CN109183143A - A method of AlN single crystal purity is improved using reducing gas - Google Patents

A method of AlN single crystal purity is improved using reducing gas Download PDF

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Publication number
CN109183143A
CN109183143A CN201811196690.7A CN201811196690A CN109183143A CN 109183143 A CN109183143 A CN 109183143A CN 201811196690 A CN201811196690 A CN 201811196690A CN 109183143 A CN109183143 A CN 109183143A
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furnace body
temperature
gas
aln
purity
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CN109183143B (en
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于彤军
赵起悦
吴洁君
朱星宇
李孟达
韩彤
沈波
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Peking University
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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
    • C30B23/02—Epitaxial-layer growth
    • 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

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  • 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 methods for improving AlN single crystal purity using reducing gas, using gently mixing reactive atmosphere technology, at high temperature with the active gases compared with strong reducing property as atmosphere；Powder purification and crystal growth stage in physical vapor transport, are passed through micro active gases step by step and are gently mixed；In heating powder purification phase and high temperature crystal growth stage, with impurity element reduction reaction occurs for active gases at high temperature, to remove impurity element, growth obtains high-purity AlN crystal.Using technical solution of the present invention, reduce time and cost, so that impurity content is decreased obviously in AlN monocrystalline, to improve the optical quality of AlN substrate, extends the application of AlN crystal.

Description

A method of AlN single crystal purity is improved using reducing gas
Technical field
The present invention relates to technical field of crystal growth more particularly to a kind of AlN single crystal purity is improved using reducing gas Method.
Background technique
AlN monocrystalline can significantly improve outer because its lattice constant and thermal expansion coefficient and high Al contents AlGaN are very close Prolong a layer lattice quality, reduces defect concentration to improve the internal quantum efficiency of device and have become epitaxial growth AlGaN at present Make the best substrate of deep ultraviolet device, including deep ultraviolet LED and deep ultraviolet detector.Meanwhile AlN monocrystalline is with many excellent Point, including high breakdown field strength, high heat conductance, high rigidity, electric property are excellent etc., this makes it in high-temperature high-frequency power electronic device Also it can play the part of important role in part.The AlN monocrystalline of high quality is obtained, successfully realizes large scale AlN monocrystalline in the world at present Growing method be physical carbon burdening (PVT method).The equipment of PVT growing AIN mainly have graphite furnace induction heating system and Tungsten furnace resistive heating system, basic principle is all that the source AlN powder distils at crucible bottom high temperature, by transporting in crucible top It is crystallized at low temperature.Correspondingly, in graphite induction furnace, SiC seed crystal hetero-epitaxy AlN, or in tungsten resistance furnace, homoepitaxy Growing AIN monocrystalline, mostly generation are eliminated and obtain the AlN monocrystalline of high quality, and the core of this route is how to improve crystal quality；Two It is in tungsten resistance furnace, spontaneous nucleation obtains the AlN single crystal seed that a size is smaller but is of high quality, and then homoepitaxy obtains To AlN monocrystalline, the core of this route is how to expand crystalline size.
Currently, existing research group can obtain the lower 2 inches of high quality of dislocation density by PVT method in the world AlN monocrystalline, but wherein impurity content is high, includes mainly O, C, Si, based on O impurity.The growth temperature of AlN is up in PVT method 2000 DEG C, in this hot environment, the impurity in the powder of source and in atmosphere will be decomposed, very active, be easy to happen reaction, Primarily form AlxOyAnd AlON, it can further be incorporated to AlN lattice.The introduced impurity of these processes can introduce in AlN energy band Defect level causes serious light absorption, and it is unfavorable to prepare to photoelectric device.The purity for how improving AlN seed crystal has become AlN One of main task in single crystalline substrate development.
Summary of the invention
In order to overcome the above problem, the present invention provides a kind of method for improving AlN single crystal purity using reducing gas, can Impurity content in AlN crystal is effectively reduced, and, to improve its purity, the AlN single crystal purity being prepared is high.
The core that the preparation method is different from the prior art is: the powder in physical vapor transport method (PVT method) Purifying and crystal growth stage, it is passed through trace active gas step by step, has for (1500 DEG C or more) at high temperature using active gases There is the characteristic of stronger reproducibility, in heating powder purification phase and high temperature crystal growth stage, active gases and impurity element It reacts, generates the corresponding oxide of active gases (such as protium reduction oxygen element obtains hydrone), these oxides exist It is not easy deposition under high temperature and is incorporated to lattice, but as air-flow leaves crucible, to achieve the purpose that remove major impurity O element. Active gases includes but is not limited to methane, ammonia, hydrogen, acetylene etc. and its mixed gas, and methane, acetylene, ammonia are in reaction chamber At a high temperature of can crack, can all generate hydrogen, hydrogen further functions as the effect of reduction oxygen element.It is grown using the method High-purity AlN monocrystalline is needed according to PVT equipment different heating mode and different stages of growth, and active gas is specifically gently mixed in adjustment Atmosphere composition, concentration and Optimal Temperature, to guarantee to purify in powder and the crystal growth stage, ambiance, crucible surface, heating and Heat insulation material surface, impurity element effectively removes inside powder and in sublimation gases, while micro active gases again will not Adverse effect is caused to hot-zone material and material powder.In the whole process, the applicable temperature range 1500-2500 of this method DEG C, the mass concentration ratio that reactive atmosphere accounts for total atmosphere is 10~10000ppm.
Present invention provide the technical scheme that
A method of AlN single crystal purity being improved using reducing gas, in physical vapor transport method (PVT method) Powder purification and crystal growth stage, it is passed through trace active gas (atmosphere) step by step and is gently mixed；The active gases is at high temperature (1500 DEG C or more) have stronger reproducibility；Exist in heating powder purification phase and high temperature crystal growth stage, active gases Reduction reaction occurs with impurity element under high temperature, to remove impurity element, growth obtains high-purity AlN crystal；Temperature range It is 1500-2500 DEG C；The mass concentration ratio that reactive atmosphere accounts for total atmosphere is 10~10000ppm.
The method provided by the invention for preparing AlN monocrystalline specifically comprises the following steps:
1) furnace body, which fills, substitutes gas:
The crucible equipped with raw material (high-purity source AlN powder) is placed to furnace body and closed furnace body, furnace body environment is vacuumized To 1Torr, and high pure nitrogen is filled to 500Torr, so fill in pumping displacement cavity atmosphere 3~5 times, vacuumize for last 1 time and to reach 10-4Torr；
2) furnace body inflates pressure maintaining:
After stopping vacuumizes furnace body, the height of high pure nitrogen or certain proportion (range is 0.1~0.9) is passed through into furnace body Pure nitrogen gas/high-purity argon gas mixed gas, formed ambiance, and make cavity total pressure keep stablize, pressure range be 10~ 900Torr；
3) furnace body heats up:
It selects suitable temperature gradient (1~20 DEG C/min) to heat up, and pressure is kept to stablize；
4) it is passed through trace active gas:
After temperature rises to > 1300 DEG C, opens micro flowmeter and be continually fed into trace active gas, active gas into furnace body Body is selected according to furnace interior material, including but not limited to one of methane, ammonia, hydrogen, acetylene etc. or wherein A variety of mixed gas, the mass concentration for gently mixing active gases are controlled in 10~10000ppm；
5) powder purifying/crystal growth phase:
According to the difference of growth purpose, temperature is increased to and is stabilized to setting value, wherein powder cleansing temp 1500-2000 DEG C, purification time needs to be adjusted according to powder source quality and growth, it is proposed that time range 1-48 hours；Crystal growth temperature 1800-2500 DEG C, growth time can according to growth it needs to be determined that, may generally be 4-96 hours；
6) temperature-fall period:
After powder purifying/crystal growth is completed, start that suitable temperature gradient (1~20 DEG C/min) is selected to be dropped Temperature.After temperature drops to < 1300 DEG C, closes micro flowmeter stopping and be passed through trace active gas；
7) blow-on samples:
After furnace body drops to room temperature, it is evacuated down to 1Torr, subsequent inflated with nitrogen to 500Torr so fills gas in pumping displacement cavity Atmosphere 3~5 times, last 1 inflated with nitrogen to normal pressure.Then crucible is taken out in blow-on.
Through the above steps, that is, high-purity AlN crystal is prepared.
Compared with prior art, the beneficial effects of the present invention are:
The present invention provides a kind of method for improving AlN single crystal purity using reducing gas, is that AlN crystal is effectively reduced in one kind Middle impurity content improves the processing technique scheme of its purity, improves AlN single crystalline substrate purity.Its advantage is that: first, by gently mixing Active gases can reduce in the powder of source in the processing of source powder and when growth and introduce the miscellaneous of crystal in impurity content and growth course Matter content；Second, do not need longer growth cycle, it is only necessary to which the AlN single crystalline substrate of high-purity can be obtained in a secondary growth, sufficiently Reduce time and cost.
In powder purification phase and micro reactive atmosphere is passed through in the high temperature crystal growth stage, it can powder is effectively reduced The impurity content of body purification phase and high temperature crystal growth stage, while safety and practicability are preferable.Pass through this skill Art means can be such that impurity content in AlN monocrystalline is decreased obviously, to improve the optical quality of AlN substrate, extend AlN crystal application.
Detailed description of the invention
Fig. 1 is that the basic of furnace body used in reactive atmosphere technology preparation high-purity AlN monocrystalline is gently mixed in use of the embodiment of the present invention Structure；
Wherein, 1 is furnace body shell, good airproof performance, it is ensured that vacuum degree, gas pressure intensity and atmosphere purity；2 is in furnace bodies Atmosphere, in experiment based on high pure nitrogen or the mixing of high pure nitrogen argon gas；3 be heating and insulating sections, and graphite is incuded Heating system, 3 be graphite crucible and graphite insulating layer, and for tungsten resistive heating system, 3 be heat preservation tungsten screen；4 be tantalum carbide earthenware Crucible or tungsten crucible；5 be high-purity AlN powder；6 be gas access, can input high pure nitrogen, high-purity argon gas and trace active gas Body；7 be gas vent, is evacuated by dry pump and molecular pump, is regulated and controled by vacuum valve.
Fig. 2 is the embodiment of the present invention using the flow diagram for gently mixing reactive atmosphere technology preparation high-purity AlN monocrystalline.
Specific embodiment
With reference to the accompanying drawing, the present invention, the model of but do not limit the invention in any way are further described by embodiment It encloses.
Fig. 1 is that the basic of furnace body used in reactive atmosphere technology preparation high-purity AlN monocrystalline is gently mixed in use of the embodiment of the present invention Structure.It is reaction zone in crucible, calandria provides the high temperature more than 2000 degrees Celsius for crucible, and insulating layer guarantees that high temperature continues simultaneously Certain temperature gradient is formed, the requirement of crystal growth temperature-field distribution is met.Crucible and outer layer heat tracing zone are not completely close Envelope, air-flow can pass through at gap.Dry pump and molecular pump can vacuumize and keep certain vacuum degree, while logical When entering nitrogen, vacuum pump work enables furnace gas to replace, and guarantees that pressure is stablized.During the experiment, nitrogen keeps logical Enter and maintain pressure, trace active gas is continually fed into moment.
Fig. 2 is the embodiment of the present invention using the flow diagram for gently mixing reactive atmosphere technology preparation high-purity AlN monocrystalline.
One graphite furnace of embodiment purifies AlN powder (using methane or acetylene)
1) furnace body, which fills, substitutes gas:
The carbonization tantalum crucible equipped with high-purity source AlN powder is placed to furnace body and closed furnace body, furnace body environment is vacuumized To 1Torr, and high pure nitrogen is filled to 500Torr, so fill in pumping displacement cavity atmosphere 3~5 times, vacuumize for last 1 time and to reach 10-4Torr；
2) furnace body inflates pressure maintaining:
After stopping vacuumizes furnace body, the High Purity Nitrogen that high pure nitrogen or proportional region are 0.1~0.9 is passed through into furnace body Gas/high-purity argon gas mixed gas, formed ambiance, and make cavity total pressure keep stablize, pressure range be 10~ 900Torr；
3) furnace body heats up:
It selects suitable temperature gradient (1~20 DEG C/min) to heat up, and pressure is kept to stablize；
4) it is passed through trace active gas:
After temperature rises to > 1300 DEG C, opens micro flowmeter and be continually fed into trace active gas, active gas into furnace body Body includes but is not limited to one of methane, acetylene or many of mixed gas, gently mixes the mass concentration of active gases Control is in 10~10000ppm；
5) powder purifies:
Temperature is increased to and is stabilized to setting value, 1500-2000 DEG C of powder cleansing temp, purification time is according to powder source quality It needs to be adjusted with growth, it is proposed that time range 1-48 hours；
6) temperature-fall period:
After powder purifying is completed, start that suitable temperature gradient (1~20 DEG C/min) is selected to cool down.At a temperature of After dropping to < 1300 DEG C, closes micro flowmeter stopping trace active gas and be passed through；
7) blow-on samples:
After furnace body drops to room temperature, it is evacuated down to 1Torr, subsequent inflated with nitrogen to 500Torr so fills gas in pumping displacement cavity Atmosphere 3~5 times, last 1 inflated with nitrogen to normal pressure.Then crucible is taken out in blow-on.
Two graphite furnace growing AIN monocrystalline of embodiment (using methane or acetylene)
1) furnace body, which fills, substitutes gas:
The carbonization tantalum crucible equipped with AlN sintered body is placed to graphite furnace body and closed furnace body, furnace body environment take out true Sky arrives 1Torr, and fills high pure nitrogen to 500Torr, so fills pumping and replaces in cavity atmosphere 3~5 times, vacuumizes for last 1 time and to reach To 10-4Torr；
2) furnace body inflates pressure maintaining:
After stopping vacuumizes furnace body, the High Purity Nitrogen that high pure nitrogen or proportional region are 0.1~0.9 is passed through into furnace body Gas/high-purity argon gas mixed gas, formed ambiance, and make cavity total pressure keep stablize, pressure range be 10~ 900Torr；
3) furnace body heats up:
It selects suitable temperature gradient (1~20 DEG C/min) to heat up, and pressure is kept to stablize；
4) it is passed through trace active gas:
After temperature rises to > 1300 DEG C, opens micro flowmeter and be continually fed into trace active gas, active gas into furnace body Body includes but is not limited to one of methane, ammonia, hydrogen, acetylene etc. or many of mixed gas, gently mixes active gas The mass concentration of body is controlled in 10~10000ppm；
5) crystal growth:
Temperature is increased to and is stabilized to setting value, 1800-2500 DEG C of crystal growth temperature, growth time is according to growth needs It is adjusted, it is proposed that time range 4-96 hours；
6) temperature-fall period:
After crystal growth is completed, start that suitable temperature gradient (1~20 DEG C/min) is selected to cool down.At a temperature of After dropping to < 1300 DEG C, closes micro flowmeter stopping trace active gas and be passed through；
7) blow-on samples:
After furnace body drops to room temperature, it is evacuated down to 1Torr, subsequent inflated with nitrogen to 500Torr so fills gas in pumping displacement cavity Atmosphere 3~5 times, last 1 inflated with nitrogen to normal pressure.Then crucible is taken out in blow-on.
Three tungsten furnace growing AIN monocrystalline of embodiment (using ammonia or hydrogen)
1) furnace body, which fills, substitutes gas:
The tungsten crucible equipped with AlN sintered body is placed to tungsten furnace body and closed furnace body, furnace body environment is evacuated down to 1Torr, and fill high pure nitrogen to 500Torr, so fills in pumping displacement cavity atmosphere 3~5 times, vacuumizes for last 1 time and to reach 10- 4Torr；
2) furnace body inflates pressure maintaining:
After stopping vacuumizes furnace body, the High Purity Nitrogen that high pure nitrogen or proportional region are 0.1~0.9 is passed through into furnace body Gas/high-purity argon gas mixed gas, formed ambiance, and make cavity total pressure keep stablize, pressure range be 10~ 900Torr；
3) furnace body heats up:
It selects suitable temperature gradient (1~20 DEG C/min) to heat up, and pressure is kept to stablize；
4) it is passed through trace active gas:
After temperature rises to > 1300 DEG C, opens micro flowmeter and be continually fed into trace active gas, active gas into furnace body Body includes one of ammonia, hydrogen or its mixed gas, gently mix the mass concentration control of active gases 10~ 10000ppm；
5) crystal growth:
Temperature is increased to and is stabilized to setting value, 1800-2500 DEG C of crystal growth temperature, growth time is according to growth needs It is adjusted, it is proposed that time range 4-96 hours；
6) temperature-fall period:
After crystal growth is completed, start that suitable temperature gradient (1~20 DEG C/min) is selected to cool down.At a temperature of After dropping to < 1300 DEG C, closes micro flowmeter stopping trace active gas and be passed through；
7) blow-on samples:
After furnace body drops to room temperature, it is evacuated down to 1Torr, subsequent inflated with nitrogen to 500Torr so fills gas in pumping displacement cavity Atmosphere 3~5 times, last 1 inflated with nitrogen to normal pressure.Then crucible is taken out in blow-on.
It should be noted that the purpose for publicizing and implementing example is to help to further understand the present invention, but the skill of this field Art personnel, which are understood that, not to be departed from the present invention and spirit and scope of the appended claims, and various substitutions and modifications are all It is possible.Therefore, the present invention should not be limited to embodiment disclosure of that, and the scope of protection of present invention is with claim Subject to the range that book defines.

Claims (10)

1. a kind of method for improving AlN single crystal purity using reducing gas, using gently reactive atmosphere technology is mixed, to have at high temperature There is the active gases compared with strong reducing property as atmosphere；Powder purification and crystal growth stage in physical vapor transport, substep Micro active gases is passed through gently to be mixed；In heating powder purification phase and high temperature crystal growth stage, active gases is in height Temperature is lower and reduction reaction occurs for impurity element, to remove impurity element, growth obtains high-purity AlN crystal；Including walking as follows It is rapid:
1) furnace body, which fills, substitutes gas:
The crucible equipped with high-purity source AlN powder is placed to furnace body and closed furnace body, furnace body environment is vacuumized, and fill High Purity Nitrogen Gas；Atmosphere in pumping displacement cavity is so repeatedly filled, so that furnace body reaches vacuum environment；
2) furnace body inflates pressure maintaining:
After stopping vacuumizes furnace body, the mixed of high pure nitrogen or a certain proportion of high pure nitrogen and high-purity argon gas is passed through into furnace body Gas is closed, ambiance is formed, and cavity total pressure is made to keep stablizing；
3) furnace body heats up:
Temperature gradient is selected, is heated up, and pressure is kept to stablize；
4) it is passed through trace active gas:
After temperature rises to greater than 1300 DEG C, micro flowmeter is opened, trace active gas is continually fed into furnace body；Control is light Mix the mass concentration ratio that reactive atmosphere accounts for total atmosphere；
5) temperature is increased to and is stabilized to setting value according to different growth purposes in powder purifying/crystal growth phase, and Maintain certain time；
6) temperature-fall period:
After powder purifying/crystal growth is completed, temperature gradient is selected to cool down；After temperature drops to less than 1300 DEG C, It closes micro flowmeter stopping and is passed through trace active gas；
7) blow-on samples:
It after furnace body drops to room temperature, is vacuumized, then fills high pure nitrogen；The pumping displacement intracorporal atmosphere of chamber is so repeatedly filled, most Afterwards high pure nitrogen is filled to normal pressure 1 time；Then crucible is taken out in blow-on；
Through the above steps, that is, high-purity AlN crystal is prepared.
2. the method as described in claim 1, characterized in that the temperature range of preparation process is 1500-2500 DEG C.
3. the method as described in claim 1, characterized in that in step 4), reactive atmosphere accounts for the mass concentration ratio of total atmosphere For 10~10000ppm.
4. the method as described in claim 1, characterized in that step 1) furnace body, which fills, substitutes gas, specifically: first to furnace body environment It carries out being evacuated down to 1Torr, and fills high pure nitrogen to 500Torr, so fill in pumping displacement cavity atmosphere 3~5 times, finally take out true Sky reaches 10-4Torr。
5. the method as described in claim 1, characterized in that step 2) furnace body inflates pressure maintaining, is specifically passed through into furnace body high-purity Nitrogen/high-purity argon gas mixed gas forms ambiance；The ratio of mixed gas is 0.1~0.9.
6. the method as described in claim 1, characterized in that step 2) furnace body inflates pressure maintaining, so that the range of cavity total pressure For 10~900Torr.
7. the method as described in claim 1, characterized in that in step 3) furnace body temperature-rise period, the temperature gradient that selects for 1~ 20℃/min。
8. the method as described in claim 1, characterized in that active gases is selected according to furnace interior material, including but It is not limited to one of methane, ammonia, hydrogen, acetylene or in which a variety of mixed gas.
9. the method as described in claim 1, characterized in that temperature is increased and be stabilized to setting value by step 5), it is preferable that powder Body cleansing temp is 1500-2000 DEG C, and purification time is 1-48 hours, and crystal growth temperature is 1800-2500 DEG C, growth time It is 4-96 hours；Temperature range can be adjusted according to heating method.
10. the method as described in claim 1, characterized in that in step 6) temperature-fall period, selecting suitable temperature gradient is 1 ~20 DEG C/min；And/or in step 7) blow-on sampling process, specifically after furnace body drops to room temperature, it is evacuated down to 1Torr, then Inflated with nitrogen so fills in pumping displacement cavity atmosphere 3~5 times, final inflated with nitrogen to normal pressure to 500Torr.
CN201811196690.7A 2018-10-15 2018-10-15 Method for improving AlN single crystal purity by using reducing gas Active CN109183143B (en)

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CN110015648A (en) * 2019-03-28 2019-07-16 北京中材人工晶体研究院有限公司 A kind of high-purity aluminium nitride powder and aluminium nitride powder method of purification
CN113005518A (en) * 2021-02-23 2021-06-22 哈尔滨工业大学 Method for preparing silicon carbide single crystal
CN114921849A (en) * 2022-06-08 2022-08-19 中材人工晶体研究院(山东)有限公司 Method for growing silicon carbide crystal by PVT (physical vapor transport) method

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Publication number Priority date Publication date Assignee Title
CN110015648A (en) * 2019-03-28 2019-07-16 北京中材人工晶体研究院有限公司 A kind of high-purity aluminium nitride powder and aluminium nitride powder method of purification
CN110015648B (en) * 2019-03-28 2021-05-04 中材人工晶体研究院有限公司 High-purity aluminum nitride powder and aluminum nitride powder purification method
CN113005518A (en) * 2021-02-23 2021-06-22 哈尔滨工业大学 Method for preparing silicon carbide single crystal
CN114921849A (en) * 2022-06-08 2022-08-19 中材人工晶体研究院(山东)有限公司 Method for growing silicon carbide crystal by PVT (physical vapor transport) method

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