CN109989107A - A kind of seed crystal processing method growing high quality SiC crystal - Google Patents
A kind of seed crystal processing method growing high quality SiC crystal Download PDFInfo
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- CN109989107A CN109989107A CN201711475714.8A CN201711475714A CN109989107A CN 109989107 A CN109989107 A CN 109989107A CN 201711475714 A CN201711475714 A CN 201711475714A CN 109989107 A CN109989107 A CN 109989107A
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- 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
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- 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
- C30B29/36—Carbides
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Abstract
The invention discloses a kind of seed crystal processing methods for growing high quality SiC crystal.It is placed in high temperature furnace this method comprises: the SiC seed crystal being bonded in graphite support is placed on crucible; 1750 ~ 1900 DEG C are warming up to after being filled with a certain amount of H2 in Ar protective atmosphere; it can be reacted with SiC and the bonding agent of carbonization using H2 under high temperature; not only seed crystal face scuffing had been eliminated, but also has cleaned the remaining bonding agent for being attached to surface；In addition, SiC seed crystal keeps after a certain period of time slow cooling again at high temperature, the stress that seed crystal is generated by plastic deformation during the bonding process can also be eliminated.Pretreated seed crystal is grown for SiC crystal, and the dislocation density for solving the appearance of crystal growth initial stage sharply increases this technical problem, is laid the foundation to obtain high quality SiC crystal.
Description
Technical field
The invention belongs to technical field of semiconductor material preparation, and it is brilliant to relate generally to a kind of growth high quality silicon carbide (SiC)
The seed crystal processing method of body.
Background technique
With SiC, gallium nitride (GaN) be representative semiconductor material with wide forbidden band, be after silicon (Si), GaAs (GaAs) it
Third generation semiconductor afterwards.Compared with Si and GaAs conventional semiconductor material, SiC has high heat conductance, high breakdown field strength, height full
The advantages that with electronic drifting rate and high bonding energy, excellent properties can satisfy modern electronic technology to high temperature, high frequency, Gao Gong
One of rate and anti-radiation new demand, thus be counted as the most promising material of field of semiconductor materials.Further, since six
Square SiC and GaN lattice constant and similar thermal expansion coefficient, therefore also become manufacture high brightness LED (HB-LED)
Ideal substrate material.
The method of SiC crystal preparation is mainly physical vapor transport (Physical Vapor Transport
Method), growth cell structure is as shown in Figure 1.Temperature in crucible 6 is risen to 2000~2500 DEG C, so that 5 liters of SiC raw material
China, distillation generate gas phase Si2C, SiC2 and Si, and the SiC seed crystal 3 being bonded in graphite support 1 with bonding agent 2 is placed in than SiC original
Expect the low crucible top of 5 temperature, the generated gas phase that distils is transferred to temperature from the surface of raw material under the action of temperature gradient
At lower seed crystal 3, and on seed crystal 3 crystalline at bulk crystals.The growth quality of SiC is mainly by material purity, seed crystal matter
The influence of the factors such as amount, thermal field distribution, growth parameter(s).With advances in technology, the higher raw material of purity is already available to, if
More reasonable thermal field is counted out, growing method condition is also being continued to optimize, and has grown the higher crystalline substance of quality on this basis
Body.
Segmental defect in SiC seed crystal, such as micro-pipe, dislocation and phase transformation have inheritance, are readily extended to subsequent growth
In crystal, thus the quality of seed crystal will have a direct impact on crystal quality, and improving seed crystal quality just becomes the pass improved in crystal quality
One ring of key.Due to the hard brittleness of SiC, surface is easy to produce deep scuffing (damaging layer) in SiC seed crystal process；And in seed crystal
Be bonded in graphite support and follow-up sintering process, surface can also introduce it is deep scratch and bonding agent easy to attach after sintering not
It is easy to completely remove, the deep scuffing and attachment that seed crystal face generates all can induce dislocation defects in subsequent crystallographic growth course
It generates.Further, since the face type of seed crystal and graphite support Incomplete matching, bonding agent seed crystal can be forced to be bonded in graphite support and
Seed crystal is caused to generate deformation, the stress that this deformation generates can form dislocation in subsequent crystallographic growth.
In view of the above technical problems, it does not put forward effective solutions also at present.
Summary of the invention
SiC crystal is grown for current physical vapor transport, increases this technology in early growth period crystal dislocation density
Problem, the invention proposes one kind after SiC seed crystal bonding, the processing method before crystal growth.It, can be with by implementing this method
The deep scratch that chip is processed and bonding process is left in seed crystal face is eliminated, the bonding agent of seed crystal face remnants is removed, reduces seed
The stress that crystalline substance bonding deformation generates, so that the dislocation density for solving the appearance of crystal growth initial stage sharply increases this technical problem.
To achieve the above object, the present invention provides a kind of seed crystal processing method for growing high quality SiC crystal, this method
It include: that will be bonded in seed crystal in graphite support and be placed on crucible to be placed in the good high temperature furnace of leakproofness, heat insulating ability；It is evacuated to 5
It is filled with Ar to 30~50 kPas after pa, then after being evacuated to 5 pas, is passed through H2/Ar gaseous mixture according to a certain percentage；Slowly it is warming up to
1750~1900 DEG C and constant temperature are slowly dropped to room temperature after for a period of time again.
Wherein, high temperature furnace is pyrographite heating furnace or Medium frequency induction coil heats furnace, and heating temperature is not less than 2200 DEG C；
The leakproofness of high temperature furnace is good, and gas leakage in 12 hours is no more than 10 pas.
Further, high temperature furnace thermal insulation property is good, and temperature gradient is less than 5 DEG C/cm at high-temperature region, that is, seed crystal, preferably smaller than
1℃ /cm。
Further, it is passed through H2/Ar mixed gas, mixed proportion is between 0.1~0.5, and preferably 0.2~0.3.Further
Ground, then after being evacuated to 5 pas, is passed through the pressure of H2/Ar gaseous mixture to 5~8 kPas according to a certain percentage, and preferably 7~8 kPas.
Further, slow temperature-rise period needs 3~5 hours.
Further, the maximum temperature slowly to heat up is at 1750~1900 DEG C, and preferably 1800~1850 DEG C.
Further, 1750~1900 DEG C and constant temperature 5~8 hours are slowly warming up to.
Further, constant temperature was cooled to room temperature with 10~20 hours afterwards for a period of time.
The present invention is the SiC seed crystal table after etching bonding at 1750~1900 DEG C by introducing H2 in Ar protective atmosphere
Face can be reacted with the bonding agent and SiC of carbonization at high temperature using H2, not only clean and be attached to wafer surface
Remaining bonding agent, and wafer surface surface damage layer is eliminated, obtain atomic flat surface；In addition, at high temperature
It anneals to the seed crystal after bonding, stress caused by seed crystal plastic deformation caused by effectively eliminating because of bonding.By implementing to be somebody's turn to do
Method effectively avoids early growth period crystal dislocation from increased dramatically this problem, and the SiC crystal for long high quality of making a living provides safeguard.
Detailed description of the invention
Fig. 1 is growth room's structural schematic diagram of physical vapor transport growth SiC crystal；Wherein, 1, seed crystal support (graphite
Support)；2, bonding agent；3, SiC seed crystal；4, SiC raw material distillation steam；5, SiC raw material；6, graphite external member.
Fig. 2 is the seed crystal structural schematic diagram being bonded in graphite support to high temperature etching；
Fig. 3 is bonded in the structural schematic diagram that the seed crystal in graphite support is placed on crucible.
Specific embodiment
Referring to the drawings, seed crystal preprocess method increased dramatically with to solve SiC crystal early growth period dislocation density and asks
Topic elaborates.
Fig. 1 is the growth room's structural schematic diagram for the physical vapor transport growth SiC crystal being commonly used.Wherein stone
Black crucible 6 and graphite support 1 are formed with three high machining graphites；In crystal growing process, temperature highest at SiC raw material 5 is former
Material, which decomposes, generates SiC gaseous substance 4, and the temperature of 3 position of seed crystal is set as lower than SiC raw material 5, i.e., SiC gaseous substance 4 exists
Reach supersaturation at seed crystal 3 and crystallizes.The SiC gaseous substance 4 that thus SiC raw material 5 generates continually crystallizes at seed crystal 3,
To which growth obtains SiC crystal.
Fig. 2 is the seed crystal structural schematic diagram being bonded in graphite support to high temperature etching.The step of seed crystal bonds are as follows: in stone
The inner surface of black support 1 uniformly applies one layer of bonding agent 2, also uniformly applies one layer of bonding agent 2 in the adhesive surface of seed crystal 3, the two is bonded
Face is stacked together, and then heating a period of time allows bonding agent 2 to solidify under heater, to avoid growing in SiC crystal
Seed crystal 3 falls off from graphite support 1 in journey.Since SiC is hard brittle material, seed crystal 3 is in cutting, grinding and polishing process, seed crystal 3
Aufwuchsplate is easy to produce scuffing (damaging layer), and also can be in seed crystal when cleaning seed crystal face after bonding, sintering process and sintering
Face, which introduces, to be scratched.Scratch this means that seed crystal regional area because caused by mechanical stress lattice it is imperfect, grown in subsequent crystallographic
When be readily incorporated dislocation defects.In addition, when carrying out cleaning seed crystal 3 after sintering, can still have on surface it is a small amount of do not clean it is dry
Net bonding agent 2, these bonding agents 2 form wrappage in subsequent growth, and then derive dislocation.Finally, although we select
The good seed crystal 3 of flatness and graphite support 1 (flatness is both less than 10 μm), but bond and will can form between the two rigid connection, two
Person's flatness difference can make seed crystal 3 occur plastic deformation, if deformational stress do not eliminate will subsequent growth can generate dislocation lack
It falls into.It above may be the main reason for crystal growth initial stage dislocation density is significantly increased compared with seed crystal.
To avoid the occurrence of the above problem, it is proposed that carrying out high temperature to seed crystal 3 before SiC crystal growth after the bonding of seed crystal 3
Etching processing.First by after bonding seed crystal 3 and graphite support 1 be put on graphite crucible 6 together, as shown in Figure 3；Then by crucible
It is placed in the good high-temperature heater of leakproofness, heat insulating ability, by being evacuated the residual air filled in Ar reduction furnace；After being evacuated again so
After be filled with a certain amount of H2/Ar gaseous mixture, and be warming up to 1750~1900 DEG C, drop to room temperature again after being kept for a period of time.Due to
H2 can be reacted with SiC at high temperature, and mechanical stress region, that is, seed crystal scratches region, be easier because lattice defect is more and H2
It reacts, thus is passed through H2 to eliminate lattice mismatch caused by SiC seed crystal 3 scratches, and then reduce the crystal of late growth
In the dislocation defects probability for scratching region generation；H2 is also reacted with carbon under high temperature, the bonding agent 2 of the carbonization remained on surface of seed crystal 3
Production hydrocarbon is reacted with H2, to avoid residual bonding agent insertion Crystallization package after the carbonization of growth course initial stage
Object, and then induce dislocation defects；Using high temperature etched seed under the conditions of H2, slowly in order to avoid seed crystal heat-shock when heating
Too big and damaged, holding time enough is to allow the 3 surface scratch region of bonding agent and seed crystal of H2 and carbonization at high temperature
Sufficiently reaction, while can also thoroughly eliminate seed crystal 3 and generate stress because of plastic deformation during the bonding process, and use temperature ladder
Spend small heat-retaining condition and slow cooling be then in order to avoid seed crystal 3 newly generates stress in subsequent temperature-fall period, it is newly generated
Stress also can in subsequent growth product dislocation.It is grown by the seed crystal that this method is handled for SiC crystal, can effectively avoid crystalline substance
Body early growth period dislocation density sharply increases this technical problem.
Embodiment 1
Be bonded in graphite support 14 inches of SiC seed crystals 3 are placed on crucible 5 and are placed in leakproofness and the good high temperature of heat insulating ability
In graphite heater furnace, Ar to 30 kPas is filled with after being evacuated to 5 pas；It is evacuated down to 5 pas again, is passed through H2/Ar=0.1 gaseous mixture extremely
5 kPas；It was warming up to after 1750 DEG C, constant temperature 8 hours with 3 hours and was down to room temperature with 10 hours.
Embodiment 2
Be bonded in graphite support 16 inches of conduction SiC seed crystals 3 are placed on crucible 5 and are placed in leakproofness and heat insulating ability is good
In high temperature Medium Frequency Induction Heating Furnace, 5 pas are evacuated to, are filled with Ar to 50 kPas；It is evacuated down to 5 pas again, is passed through H2/Ar=0.3
Gaseous mixture is to 8 kPas；It was warming up to after 1850 DEG C, constant temperature 7 hours with 4 hours and was down to room temperature with 15 hours.
Embodiment 3
Be bonded in graphite support 16 inches of conduction SiC seed crystals 3 are placed on crucible 5 and are placed in leakproofness and heat insulating ability is good
In high temperature Medium Frequency Induction Heating Furnace, 5 pas are evacuated to, are filled with Ar to 40 kPas；It is evacuated down to 5 pas again, is passed through H2/Ar=0.2
Gaseous mixture is to 8 kPas；It was warming up to after 1800 DEG C, constant temperature 8 hours with 4 hours and was down to room temperature with 12 hours.
Embodiment 4
Be bonded in graphite support 14 inches of SiC seed crystals 3 are placed on crucible 5 and are placed in leakproofness and the good high temperature of heat insulating ability
In graphite heater furnace, Ar to 30 kPas is filled with after being evacuated to 5 pas；It is evacuated down to 5 pas again, is passed through H2/Ar=0.5 gaseous mixture extremely
6 kPas；It was warming up to after 1900 DEG C, constant temperature 5 hours with 5 hours and was down to room temperature with 20 hours.
Claims (14)
1. a kind of seed crystal processing method for growing high quality SiC crystal, this method is used to improve physical vapor transport growth
SiC single crystal quality, comprising: seed crystal in graphite support will be bonded in be placed on crucible and be placed in the good high temperature of leakproofness, heat insulating ability and move back
In stove；It is filled with 30 ~ 50 kPas of Ar after being evacuated to 5 pas or less, then is evacuated to 5 pas or less and is passed through a certain amount of H in proportion2/
Ar gaseous mixture；1750 DEG C ~ 1900 DEG C are to slowly warm up to, constant temperature is slowly dropped to room temperature afterwards for a period of time.
2. high-temperature annealing furnace as described in claim 1 is graphite heater furnace or Medium frequency induction coil heats furnace, heating temperature is not
Lower than 2200 DEG C.
3. high-temperature annealing furnace leakproofness as described in claim 1 is good, gas leakage in 12 hours is no more than 10 pas.
4. high-temperature annealing furnace thermal insulation property as described in claim 1 is good, in high annealing seed crystal, at high-temperature region, that is, seed crystal
Temperature gradient is less than 5 DEG C/cm.
5. high-temperature annealing furnace thermal insulation property as claimed in claim 4 is good, in high annealing seed crystal, at high-temperature region, that is, seed crystal
Temperature gradient is less than 1 DEG C/cm.
6. being evacuated to 5 pas again hereinafter, being passed through H as described in claim 12/ Ar ratio of gas mixture is between 0.1 ~ 0.5.
7. being evacuated to 5 pas again hereinafter, being passed through H as claimed in claim 62/ Ar ratio of gas mixture is between 0.2 ~ 0.3.
8. being passed through H after being evacuated to 5 pas or less again as described in claim 12Pressure after/Ar mixed gas in furnace is at 5 ~ 8 kPas.
9. being passed through H after being evacuated to 5 pas or less again as claimed in claim 82Pressure after/Ar mixed gas in furnace is at 7 ~ 8 kPas.
10. being bonded in seed crystal in graphite support as described in claim 1 need to slowly heat up, the heating-up time was at 3 ~ 5 hours.
11. being bonded in seed crystal in graphite support is warming up to 1750 DEG C ~ 1900 DEG C as described in claim 1.
12. being bonded in seed crystal in graphite support is warming up to 1800 DEG C ~ 1850 DEG C as claimed in claim 11.
13. the seed crystal being bonded in graphite support as described in claim 1 needs after being to slowly warm up to 1750 DEG C ~ 1900 DEG C
For a period of time, constant temperature time was at 5 ~ 8 hours for constant temperature.
14. the seed crystal constant temperature being bonded in graphite support as described in claim 1 is slowly dropped to room temperature, temperature fall time afterwards for a period of time
It is 10 ~ 20 hours.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113529171A (en) * | 2021-07-01 | 2021-10-22 | 山东天岳先进科技股份有限公司 | Seed crystal with high surface cleanliness and cleaning method thereof |
| CN114134576A (en) * | 2021-12-02 | 2022-03-04 | 中国电子科技集团公司第四十六研究所 | Seed crystal processing method for low dislocation density CdS single crystal growth |
| CN114574956A (en) * | 2022-03-09 | 2022-06-03 | 北京世纪金光半导体有限公司 | Growth method and growth device of doped aluminum nitride crystal |
| CN115627522A (en) * | 2022-12-12 | 2023-01-20 | 北京青禾晶元半导体科技有限责任公司 | Method for improving crystal growth quality |
| CN116837456A (en) * | 2023-07-17 | 2023-10-03 | 江苏超芯星半导体有限公司 | Seed crystal treatment method and silicon carbide crystal growth method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113529171A (en) * | 2021-07-01 | 2021-10-22 | 山东天岳先进科技股份有限公司 | Seed crystal with high surface cleanliness and cleaning method thereof |
| CN113529171B (en) * | 2021-07-01 | 2022-08-02 | 山东天岳先进科技股份有限公司 | Seed crystal with high surface cleanliness and cleaning method thereof |
| CN114134576A (en) * | 2021-12-02 | 2022-03-04 | 中国电子科技集团公司第四十六研究所 | Seed crystal processing method for low dislocation density CdS single crystal growth |
| CN114574956A (en) * | 2022-03-09 | 2022-06-03 | 北京世纪金光半导体有限公司 | Growth method and growth device of doped aluminum nitride crystal |
| CN114574956B (en) * | 2022-03-09 | 2024-02-09 | 北京世纪金光半导体有限公司 | Growth method and growth device of doped aluminum nitride crystal |
| CN115627522A (en) * | 2022-12-12 | 2023-01-20 | 北京青禾晶元半导体科技有限责任公司 | Method for improving crystal growth quality |
| CN116837456A (en) * | 2023-07-17 | 2023-10-03 | 江苏超芯星半导体有限公司 | Seed crystal treatment method and silicon carbide crystal growth method |
| CN116837456B (en) * | 2023-07-17 | 2024-02-23 | 江苏超芯星半导体有限公司 | Seed crystal treatment method and silicon carbide crystal growth method |
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Application publication date: 20190709 |