CN107904661A - A kind of growing method of low stress nitride aluminium crystal - Google Patents
A kind of growing method of low stress nitride aluminium crystal Download PDFInfo
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- CN107904661A CN107904661A CN201711284009.XA CN201711284009A CN107904661A CN 107904661 A CN107904661 A CN 107904661A CN 201711284009 A CN201711284009 A CN 201711284009A CN 107904661 A CN107904661 A CN 107904661A
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- 239000013078 crystal Substances 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 26
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 239000004411 aluminium Substances 0.000 title claims abstract description 14
- 150000004767 nitrides Chemical class 0.000 title claims abstract description 14
- 230000012010 growth Effects 0.000 claims abstract description 32
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000001963 growth medium Substances 0.000 claims abstract description 3
- 229910017083 AlN Inorganic materials 0.000 claims description 13
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 7
- 238000010583 slow cooling Methods 0.000 claims description 6
- 238000012512 characterization method Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 abstract description 19
- 230000006911 nucleation Effects 0.000 abstract description 8
- 238000010899 nucleation Methods 0.000 abstract description 8
- 230000009466 transformation Effects 0.000 abstract description 6
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 abstract description 5
- 229910010271 silicon carbide Inorganic materials 0.000 abstract description 5
- 230000006837 decompression Effects 0.000 abstract description 3
- 230000008021 deposition Effects 0.000 abstract description 3
- 230000035876 healing Effects 0.000 abstract description 3
- 208000037656 Respiratory Sounds Diseases 0.000 abstract description 2
- 230000007773 growth pattern Effects 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 206010037660 Pyrexia Diseases 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000003708 ampul Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000002109 crystal growth method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 230000034655 secondary growth Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
Classifications
-
- 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
-
- 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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/002—Controlling or regulating
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a kind of growing method of low stress nitride aluminium crystal, the growing method in growth course by alternating temperature transformation by way of, realize AlN crystal fast two-dimensional pattern growths, reduce the stress of aluminum-nitride single crystal.Obtain crystal growth plane and do not include crackle and the aluminum nitride body monocrystalline containing nature growth step.The application uses temperature control technique, the mode of specified temp section alternating temperature transformation in growth course, early period, high pressure low temperature reduced atomic nucleation speed, increase nucleation regularity at initial stage simultaneously suppresses substrate decomposition failure, growth medium decompression improves growth rate, slow down substrate decomposition, Later growth, heating pressurization, increase nitrogen source supply avoids 3-dimensional island growth pattern, it is uneven to reduce deposition, the larger phenomenon of stress, secondary temperature elevation is carried out after cooling, reduce crystals stress, allow plane of crystal crack healing, so that silicon carbide substrates are decomposed, obtained from the aluminum-nitride single crystal of the high quality of stripping.
Description
Technical field
The present invention relates to aluminum-nitride single crystal preparation field, and in particular to a kind of growing method of low stress nitride aluminium crystal.
Background technology
AlN crystal is a kind of important broad stopband (6.2eV) semi-conducting material, has high heat conductance (3.2W.cm-1K-1)、
The excellent physical property such as high resistivity and the high surface velocity of sound (5600-6000m/s), in laser, high-power electronic device, light
It is used widely in electronic device and SAW device.At present, physical vapor transmission method (PVT) is generally acknowledged to prepare big ruler
The effective way of very little aluminum-nitride single crystal, is the method that large single crystal is more easily prepared relative to self-contained nucleus growth using seed crystal bottom.
By sublimed method in the method for grown on foreign substrates AlN crystal, can be grown using the foreign substrate of major diameter
Large-sized AlN crystal, yet between substrate seed crystal, there are lattice mismatch and thermal mismatching, and aluminum nitride crystal c-axis and a
The anisotropy of axis thermal coefficient of expansion is larger into crystalline anisotropy, causes crystal stress larger, serious cracking.
In order to obtain high quality, the aluminum-nitride single crystal of low stress, passes through alternating temperature transformation, adjusting crucible position in growth course
Put, the methods of Heating tube wall thickness is thinned so that crucible can realize the purpose of heat stepwise, it is ensured that aufwuchsplate is axially and radially given birth to
Long temperature gradient, realizes larger sedimentation rate.
The content of the invention
For problems of the prior art, it is an object of the invention to provide a kind of life of low stress nitride aluminium crystal
Long method, different pressures and temperature are respectively adopted by the growth techniques of alternating temperature transformations a series of, preceding middle and later periods in it, and latter stage is secondary
Heating, overcome foreign substrate growth in substrate decompose, substrate deposition bed boundary crystal quality is poor, crystals stress compared with
Greatly, crack the problem of more.
To achieve the above object, the present invention uses following technical scheme：
A kind of growing method of low stress nitride aluminium crystal, the growing method include the following steps：
1) in the early growth period of aluminum nitride crystal, growing environment is vacuumized, and is filled with nitrogen, until gas in growing environment
Pressure reaches the first setting pressure, and is raised to the first design temperature with the heating rate of 20 DEG C/h-40 DEG C/h, and keeps the temperature half an hour；
2) air pressure in growing environment is dropped into the second setting pressure in the growth medium of aluminum nitride crystal, ten minutes,
And temperature is stepped up as the second design temperature in two hours, when growth time 8-15 is small；
3) in the Later growth of aluminum nitride crystal, rise crucible position, improves seed crystal face gradient, increase material source to seed crystal
Axial-temperature gradient, pressure is raised to the 3rd setting pressure by air pressure in growing environment；And by growing environment in 20 minutes
Temperature be increased to the 3rd design temperature, keep 4 it is small when；
4) in the growth latter stage of aluminum nitride crystal, with the speed slow cooling of 40 DEG C/h, by growing environment under 95KPa pressure
Interior temperature drops to 1850 DEG C of the decomposition temperature of aluminium nitride material source, is kept for half an hour；
5) heat up again under 95KPa pressure, the temperature in growing environment is increased to the 4th design temperature；
6) 1000 DEG C are slow cooling to 30 DEG C/h speed under 95KPa pressure, natural cooling, blow-on, tests characterization.
Further, described first pressure is set as 40KPa.
Further, first design temperature is 1900 DEG C.
Further, described second pressure is set as 20KPa.
Further, second design temperature is 1930-1940 DEG C.
Further, the described 3rd pressure is set as 95KPa.
Further, the 3rd design temperature is 2000 DEG C.
Further, the 4th design temperature is 2000 DEG C.
The present invention has following advantageous effects：
The application by the way of specified temp section alternating temperature transformation in growth course, early period high pressure low temperature reduce atom into
Core speed, increase nucleation at initial stage regularity reduce substrate decomposition failure, during mid-term decompression improve growth rate so that sedimentary is covered
Lid substrate, avoids substrate because aluminium nitride material source big saturation degree etching causes to fail, Later growth, heats up and increases nitrogen partial pressure,
Increase nitrogen partial pressure avoids island growth so that it is guaranteed that nitrogen source supply, and secondary temperature elevation is carried out after cooling, and reducing crystals should
Power, face crack healing so that silicon carbide decomposition, obtained from the aluminum-nitride single crystal of the high quality of stripping.
Brief description of the drawings
Fig. 1 is the structural representation of the aluminum-nitride single crystal growth furnace used in aluminum nitride crystal growth method of the embodiment of the present invention
Figure.
Embodiment
In the following, refer to the attached drawing, more fully illustrates the present invention, shown in the drawings of the exemplary implementation of the present invention
Example.However, the present invention can be presented as a variety of multi-forms, it is not construed as being confined to the exemplary implementation described here
Example.And these embodiments are to provide, so that the present invention is fully and completely, and it will fully convey the scope of the invention to this
The those of ordinary skill in field.
As shown in Figure 1, the heterogeneous lining of major diameter is used in the method for grown on foreign substrates AlN crystal by sublimed method
The AlN crystal of growing large-size is capable of at bottom, yet with there are lattice mismatch and thermal mismatching, and deposition is not between substrate seed crystal
Cause crystalline anisotropy larger, by the present invention in that with the Heating tube of uneven thickness one, so that radial symmetry gradient is adjusted,
So as to be accurately controlled thermal field.Wherein, position thickness is 1/3rd of both sides thickness centered on Heating tube, is only 5mm, up and down
Base fever barrel thickness is 15mm so that under the conditions of identical thermal field, axial-temperature gradient is kept constant.
By thermal field design and gradient demand, the dimensional thickness of seed crystal Heating tube top and side insulation quilt is determined.Filler
And make it that 8 spacing of material source is 60mm, silicon carbide seed 11 is bonded in seed crystal covers, and using aluminium nitride block after sintering, determines
Crucible opposed coil position, adjusts crucible opposed coil position, by ramet (TaC) crucible by regulation heating cylinder lifting platform 5
10 centres are relatively thin, in the thicker Heating tube in Heating tube top 6 and Heating tube lower part 7, protected using graphite insulation quilt 9
Temperature, carries out thermometric by upper and lower thermometer hole 3,4, graphite felt overall structure is placed on lifting platform 5, can be changed by adjusting position
Become the axial-temperature gradient per heat.The graphite felt cylinder is located in quartz ampoule 2, which is located in coil 1.
Shove charge, vacuumizes, and is filled with nitrogen 40KPa, and insulation half at 1900 DEG C is raised to the heating rate of 20 DEG C/h-40 DEG C/h
Hour, nucleation rate on substrate at aluminium nitride initial stage is reduced, suppresses seed crystal decomposition failure, improves atomic rearrangement regularity.
Pressure is dropped into 20KPa in ten minutes, properly increases aluminium nitride sedimentation rate on silicon carbide substrates, suppresses carbonization
The decomposition of silicon seed.Temperature is adjusted to 1930-1940 DEG C in two hours.When growth time 8-15 is small.
As deposit thickness increases, to change due to growth interface energy variation and seed crystal face gradient is excessive makes
Become the phenomenon of vertebra shape nucleation by two-dimensional nucleation into aluminium nitride, rise crucible position, improves seed crystal face gradient, increase material source axis
To gradient, rise pressure to 95KPa；Temperature is increased to 2000 DEG C in 20 minutes.4h is kept, heal plane of crystal crackle and island
Shape is nucleated.
In growth latter stage, temperature is reduced to aluminium nitride with 40 DEG C/h slow coolings, under 95KPa and decomposes window temperature 1850
DEG C, kept for half an hour.
Secondary temperature elevation, heats up again under 95KPa pressure, and rise temperature is to 2000 DEG C, by post annealed, by surface column
Shape structure is changed into two-dimensional structure, reduces crystals stress.
1000 DEG C are slow cooling to 30 DEG C/h speed under 95KPa, natural cooling, blow-on, tests characterization.
Lower secondary growth is as seed crystal diauxic growth.The aluminum-nitride single crystal surface nature step is good nucleation substrate.
The present invention using specified temp section alternating temperature transformation in growth course by the way of, early period high pressure low temperature reduction atom into
Core speed, increase nucleation at initial stage regularity reduce substrate decomposition failure, during growth decompression improve growth rate so that sedimentary is covered
Lid substrate, avoids failing, Later growth, heating pressurization, and increase nitrogen source supply, carries out secondary temperature elevation, reduce in crystal after cooling
Portion's stress, face crack healing so that silicon carbide decomposition, obtained from the aluminum-nitride single crystal of the high quality of stripping.
It is described above simply to illustrate that of the invention, it is understood that the invention is not limited in above example, meets
The various variants of inventive concept are within protection scope of the present invention.
Claims (8)
1. a kind of growing method of low stress nitride aluminium crystal, it is characterised in that the growing method includes the following steps：
1) in the early growth period of aluminum nitride crystal, growing environment is vacuumized, and is filled with nitrogen, until air pressure reaches in growing environment
To the first setting pressure, and the first design temperature is raised to the heating rate of 20 DEG C/h-40 DEG C/h, and keeps the temperature half an hour；
2) air pressure in growing environment is dropped into the second setting pressure in the growth medium of aluminum nitride crystal, ten minutes, and
Temperature is stepped up as the second design temperature in two hours, when growth time 8-15 is small；
3) seed crystal face gradient is improved in the Later growth of aluminum nitride crystal, rise crucible position, increase material source is axial to seed crystal
Temperature gradient, pressure is raised to the 3rd setting pressure by air pressure in growing environment；And by the temperature in growing environment in 20 minutes
Degree is increased to the 3rd design temperature, when holding 4 is small；
4) in the growth latter stage of aluminum nitride crystal, with the speed slow cooling of 40 DEG C/h, by growing environment under 95KPa pressure
Temperature drops to 1850 DEG C of the decomposition temperature of aluminium nitride material source, is kept for half an hour；
5) heat up again under 95KPa pressure, the temperature in growing environment is increased to the 4th design temperature；
6) 1000 DEG C are slow cooling to 30 DEG C/h speed under 95KPa pressure, natural cooling, blow-on, tests characterization.
2. the growing method of low stress nitride aluminium crystal according to claim 1, it is characterised in that the first setting pressure
Power is 40KPa.
3. the growing method of low stress nitride aluminium crystal according to claim 1, it is characterised in that the first setting temperature
Spend for 1900 DEG C.
4. the growing method of low stress nitride aluminium crystal according to claim 1, it is characterised in that the second setting pressure
Power is 20KPa.
5. the growing method of low stress nitride aluminium crystal according to claim 1, it is characterised in that the second setting temperature
Spend for 1930-1940 DEG C.
6. the growing method of low stress nitride aluminium crystal according to claim 1, it is characterised in that the 3rd setting pressure
Power is 95KPa.
7. the growing method of low stress nitride aluminium crystal according to claim 1, it is characterised in that the 3rd setting temperature
Spend for 2000 DEG C.
8. the growing method of low stress nitride aluminium crystal according to claim 1, it is characterised in that the 4th setting temperature
Spend for 2000 DEG C.
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| CN107904661B CN107904661B (en) | 2021-04-27 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108642561A (en) * | 2018-07-06 | 2018-10-12 | 中国电子科技集团公司第四十六研究所 | A method of protecting seed crystal face in the growth of aluminum-nitride single crystal |
| CN110098287A (en) * | 2019-03-19 | 2019-08-06 | 华灿光电股份有限公司 | The manufacturing method of AlN template and LED epitaxial slice |
| CN110791811A (en) * | 2019-11-21 | 2020-02-14 | 北京大学 | Method and device for expanding growth of AlN single crystal |
| CN111472045A (en) * | 2020-04-30 | 2020-07-31 | 北京大学 | Aluminum nitride single crystal preparation method based on large-size seed crystals |
| CN111647945A (en) * | 2018-05-18 | 2020-09-11 | 北京华进创威电子有限公司 | Preparation method of aluminum nitride crystal |
| CN113130017A (en) * | 2020-06-05 | 2021-07-16 | 北京世纪金光半导体有限公司 | Crystal growth analysis method and system based on artificial intelligence |
| CN113913749A (en) * | 2021-09-30 | 2022-01-11 | 松山湖材料实验室 | Aluminum nitride film, preparation method thereof and optoelectronic device |
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| CN108642561B (en) * | 2018-07-06 | 2021-01-05 | 中国电子科技集团公司第四十六研究所 | Method for protecting seed crystal surface in growth of aluminum nitride single crystal |
| CN110098287A (en) * | 2019-03-19 | 2019-08-06 | 华灿光电股份有限公司 | The manufacturing method of AlN template and LED epitaxial slice |
| CN110791811A (en) * | 2019-11-21 | 2020-02-14 | 北京大学 | Method and device for expanding growth of AlN single crystal |
| CN111472045A (en) * | 2020-04-30 | 2020-07-31 | 北京大学 | Aluminum nitride single crystal preparation method based on large-size seed crystals |
| CN113130017A (en) * | 2020-06-05 | 2021-07-16 | 北京世纪金光半导体有限公司 | Crystal growth analysis method and system based on artificial intelligence |
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| CN113913749A (en) * | 2021-09-30 | 2022-01-11 | 松山湖材料实验室 | Aluminum nitride film, preparation method thereof and optoelectronic device |
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