
9. LED epitaxial wafer according to claim 8, wherein described AlN layers with a thickness of 0.5~2 μm；It is u-GaN layers described
With a thickness of 1~3 μm；Described n-GaN layers with a thickness of 0.5~5 μm；The active layer includes multiple Al0.5Ga0.5N layers and more
A AlyGa1-yN layers, 0.2≤y≤0.7, the Al0.5Ga0.5N layers and the AlyGa1-yN layers are arranged alternately；The p-GaN layer
With a thickness of 50~200nm.
10. a kind of preparation method of AlN film, comprising:
Graphene layer is set in substrate；
AlN layers are arranged on the graphene layer；And
Described AlN layers is removed from the substrate using adhesive tape.
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