CN107955969A - A kind of SiC single crystal growing system being persistently fed - Google Patents
A kind of SiC single crystal growing system being persistently fed Download PDFInfo
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- CN107955969A CN107955969A CN201711465087.XA CN201711465087A CN107955969A CN 107955969 A CN107955969 A CN 107955969A CN 201711465087 A CN201711465087 A CN 201711465087A CN 107955969 A CN107955969 A CN 107955969A
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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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- 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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Abstract
The present invention relates to a kind of SiC single crystal growing system being persistently fed, mainly include：Growth furnace, crucible and transmission device, wherein, the crucible includes：Upper crucible and lower crucible, wherein, the upper crucible is fixed on the top of furnace chamber, and the top on described in crucible is fixed with seed crystal；The lower crucible is located at the lower part of furnace chamber, SiC powders are equipped with the lower crucible, and multiple lower crucibles are respectively arranged on the transmission device, the top that the multiple lower crucible is alternately risen to furnace chamber by the transmission device is connected with the upper crucible, carries out the lasting replacement of the SiC powders.Crucible is separated into two parts up and down by the present invention, seed crystal is fixed on top, lower part fills powder, crystal growth is to after certain phase, the powder consumed using the carbonization of transmission device lower part is substituted for new powder, powder can be replaced constantly in crystal growing process, realize the continuous growth and the reduction of C wrappages of crystal.
Description
Technical field
The invention belongs to SiC single crystal growing technology field, and in particular to a kind of SiC single crystal growing system being persistently fed.
Background technology
SiC is as wide bandgap semiconductor materials with its high energy gap（For 3 times of Si）, high breakdown critical field strength
（About the 9 of Si times）, high electronics saturation drift velocity（For 2 times of Si）And high heat conductance（About the 3 of Si times）, small dielectric is normal
Number, and capability of resistance to radiation is strong, the solid characteristic such as wear-resistant and as making high frequency, high-power, high temperature resistant and radioresistance device
Ideal material.Thus as one of current widely studied material.In terms of SiC single crystal growing technology, lead in the world at present
To use physical vapor transport（PVT）SiC single crystal is grown, its cardinal principle is the distillation at high temperature of Si-C systems and ties again
It is brilliant.The thermodynamical equilibrium process of gas phase species carries out research discovery in Si-C systems, the dominant species in SiC growth systems
For Si, Si2C, SiC2, in the range of certain crystal growth required temperature, the partial pressure of 3 species presses Si-SiC2-Si2C orders
Successively decrease, the partial pressure of Si is maximum.Since powder quality is certain, the transmission of Si material streams can constantly decline with the increase of growth course
Subtract, i.e. Si can premature distillation, remaining powder premature can be carbonized.Plus the difference of crucible inner powder material temperature degree, crucible
Temperature overheating at wall, can aggravate this process so that in the middle and later periods of SiC growths, the C particles in a large amount of powders are carried to crystalline substance
Body surface face, the C wrappages in crystal increase.Simultaneously because the influence of C wrappages, SiC single crystal secondary crystallization degradation is derivative
Go out many micro-pipes, the defects of dislocation, or even polycrystalline occur.This SiC crystal for also resulting in the growth of PVT methods cannot be grown very
Thickness, have impact on yield, add cost.And the prior art absorbs crucible edge etc. largely using the absorbent carbon of such as tantalum
The carbonization powder at place, reduces powder carbonizing degree, so as to reduce the generation of parcel material resource, or porous stone is used in growth chamber
Black net stops transporting for carbon particle, is reduced to the carbon particle concentration up to crystal growth plane, so that the generation of wrappage is reduced, but
It is to have the following disadvantages：The metal prices such as tantalum costly, make the extra technical process of the increases such as crucible coating layer, cause cost
Increase, in addition environment introducing additional impurities, crystal is caused a hidden trouble into crystalloid amount；Had at porous graphite net in growth chamber
SiC crystal crystallizes, and blocks the upward of SiC gaseous components in powder and transports, growth rate substantially reduces, and have impact on yield, increases
Cost is added.
The content of the invention
In order to solve the above technical problems, the technical solution that the present invention takes is：
The present invention proposes a kind of SiC single crystal growing system being persistently fed, including：Growth furnace, crucible and transmission device, its
In, the crucible includes：Upper crucible and lower crucible, wherein, the upper crucible is fixed on the top of furnace chamber, on described in crucible
Top be fixed with seed crystal；The lower crucible is located at the lower part of furnace chamber, and SiC powders, and multiple institutes are equipped with the lower crucible
State lower crucible to be respectively arranged on the transmission device, the multiple lower crucible is alternately risen to by stove by the transmission device
The top of chamber is connected with the upper crucible, carries out the lasting replacement of the SiC powders.
Further, the transmission device includes：Driver, drive link and support plate, wherein, described drive link one end is stretched
Enter furnace body with the support plate to be connected, the lower crucible is arranged in the support plate, and the other end of the drive link is located at stove
It is connected outside and with the driver.
Further, the junction of the drive link and furnace body is sealed using seal.
Further, the upper crucible and lower crucible are clamped.
Further, further include：The thermal insulation layer and induction coil of furnace chamber are arranged at, wherein, the crucible is arranged at described
In thermal insulation layer, the induction coil is arranged at the outside of the thermal insulation layer.
Further, the bottom of the thermal insulation layer is opening, and the support plate is risen by the opening, by the opening
Sealed.
Further, the support plate is identical with the material of thermal insulation layer.
Further, the top of the thermal insulation layer is equipped with thermometer hole.
Further, gas access is additionally provided with the furnace body, the pressure for regulating stove intracavitary.
In another aspect of this invention, it is proposed that a kind of to grow monocrystalline using foregoing SiC single crystal growing system
Method, comprises the following steps：
（1）SiC powders are placed in lower crucible, seed crystal is fixed on the top in upper crucible；
（2）The top that lower crucible is risen to furnace chamber by transmission device is connected with the upper crucible；
（3）Gas is filled with into furnace chamber, makes to maintain certain pressure in furnace chamber, sensing heating causes the temperature liter in upper chamber
It is high；
（4）Stove cavity pressure is reduced, makes SiC powders start to distil, crystal growth began；
（5）Growth after a certain period of time, raises stove cavity pressure so that crystal stops growing；
（6）Fallen by transmission device the lower crucible for consuming SiC powders is filled, fill new SiC powders another
Lower crucible is raised to furnace chamber top, is connected with upper crucible, and sensing heating is for a period of time；
（7）Repeating said steps（4）-（6）, until the new SiC powders in multiple lower crucibles are all exhausted；
（8）Temperature is reduced, takes out the crystal that growth finishes.
Beneficial effects of the present invention include at least：The present invention is replaced the powder that lower part carbonization consumed using transmission device
Into new powder, the Si/C ratios of gas phase much deviate SiC stoichiometric ratios when solving PVT methods from source because of growth, in crystal
The middle and late growth stage easily forms C wrappages, then derives defect even polycrystalline, causes SiC single crystal to grow very thick
Problem.After the powder being carbonized is substituted for new powder, Si/C ratios greatly increase, without unnecessary carbon in growing environment
Grain, so as to be inherently eliminated the formation of wrappage, while the PVT method crystal allow grows very thick, substantially increases
Yield, reduces cost.
Brief description of the drawings
Fig. 1 is present system working state figure one.
Fig. 2 is present system working state figure two.
Fig. 3 is present system working state figure three.
Wherein, growth furnace 1, upper crucible 2, lower crucible 3, drive link 4, support plate 5, seed crystal 6, induction coil 7, thermal insulation layer 8,
Thermometer hole 9.
Embodiment
In order to make those skilled in the art more fully understand technical scheme, with reference to specific embodiment to this
Invention is described in further detail.The embodiments described below is exemplary, and is only used for explaining the present invention, without being understood that
For limitation of the present invention.Particular technique or condition are not specified in embodiment, according to the described skill of document in the art
Art or condition are carried out according to product description.
According to an embodiment of the invention, Fig. 1 is present system working state figure one, and Fig. 2 is present system work shape
State figure two, Fig. 3 are present system working state figure three, with reference to shown in Fig. 1-3, the SiC single crystal of the present invention being persistently fed
Growing system, including：Growth furnace, crucible, transmission device, the thermal insulation layer and induction coil for being arranged at growth furnace furnace chamber.
According to an embodiment of the invention, with reference to shown in Fig. 1-3, the crucible is arranged in the thermal insulation layer, the sensing
Coil is arranged at the outside of the thermal insulation layer.
According to an embodiment of the invention, with reference to shown in Fig. 1-3, the crucible includes：Upper crucible and lower crucible, wherein, institute
The top that crucible is fixed on furnace chamber is stated, the top on described in crucible is fixed with seed crystal；The lower crucible is located at furnace chamber
Lower part, is equipped with SiC powders in the lower crucible, and multiple lower crucibles are respectively arranged on the transmission device, are passed through
The top that the multiple lower crucible is alternately risen to furnace chamber by the transmission device is clamped with the upper crucible, described in progress
The lasting replacement of SiC powders.
According to an embodiment of the invention, with reference to shown in Fig. 1-3, the transmission device includes：Driver, drive link and support
Plate, wherein, described drive link one end stretches into furnace body and is connected with the support plate, and the lower crucible is arranged in the support plate,
The other end of the drive link is located at outside stove and is connected with the driver.
According to some embodiments of the present invention, the junction of the drive link and furnace body is sealed using seal.
According to some embodiments of the present invention, the bottom of the thermal insulation layer is opening, and the support plate passes through the opening
Rise, the opening is sealed；More specifically, the support plate is identical with the material of thermal insulation layer.
According to some embodiments of the present invention, the top of the thermal insulation layer is equipped with thermometer hole；Gas is additionally provided with the furnace body
Body entrance, the pressure for regulating stove intracavitary.
In another aspect of this invention, it is proposed that a kind of to grow monocrystalline using foregoing SiC single crystal growing system
Method, comprises the following steps：
（1）SiC powders are placed in lower crucible, seed crystal is fixed on the top in upper crucible；
（2）The top that lower crucible is risen to furnace chamber by transmission device is connected with the upper crucible；
（3）Gas is filled with into furnace chamber, makes to maintain certain pressure in furnace chamber, sensing heating causes the temperature liter in upper chamber
It is high；
（4）Stove cavity pressure is reduced, makes SiC powders start to distil, crystal growth began；
（5）Growth after a certain period of time, raises stove cavity pressure so that crystal stops growing；
（6）Fallen by transmission device the lower crucible for consuming SiC powders is filled, fill new SiC powders another
Lower crucible is raised to furnace chamber top, is clamped with upper crucible, sensing heating is for a period of time；
（7）Repeating said steps（4）-（6）, until the new SiC powders in multiple lower crucibles are all exhausted；
（8）Temperature is reduced, takes out the crystal that growth finishes.
Embodiment 1：
Instantly when crucible number is two, it is respectively：Lower crucible a and lower crucible b, one kind are given birth to using foregoing SiC single crystal
The method of long system growth monocrystalline, comprises the following steps：
（1）SiC powders are placed in lower crucible a and lower crucible b, seed crystal is fixed on the top in upper crucible；
（2）The top that lower crucible a is risen to furnace chamber by transmission device is connected with the upper crucible；
（3）Gas is filled with into furnace chamber, makes to maintain 100Mpa in furnace chamber, sensing heating causes the temperature in upper chamber to rise to
2000℃；
（4）Stove cavity pressure is reduced to 100pa, makes SiC powders start to distil, crystal growth began；
（5）After growing 100h, rise stove cavity pressure to 100Mpa so that crystal stops growing；
（6）Fallen by transmission device the lower crucible a for consuming SiC powders is filled, the lower crucible b for filling new SiC powders
Furnace chamber top is raised to, is clamped with upper crucible, sensing heating 10h；
（7）Stove cavity pressure is reduced again to 100pa, makes SiC powders start to distil, crystal growth began, until in lower crucible b
New SiC powders be all exhausted；
（8）Temperature is reduced to room temperature, takes out the crystal that growth finishes.
It was found that crystal growth is very thick, and generated without obvious C wrappages.
Embodiment 2：
Instantly when crucible number is three, it is respectively：Lower crucible a, lower crucible b and lower crucible c, one kind utilize foregoing
The method that SiC single crystal growing system grows monocrystalline, comprises the following steps：
（1）SiC powders are placed in lower crucible a, lower crucible b and lower crucible c, seed crystal is fixed on the top in upper crucible；
（2）The top that lower crucible a is risen to furnace chamber by transmission device is connected with the upper crucible；
（3）Gas is filled with into furnace chamber, makes to maintain 100Mpa in furnace chamber, sensing heating causes the temperature in upper chamber to rise to
2000℃；
（4）Stove cavity pressure is reduced to 100pa, makes SiC powders start to distil, crystal growth began；
（5）After growing 100h, rise stove cavity pressure to 100Mpa so that crystal stops growing；
（6）Fallen by transmission device the lower crucible a for consuming SiC powders is filled, the lower crucible b for filling new SiC powders
Furnace chamber top is raised to, is clamped with upper crucible, sensing heating 10h；
（7）Stove cavity pressure is reduced again to 100pa, makes SiC powders start to distil, crystal growth began；
（8）After growing 100h, rise stove cavity pressure to 100Mpa so that crystal stops growing；
（9）Fallen by transmission device the lower crucible b for consuming SiC powders is filled, the lower crucible c for filling new SiC powders
Furnace chamber top is raised to, is clamped with upper crucible, sensing heating 10h；
（10）Stove cavity pressure is reduced again to 100pa, makes SiC powders start to distil, crystal growth began, until lower crucible c
Interior new SiC powders are all exhausted；
（8）Temperature is reduced to room temperature, takes out the crystal that growth finishes.
It was found that crystal growth is very thick, and generated without obvious C wrappages.
Crucible is separated into two parts up and down by the present invention, and seed crystal is fixed on top, and lower part dress powder, crystal growth is to necessarily
After stage, new powder is substituted for using the transmission device lower part powder that consumed of carbonization, powder can be with crystal growing process
Constantly replace, realize the continuous growth and the reduction of C wrappages of crystal.
In the description of the present invention, it is to be understood that the orientation or position relationship of the instruction such as term " on ", " under " are base
In orientation shown in the drawings or position relationship, description description of the invention and simplified, rather than instruction or hint are for only for ease of
Signified device or element must have specific orientation, with specific azimuth configuration and operation, therefore it is not intended that to this
The limitation of invention.
In the present invention, unless otherwise clearly defined and limited, the term such as term " connected ", " connection " should do broad sense reason
Solution, for example, it may be fixedly connected or be detachably connected, or integrally；Can be mechanical connection or electricity
Connection；It can be directly connected, can also be indirectly connected by intermediary, can be the connection inside two elements or two
The interaction relationship of element.For the ordinary skill in the art, above-mentioned term can be understood as the case may be
Concrete meaning in the present invention.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or the spy for combining the embodiment or example description
Point is contained at least one embodiment of the present invention or example.In the present specification, schematic expression of the above terms is not
It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be any
Combined in an appropriate manner in a or multiple embodiments or example.In addition, without conflicting with each other, the technology of this area
Different embodiments or example described in this specification and different embodiments or exemplary feature can be combined by personnel
And combination.
Although the embodiment of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, those of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changes, replacing and modification, meanwhile, for those of ordinary skill in the art, the think of according to the application
Think, in specific embodiments and applications there will be changes.
Claims (10)
1. a kind of SiC single crystal growing system being persistently fed, including：Growth furnace, crucible and transmission device, it is characterised in that its
In,
The crucible includes：Upper crucible and lower crucible, wherein, the upper crucible is fixed on the top of furnace chamber, the crucible on described
Interior top is fixed with seed crystal；
The lower crucible is located at the lower part of furnace chamber, SiC powders is equipped with the lower crucible, and multiple lower crucibles are set respectively
Be placed on the transmission device, the multiple lower crucible is alternately risen to by the transmission device top of furnace chamber with it is described
Upper crucible connection, carries out the lasting replacement of the SiC powders.
2. SiC single crystal growing system according to claim 1, it is characterised in that the transmission device includes：Driver,
Drive link and support plate, wherein, described drive link one end stretches into furnace body and is connected with the support plate, and the lower crucible is arranged at institute
State in support plate, the other end of the drive link is located at outside stove and is connected with the driver.
3. SiC single crystal growing system according to claim 2, it is characterised in that the junction of the drive link and furnace body
Sealed using seal.
4. SiC single crystal growing system according to claim 2, it is characterised in that the upper crucible and lower crucible card
Connect.
5. SiC single crystal growing system according to claim 2, it is characterised in that further include：It is arranged at the thermal insulation layer of furnace chamber
And induction coil, wherein, the crucible is arranged in the thermal insulation layer, and the induction coil is arranged at the outer of the thermal insulation layer
Portion.
6. SiC single crystal growing system according to claim 5, it is characterised in that the bottom of the thermal insulation layer is opening, institute
State support plate by the opening to rise, the opening is sealed.
7. SiC single crystal growing system according to claim 6, it is characterised in that the support plate and the material of thermal insulation layer
It is identical.
8. SiC single crystal growing system according to claim 5, it is characterised in that the top of the thermal insulation layer is equipped with thermometric
Hole.
9. SiC single crystal growing system according to claim 2, it is characterised in that gas access is additionally provided with the furnace body,
Pressure for regulating stove intracavitary.
10. a kind of method of SiC single crystal growing system growth monocrystalline using any one of claim 1-9, its feature
It is, comprises the following steps：
（1）SiC powders are placed in lower crucible, seed crystal is fixed on the top in upper crucible；
（2）The top that lower crucible is risen to furnace chamber by transmission device is connected with the upper crucible；
（3）Gas is filled with into furnace chamber, makes to maintain certain pressure in furnace chamber, sensing heating causes the temperature liter in upper chamber
It is high；
（4）Stove cavity pressure is reduced, makes SiC powders start to distil, crystal growth began；
（5）Growth after a certain period of time, raises stove cavity pressure so that crystal stops growing；
（6）Fallen by transmission device the lower crucible for consuming SiC powders is filled, fill new SiC powders another
Lower crucible is raised to furnace chamber top, is connected with upper crucible, and sensing heating is for a period of time；
（7）Repeating said steps（4）-（6）, until the new SiC powders in multiple lower crucibles are all exhausted；
（8）Temperature is reduced, takes out the crystal that growth finishes.
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| CN109321981A (en) * | 2018-11-02 | 2019-02-12 | 山东天岳先进材料科技有限公司 | A kind of high quality single crystal silicon carbide and preparation method thereof |
| CN109355705A (en) * | 2018-11-02 | 2019-02-19 | 山东天岳先进材料科技有限公司 | A kind of device preparing high quality single crystal silicon carbide and its application |
| CN111041553A (en) * | 2019-12-04 | 2020-04-21 | 山东天岳先进材料科技有限公司 | Crystal growth device and method |
| WO2020087720A1 (en) * | 2018-11-02 | 2020-05-07 | 山东天岳先进材料科技有限公司 | High-quality single crystal silicon carbide, and method and apparatus for preparing same |
| CN112553691A (en) * | 2020-12-02 | 2021-03-26 | 中电化合物半导体有限公司 | Silicon carbide crystal growth method and growth device |
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| CN115323478A (en) * | 2022-07-20 | 2022-11-11 | 中国电子科技集团公司第二十六研究所 | Method for realizing continuous growth of crystal |
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| EP3922762A4 (en) * | 2020-04-14 | 2022-01-05 | Meishan Boya Advanced Materials Co., Ltd. | Crystal growth method and device |
| US11926922B2 (en) * | 2020-04-14 | 2024-03-12 | Meishan Boya Advanced Materials Co., Ltd. | Methods for crystal growth by replacing a sublimated target source material with a candidate source material |
| CN112663136A (en) * | 2020-12-02 | 2021-04-16 | 中电化合物半导体有限公司 | Silicon carbide crystal growth method and growth device |
| CN112553691A (en) * | 2020-12-02 | 2021-03-26 | 中电化合物半导体有限公司 | Silicon carbide crystal growth method and growth device |
| CN114752997A (en) * | 2022-04-25 | 2022-07-15 | 哈尔滨工业大学 | Double-crucible liquid phase epitaxial growth device |
| CN115074820A (en) * | 2022-06-17 | 2022-09-20 | 哈尔滨工业大学 | Double-crucible liquid phase epitaxy preparation method of single crystal RIG thick film |
| CN115323478A (en) * | 2022-07-20 | 2022-11-11 | 中国电子科技集团公司第二十六研究所 | Method for realizing continuous growth of crystal |
| CN115404538A (en) * | 2022-07-20 | 2022-11-29 | 中国电子科技集团公司第二十六研究所 | Device capable of realizing continuous growth of crystal |
| CN115404538B (en) * | 2022-07-20 | 2023-08-22 | 中国电子科技集团公司第二十六研究所 | Device capable of realizing continuous growth of crystals |
| CN115323478B (en) * | 2022-07-20 | 2023-11-21 | 中国电子科技集团公司第二十六研究所 | Method for realizing continuous growth of crystal |
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