CN110079863A - A kind of reactor for crystal growth - Google Patents
A kind of reactor for crystal growth Download PDFInfo
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- CN110079863A CN110079863A CN201910325375.8A CN201910325375A CN110079863A CN 110079863 A CN110079863 A CN 110079863A CN 201910325375 A CN201910325375 A CN 201910325375A CN 110079863 A CN110079863 A CN 110079863A
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- crucible
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- helical baffle
- gas phase
- crystal
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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
- C30B23/002—Controlling or regulating
- C30B23/005—Controlling or regulating flux or flow of depositing species or vapour
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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
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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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- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
This application involves a kind of reactors for crystal growth, belong to crystalline material preparation field.The reactor for being used for crystal growth includes: crucible assembly, comprising: Crucible body, crucible cover and the helical baffle component being arranged in Crucible body, crystal growth is carried out after the helical airflow passages at least partly formed through helical baffle component after the raw material distillation being loaded in Crucible body；Support member and heating element, crucible assembly can also rotate.The reactor of the application changes traditional gas phase transmission mode, is converted to spiral by traditional transmission vertically upward and transmits upwards, realizes and keeps off to effective lattice of large granular impurity in crystal growing process, reduce the defect density in crystal, improves crystal quality；And it not will cause gas phase and transmit difficulty upwards, be not necessarily to excessively high growth temperature, reduce energy consumption；The application can play control action to the gas phase transmission under vacuum, and the single crystal growth rate under vacuum is fast, growth temperature is low, and gas phase can be transmitted orderly upwards, and the defect of the crystal of growth is few, cost efficiency.
Description
Technical field
This application involves a kind of reactors for crystal growth, belong to crystalline material preparation field.
Background technique
Silicon carbide is typical semiconductor material with wide forbidden band, is the third generation semiconductor material generation after silicon, GaAs
One of table.Carbofrax material has the excellent characteristics such as high heat conductance, high breakdown field strength, high saturated electrons mobility, becomes preparation
One of high temperature, high frequency, high power and active material of anti-radiation device.
The method of growth of silicon carbide mainly has physical vapor transport (PVT), liquid phase epitaxial method (LPE), chemical gas at present
Phase sedimentation (CVD) etc., wherein PVT method is can to provide commercial carbon using most mature method and currently the only one kind
The growing method of silicon substrate demand.The growth course of PVT method growth single-crystal silicon carbide carries out in closed graphite crucible, because
Growing environment is under carbon rich atmosphere at high temperature for this.It is crystal growth initial stage, brilliant since the partial vapour pressure of silicon components is higher
The state that body growth interface is in silicon components and carbon component balances each other.Silicon with the progress of crystal growth, in sic raw material
Component constantly distils reduction, causes the indoor gaseous component of growth chamber is gradually unbalance to become rich carbon state.In the growth ring of rich carbon
Under border, the front interface of crystal growth has the enrichment of carbon and forms the carbon wrappage defect of bulky grain.In addition, sic raw material
In bulky grain metal impurities, silicon inclusion enclave etc. can also follow gas phase in traditional silicon carbide gas phase from bottom to top transmission process
It enters in single-crystal silicon carbide and then forms large granular impurity defect.Bulky grain defect can induce micro-pipe, dislocation, fault etc. and lack
It falls into, seriously affect silicon carbide substrates quality and then influences epitaxial layer quality and device performance.
Solving a big main flow direction of large granular impurity defect in single-crystal silicon carbide at present is on silicon carbide gas phase transmission road
On diameter be arranged graphite strainer play the role of be isolated large granular impurity transmit upwards.207498521 U of Chinese patent application CN is public
A kind of silicon carbide monocrystal growth device for promoting quality, including graphite crucible, graphite cover and graphite soft felt insulating layer have been opened, it is described
Graphite cover is located at the top closed graphite crucible of graphite crucible, and the graphite cover medial center outburst area is bonded with seed crystal
Piece, the graphite soft felt insulating layer coats around the graphite crucible, top, bottom, is placed with carbon in the graphite crucible
SiClx powder, the region in the graphite crucible between silicon carbide powder and seed wafer set up graphite support ring, the graphite branch
Guide shell is installed on pushing out ring, fixes one or more layers metal filtration piece in the guide shell, in the metal filtration piece
It is even that through-hole is distributed with.The utility model is installed metal filtration piece resistant to high temperature and is led in the space in crucible between raw material and seed crystal
Flow cartridge can effectively filter out carbon impurity, avoid forming carbon wrappage in crystal growing process, and then cause micro-pipe, dislocation
The defects of generation, generate the single-crystal silicon carbide of high quality.The patent application scheme can effectively control big in single-crystal silicon carbide
The density of granule foreign defect, but the presence of graphite strainer often will cause the difficulty that silicon carbide gas phase is transmitted upwards, need
Improve temperature and be just able to achieve the stability that gas phase is transmitted to seed crystal, and the raising of temperature can then greatly increase in crystal stress and its
The output probability of his defect, the quality of single-crystal silicon carbide are unable to get guarantee.And in crystal growing process, traditional gas phase
Gas phase under the vacuum growth of transmission mode is unable to get effective control, and single crystal growth rate is exceedingly fast and crystalline quality is very poor, micro-
The defects of pipe, many types of, dislocation, increased significantly.
Summary of the invention
To solve the above-mentioned problems, present applicant proposes a kind of reactor for crystal growth, the application changes tradition
PVT method prepare the gas phase transmission mode of crystal, spiral is converted to by traditional transmission vertically upward and is transmitted upwards, is realized to crystalline substance
Effective lattice gear of large granular impurity, reduces the defect density in crystal, improves crystal quality in body growth course；And it will not make
Difficulty is transmitted upwards at gas phase, is not necessarily to excessively high growth temperature, reduces energy consumption；The application can play the gas phase transmission under vacuum
Control action, single crystal growth rate under vacuum is fast, growth temperature is low, and gas phase can be transmitted orderly upwards, the crystal of growth
Defect is few, cost efficiency.
This is used for the reactor of crystal growth, comprising: crucible assembly comprising: Crucible body, crucible cover and setting are in earthenware
At least one intracorporal helical baffle component of crucible master is loaded in after the raw material distillation in Crucible body at least partly through helical baffle
Crystal growth is carried out after the helical airflow passages that component is formed；On the inside of crucible cover and it is suitable for supporting the support portion for growing crystal
Part；And the heating element of the temperature suitable for the crucible assembly to be maintained to growth crystal.
Optionally, the crucible assembly can be rotated.Preferably, the velocity of rotation of the crucible assembly is that 10-200 turns/h.
Optionally, at least partly diameter of the helical baffle component is identical with its mutually level Crucible body internal diameter.
Preferably, the diameter of Crucible body lower part is less than top.
Preferably, the construction of the helical baffle component and Crucible body inner wall includes forming uniform spiral airflow channel.
Optionally, the axis of the helical baffle component is parallel with the axis of the Crucible body.
Optionally, the helical baffle component includes 2-6 helical blade.Preferably, the spiral shell baffle assembly includes 4
Helical blade.
Optionally, the helical baffle component is the helical axis for including helical blade, and helical baffle includes having certain thickness
The shaft portion diameter ratio of the helical blade of degree, helical blade diameter and helical axis is greater than 2:1.
Preferably, the spacing of the helical blade is identical.
Optionally, the helical baffle component includes the raw material area helical baffle that raw material area is arranged in.
Preferably, the helical angle of raw material area helical baffle is 60 ° -90 °, and the single blade face angle of vertical direction is
90°-360°.The spiral of silicon carbide gas phase may be implemented in the angular compliance crucible rotation, and will not cause to gas phase transmission
Too big obstruction.
Optionally, the helical baffle component further includes the gas phase transmission area helical baffle that gas phase transmission area is arranged in.
Preferably, the helical angle of gas phase transmission area helical baffle is 60 ° -90 °, the single blade face angle of vertical direction
It is 60 ° -180 °., which preferably can keep off large granular impurity by lattice, and not need to improve long brilliant temperature.
Optionally, the height ratio of raw material area helical baffle and gas phase transmission area helical baffle are as follows: 48-180:
12-45。
Optionally, raw material area helical baffle includes 2-6 helical blade, and gas phase transmission area helical baffle includes
2-6 helical blade.
Optionally, the gas phase transmission area spiral gauge with a distance from raw material, gas phase transmission area helical baffle length it is gentle
The ratio of distance of the phase transmission range helical baffle apart from seed crystal are as follows: 20-80:12-45:68-245.Optionally, the helical baffle
Component includes the gas phase transmission area helical baffle that gas phase transmission area is arranged in.
Optionally, the helical baffle component further includes the raw material area helical baffle that raw material area is arranged in.
Optionally, gas phase transmission area helical baffle is different from the hand of spiral of raw material area helical baffle.Preferably, earthenware
The rotation direction of crucible component and the hand of spiral of raw material area helical baffle are on the contrary, the hand of spiral with gas phase transmission area helical baffle
It is identical.
After the position of gas phase transmission area helical baffle loads upper surface and the brilliant length of raw material substantially in Crucible body
Crystal lower surface gas phase transmission area；The region of raw material is placed in raw material area substantially Crucible body.
Optionally, the crucible assembly is adiabatic material and is surrounded, and the crucible assembly is inserted into quartz container, described
Heating element is induction type, and the material of the crucible assembly includes graphite.
Preferably, the crucible and heat-insulating material can be rotated.Pass through the orientation of raw material area helical baffle and crucible assembly
Rotation, is converted to spiral by traditional transmission vertically upward for the path that raw material area silicon carbide gas phase is transmitted upwards and transmits upwards,
Lattice gear filtering is carried out in conjunction with the gas phase transmitted in gas phase transmission area helical baffle opposite direction, large granular impurity is prevented to pass to crystallographic direction
It is input into the defect concentration that single-crystal silicon carbide is reduced into crystal.Preferably raw material area helical baffle and gas phase transmission area helical baffle
The hand of spiral it is different.
According to the another aspect of the application, provides a kind of reactor for crystal growth and preparing silicon carbide or three groups
The application of the aspect of the crystal of element nitride.
The beneficial effect that the application can generate includes but is not limited to:
1. the reactor provided herein for crystal growth, by the way that helical baffle is arranged in the Crucible body of reactor
Component changes traditional silicon carbide gas phase transmission mode, is converted to spiral by traditional transmission vertically upward and transmits upwards, spiral shell
The gas phase transmitted in rotation baffle assembly opposite direction carries out lattice gear filtering, and large granular impurity is prevented to be transferred into crystal to crystallographic direction,
Reduce the defect concentration of the monocrystalline such as silicon carbide；Not only effective lattice gear can be carried out to large granular impurity, but not will cause gas phase to
Upper transmission is difficult, is not necessarily to excessively high growth temperature, reduces energy consumption.
2. under conventional gas-phase transmission mode, the gas phase under vacuum growth is unable to get effective control, single crystal growth rate pole
The defects of fast and crystalline quality is very poor, micro-pipe, many types of, dislocation increased significantly, the reaction provided herein for crystal growth
Device passes through the directional-rotation of two helical baffles and crucible assembly, rises while changing gas phase transmission path to gas phase transmission rate
Inhibit regulating and controlling effect to obvious, control action can be played to the gas phase transmission under vacuum, the single crystal growth rate under vacuum compared with
Fast and gas phase can be transmitted orderly upwards, and the defect of the crystal of growth is less, realize vacuum and low temperature fast-growth, reduce growth temperature
Degree reduces growth time, energy saving and cost lowering synergy.
3. the reactor provided herein for crystal growth, helical baffle component sufficiently connect with Crucible body inner wall
Touching, makes that Crucible body heat conduction is more uniform, thermal field is more stable, improves crystal quality；Raw material area helical baffle and raw material
It comes into full contact with, and outer wall and crucible internal walls come into full contact with inwardly conduction heat, are uniformly heated sic raw material, reduce raw material
Edge carbonization, vapor are more uniform orderly.
Detailed description of the invention
The drawings described herein are used to provide a further understanding of the present application, constitutes part of this application, this Shen
Illustrative embodiments and their description please are not constituted an undue limitation on the present application for explaining the application.In the accompanying drawings:
Fig. 1 be the invention relates to a kind of embodiment the reactor for crystal growth schematic diagram.
Fig. 2 be the invention relates to a kind of embodiment crucible assembly schematic cross-sectional view.
Fig. 3 is the schematic top plan view of the gas phase transmission area helical baffle in Fig. 2.
Fig. 4 is a kind of stereoscopic schematic diagram of the gas phase transmission area helical baffle in Fig. 2.
Fig. 5 is a kind of stereoscopic schematic diagram of the gas phase transmission area helical baffle in Fig. 2.
Fig. 6 is the schematic elevation view of the gas phase transmission area helical baffle in Fig. 2.
Fig. 7 is a kind of stereoscopic schematic diagram of the raw material area helical baffle in Fig. 2.
Fig. 8 is a kind of stereoscopic schematic diagram of the raw material area helical baffle in Fig. 2.
Specific embodiment
For the clearer general idea for illustrating the application, carry out in an illustrative manner with reference to the accompanying drawings of the specification detailed
It describes in detail bright.
It can be more clearly understood that the above objects, features, and advantages of the application, with reference to the accompanying drawing and specific implementation
The application is further described in detail in mode.It should be noted that in the absence of conflict, embodiments herein
And the feature in embodiment can be combined with each other.
Many details are explained in the following description in order to fully understand the application, still, the application may be used also
To be implemented using other than the one described here other modes, therefore, the protection scope of the application is not by described below
Specific embodiment limitation.
In addition, in the description of the present application, it is to be understood that term " center ", "upper", "lower", "front", "rear",
The orientation of the instructions such as "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outside", " axial direction ", " radial direction ", " circumferential direction "
Or positional relationship is to be based on the orientation or positional relationship shown in the drawings, and is merely for convenience of description the application and simplifies description, and
It is not that the device of indication or suggestion meaning or element must have a particular orientation, be constructed and operated in a specific orientation, therefore
It should not be understood as the limitation to the application.
In addition, term " first ", " second " are used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance
Or implicitly indicate the quantity of indicated technical characteristic.Define " first " as a result, the feature of " second " can be expressed or
Implicitly include one or more this feature.In the description of the present application, the meaning of " plurality " is two or more, remove
It is non-separately to have clearly specific restriction.
In this application unless specifically defined or limited otherwise, term " installation ", " connected ", " connection ", " fixation " etc.
Term shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or integral；It can be mechanical connect
It connects, is also possible to be electrically connected, can also be communication；It can be directly connected, can also indirectly connected through an intermediary, it can be with
It is the interaction relationship of the connection or two elements inside two elements.For the ordinary skill in the art, may be used
To understand the concrete meaning of above-mentioned term in this application as the case may be.
In this application unless specifically defined or limited otherwise, fisrt feature in the second feature " on " or " down " can be with
It is that the first and second features directly contact or the first and second features pass through intermediary mediate contact.In retouching for this specification
In stating, the description of reference term " one embodiment ", " some embodiments ", " example ", " specific example " or " some examples " etc.
Mean that particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one of the application
In embodiment or example.In the present specification, schematic expression of the above terms are not required to be directed to identical implementation
Example or example.Moreover, particular features, structures, materials, or characteristics described can be in any one or more embodiment or examples
In can be combined in any suitable manner.
Analysis method is as follows in embodiments herein:
1, microcosmic test uses the BX51 type microscope of OLYMPUS company.
2, many types of test uses the HR800 type Raman spectrometer of HORIBA company.
3, dislocation test is after potassium hydroxide corrodes using the BX51 type microscope using OLYMPUS company.
4, inclusion enclave test uses the BX51 type microscope of OLYMPUS company.
Unless otherwise instructed, the raw material in embodiments herein, catalyst and gas are bought by commercial sources,
In, the purity of sic raw material is 99.99%, and the purity of high purity inert gas (Ar or He) is greater than 99.99%.
With reference to Fig. 1, the reactor of the application can be used for preparing single-crystal silicon carbide or group iii elements nitride such as gallium nitride or
The diagrammatic sectional view of the crystal growth of aluminium nitride grows silicon carbide especially suitable for physical vapor transport (abbreviation PVT method)
Monocrystalline.
Reactor for growing crystals includes crucible assembly, and crystal growth occurs in crucible assembly.Reactor packet in Fig. 1
Include crucible assembly；Positioned at 3 inside of crucible cover and it is suitable for supporting the support member for growing crystal；And suitable for crucible assembly is kept
In the heating element of the temperature of growth crystal.
One of one embodiment crucible assembly, with reference to Fig. 2, which includes Crucible body 2,3 and of crucible cover
Helical baffle component 4, the settable seed crystal 31 of the support member of the inside of crucible cover 3, helical baffle component 4 are arranged in Crucible body
In 2, the construction of helical baffle component 4 can form helical airflow passages.The quantity of helical baffle component 4 is at least one, Fig. 2 institute
The quantity of helical baffle component 4 in the embodiment of the crucible assembly shown is 2.Helical baffle component 4 is in Crucible body 2
Upper surface is at least not higher than the position of the crystal face after raw material grows crystalline substance.
Helical baffle component 4 can be fixed by chuck and Crucible body 2 that 2 inner sidewall of Crucible body is arranged in, or
It can be placed in Crucible body 2.The top of helical baffle component 4 is not contacted with seed crystal 31.Preferably, helical baffle component 4
Length direction is parallel to the length of Crucible body 2.
4 diameter of helical baffle component in embodiment shown in Fig. 2 and its mutually level 2 internal diameter phase of Crucible body
Together.In the embodiment being not shown, 4 diameter of helical baffle component can not with its mutually level 2 internal diameter of Crucible body
Together or 2 internal diameter of Crucible body of the same height of 4 diameter of part helix baffle assembly is different.Helical baffle component 4 and earthenware
Crucible main body comes into full contact with so that more uniform, the raising crystal quality that conducts heat in crucible.
As a preferred embodiment, the construction of 2 inner wall of helical baffle component 4 and Crucible body includes forming single
Helical airflow passages.With reference to Fig. 2, helical baffle component 4 is 2, then the construction of 2 inner wall of helical baffle component 4 and Crucible body
Including forming 2 single helical airflow passages, and so on.Preferred single helical airflow passages are uniform channel, i.e. single
The internal diameter of helical duct is uniform.
Further, helical baffle component 4 can be hollow helical blade or be the spiral for including helical blade 43
Axis, preferably helical axis, such as Fig. 3, helical baffle component 4 include 2-6 helical blade 43, and the spacing of helical blade 43 can not
Together, the spacing of preferred helical blade 43 is identical.
With reference to Fig. 1,2, helical baffle component 4 includes 41 He of gas phase transmission area helical baffle that gas phase transmission area is arranged in,
The raw material area helical baffle 42 in raw material area is set.With reference to Fig. 3-6, the pitch angle alpha of gas phase transmission area helical baffle 41 is 60 °-
90 °, which preferably can keep off large granular impurity by lattice, and not need to improve long brilliant temperature.Gas phase transmission area helical baffle
The single blade face angle beta of vertical direction is 60 ° -180 °, and it is miscellaneous to have advanced optimized gas phase transmission area helical baffle lattice gear bulky grain
The efficiency of matter.With reference to Fig. 7,8, the pitch angle alpha of raw material area helical baffle 42 is 60 ° -90 °, which can be with
It realizes the spiral of silicon carbide gas phase, and too big obstruction will not be caused to gas phase transmission.Raw material area helical baffle vertical direction
Single blade face angle beta be 90 ° -360 °, advanced optimized gas phase transmission path.Gas phase transmission area helical baffle 41 and raw material
The hand of spiral of area's helical baffle 42 is different, can to keep off the more effective lattice of large granular impurity progress in gas phase transmission
Filter.
In order to which effective lattice keep off bulky grain and will not cause big obstruction to gas phase transmission, by raw material area helical baffle 42 and gas
The height of phase transmission range helical baffle 41 sets ratio are as follows: 48-180:12-45, raw material area helical baffle 42 include 2-6 helical-blade
Piece, gas phase transmission area helical baffle 41 include 2-6 helical blade.
Distance, gas phase transmission area helical baffle 41 height and gas phase transmission of the gas phase transmission area helical baffle 41 apart from raw material
The ratio of distance of the area's helical baffle 41 apart from seed crystal 31 are as follows: 20-80:12-45:68-245.In preferred embodiment, raw material
Height be about the 1/3 of crucible height, gas phase transmission area spiral is fixed at about the 1/2 of Crucible body 2 every 41 bottom degree, gas phase
The height of transmission range helical baffle 41 is about the 1/10 of crucible height, and the height of raw material area helical baffle 42 is slightly below the height of raw material
Degree, raw material area helical baffle 42 just bury in the feed.Preferably, the height of the height of raw material and raw material area helical baffle 42
Ratio be 1:0.7-0.98.When raw material area helical baffle 42 and 2 inner wall of Crucible body come into full contact with, raw material area helical baffle 42
It is come into full contact with raw material, raw material area helical baffle 42 and 2 inner wall of Crucible body come into full contact with inwardly conduction heat, keep raw material heated more
Add uniformly, reduces raw edges carbonization, improve crystal quality, such as raw material can be sic powder.
Crucible assembly is adiabatic material 5 and is surrounded, and heat-insulating material is preferably graphite fibre such as graphite felt；Crucible assembly is inserted
Enter in quartz container 6；Heating element 7 is induction type, such as heating coil；The material of crucible assembly includes graphite.
As a preferred embodiment, crucible assembly and heat-insulating material 5 are spindle rotationally arranged in quartz container 6.
Optionally, the crucible assembly for surrounding thermal insulation material 5 is arranged on pallet 8, pallet 8 passes through the tray bar across quartz container 6
81 is fixed, and the bottom end of tray bar 81 drives rotation to which Rotary tray 8 drives crucible assembly and thermal insulation material 5 by motor 9.
Reactor passes through 83 fixed placement of support plate 82 and supporting plate.For the heat insulation effect in enhancing reactor, by the outer of quartz container 6
Screwed pipe is set on the tray bar 8 in portion.
Preferably raw material area helical baffle 42 is different with the hand of spiral of gas phase transmission area helical baffle 41.Raw material area spiral
The hand of spiral of partition 42 and the direction of rotation of crucible assembly are identical, the road that raw material such as silicon carbide gas phase in raw material area is transmitted upwards
Diameter is converted to spiral by traditional transmission vertically upward and transmits upwards, the hand of spiral and raw material of gas phase transmission area helical baffle 41
The hand of spiral of area's helical baffle 42 is different, keeps off so that the gas phase transmitted in 41 opposite direction of gas phase transmission area helical baffle carries out lattice
Filter prevents large granular impurity from being transferred into crystal to crystallographic direction, reduces the defect concentration of the crystal such as single-crystal silicon carbide of growth.
Under the long brilliant gas phase transmission mode of traditional PVT method, the gas phase under vacuum growth is unable to get effective control, and monocrystalline is raw
The defects of long rate is exceedingly fast and crystalline quality is very poor, micro-pipe, many types of, dislocation increased significantly.The application passes through in Crucible body
The directional-rotation of gas phase transmission area helical baffle and raw material area helical baffle and crucible assembly is set, gas phase transmission road is changed
Obvious inhibition regulating and controlling effect is played to gas phase transmission rate while diameter, control can be played to the gas phase transmission under vacuum and is made
With the single crystal growth rate under vacuum is very fast and gas phase can be transmitted orderly upwards, and defect is less, realizes the fast fast-growing of vacuum and low temperature
It is long, it reduces growth temperature, reduce growth time, cost efficiency.
A kind of preparation method preparing single-crystal silicon carbide, including that will be included at least one after the raw material distillation in Crucible body
Helical airflow passages gas phase transmission to the seed crystal face that a helical baffle is formed carries out long crystalline substance, and carborundum crystals are made.The application
Preparation method any of the above-described kind of reactor can be used to realize the purpose of the application, that is, include that helical baffle is set in Crucible body
The effect to the bulky grain lattice gear in gas phase transmission can be realized, defect concentration can be reduced, improve the carborundum crystals of preparation
Quality.
Preferably, a kind of preparation method preparing single-crystal silicon carbide, includes the following steps:
(1) the high purity graphite crucible of sic powder, raw material area helical baffle, transmission range helical baffle and seed crystal will be filled with
It is placed in monocrystal growing furnace body and seals, wherein raw material height is slightly above raw material area helical baffle, keeps raw material area helical baffle complete
It buries in raw material entirely；
(2) vacuum in furnace body is evacuated to 10-6Mbar is hereinafter, then pass to high purity inert gas to 300-500mbar, repetition
Vacuum in furnace body is finally evacuated to 10 by this process 2-3 times-6Mbar or less；
(3) high purity inert gas is passed through into furnace body, 1-3h is interior to rise to 10-100mbar for pressure, is continually fed into high-purity lazy
Property gas simultaneously keeps pressure constant；
(4) first crystal growing stages: in the case where keeping pressure constant, furnace body temperature is risen into crystal growth in 3-5h
1950-2150 DEG C of temperature, growth time 5-10h；
(5) second crystal growing stages: it keeps growth temperature constant, pressure in furnace body is down to vacuum 10 in 3-5h-4mbar
It below and remains unchanged, while directional rotating crucible assembly, direction of rotation is consistent with the raw material area helical baffle hand of spiral, turns
Speed is that 10-200 turns/h, while position is constant in crucible vertical direction, growth time 30-100h；
(6) crystal growth terminates, and opens furnace body, and taking out graphite crucible can be obtained the single-crystal silicon carbide of low-defect-density.
Reactor used in the preparation method refers to Fig. 1, is the preferred embodiment in presently filed embodiment.
Single-crystal silicon carbide 1#-3# and comparison single-crystal silicon carbide D1#-D4#, specific preparation method are prepared according to the method described above
It is as shown in table 1 with above method difference.
Table 1
Micro-pipe, many types of, dislocation, inclusion enclave of single-crystal silicon carbide 1#-3# and comparison single-crystal silicon carbide D1#-D4# to preparation
Isostructuralism defect is detected, and testing result is as shown in table 2.
Table 2
From the result of Tables 1 and 2:
1, single-crystal silicon carbide 1# is the single-crystal silicon carbide grown after one group long brilliant parameter optimization combines, is not occurred micro-
The defects of pipe, many types of and inclusion enclave, dislocation density is also maintained at 1000/cm2Within；
2, single-crystal silicon carbide 2# on the basis of single-crystal silicon carbide 1# by crucible assembly revolving speed from 80 turns/h be adjusted to 30 turns/
H, according to table 2, related defects are not obviously increased, and monocrystalline quality is higher；
3, single-crystal silicon carbide 3# is on the basis of single-crystal silicon carbide 1# by the raw material area helical baffle hand of spiral and gas phase zone
The helical baffle hand of spiral is set as identical, and output monocrystalline micropipe density significantly improves, and starts package volume defect, surface two occur
A helical baffle hand of spiral is identical to be unfavorable for micro-pipe and inclusion enclave defects controlling；
4, crucible assembly revolving speed is adjusted to by comparison single-crystal silicon carbide D1# on the basis of single-crystal silicon carbide 1# from 80 turns/h
0 turn/h, according to table 2, output monocrystalline micropipe density and single-crystal silicon carbide 3# are essentially identical, but wrap up volume defect and obviously add
Weight, the combination of crucible assembly directional-rotation and two helical baffles can significantly inhibit the output of package volume defect；
5, two step-length crystallization growth single-crystal silicon carbide is not used in comparison single-crystal silicon carbide D2#, and the crystal growth time is double, raw
Long temperature improves 50 DEG C, and each defect index increases substantially, and shows to grow in the case where more time-consuming, more high energy consumptions
Single-crystal silicon carbide, monocrystalline quality decline to a great extent；
6, comparison single-crystal silicon carbide D3#, D4# further removes raw material area spiral shell on the basis of comparing single-crystal silicon carbide D2#
Partition, gas phase transmission area helical baffle are revolved, every defect index continues to rise appreciably, and shows resistance of no helical baffle to gas phase
Every filtration, monocrystalline quality is unable to get control.
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.Especially for system reality
For applying example, since it is substantially similar to the method embodiment, so being described relatively simple, related place is referring to embodiment of the method
Part explanation.
The above description is only an example of the present application, is not intended to limit this application.For those skilled in the art
For, various changes and changes are possible in this application.All any modifications made within the spirit and principles of the present application are equal
Replacement, improvement etc., should be included within the scope of the claims of this application.
Claims (10)
1. a kind of reactor for crystal growth, which is characterized in that the reactor includes: crucible assembly comprising: crucible master
Body, crucible cover and at least one the helical baffle component being arranged in Crucible body, the raw material distillation being loaded in Crucible body
Crystal growth is carried out after the helical airflow passages at least partly formed afterwards through helical baffle component；On the inside of crucible cover and it is suitable for
The support member of support growth crystal；And the heating element of the temperature suitable for the crucible assembly to be maintained to growth crystal.
2. the reactor according to claim 1 for crystal growth, which is characterized in that the crucible assembly can be rotated.
3. the reactor according to claim 1 for crystal growth, which is characterized in that the helical baffle component is extremely
Small part diameter is identical with its mutually level Crucible body internal diameter；
Preferably, the construction of the helical baffle component and Crucible body inner wall includes forming uniform spiral airflow channel.
4. the reactor according to claim 1 for crystal growth, which is characterized in that the axis of the helical baffle component
Line and the axis of Crucible body are substantially parallel.
5. the reactor according to claim 1 for crystal growth, which is characterized in that the helical baffle component includes
2-6 helical blade.
6. the reactor according to claim 1 for crystal growth, which is characterized in that the helical baffle component is packet
Include the helical axis of helical blade；
Preferably, the spacing of the helical blade is identical.
7. the reactor according to claim 1 to 6 for crystal growth, which is characterized in that the spiral every
Board group part includes the raw material area helical baffle that raw material area is arranged in；
Preferably, the helical angle of raw material area helical baffle is 60 ° -90 °, the single blade face angle of vertical direction is 90 ° -
360°。
8. the reactor according to claim 7 for crystal growth, which is characterized in that the helical baffle component also wraps
Include the gas phase transmission area helical baffle that gas phase transmission area is set；
Preferably, the helical angle of gas phase transmission area helical baffle is 60 ° -90 °, and the single blade face angle of vertical direction is
60°-180°。
9. the reactor according to claim 8 for crystal growth, which is characterized in that gas phase transmission area spiral every
Plate is different from the hand of spiral of raw material area helical baffle.
10. the reactor of crystal growth is used for described in -9 according to claim 1, which is characterized in that the crucible assembly is exhausted
Hot material is surrounded, and the crucible assembly is inserted into quartz container, and the heating element is induction type, the crucible assembly
Material includes graphite；
Preferably, the crucible assembly and heat-insulating material can be rotated.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111748843A (en) * | 2020-07-09 | 2020-10-09 | 北京北方华创微电子装备有限公司 | Silicon carbide single crystal growth device |
| CN111945219A (en) * | 2020-09-11 | 2020-11-17 | 山东天岳先进材料科技有限公司 | Silicon carbide crystal growth method and device |
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| JPH09235176A (en) * | 1996-03-04 | 1997-09-09 | Sumitomo Sitix Corp | Quartz crucible for melting silicon |
| CN206173480U (en) * | 2016-09-19 | 2017-05-17 | 山东天岳晶体材料有限公司 | Crucible |
| CN109355706A (en) * | 2018-11-02 | 2019-02-19 | 山东天岳先进材料科技有限公司 | A kind of silicon carbide monocrystal growth device |
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2019
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| JPH0558774A (en) * | 1991-09-03 | 1993-03-09 | Sanyo Electric Co Ltd | Vessel for silicone carbide single crystal growing device |
| JPH09235176A (en) * | 1996-03-04 | 1997-09-09 | Sumitomo Sitix Corp | Quartz crucible for melting silicon |
| CN206173480U (en) * | 2016-09-19 | 2017-05-17 | 山东天岳晶体材料有限公司 | Crucible |
| CN109355706A (en) * | 2018-11-02 | 2019-02-19 | 山东天岳先进材料科技有限公司 | A kind of silicon carbide monocrystal growth device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111748843A (en) * | 2020-07-09 | 2020-10-09 | 北京北方华创微电子装备有限公司 | Silicon carbide single crystal growth device |
| CN111748843B (en) * | 2020-07-09 | 2022-02-22 | 北京北方华创微电子装备有限公司 | Silicon carbide single crystal growth device |
| CN111945219A (en) * | 2020-09-11 | 2020-11-17 | 山东天岳先进材料科技有限公司 | Silicon carbide crystal growth method and device |
| CN111945219B (en) * | 2020-09-11 | 2021-07-09 | 山东天岳先进科技股份有限公司 | Silicon carbide crystal growth method and device |
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| CN110079863B (en) | 2020-07-14 |
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