CN109355705A - A kind of device preparing high quality single crystal silicon carbide and its application - Google Patents
A kind of device preparing high quality single crystal silicon carbide and its application Download PDFInfo
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- CN109355705A CN109355705A CN201811302576.8A CN201811302576A CN109355705A CN 109355705 A CN109355705 A CN 109355705A CN 201811302576 A CN201811302576 A CN 201811302576A CN 109355705 A CN109355705 A CN 109355705A
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- crucible
- silicon carbide
- high quality
- single crystal
- silicon
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 44
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 70
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 69
- 239000010703 silicon Substances 0.000 claims abstract description 65
- 238000010438 heat treatment Methods 0.000 claims abstract description 51
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 40
- 239000013078 crystal Substances 0.000 claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 36
- 230000012010 growth Effects 0.000 claims abstract description 36
- 238000009413 insulation Methods 0.000 claims abstract description 26
- 238000010276 construction Methods 0.000 claims abstract description 22
- 239000013589 supplement Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims description 31
- 239000000126 substance Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- 230000006698 induction Effects 0.000 claims description 6
- 238000004891 communication Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000011863 silicon-based powder Substances 0.000 claims description 5
- 238000010891 electric arc Methods 0.000 claims description 2
- 238000010894 electron beam technology Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000428 dust Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 11
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 20
- 229910010271 silicon carbide Inorganic materials 0.000 description 12
- 230000007547 defect Effects 0.000 description 10
- 238000004821 distillation Methods 0.000 description 8
- 229910052571 earthenware Inorganic materials 0.000 description 8
- 230000001681 protective effect Effects 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 4
- 239000001307 helium Substances 0.000 description 4
- 229910052734 helium Inorganic materials 0.000 description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 230000002401 inhibitory effect Effects 0.000 description 3
- 238000005192 partition Methods 0.000 description 3
- 229910003978 SiClx Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052743 krypton Inorganic materials 0.000 description 2
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052754 neon Inorganic materials 0.000 description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 101000623895 Bos taurus Mucin-15 Proteins 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000003698 anagen phase Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000021332 multicellular organism growth Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 238000001291 vacuum drying 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
- C30B29/36—Carbides
-
- 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
-
- 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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
- C30B23/06—Heating of the deposition chamber, the substrate or the materials to be evaporated
- C30B23/066—Heating of the material to be evaporated
Landscapes
- 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 proposes a kind of devices for preparing high quality single crystal silicon carbide, which is characterized in that described device includes: at least the first crucible and the second crucible, at least two heating elements and insulation construction；Wherein, at least two crucible is interconnected；Each crucible corresponds at least one heating element；The heating of each crucible is independent control；First crucible is used for the growth of carbide silicon crystal, and second crucible is used for the supplement of silicon atmosphere.The present invention also provides a kind of applications of device for preparing high quality single crystal silicon carbide.Silicon atmosphere supplement can be provided for long brilliant crucible in the middle and later periods in growing silicon carbice crystals stage using preparation facilities of the present invention, the formation of crystal carbon inclusion enclave can be decreased or even eliminated.
Description
Technical field
The present invention relates to crystalline material preparation facilities technical field more particularly to a kind of preparations of high quality single crystal silicon carbide
Device, the device for further relating to prepare high quality single crystal silicon carbide are preparing the application in high quality single crystal silicon carbide.
Background technique
Single-crystal silicon carbide is one of most important third generation semiconductor material, because its with forbidden bandwidth big, saturated electrons
The excellent properties such as mobility is high, breakdown field is powerful, thermal conductivity is high, are widely used in power electronics, radio-frequency devices, photoelectron device
The fields such as part.Physical vapor transport (PVT) method is the main growing technology for producing single-crystal silicon carbide at present, i.e., makes carbon at high temperature
The gaseous sources that the distillation of SiClx raw material generates, which are transported at seed crystal, to be recrystallized.
The growth course that PVT method grows single-crystal silicon carbide is to carry out in closed graphite crucible, therefore give birth at high temperature
Long environment is under carbon rich atmosphere.Crystal growth initial stage, since the partial vapour pressure of silicon components is higher, at crystal growth interface
In the state of silicon components and carbon component relative equilibrium.With the progress of crystal growth, the silicon components in sic raw material are constantly
Distillation is reduced, and causes the indoor gaseous component of growth chamber is gradually unbalance to become rich carbon state.Under the growing environment of rich carbon, crystal
The front interface of growth has the enrichment of carbon and forms carbon package volume defect.Package volume defect can induce micro-pipe, dislocation, fault etc.
Defect seriously affects silicon carbide substrates quality, and then influences epitaxial layer quality and device performance.
When PVT method grows carborundum crystals, it is long brilliant to carry out silicon carbide usually using crucible, in crystal growth after
Phase, due to a large amount of volatilizations and loss of silicon components, the sic raw material carbonization of bottom is serious, leads to the indoor gas phase group of growth chamber
Divide gradually unbalance as rich carbon state.Under the growing environment of rich carbon, the front interface of crystal growth has the enrichment of carbon and shape
Volume defect is wrapped up at carbon.In order to eliminate the package volume defect of carbon present in carborundum crystals, the Wang Fengfu etc. of Xi'an University of Technology
The small crucible that Silicon-rich raw material is housed is added in original long brilliant crucible, to wish in crystal growing process as silicon components
Supplementary source, to reduce the generation of rich carbon component, and then the formation of carbon inclusion enclave is inhibited [to mix Si powder in the raw material of the mansion Wang Feng
Influence [D] Xi'an University of Technology to SiC crystal quality, 2013.].This method cannot flexibly control the liter of silicon in small crucible
The magnificent time, it is possible to cause the distillation in advance or lag distillation of silicon, silicon distils in advance, and to will cause silicon atmosphere in growth chamber excessive,
The defects of silicon inclusion enclave easy to form, micro-pipe；Silicon lag distillation cannot then be played the role of inhibiting carbon inclusion enclave.
CN105671637A and CN205653539U discloses a kind of device of PVT method growth single-crystal silicon carbide sustained release, earthenware
Partition is provided in crucible, the carborundum powder source is separated into upper layer and lower layer by the partition, and setting is by several connections on partition
The hole in upper layer and lower layer carborundum powder source.CN207062351U discloses a kind of vacuum drying oven of two sections of distillations, and crucible I and crucible II are logical
Gas-guide tube connection is crossed, temperature control heating component I is connect with crucible I, and temperature control heating component II is connect with crucible II, and thermocouple I is arranged
In crucible I, thermocouple II is arranged in crucible II, and two crucibles are heated in realization respectively, realizes to metalliferous material twice
Vacuum distillation.Patent documents above is undesirable to the loss control effect of element silicon during the long crystalline substance of monocrystalline silicon carbide, and control is not
It is enough accurate.
Summary of the invention
Existing technology is unable to fully inhibit the carbonization of sic raw material, causes to occur in the later period of crystal growth more highly concentrated
The carbon of degree wraps up volume defect, and crystal quality and substrate quality is caused to be greatly reduced.Mansion Xi'an University of Technology Wang Feng etc. is in original length
The small crucible that Silicon-rich raw material is housed is added in brilliant crucible, to wish in crystal growing process as the supplementary source of silicon components
Method, cannot flexibly control the sublimation time of silicon in small crucible, it is possible to cause silicon distillation in advance or lag distillation,
The defects of silicon distils in advance, and to will cause silicon atmosphere in growth chamber excessive, silicon inclusion enclave easy to form, micro-pipe；Silicon lag distils then not
It can play the role of inhibiting carbon inclusion enclave.In addition, the addition of small crucible will increase the risk for introducing additional impurities.Furthermore small crucible
It is size-constrained, the available silicon atmosphere of raw material also will receive limitation in small crucible, may cause at later stages silicon atmosphere benefit
Fill not total, the formation that crystal growth later period carbon cannot be inhibited to wrap up well.High quality single crystal silicon carbide proposed by the present invention
Preparation facilities can flexibly control the time of silicon atmosphere supplement, and the production of problem above can also be avoided while inhibiting carbon inclusion enclave
It is raw.
The present invention is for more carbon inclusion enclave easy to form in monocrystalline silicon carbide preparation process in the prior art, micro-pipe etc.
The problem of defect, a kind of device for preparing high quality single crystal silicon carbide is provided, the preparation facilities includes: at least the first crucible
With the second crucible, at least two heating elements and insulation construction；Wherein, at least two crucible is interconnected；Each earthenware
Crucible corresponds at least one heating element；The heating of each crucible is independent control；First crucible is used for monocrystalline silicon carbide
The growth of crystal, second crucible are used for the supplement of silicon atmosphere.Increase at least one for supplementing the crucible of silicon atmosphere, in crystalline substance
The silicon atmosphere of body growth phase middle and later periods, supplement can be entered in growth chamber by connecting pipe, so that the silicon carbon ratio in growth chamber
Reach balance, decreases or even eliminates the formation of carbon inclusion enclave.The temperature of each crucible is controlled by individual intermediate frequency coil, is improved
Temperature controlled flexibility.
On the one hand, the present invention provides a kind of device for preparing high quality single crystal silicon carbide, described device includes: at least
One crucible and the second crucible, at least two heating elements and insulation construction；Wherein, at least two crucible is interconnected；
Each crucible corresponds at least one heating element；The heating of each crucible is independent control；First crucible is used for monocrystalline
The growth of carborundum crystals, second crucible are used for the supplement of silicon atmosphere.
Further, first crucible and the upper and lower serial communication of second crucible.
Further, first crucible and second crucible are interconnected by connecting pipe, first earthenware
Crucible and second crucible are to be threadedly coupled with the connection type of connecting pipe.
Further, increase one or more crucibles between first crucible and second crucible, and all
Crucible is interconnected.
Further, the heating element is selected from resistance heating circle, induction heating circle, electric arc heated circle, electron beam heating
One of circle, infrared heating circle or medium heating coil.
Further, the heating element is induction heating circle, and induction heating circle can be intermediate frequency coil or high frequency coil
One of.Preferably, the heating element can be intermediate frequency coil.
Further, first crucible is provided with raw material and seed crystal for crystal growth, the second crucible setting
There is the Silicon-rich raw material for silicon atmosphere supplement.
Further, the raw material for crystal growth is selected from high-purity silicon carbide powder, high-purity silicon powder and high-purity carbon
The mixture of powder.
Further, the Silicon-rich raw material is selected from the material that element silicon ratio is higher than carbon ratio.It is preferred that the richness
Silicon raw material is high-purity silicon powder.
Further, the insulation construction can be a set of insulation construction, be also possible to more set insulation constructions, wherein more
The quantity for covering insulation construction is consistent with the quantity of crucible.
Further, the insulation construction can be seperated loosely filled insulation structure, including holder part and filling part
Point.
Further, first crucible and the upper and lower serial communication of second crucible.First crucible bottom is set
Striker plate is set, the striker plate is connected through a screw thread mode with the bottom of first crucible and is connected.
Further, the length of the striker plate is the 1/3-2/3 of the height of first crucible.Preferably, described
The length of striker plate is the 1/2 of the height of first crucible.
Further, the cross-sectional area of the connecting pipe is the 1/12-1/6 of the first crucible cross-sectional area.It is excellent
Choosing, the cross-sectional area of the connecting pipe is the 1/10-1/8 of the first crucible cross-sectional area.It is furthermore preferred that the connection
The cross-sectional area of pipeline is the 1/9 of the first crucible cross-sectional area.
Further, the connection type of the connecting pipe and first crucible and second crucible is screw thread company
It connects.
The shape of the cross section of further connecting pipe can be circle, ellipse, square, rectangle, diamond shape, more
One of side shape；It is preferably circular shape at each angle of square, rectangle, diamond shape, polygon.
On the other hand, the present invention also provides the above-mentioned devices for preparing high quality single crystal silicon carbide to prepare high quality single crystal
Application in silicon carbide.
Further, the application method specifically includes the following steps:
Growth chamber in first crucible is evacuated to 5-80mbar, long brilliant temperature is heated to first crucible
2000-2500 DEG C, it is long brilliant to carry out the first stage, when Si and C ratio are less than 1.1 in gas phase in first crucible, terminates the
Single order segment length is brilliant；Second crucible is carried out to be heated to long brilliant 2000-2500 DEG C of temperature, the silicon atmosphere in second crucible
It is added in first crucible, carries out second-order segment length crystalline substance 10-50h.
Further, when Si and C ratio reach 1.0-1.1:1 in gas phase in first crucible, terminate the first rank
Segment length is brilliant.Preferably, when Si and C ratio reach 1.0-1.05:1 in gas phase in first crucible, it is long to terminate the first stage
It is brilliant.It is furthermore preferred that it is long brilliant to terminate the first stage when Si and C ratio reach 1.0-1.01:1 in gas phase in first crucible.
Further, before the first stage of the growing silicon carbice crystals starts, the application method further include:
It is packed into long brilliant raw material and seed crystal in first crucible, is packed into the raw material of Silicon-rich component in second crucible, and to described
Protective gas is passed through in first crucible and second crucible.
The protective gas is one or more in helium, neon, argon gas, Krypton, xenon, hydrogen.
Further, after the second stage of the growing silicon carbice crystals, the application method further include as
Lower step: being passed through protective gas into first crucible and the second crucible, until pressure reaches an atmospheric pressure in crucible, simultaneously
Cooled to room temperature can be prepared by the monocrystalline silicon carbide of high quality.
The protective gas is one or more in helium, neon, argon gas, Krypton, xenon, hydrogen.
The invention has the following beneficial effects:
1. the present invention uses more than two interconnected crucibles, the long brilliant needs of silicon carbide can be placed in each crucible
Raw material；One of crucible places seed crystal and carries out long crystalline substance, and the raw material in remaining crucible is the raw material of Silicon-rich, in crystal growth phase
Middle and later periods can provide silicon atmosphere supplement for long brilliant crucible, can decrease or even eliminate the formation of crystal carbon inclusion enclave.
2. the present invention can be realized using two sections or more of heating element and individually be controlled each crucible, can be according to practical life
Produce need stage by stage, between timesharing, division technique control, improve the flexibility of control, can reduce due to the silicon atmosphere prolongation
Control it is improper caused by silicon inclusion enclave, micro-pipe the defects of.
Detailed description of the invention
The drawings described herein are used to provide a further understanding of the present invention, constitutes a part of the invention, this hair
Bright illustrative embodiments and their description are used to explain the present invention, and are not constituted improper limitations of the present invention.In the accompanying drawings:
Fig. 1 is the signal of the device for preparing high quality single crystal silicon carbide of crucible of the present invention including upper and lower serial communication
Figure.
Wherein: 1. first thermometer holes；2. the first crucible；3. seed crystal；4. striker plate；5. the first heating element；6. long brilliant former
Material；7. connecting pipe；8. the second crucible；9. the second heating element；10. Silicon-rich raw material；11. insulation construction；12. the second thermometric
Hole.
Specific embodiment
General idea of the invention is illustrated in order to clearer, is described in detail below with reference to following specific embodiments,
But it does not limit the scope of the invention.
Embodiment 1
The device of high quality single crystal silicon carbide is prepared as shown in Figure 1, the preparation facilities includes: raw for single-crystal silicon carbide
Long the first crucible (2), the second crucible (8) for supplementing silicon atmosphere, the connection for connecting the first crucible and the second crucible
Pipeline (7), for the first crucible heating the first heating element (5), for the second crucible heating the second heating element (9),
Striker plate (4) and insulation construction (11) further include the first measured hole (1) for measuring the temperature of the first crucible, for measuring
The second measured hole (12) of the temperature of second crucible, wherein first crucible, second crucible and the connecting pipe
Connection type is to be threadedly coupled, and the striker plate is to be threadedly coupled with the connection type of the first crucible, first heating element
It is independent control with second heating element.
The mode of communicating of first crucible and second crucible is upper and lower serial communication.
First heating element and second heating element are intermediate frequency coil.
Seed crystal (3) and the long brilliant raw material (6) for silicon carbide monocrystal growth are equipped in first crucible；Second earthenware
The Silicon-rich raw material (10) for silicon atmosphere supplement is equipped in crucible.
The length of the striker plate is the 1/3-2/3 of the height of first crucible.
The cross-sectional area of the connecting pipe is the 1/12-1/6 of the first crucible cross-sectional area.
The insulation construction of the invention is not particularly limited, as long as insulation effect can be played, the insulation construction
It can be a set of insulation construction, be also possible to more set insulation constructions, wherein the quantity of more set insulation constructions and the quantity one of crucible
It causes.
The insulation construction can be seperated loosely filled insulation structure, including holder part and fill part.
Embodiment 2
The method for preparing high quality single crystal silicon carbide, the preparation method comprises the following steps:
(1) it is packed into long brilliant raw material sic powder and seed crystal in first crucible, is packed into second crucible
The raw material of Silicon-rich component, and protective gas helium is passed through into first crucible and second crucible；
(2) growth chamber in first crucible is vacuumized into 5mbar, and the control switch of first heating element is beaten
It opens, first crucible is heated, step up the temperature of first crucible to long brilliant 2000 DEG C of temperature, carry out the
Single order segment length's crystalline substance 50h；
(3) after the long crystalline substance of the first stage in step (2), at this point, the growth gas in first crucible in growth chamber
The silicon carbon ratio of atmosphere is 1.0, opens the control switch of second heating element, heats to second crucible, is made described
The temperature of second crucible is stepped up to brilliant 2500 DEG C of temperature is grown, and the silicon atmosphere in second crucible is added to first earthenware
In crucible, second-order segment length crystalline substance 30h is carried out；
(4) after second-order segment length's crystalline substance in step (3), guarantor is passed through into first crucible and second crucible
It protects gas and can be prepared by the carbide of high quality until pressure reaches an atmospheric pressure, while cooled to room temperature in crucible
Silicon.
Embodiment 3
The method for preparing high quality single crystal silicon carbide, the preparation method comprises the following steps:
(1) it is packed into long brilliant raw material sic powder and seed crystal in first crucible, is packed into second crucible
The raw material of Silicon-rich component, and protective gas hydrogen is passed through into first crucible and second crucible；
(2) growth chamber in first crucible is vacuumized into 80mbar, and by the control switch of first heating element
It opens, first crucible is heated, step up the temperature of first crucible to long brilliant 2500 DEG C of temperature, carry out
First stage grows crystalline substance 10h；
(3) after the long crystalline substance of the first stage in step (2), at this point, the growth gas in first crucible in growth chamber
The silicon carbon ratio of atmosphere is 1.01, opens the control switch of second heating element, heats to second crucible, is made described
The temperature of second crucible is stepped up to brilliant 2000 DEG C of temperature is grown, and the silicon atmosphere in second crucible is added to first earthenware
In crucible, second-order segment length crystalline substance 50h is carried out；
(4) after second-order segment length's crystalline substance in step (3), guarantor is passed through into first crucible and second crucible
It protects gas and can be prepared by the carbide of high quality until pressure reaches an atmospheric pressure, while cooled to room temperature in crucible
Silicon.
Embodiment 4
The method for preparing high quality single crystal silicon carbide, the preparation method comprises the following steps:
(1) it is packed into long brilliant raw material sic powder and seed crystal in first crucible, is packed into second crucible
The raw material of Silicon-rich component, and protective gas helium is passed through into first crucible and second crucible；
(2) growth chamber in first crucible is vacuumized into 50mbar, and by the control switch of first heating element
It opens, first crucible is heated, step up the temperature of first crucible to long brilliant 2200 DEG C of temperature, carry out
First stage grows crystalline substance 40h；
(3) after the long crystalline substance of the first stage in step (2), at this point, the growth gas in first crucible in growth chamber
The silicon carbon ratio of atmosphere is 1.05, opens the control switch of second heating element, heats to second crucible, is made described
The temperature of second crucible is stepped up to brilliant 2400 DEG C of temperature is grown, and the silicon atmosphere in second crucible is added to first earthenware
In crucible, second-order segment length crystalline substance 20h is carried out；
(4) after second-order segment length's crystalline substance in step (3), guarantor is passed through into first crucible and second crucible
It protects gas and can be prepared by the carbide of high quality until pressure reaches an atmospheric pressure, while cooled to room temperature in crucible
Silicon.
There is less carbon using the monocrystalline silicon carbide that the preparation facilities of high quality single crystal silicon carbide of the invention is prepared
Wrap up bulk concentration.10 pieces of monocrystalline silicon carbide that common crucible structure and crucible structure of the invention are grown, monocrystalline are chosen respectively
The concentration levels of carbon inclusion enclave are observed after silicon carbide slice under the microscope.Every piece of monocrystalline silicon carbide is unified to extract the 10th and the
20, under 50 times of amplification factors, the carbon inclusion enclave concentration data of statistics is as shown in table 1.
Table 1 is using common crucible and crucible output single crystal silicon carbide wafer of the present invention 10th and the 20th package bulk concentration
(/cm3)
The carbon package bulk concentration that can be seen that the monocrystalline silicon carbide produced using crucible of the invention from upper table data is bright
The aobvious carbon package bulk concentration lower than the monocrystalline silicon carbide produced using common crucible.The single crystal carbon produced using crucible of the present invention
The 10th of SiClx and the carbon inclusion enclave mean concentration of the 20th wafer are only 0.36/cm3And 0.71/cm3, and use common earthenware
The 10th of monocrystalline silicon carbide of crucible production and the carbon inclusion enclave mean concentration of the 20th wafer are 1.24/cm3And 1.77/cm3。
All the embodiments in this specification are described in a progressive manner, same and similar portion between each embodiment
Dividing may refer to each other, and each embodiment focuses on the differences from other embodiments.
The above description is only an embodiment of the present invention, is not intended to restrict the invention.For those skilled in the art
For, the invention may be variously modified and varied.All any modifications made within the spirit and principles of the present invention are equal
Replacement, improvement etc., should be included within scope of the presently claimed invention.
Claims (10)
1. a kind of device for preparing high quality single crystal silicon carbide, which is characterized in that described device includes: at least the first crucible and
Two crucibles, at least two heating elements and insulation construction；
Wherein, at least two crucible is interconnected；
Each crucible corresponds at least one heating element；
The heating of each crucible is independent control；
First crucible is used for the growth of carbide silicon crystal, and second crucible is used for the supplement of silicon atmosphere.
2. the device according to claim 1 for preparing high quality single crystal silicon carbide, which is characterized in that
Serial communication above and below first crucible and second crucible.
3. the device according to claim 1 for preparing high quality single crystal silicon carbide, which is characterized in that
The heating element is selected from resistance heating circle, induction heating circle, electric arc heated circle, electron beam heating coil, infrared heating
One of circle or medium heating coil.
4. the device according to claim 3 for preparing high quality single crystal silicon carbide, which is characterized in that
The heating element is induction heating circle, and induction heating circle can be one of intermediate frequency coil or high frequency coil；Preferably,
The heating element can be intermediate frequency coil.
5. the device according to claim 1 for preparing high quality single crystal silicon carbide, which is characterized in that
First crucible is provided with raw material and seed crystal for crystal growth, and second crucible is provided with to be mended for silicon atmosphere
The Silicon-rich raw material filled.
6. the device according to claim 5 for preparing high quality single crystal silicon carbide, which is characterized in that
The raw material for crystal growth is selected from the mixture of high-purity silicon carbide powder, high-purity silicon powder and high-purity carbon dust；
The Silicon-rich raw material is selected from the material that element silicon ratio is higher than carbon ratio, preferably high-purity silicon powder.
7. the device according to claim 1 for preparing high quality single crystal silicon carbide, which is characterized in that
The insulation construction can be a set of insulation construction, be also possible to more set insulation constructions, wherein the number of more set insulation constructions
It measures consistent with the quantity of crucible.
8. the device according to claim 7 for preparing high quality single crystal silicon carbide, which is characterized in that
The insulation construction can be seperated loosely filled insulation structure, including holder part and fill part.
9. any device for preparing high quality single crystal silicon carbide of claim 1-8 is in preparing high quality single crystal silicon carbide
Application.
10. the application of the device according to claim 9 for preparing high quality single crystal silicon carbide, which is characterized in that described to answer
With method specifically includes the following steps:
Growth chamber in first crucible is evacuated to 5-80mbar, long brilliant temperature 2000- is heated to first crucible
2500 DEG C, carrying out first stage long crystalline substance terminates the first stage when Si and C ratio are less than 1.1 in gas phase in first crucible
It is long brilliant；
Second crucible is carried out to be heated to long brilliant 2000-2500 DEG C of temperature, the silicon atmosphere in second crucible is added to
In first crucible, second-order segment length crystalline substance 10-50h is carried out.
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| CN201811302576.8A CN109355705B (en) | 2018-11-02 | 2018-11-02 | Device for preparing high-quality monocrystalline silicon carbide and application thereof |
| PCT/CN2018/123713 WO2020087720A1 (en) | 2018-11-02 | 2018-12-26 | High-quality single crystal silicon carbide, and method and apparatus for preparing same |
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| CN201811302576.8A CN109355705B (en) | 2018-11-02 | 2018-11-02 | Device for preparing high-quality monocrystalline silicon carbide and application thereof |
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| CN113862789A (en) * | 2021-12-01 | 2021-12-31 | 浙江大学杭州国际科创中心 | Crucible structure, device and method for preparing p-type 4H-SiC single crystal |
| CN114836834A (en) * | 2022-07-04 | 2022-08-02 | 浙江大学杭州国际科创中心 | Device and method for continuously growing single crystal silicon carbide by PVT (physical vapor transport) method |
| CN115595657A (en) * | 2022-10-28 | 2023-01-13 | 深圳腾睿微电子科技有限公司（Cn） | growing equipment |
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| CN117265664B (en) * | 2023-09-26 | 2024-04-30 | 江苏超芯星半导体有限公司 | Growth method of silicon carbide crystal and silicon carbide crystal |
| CN119177495A (en) * | 2024-11-26 | 2024-12-24 | 湖南顶立科技股份有限公司 | Silicon carbide single crystal growth equipment and preparation process thereof |
| CN120925079A (en) * | 2025-10-15 | 2025-11-11 | 山西烁科晶体有限公司 | A high-quality, large-size silicon carbide crystal growth apparatus and method |
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