CN109119327A - The method of epitaxial growth aluminium nitride on nano-patterned sapphire substrate - Google Patents
The method of epitaxial growth aluminium nitride on nano-patterned sapphire substrate Download PDFInfo
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- CN109119327A CN109119327A CN201810973406.6A CN201810973406A CN109119327A CN 109119327 A CN109119327 A CN 109119327A CN 201810973406 A CN201810973406 A CN 201810973406A CN 109119327 A CN109119327 A CN 109119327A
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- epitaxial growth
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- 239000000758 substrate Substances 0.000 title claims abstract description 58
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 49
- 239000010980 sapphire Substances 0.000 title claims abstract description 49
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910017083 AlN Inorganic materials 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 49
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 47
- 238000003851 corona treatment Methods 0.000 claims abstract description 19
- 238000012545 processing Methods 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000005229 chemical vapour deposition Methods 0.000 claims description 5
- 230000003746 surface roughness Effects 0.000 claims description 4
- 238000000407 epitaxy Methods 0.000 claims description 3
- 150000004678 hydrides Chemical class 0.000 claims description 3
- 238000001451 molecular beam epitaxy Methods 0.000 claims description 3
- 238000004544 sputter deposition Methods 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052782 aluminium Inorganic materials 0.000 abstract description 7
- 239000004411 aluminium Substances 0.000 abstract description 4
- 150000004767 nitrides Chemical class 0.000 abstract description 4
- 239000010408 film Substances 0.000 description 32
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 238000001069 Raman spectroscopy Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 5
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- 230000005012 migration Effects 0.000 description 3
- 125000004433 nitrogen atom Chemical group N* 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- -1 graphite Alkene Chemical class 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000000059 patterning Methods 0.000 description 2
- 238000009832 plasma treatment Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Classifications
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- 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
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02538—Group 13/15 materials
- H01L21/0254—Nitrides
-
- 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
- H01L21/02656—Special treatments
- H01L21/02658—Pretreatments
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/26—Materials of the light emitting region
- H01L33/30—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table
- H01L33/32—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table containing nitrogen
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The present invention provides a kind of method of epitaxial growth aluminium nitride on nano-patterned sapphire substrate, comprising: deposits graphene layer on the surface of nano-patterned sapphire substrate;Corona treatment is carried out to the graphene layer;And the epitaxial growth aln layer on the graphene layer after processing.The present invention is using graphene nano graphical sapphire substrate as the substrate of aluminium nitride epitaxial growth, and corona treatment is carried out to graphene layer, by means of graphene as buffer layer, utilize the property of Van der Waals extension, high stress caused by lattice mismatch and thermal mismatching and high dislocation density can be reduced, to effectively promote the quality of epitaxial nitride aluminium film.
Description
Technical field
The present invention relates to Material Fields, in particular to one kind epitaxial growth aluminium nitride on nano-patterned sapphire substrate
Method.
Background technique
Aluminium nitride (AlN) is a kind of III-V semiconductor with wide direct band gap, have high heat conductance, high mechanical strength,
The properties such as high chemical stability and strong Radiation hardness are answered in photoelectron, high temperature high power device and high-frequency wideband communication device
There is wide prospect with aspect.Nano-patterned sapphire substrate is a kind of novel nitride epitaxial substrate, and light can be improved and mention
Take efficiency.
Aluminium nitride film is the core base material of ultraviolet LED, but aluminium nitride and nano patterning sapphire epitaxial substrate
Between there are huge lattice mismatch and thermal mismatchings, lead to the aluminium nitride film poor quality of epitaxial growth.Moreover, aluminium atom,
Nitrogen-atoms migration rate will be far below plane sapphire substrate in patterned substrate, difficult by changing the modes such as pressure, air-flow
To obtain smooth aluminium nitride film.Therefore, how effectively to buffer between aluminium nitride and sapphire epitaxial substrate that there are huge crystalline substances
Lattice mismatch and thermal mismatching increase aluminium atom, nitrogen-atoms migration rate, so that the quality of aluminium nitride film is promoted, it is ultraviolet to being promoted
The performance of LED has great importance.
Summary of the invention
The method of the object of the present invention is to provide a kind of on nano-patterned sapphire substrate epitaxial growth aluminium nitride, has
There are huge lattice mismatch and thermal mismatchings between effect buffering aluminium nitride and sapphire epitaxial substrate, increase aluminium atom, nitrogen-atoms
Migration rate.
To achieve the above object, scheme of the present invention are as follows:
The method of epitaxial growth aluminium nitride on nano-patterned sapphire substrate, comprising:
Graphene layer is deposited on the surface of nano-patterned sapphire substrate;
Corona treatment is carried out to the graphene layer;And
The epitaxial growth aln layer on the graphene layer after processing.
In some embodiments, the corona treatment is carried out using nitrogen plasma.
In some embodiments, the power of the corona treatment is 10-200W.
In some embodiments, the flow of the corona treatment is 10-500sccm.
In some embodiments, the time of the corona treatment is 10s-60s.
In some embodiments, the pressure of the corona treatment is 100-1000Pa.
In some embodiments, the surface roughness of the aln layer is 0.2-1nm.
In some embodiments, the aln layer by Metallo-Organic Chemical Vapor deposition, hydride gas-phase epitaxy, splash
Penetrate or molecular beam epitaxy and formed.
The present invention is using graphene nano graphical sapphire substrate as the substrate of aluminium nitride epitaxial growth, and to graphite
Alkene layer carries out corona treatment, reduces lattice mismatch using the property of Van der Waals extension as buffer layer by means of graphene
With high stress caused by thermal mismatching and high dislocation density, thus effectively promoted epitaxial nitride aluminium film quality.Present invention preparation
Method is simple, and universality is high, is suitble to industrial mass manufacture.
Detailed description of the invention
Figure 1A is the scanning electron microscopy of the aluminium nitride film of epitaxial growth on Conventional nano graphical sapphire substrate
Mirror figure;
Figure 1B is that the scanning electron of the aluminium nitride film of epitaxial growth on graphene nano graphical sapphire substrate is aobvious
Micro mirror figure;
Fig. 2 is the atomic force microscope of the aluminium nitride film of epitaxial growth on graphene nano graphical sapphire substrate
Figure;
Fig. 3 A is that the X-ray diffraction of the aluminium nitride film of epitaxial growth on Conventional nano graphical sapphire substrate waves
Curve;
Fig. 3 B is that the X-ray diffraction of the aluminium nitride film of epitaxial growth on graphene nano graphical sapphire substrate shakes
Put curve;
Fig. 4 is the epitaxial growth on Conventional nano graphical sapphire substrate and graphene nano graphical sapphire substrate
Aluminium nitride film Raman test chart.
Specific embodiment
Below according to specific embodiment, technical scheme is described further.Protection scope of the present invention is unlimited
In following embodiment, these examples are enumerated merely for exemplary purpose without limiting the invention in any way.
The method of epitaxial growth aluminium nitride on nano-patterned sapphire substrate of the invention, is in nano graph first
The surface for changing Sapphire Substrate deposits graphene layer, obtains graphene nano graphical sapphire substrate.
The method for depositing graphene layer can be chemical vapour deposition technique, step can include: by nano patterning sapphire
Substrate is placed in reaction cavity, and reaction temperature (such as 1000-1200 DEG C) is warming up under oxygen atmosphere, and annealing is pre- under this condition
4h is handled, oxygen is closed later, is drained oxygen in system using inert gas, hydrogen is passed through and carbon source carries out the change of graphene
Vapor deposition reaction is learned, so that graphene layer is deposited on nano-patterned sapphire substrate.
Nano-patterned sapphire substrate has specific nano graph, such as cone cell, platform-like, pothole shape etc..Graphite
Alkene layer may include one or more layers graphene, such as 1-3 layers of graphene.
It needs to carry out corona treatment to graphene layer after deposition graphene layer, so that the aln layer of itself and subsequent growth
Form good matching effect.
Corona treatment can be nitrogen plasma treatment, and wherein nitrogen flow is 10-500sccm, power 10-
200w, time 10-60s, pressure 100-1000Pa.
It is plasma treated, the epitaxial growth aln layer on graphene layer, the rough surface of gained aln layer
Degree is 0.2-1nm, it is sufficient to meet the level requirements of subsequent technique.The method of growing aluminum nitride layer can be Metallo-Organic Chemical Vapor
Deposition, hydride gas-phase epitaxy, sputtering or molecular beam epitaxy etc..
The present invention is described in further detail by the following examples.
Embodiment
Unless otherwise specified, experimental method used in following embodiments is conventional method.
Unless otherwise specified, the materials, reagents and the like used in the following examples is commercially available.
The epitaxial growth aluminium nitride film on graphene nano graphical sapphire substrate of embodiment 1.
1) graphene layer is deposited on the surface of nano-patterned sapphire substrate.
Nano-patterned sapphire substrate is placed in reaction cavity, 1100 DEG C are warming up under 300sccm oxygen atmosphere,
And annealing pre-processes 4h under this condition, closes oxygen later, is drained oxygen in system using argon gas, holding flow is
500sccm is passed through 200sccm hydrogen and 15sccm methane, carries out the chemical vapour deposition reaction of graphene, reaction time 8h,
To which graphene layer is deposited on nano-patterned sapphire substrate.
2) nitrogen plasma treatment is carried out to graphene nano graphical sapphire substrate.
Graphene nano graphical sapphire substrate is put into plasma process chamber, adjusting nitrogen flow is
15sccm, power 90w, pressure 500Pa carry out 30s corona treatment.
3) the epitaxial growth aluminium nitride film on plasma treated graphene nano graphical sapphire substrate.
Plasma treated graphene graphical sapphire substrate is put into mocvd growth chamber, heating substrate is extremely
1200 DEG C, adjust TMAl flow 50sccm, NH3Flow 500sccm, growth chamber pressure are 50torr, use N2It is raw as carrier gas
Long 1h obtains the AlN film of high quality.
With scanning electron microscope, measure respectively graphical in Conventional nano graphical sapphire substrate and graphene nano
The surface topography of the aluminium nitride film of Grown on Sapphire Substrates, as a result as shown in FIG. 1A and 1B, wherein Figure 1A be
The scanning electron microscope diagram of the aluminium nitride film of epitaxial growth on Conventional nano graphical sapphire substrate;Figure 1B is in graphite
The scanning electron microscope diagram of the aluminium nitride film of epitaxial growth on alkene nano-patterned sapphire substrate.It can from Figure 1A
Out, growing aluminum nitride film is discontinuous island structure on Conventional nano graphical sapphire substrate, irregular;And from
Figure 1B can be seen that the aluminum nitride thin film surface continuous formation grown on graphene nano graphical sapphire substrate.
For further verify growth aluminium nitride film profile pattern, use atomic force microscope measure aluminum nitride thin
The surface roughness of film, as a result as shown in Figure 2.From figure 2 it can be seen that raw on graphene nano graphical sapphire substrate
The surface roughness of long aluminium nitride film is 0.3nm, is atomically flating.
Using the rocking curve of X-ray diffraction test aluminium nitride film, the dislocation in film can be assessed by halfwidth
As a result density is schemed as shown in Figure 3A and Figure 3B, wherein Fig. 3 A is the epitaxial growth on Conventional nano graphical sapphire substrate
The X-ray diffraction rocking curve of aluminium nitride film;Fig. 3 B is the epitaxial growth on graphene nano graphical sapphire substrate
The X-ray diffraction rocking curve of aluminium nitride film.As can be seen from Figure 3A, the nitrogen grown in graphene nano patterned substrate
Changing aluminium film (0002) peak has smaller halfwidth.As can be seen from Figure 3B, it is grown in graphene nano patterned substrate
The aluminium nitride film peak (10-12) have smaller halfwidth.It is converted to dislocation density, threading dislocation density 2.70E+08, sword
Dislocation density 6.82E+09 reduces an at least number compared to the Conventional nano patterned substrate dislocation density in not graphene
Magnitude.
Using Raman spectrum test in the Raman shift of aluminium nitride film, answering in film can be assessed by Raman peak position
Power size, as a result as shown in Figure 4.It can be seen from the figure that with the epitaxial growth on Conventional nano graphical sapphire substrate
Aluminium nitride film is compared, the aluminium nitride film Raman peak position grown in graphene nano patterned substrate more towards with intrinsic body
Peak position, Raman shift is from 662.5cm-1Become 658.8cm-1, stress intensity is reduced into 0.378GPa from 1.378Ga, significantly reduces
Stress.
In conclusion the present invention is using graphene nano graphical sapphire substrate as the lining of aluminium nitride epitaxial growth
Bottom, and corona treatment is carried out to graphene layer, by means of graphene as buffer layer, using the property of Van der Waals extension,
High stress and high dislocation density caused by lattice mismatch and thermal mismatching are reduced, to effectively promote the matter of epitaxial nitride aluminium film
Amount.Preparation method of the present invention is simple, and universality is high, is suitble to industrial mass manufacture.
Those skilled in the art should be noted that embodiment described in the invention is only exemplary, can be
Various other replacements, changes and improvements are made in the scope of the present invention.Thus, the present invention is not limited to the above embodiments, and only
It is defined by the claims.
Claims (8)
1. a kind of method of the epitaxial growth aluminium nitride on nano-patterned sapphire substrate, comprising:
Graphene layer is deposited on the surface of nano-patterned sapphire substrate;
Corona treatment is carried out to the graphene layer;And
The epitaxial growth aln layer on the graphene layer after processing.
2. according to the method described in claim 1, wherein the corona treatment is carried out using nitrogen plasma.
3. according to the method described in claim 2, wherein the power of the corona treatment is 10-200W.
4. according to the method described in claim 2, wherein the flow of the corona treatment is 10-500sccm.
5. according to the method described in claim 2, wherein the time of the corona treatment is 10-60s.
6. according to the method described in claim 2, wherein the pressure of the corona treatment is 100-1000Pa.
7. according to the method described in claim 1, wherein the surface roughness of the aln layer is 0.2-1nm.
8. method according to any one of claim 1 to 7, wherein the aln layer passes through Metallo-Organic Chemical Vapor
Deposition, hydride gas-phase epitaxy, sputtering or molecular beam epitaxy and formed.
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CN201810973406.6A CN109119327A (en) | 2018-08-24 | 2018-08-24 | The method of epitaxial growth aluminium nitride on nano-patterned sapphire substrate |
PCT/CN2019/092806 WO2020038103A1 (en) | 2018-08-24 | 2019-06-25 | Nano patterned sapphire substrate with graphene, preparation method therefor and use thereof, graphene ultraviolet led and preparation method therefor |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2020038103A1 (en) * | 2018-08-24 | 2020-02-27 | 北京石墨烯研究院 | Nano patterned sapphire substrate with graphene, preparation method therefor and use thereof, graphene ultraviolet led and preparation method therefor |
CN112086343A (en) * | 2020-08-24 | 2020-12-15 | 中国科学院长春光学精密机械与物理研究所 | Hexagonal boron nitride film growth method and hexagonal boron nitride film |
CN114284397A (en) * | 2020-09-27 | 2022-04-05 | 中国科学院半导体研究所 | Method for growing high-quality aluminum nitride film on foreign substrate |
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US20110129675A1 (en) * | 2009-12-01 | 2011-06-02 | Samsung Electronics Co., Ltd. | Material including graphene and an inorganic material and method of manufacturing the material |
CN106868472A (en) * | 2017-01-19 | 2017-06-20 | 中国工程物理研究院电子工程研究所 | The growing method and gallium nitride lasers of a kind of nitride epitaxial piece |
CN108010995A (en) * | 2017-12-01 | 2018-05-08 | 北京大学 | A kind of high light efficiency LED chip based on graphene Sapphire Substrate |
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2018
- 2018-08-24 CN CN201810973406.6A patent/CN109119327A/en active Pending
Patent Citations (3)
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US20110129675A1 (en) * | 2009-12-01 | 2011-06-02 | Samsung Electronics Co., Ltd. | Material including graphene and an inorganic material and method of manufacturing the material |
CN106868472A (en) * | 2017-01-19 | 2017-06-20 | 中国工程物理研究院电子工程研究所 | The growing method and gallium nitride lasers of a kind of nitride epitaxial piece |
CN108010995A (en) * | 2017-12-01 | 2018-05-08 | 北京大学 | A kind of high light efficiency LED chip based on graphene Sapphire Substrate |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2020038103A1 (en) * | 2018-08-24 | 2020-02-27 | 北京石墨烯研究院 | Nano patterned sapphire substrate with graphene, preparation method therefor and use thereof, graphene ultraviolet led and preparation method therefor |
CN112086343A (en) * | 2020-08-24 | 2020-12-15 | 中国科学院长春光学精密机械与物理研究所 | Hexagonal boron nitride film growth method and hexagonal boron nitride film |
CN114284397A (en) * | 2020-09-27 | 2022-04-05 | 中国科学院半导体研究所 | Method for growing high-quality aluminum nitride film on foreign substrate |
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