CN110067026A - A kind of single-crystal silicon carbide and its PVT long crystal method - Google Patents
A kind of single-crystal silicon carbide and its PVT long crystal method Download PDFInfo
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- CN110067026A CN110067026A CN201910344555.0A CN201910344555A CN110067026A CN 110067026 A CN110067026 A CN 110067026A CN 201910344555 A CN201910344555 A CN 201910344555A CN 110067026 A CN110067026 A CN 110067026A
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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
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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
- C30B23/06—Heating of the deposition chamber, the substrate or the materials to be evaporated
- C30B23/066—Heating of the material to be evaporated
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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)
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Abstract
This application involves a kind of single-crystal silicon carbide and its PVT long crystal methods, belong to field of crystal growth.The PVT long crystal method of the single-crystal silicon carbide includes the following steps: to provide a Crystal growth device, the Crystal growth device includes weight sensor, crucible and the liftable charging portion in crucible, the charging portion is for loading sic raw material, and the weight sensor is for detecting sic raw material weight in charging portion；Long crystalline substance is carried out after charging portion is loaded sic powder, long crystalline substance includes the first crystal growing stage and the second crystal growing stage, and the different piece in adjustment charging portion is placed in the high-temperature region in crucible and carries out long crystalline substance.The PVT long crystal method can accurately automatically control position of the charging portion in thermal field, and the long brilliant ambient stable of single-crystal silicon carbide, the quality of the carborundum crystals of growth is high, and the long brilliant raw material of the silicon carbide that can sufficiently volatilize improves the utilization rate of long brilliant raw material, saved production cost.
Description
Technical field
This application involves a kind of single-crystal silicon carbide and its PVT long crystal methods, belong to field of crystal growth.
Background technique
Silicon carbide has high voltage, false loss, high thermal conductivity, low-leakage current etc. excellent as a kind of novel semiconductor material
Different performance.It is generally considered the substitution optimal semiconductor device of silicon-based power devices.Physical vapor transport
(Physical Vapor Transport-PVT) is the common method for growing carborundum crystals, and this method is by silicon carbide seed
Crystalline substance setting is covered in graphite crucible or top, graphite crucible are provided with the silicon carbide powder as growth raw material, control growth temperature
Degree is so that growth raw material resolves into is transported at seed crystal inside the graphite crucible under the driving of axial-temperature gradient after gaseous component
Crystalline growth carborundum crystals.
Chinese patent application CN1069299123A provides a kind of split type growing silicon carbice crystals crucible, comprising: uses
In the raw material cavity for holding SiC crystal growth raw material；It is nested in the top of the raw material cavity relatively movably to form crystal knot
The growth chamber in crystalline region domain, described be grown in have growth room and the seed crystal support on the roof of the growth room；The growth
The side wall of room is formed as the double-layer structure being made of interior bucket and outer barrel.Seperated crucible in the patent application is mobile main body crucible
Charging chamber, the environment of crystal growth stability of the set-up mode of the fission crucible is poor, influences crystal growth quality, and the fission
Distillation raw material in crucible, which easily enters at the gap of nested parts, easily causes blocking after cooling, so that the stability of crucible movement,
Accuracy and flexibility are poor, and then influence the quality of growth crystal.
Summary of the invention
To solve the above-mentioned problems, present applicant proposes a kind of single-crystal silicon carbides and its PVT long crystal method, this method not to move
Moveable charging portion is arranged in crucible, and adjusts charging portion in crucible according to different crystal growing stages for dynamic seed crystal and crucible
Interior high temperature zone position, the PVT long crystal method can stable crystal growing environment, improve long brilliant quality, can sufficiently volatilize long brilliant former
Material improves the utilization rate of long brilliant raw material, saves production cost.
According to the one aspect of the application, a kind of PVT long crystal method of single-crystal silicon carbide is provided, which is characterized in that packet
Include following step:
A Crystal growth device is provided, which includes seed crystal, crucible and the dress that can be gone up and down to seed crystal direction in crucible
Material portion, the charging portion is for loading sic raw material；
Long crystalline substance will be carried out after charging portion loading sic powder and prepares single-crystal silicon carbide, and the long brilliant step includes:
First crystal growing stage: the 1/2 height any portion below in charging portion is placed in the high-temperature region in crucible, this stage carbon
SiClx raw material sublimation rate is less than the first sublimation rate；
Second crystal growing stage: when sic raw material sublimation rate be the first sublimation rate when, reduce charging portion so that charging portion by
The part of high-temperature region heating moves up, and when sic raw material sublimation rate is the second sublimation rate, stops reducing charging portion, cool down cold
But, the single-crystal silicon carbide is obtained；
Wherein, first sublimation rate is 30%-60%, and second sublimation rate is 70%-90%.
Optionally, the rate that charging portion is reduced in second crystal growing stage is 0.2-2mm/h.Further, the drop
The rate in low charging portion is 0.5-1.5mm/h.Further, the rate for reducing charging portion is 1mm/h.
Optionally, the 1/4 height any portion below in the charging portion in first crystal growing stage is placed in crucible
High-temperature region.Further, the bottom part in the charging portion in first crystal growing stage is placed in the high-temperature region in crucible.
Optionally, first sublimation rate is 35%.
Preferably, the temperature of crystal growing stage is 2273-2473K, time 50-200h, and the pressure for being filled with inert gas is
0-104Pa.Further, the temperature of crystal growing stage is 2373K, time 130h, pressure 103In the inert atmosphere of Pa.It is described
Preferably, the inert gas is selected from argon gas or helium.
Preferably, the cooling down step include: by electric current near 0 in 10h after cooled to room temperature.
Optionally, first crystal growing stage further includes removal step, and the temperature of the removal step is 1700K-
1800K, time are not less than 1.5h, pressure 5-105Pa.Further, first crystal growing stage further includes removal step, institute
The temperature for stating removal step is 1700K-1800K, and the time is not less than 1.5h, pressure 5-105Pa。
Optionally, the Crystal growth device includes: crucible, be oppositely arranged in the crucible charging portion for loading raw material and
Seed crystal, the charging portion include at least one gas vent, and the charging portion can back and forth be moved by regulating mechanism to seed crystal direction
It is dynamic；
Heating device makes distillation raw material from gas phase transmission after gas vent outflow by induction heating mode heating crucible
It is long brilliant to seed crystal face；And
Insulation construction, the crucible setting is intracavitary in insulation construction, for controlling crucible heat dissipation.
Optionally, the crucible and the diameter in charging portion ratio are 100-280:60-240, the thickness of the crucible and charging portion
Ratio is spent for 15-25:5-10, and the height ratio in the crucible and charging portion is 140-350:60-150.Further, the crucible and
The diameter ratio in charging portion is 120-250:80-210.Further, the crucible and the diameter in charging portion ratio are 140-230:
The thickness ratio in 100-190, the crucible and charging portion is 15-23:5-9, and the height ratio in the crucible and charging portion is 180-
310:70-130.Further, the crucible and the diameter in charging portion ratio are 185:110, the thickness of the crucible and charging portion
Ratio is spent for 16:5, and the height ratio in the crucible and charging portion is 260:70.
Optionally, the gas phase transmission path length of the sic raw material of the distillation be greater than the sic raw material surface with
The distance between seed crystal.
Optionally, the charging portion includes charging main body and to be arranged in the cover of its overthe openings, the cover and charging
Main body forms the gas vent.
Preferably, the cover is greater than the charging body openings to the projected area in the charging body openings direction
Area.
Preferably, the charging main body is charging ladle.
Optionally, the cover includes lid ontology and supporting element, the supporting element setting lid ontology and charging main body it
Between.
Preferably, the supporting element is removably connect with the lid ontology and/or the charging main body.
Preferably, the supporting element includes first end and second end, and the first end is fixedly connected with the lid ontology, institute
Charging main body is stated removably to connect with the second end.
Preferably, the second end of the supporting element is plugged in the groove of the wall portion top end face of the charging body openings.
Preferably, the supporting element includes that at least two is respectively perpendicular and is set to the lid ontology and the charging main body
Support rod.
Optionally, it is described at least partly distillation raw material from the direction that gas vent flow out be first direction, the first party
To the first angle α having with the axis of the seed crystal less than 90 DEG C.Preferably, first angle α is 0-60 DEG C.More preferably
Ground, first angle α are 0 DEG C.
Preferably, the cover includes lid ontology, supporting element and baffle, and the baffle is fixedly connected with lid ontology, described
At least two parts in the elongated end of baffle, charging main body and supporting element constitute the gas vent, and at least baffle end is prolonged
Stretching direction and the seed crystal axis has the first angle α, and the projected area in the baffle to the charging body openings direction is big
In the area of the charging body openings.
Preferably, the elongated end of the baffle is not less than the charging body openings；It is highly preferred that the extension of the baffle
End is higher than the charging body openings.
Preferably, the baffle be vertically set on the lid ontology and/or, the opening that the elongated end of the baffle is constituted with
The shape of the charging body openings is roughly the same.
Preferably, the lid ontology and the baffle are integrally formed.
Optionally, the cover is by the roughness on at least partly surface of heat radiation less than 6.3 μm.Preferably, described
The roughness on cover surface substantially parallel with the seed crystal is less than 3.2 μm.
Optionally, the Crystal growth device further includes weight sensor, the weight sensor can measure charging portion and/or
The weight of raw material.
Preferably, the Crystal growth device further includes control unit, and described control unit is measured according to weight sensor
The weight of charging portion and/or raw material controls the movement of charging portion by regulating mechanism.Control unit can be automatic control or manual
Control.
Optionally, the regulating mechanism is elevating mechanism or shift mechanism.
Optionally, the Crystal growth device further includes furnace body, and the insulation construction is arranged in furnace body, the heating device ring
Around setting outside furnace body；
The regulating mechanism includes tray bar, lead screw, lifting platform and screw drives assembly, the screw drives assembly and silk
Thick stick worm drive cooperation controls lifting of lifting table, tray bar is arranged on the lifting platform, the tray bar is through crucible, heat preservation knot
Structure and furnace body simultaneously can drive charging portion to go up and down.
Preferably, the regulating mechanism further includes the pallet being arranged on the tray bar, and the charging portion setting is being held in the palm
On disk.
Preferably, the regulating mechanism further includes bellows, and the bellows-sheathed is located on tray bar, the bellows point
It is not abutted with lifting platform and furnace body.
Preferably, the material of the crucible, charging portion and insulation construction is graphite, and the heating device is intermediate frequency coil.
Optionally, the weight sensor is arranged on lifting platform, and the tray bar is contacted with the weight sensor.
According to further aspect of the application, a kind of single-crystal silicon carbide is provided, it is brilliant by any of the above-described PVT long
Method is prepared.
In the application, the high-temperature region refers to the highest region of the temperature in crucible, the generally centre-height of crucible
The high-temperature region in region, but used crucible, thermal field can shift.
In the application, sic raw material quality and the silicon carbide before long crystalline substance that the sic raw material sublimation rate refers to distillation
The ratio of total mass of raw material.
In the application, the height that sic raw material is loaded in the charging portion accounts for the 70-100% of charging portion height.
The beneficial effect that the application can generate includes but is not limited to:
1. silicon carbide PVT long crystal method provided herein passes through the dress of the accurately different crystal growing stages of control silicon carbide
The position of thermal field of the material portion in crucible, and guarantee the stability of the environment of crystal growth, the single-crystal silicon carbide of high quality is made.
2. PVT long crystal method provided herein can be filled by accurately automatically controlling position of the charging portion in thermal field
Divide volatilization long brilliant raw material, improves the utilization rate of long crystalline substance raw material, saved production cost.
3. preventing big by increasing the transmitting range of distillation raw material atmosphere in PVT long crystal method provided herein
The movement to seed crystal direction of grain carbon particle, avoids micro-pipe in crystal growing process, many types of, dislocation, inclusion enclave isostructuralism
The appearance of defect.
4. the cover in the charging portion of Crystal growth device used in PVT long crystal method provided herein is parallel with seed crystal
The roughness of upper surface is small, and the heat radiation that may make distillation raw material to be subject to is uniform.
5. Crystal growth device provided herein can detect the weight of raw material, and accurately adjust charging according to the weight of raw material
Position of the portion in thermal field, control accuracy is high, and the quality of the carborundum crystals of growth is high.
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 Crystal growth device positive schematic cross-sectional view.
Fig. 2 be the invention relates to a kind of Crystal growth device positive schematic cross-sectional view.
Fig. 3 be the invention relates to a kind of Crystal growth device positive schematic cross-sectional view.
Fig. 4 be the invention relates to a kind of Crystal growth device positive schematic cross-sectional view.
Fig. 5 be the invention relates to a kind of Crystal growth device positive schematic cross-sectional view.
Fig. 6 be the invention relates to Crystal growth device part regulating mechanism schematic diagram.
Fig. 7 be the invention relates to a kind of Crystal growth device perspective cross-sectional schematic diagram.
Fig. 8 be the invention relates to a kind of PVT long crystal method flow chart.
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.
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%.
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.
The calculation method of the silicon carbide sublimation rate of the application is as follows:
Silicon carbide sublimation rate %=(total silicon carbide material quality-surplus stock quality)/total silicon carbide material quality
With reference to Fig. 1, one embodiment of the application discloses a kind of Crystal growth device, which includes crucible 2, heating
Device 3, insulation construction 4, seed crystal 5, regulating mechanism 6 and charging portion 7.It is oppositely arranged in crucible 2 for loading sic raw material
Charging portion 7 and seed crystal 5, charging portion 7 include at least one gas vent, and charging portion 7 can be past to 5 direction of seed crystal by regulating mechanism
It is multiple mobile；Heating device 3 passes distillation raw material from gas phase after gas vent outflow by induction heating mode heating crucible 2
It is long brilliant to transport to 5 surface of seed crystal；And insulation construction 4, the setting of crucible 2 is intracavitary in insulation construction 4, radiates for controlling crucible 2.It is logical
Moving up and down for charging portion 7 is crossed, the sic raw material in charging portion 7 can be allowed sufficiently to be sublimed into silicon carbide atmosphere, it is possible to reduce
Charge improves the utilization rate of sic powder；Reduce charge, increases growing silicon carbice crystals space, stabilize growth
Environment.
Preferably, crucible 2 is graphite crucible, and charging portion 7 is graphite material, and insulation construction 4 is graphite felt, but is not limited to
Above-mentioned material.Preferably the ratio of the diameter of crucible, thickness and height is 100-280:15-25:140-350, such as can be
The diameter of crucible is 120-250mm, thickness 15-25mm, height 140-350mm, but is not limited to above range numerical value.
More specifically, charging portion 7 is arranged in the seal chamber of crucible 2, and crucible 2 is arranged in the cavity of insulation construction 4.
In one embodiment, charging portion 7 is charging barrel-like structure, and the opening of charging ladle is gas vent, charging ladle
Seed crystal 5 is arranged in the crucible cover inside of interior filling sic raw material, the relative direction of sic raw material, and charging ladle can pass through adjusting machine
Structure is gone up and down to 5 direction of seed crystal.
As an implementation, heating device 3 can be Medium frequency induction coil, and Medium frequency induction coil passes through induction mode pair
Crucible is heated, and is heated by heat radiation mode to charging portion inside crucible, so that sic raw material distils from gas vent
I.e. gas phase transmission is long brilliant to 5 surface of seed crystal after the outflow of charging ladle opening.
With reference to Fig. 2, preferably in a kind of embodiment, charging portion 7 includes charging main body 71 and is arranged in its overthe openings
Cover 72, cover 72 and charging main body 71 formed gas vent.Cover 72 and charging the non-contact setting of main body 71, cover 72 with
Gap between the main body 71 that charges is gas vent, the sic raw material gas of distillation from charging main body 71 flow out after at least partly
It is flowed out after colliding cover 72 from gas vent.In preferred embodiment, cover 72 is to charging 71 opening direction of main body
Projected area is greater than the area that charging main body 71 is open.Such as, but not limited to, cover 72 and the charging opening of main body 71 are concentric
Circular shape, 72 area of cover be greater than charging main body 71 be open area.More specifically, charging main body 71 can be bucket
Shape structure.
With reference to Fig. 3, as a kind of specific embodiment, cover 72 includes lid ontology 721 and supporting element 722, supporting element
Between lid ontology 721 and charging main body 71, supporting element 722 includes first end and second end, first end and Gai Benti for 722 settings
721 are fixedly connected, and charging main body 71 is removably connect with second end；It specifically can be the second end grafting of supporting element 722
In the groove for the wall portion top end face that charging main body 71 is open, supporting element 722 is respectively perpendicular including at least two and is set to lid ontology
721 and charging main body 71 support rod.Preferably, the quantity of supporting element 722 is 4, and supporting element 722 is strip structure.
The principle of single-crystal silicon carbide is prepared according to PVT method, sic raw material is after by heat sublimation from charging portion 7 through gas vent
Outflow carries out the long crystalline substance of single-crystal silicon carbide through gas phase transmission to seed crystal.At least partly distillation raw material is from the direction that gas vent flows out
The axis of first direction A, first direction A and seed crystal 5 has the first angle α less than 90 DEG C.Preferably, the first angle α is 0-
60℃.It is furthermore preferred that the first angle α is 0 DEG C.
With reference to Fig. 4, it is preferable that cover 72 includes lid ontology 721, supporting element 722 and baffle 723, baffle 723 and Gai Benti
721 are fixedly connected, and the extending direction of baffle 723 is first direction A, elongated end, charging main body 71 and the supporting element of baffle 723
722 constitute gas vent.Baffle 723 can be for around the ring structure of the open loop of charging main body 71 or closed loop；Baffle 723 can be with
For plate or twisted plate, the extending direction of the baffle 723 when baffle 723 is straight panel is first direction A, first direction A and seed
Brilliant 5 axis have the first angle α；When baffle 723 is twisted plate, 723 end extending direction of baffle is first direction A, first party
There is the first angle α to A and 5 axis of seed crystal.Preferably, baffle 723 is greater than to the projected area of charging 71 opening direction of main body
The area that the main body 71 that charges is open.Baffle 723 is attached to the end of lid ontology 721 or inside or baffle 723 are Gai Benti
721 bending parts being integrally formed.At the initial stage of silicon carbide monocrystal growth, the lower part in charging portion 7 is placed in crucible 2
High-temperature region, baffle 723 convey distillation raw material atmosphere down backward to lid ontology 721, behind the high-temperature region of 2 lower section of crucible
Raw material atmosphere can be conveyed up at seed crystal 5, and the transmitting range that can increase SiC atmosphere to seed crystal 5 is arranged such, prevent due to
SiC powder silicon carbide seriously after carbon particle be delivered up, avoid micro-pipe in crystal growing process, many types of, dislocation, inclusion enclave
The appearance of isostructuralism defect.
In preferred embodiment, the elongated end of baffle 723 is higher than charging main body 71 and is open, Gai Benti 721 and baffle 723
It is integrally formed, baffle 723 is vertically set on lid ontology 721, and the opening and charging main body 71 that the elongated end of baffle 723 is constituted are open
Shape it is roughly the same.The cover 72 of the Crystal growth device and the relative position of charging main body 71, the elongated end such as baffle 723 are high
It is open in charging main body 71, the exposure concentration of distillation raw material atmosphere and the main body 71 that charges can be reduced, it is former by distillation to reduce charging portion 7
Expect the corrosion of atmosphere.
Preferably, charging main body 71 be charging tubular structure, charge main body 71 diameter 60-240mm, thickness 5-10mm,
Height 60-150mm；The diameter 80-250mm of lid ontology 721, thickness 5-10mm, height 5-20mm；The height 10- of supporting element 722
50mm, width 5-40mm, thickness 2-8mm；The width of the groove for the wall portion top end face that the insertion charging main body 71 of supporting element 722 is open
2-8mm, depth 3-5mm.The size in above-mentioned charging portion 7 can be expanded or shunk in proportion, limit its dimension scale, but be not limited to
Above-mentioned specific value.Crystal growth quality can be improved in the dimensional structure of the Crystal growth device.
The heat radiation of the upper surface of lid ontology 721 acts on, in order to pass the sic raw material after distillation in gas phase
It is heated evenly, the roughness of lid ontology 721 is controlled less than 6.3 μm, but be not limited to the upper surface of lid ontology 721 during defeated,
It is preferred that by the control of the roughness of lid ontology 721 or cover 72 for less than 3.2 μm.
With reference to Fig. 5, during Crystal growth device use, in order to more accurately adjust thermal field ring of the charging portion 7 in crucible 2
Border in embodiment as one preferred, will install weight sensor 8 and control unit 9, weight sensor in Crystal growth device
8 can measure the raw material weight in charging portion 7, and the raw material weight measured is transmitted to control unit 9, and control unit 9 is according to
Raw material weight through storing is judged that control unit 9 is logical according to judging result with height relationships of the charging portion 7 in crucible 2
It crosses and controls to adjust mechanism 6 and then adjust position of the charging portion 7 in thermal field.Position of the charging portion 7 in thermal field can not only lead to
Crossing the automatic control of control unit 9 can also manually control, and manually control adjusting machine according to the raw material weight that weight sensor 8 is shown
The lifting of structure 6 and then the position for adjusting thermal field of the charging portion 7 in crucible 2.
Regulating mechanism 6 can be elevating mechanism or can be shift mechanism.
As an implementation, Crystal growth device further includes furnace body 10, and insulation construction 4 is arranged in furnace body 10, heating dress
3 are set to be circumferentially positioned at outside furnace body 10；Regulating mechanism 6 includes tray bar 61, lead screw 62, lifting platform 63 and screw drives assembly 64,
Screw drives assembly 64 and 62 worm drive of lead screw cooperation control lifting platform 63 are gone up and down, and tray bar 61, support are arranged on lifting platform 63
Disk bar 61 is through crucible 2, insulation construction 4 and furnace body 10 and charging portion 7 can be driven to go up and down.Screw drives assembly 64 is servo electricity
Machine, lead screw 62 are ball-screw, and ball-screw is fixed in support plate 67, and servo motor drives ball-screw to turn by shaft coupling
Dynamic, ball screw turns drive lifting platform 63 to go up and down.It is that regulating mechanism 6 includes lifting platform 63, lead screw 62 and support plate with reference to Fig. 6
67 schematic elevation view.
With reference to Fig. 7, tray bar 61 can be directly fixedly connected with charging portion 7；Or the fixed tray 65 on tray bar 61,
Charging portion 7 is placed or is removably attachable on pallet 65, the connection relationship in pallet 65 and charging portion 7 is not limited to above-mentioned side
Formula, as long as realizing that charging portion 7 is steadily gone up and down under the drive of regulating mechanism 6.
Tray bar 61 runs through during crucible 2, insulation construction 4 and furnace body 10 drive charging portion 7 to go up and down and dissipates in order to prevent
Heat, is arranged bellows 66 on the tray bar 61 between lifting platform 63 and furnace body 10, bellows 66 respectively with lifting platform 63 and furnace
Body 10 abuts, and can prevent from radiating from through-hole during lifting platform 63 is gone up and down, and bellows 66 can further prevent holding in the palm
The heat dissipation of disk bar 61, and guarantee the thermal field ambient stable in crucible 2.
As a preferred embodiment, being arranged weight sensor 8 on lifting platform 63, tray bar 61 and weight are passed
Sensor 8 contacts, then raw material weight can be transferred to the weight of the real-time recording and displaying raw material of weight sensor 8 by tray bar 61
Amount.
With reference to Fig. 8, single-crystal silicon carbide PVT long crystal method include removal step, the first crystal growing stage, the second crystal growing stage and
The cooling down stage.Specifically, single-crystal silicon carbide PVT long crystal method include the following steps: using any of the above-described Crystal growth device into
The long brilliant step of row comprising: the first crystal growing stage: sic raw material sublimation rate is less than the first sublimation rate, 1/2 height in charging portion
Any portion below is placed in the high-temperature region in crucible；Second crystal growing stage: when sic raw material sublimation rate is the first sublimation rate
When, starting, which reduces charging portion, moves up the part that charging portion is heated by high-temperature region, when sic raw material sublimation rate is the second sublimation rate
When, stop reducing charging portion, cooling down obtains the single-crystal silicon carbide.First sublimation rate be 30%-60%, second
Sublimation rate is 70%-90%.
The long chip of single-crystal silicon carbide PVT method includes heating the middle lower half portion in charging portion first at long brilliant initial stage, i.e., will dress
The lower half portion in material portion is placed on the high-temperature region of crucible, and high-temperature region is the center of crucible, with the volatility weight of SiC raw material
It can reduce, tray bar bottom heaviness inductor can record the weight of SiC raw material in charging in real time；It is surplus after sic raw material distillation
When the weight of remaining raw material is original substantially half, the indoor Si/C of growth chamber becomes rich C environment from rich Si environment, is easy to draw
It is unbalance to play Si/C, easily causes the appearance that crystal is many types of, the heated high-temperature region for adjusting charging portion at this time is moved to the top in charging portion
It is dynamic to improve the indoor Si/C environment of growth chamber, improve crystal quality；Sic raw material sublimes up into life when original about 1/5
The long indoor Si/C of chamber is in imbalance state, and substantially C is in the majority, stops reaction.
As a kind of specific embodiment, a kind of Crystal growth device using with reference to Fig. 5 prepares the PVT long of single-crystal silicon carbide
Crystal method includes the following steps:
(1) it is packed into 1000g SiC raw material in the charging portion of tubbiness, charging portion is moved to crucible high-temperature region lower part, it is long
Brilliant program starts, and the pressure in furnace chamber is extracted into 10 with 1h-5Furnace temperature is raised to 1773K in 1h by Pa, is passed through Ar gas, and pressure is 5-
105Pa keeps 2h in this temperature；The step can remove sic powder, in crucible, aqueous vapor, the grease in charging portion etc. etc. it is miscellaneous
Matter；
(2) middle and lower part in the portion of charging is moved to high-temperature region, pressure is reduced to 0-10 with 2h4Pa, furnace temperature are raised to 2273-
2473K enters crystal growing stage afterwards；Wherein, the long brilliant time is 50-200h, is continually fed into Ar gas, wherein high-temperature region substantially earthenware
The region of the centre-height of crucible；
(3) the middle lower half portion for heating charging portion first at long brilliant initial stage, as the volatility weight of SiC raw material can be reduced,
Tray bar bottom heaviness inductor can record the weight of SiC raw material in charging portion in real time；
When raw material in charging portion reduces to 650g (the first sublimation rate), electric motor starting drives the charging portion on pallet to moving down
Dynamic, the middle and upper part of charging ladle point is moved to high-temperature region by movement speed 0.2-2mm/h；
When material in charging ladle reduces to 100g (the second sublimation rate), motor stopping moves down end；
(4) electric current is dropped to 0 by last 10h, and carborundum crystals 893g, user's legal system is made in cooled to room temperature
The yield of the carborundum crystals obtained is high, avoids micro-pipe in crystal growing process, many types of, dislocation, inclusion enclave isostructuralism defect
Appearance.
The dimensional parameters of the Crystal growth device used are as follows: crucible: diameter 185mm, thickness 16mm, height 260mm；Cartridge:
Diameter 110mm, thickness 5mm, height 70mm；Cartridge upper cover: diameter 135mm, thickness 4mm, height 11mm；Cartridge four
Leg: height 17mm, width 20mm, thickness 2mm；Charge barrel upper grooves: width 2mm, depth 3mm.
The central area of high-temperature region substantially crucible in crucible, meeting high-temperature region can occur upwards after crucible is used for multiple times
Offset, can be judged according to the convex rate of single-crystal silicon carbide obtained.
Single-crystal silicon carbide 1#-6# is prepared according to the method described above, it is as shown in table 1 with above-mentioned preparation method difference.
Table 1
The yield of the single-crystal silicon carbide 1#-6# prepared in conjunction with 1 Dui of table, micro-pipe, many types of, dislocation include screw dislocation (abbreviation
TSD it) is detected with plane surface dislocation (abbreviation BPD), inclusion enclave isostructuralism defect, testing result is as shown in table 2.
Table 2
The charging portion in conjunction with known to data analysis in Tables 1 and 2 is placed in first liter of the initial position of high-temperature region, sic raw material
Magnificent rate, the fall off rate in charging portion, the second sublimation rate of sic raw material will affect the quality of carborundum crystals obtained.The application
Preparation method made from single-crystal silicon carbide 1#-6# do not occur it is many types of.The first angle known to single-crystal silicon carbide 1#, 5# and 6#
α is affected to the micro-pipe of single-crystal silicon carbide, dislocation, yield, micro-pipe and dislocation in the single-crystal silicon carbide that the first angle is 0 °
Content it is minimum and yield is high.By 1mm/h and 2mm/h difference the single-crystal silicon carbide 3# obtained and carbon of the fall off rate in charging portion
Micro-pipe, dislocation content in SiClx monocrystalline 4# is it is found that the dislocation in single-crystal silicon carbide 3# is far below single-crystal silicon carbide 4#, charging portion
Fall off rate have to micro-pipe, the dislocation of the single-crystal silicon carbide of preparation and influence that yield is very big.Charging portion is placed in high-temperature region
Position is affected to the former first material sublimation rate of silicon carbide；It can be seen that charging portion is placed in high-temperature region from single-crystal silicon carbide 1#, 3#
Position it is larger to yield impact, and micro-pipe and dislocation when charging portion is placed in 1/4 position of high-temperature region in single-crystal silicon carbide
Content it is low.Second sublimation rate is higher, and obtained yield is higher, and inclusion enclave is more serious in single-crystal silicon carbide.
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 PVT long crystal method of single-crystal silicon carbide, which is characterized in that include the following steps:
One Crystal growth device is provided, the Crystal growth device include seed crystal, crucible and in crucible can to seed crystal direction go up and down charging portion,
The charging portion is for loading sic raw material；
Long crystalline substance will be carried out after charging portion loading sic powder and prepares single-crystal silicon carbide, and the long brilliant step includes:
First crystal growing stage: the 1/2 height any portion below in charging portion is placed in the high-temperature region in crucible, this stage silicon carbide
Raw material sublimation rate is less than the first sublimation rate；
Second crystal growing stage: when sic raw material sublimation rate is the first sublimation rate, charging portion is reduced so that charging portion is by high temperature
The part of area's heating moves up, when sic raw material sublimation rate is the second sublimation rate, stopping reduction charging portion, and cooling down, i.e.,
The single-crystal silicon carbide is made；
Wherein, first sublimation rate is 30%-60%, and second sublimation rate is 70%-90%.
2. PVT long crystal method according to claim 1, which is characterized in that reduce charging portion in second crystal growing stage
Rate be 0.2-2mm/h；Preferably, the rate for reducing charging portion is 1mm/h.
3. PVT long crystal method according to claim 1, which is characterized in that charging portion in first crystal growing stage
1/4 height any portion below is placed in the high-temperature region in crucible.
4. PVT long crystal method according to claim 1, which is characterized in that first sublimation rate is 35%.
5. PVT long crystal method according to claim 1, which is characterized in that the temperature of crystal growing stage is 2273-2473K, when
Between be 50-200h, be filled with inert gas pressure be 0-104Pa；
Preferably, the cooling down step include: by the heated current of Crystal growth device near 0 in 10h after naturally cool to
Room temperature.
6. PVT long crystal method according to claim 1, which is characterized in that first crystal growing stage further includes removal of impurities step
Suddenly, the temperature of the removal step is 1700K-1800K, and the time is not less than 1.5h, pressure 5-105Pa。
7. PVT long crystal method according to claim 1, which is characterized in that the Crystal growth device includes: crucible, the earthenware
The charging portion for loading raw material and seed crystal are oppositely arranged in crucible, the charging portion includes at least one gas vent, the dress
Material portion can be moved back and forth by regulating mechanism to seed crystal direction；
Heating device to distil raw material from gas phase transmission after gas vent outflow to seed by induction heating mode heating crucible
Brilliant surface is long brilliant；And
Insulation construction, the crucible setting is intracavitary in insulation construction, for controlling crucible heat dissipation.
8. PVT long crystal method according to claim 1, which is characterized in that the crucible and the diameter in charging portion ratio are
The thickness ratio in 100-280:60-240, the crucible and charging portion is 15-25:5-10, the height ratio of the crucible and charging portion
For 140-350:60-150.
9. PVT long crystal method according to claim 1 to 8, which is characterized in that the silicon carbide of the distillation is former
The gas phase transmission path length of material is greater than the distance between the sic raw material surface and seed crystal.
10. a kind of single-crystal silicon carbide, which is characterized in that be prepared by PVT long crystal method of any of claims 1-9
It arrives.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112410732A (en) * | 2020-11-20 | 2021-02-26 | 湖南烁科晶磊半导体科技有限公司 | In-situ pretreatment method for molecular beam epitaxy source material |
| CN113151900A (en) * | 2021-04-30 | 2021-07-23 | 山东天岳先进科技股份有限公司 | Silicon carbide crystal and preparation method thereof |
| CN113388888A (en) * | 2021-06-22 | 2021-09-14 | 山东天岳先进科技股份有限公司 | Silicon carbide crystal, seed crystal used by same and preparation method of seed crystal |
| WO2024050843A1 (en) * | 2022-09-09 | 2024-03-14 | 眉山博雅新材料股份有限公司 | Crystal growth method and apparatus |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5968261A (en) * | 1995-09-05 | 1999-10-19 | Northrop Grumman Corporation | Method for growing large silicon carbide single crystals |
| CN102586858A (en) * | 2012-04-01 | 2012-07-18 | 北京华进创威电子有限公司 | Double-crucible device for growing single crystals through induction heating physical vapor phase transfer |
| CN105671637A (en) * | 2016-02-02 | 2016-06-15 | 北京华进创威电子有限公司 | Sustained release device for growing of SiC single crystals with PVT (physical vapor transport) method |
| CN205342231U (en) * | 2016-01-13 | 2016-06-29 | 山东天岳先进材料科技有限公司 | Carborundum cutting device |
| CN106929913A (en) * | 2015-12-29 | 2017-07-07 | 中国科学院上海硅酸盐研究所 | A kind of split type growing silicon carbice crystals crucible |
| CN107385512A (en) * | 2017-06-30 | 2017-11-24 | 山东天岳先进材料科技有限公司 | The growing method of carbon parcel volume defect in a kind of suppression single-crystal silicon carbide |
-
2019
- 2019-04-26 CN CN201910344555.0A patent/CN110067026B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5968261A (en) * | 1995-09-05 | 1999-10-19 | Northrop Grumman Corporation | Method for growing large silicon carbide single crystals |
| CN102586858A (en) * | 2012-04-01 | 2012-07-18 | 北京华进创威电子有限公司 | Double-crucible device for growing single crystals through induction heating physical vapor phase transfer |
| CN106929913A (en) * | 2015-12-29 | 2017-07-07 | 中国科学院上海硅酸盐研究所 | A kind of split type growing silicon carbice crystals crucible |
| CN205342231U (en) * | 2016-01-13 | 2016-06-29 | 山东天岳先进材料科技有限公司 | Carborundum cutting device |
| CN105671637A (en) * | 2016-02-02 | 2016-06-15 | 北京华进创威电子有限公司 | Sustained release device for growing of SiC single crystals with PVT (physical vapor transport) method |
| CN107385512A (en) * | 2017-06-30 | 2017-11-24 | 山东天岳先进材料科技有限公司 | The growing method of carbon parcel volume defect in a kind of suppression single-crystal silicon carbide |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112410732A (en) * | 2020-11-20 | 2021-02-26 | 湖南烁科晶磊半导体科技有限公司 | In-situ pretreatment method for molecular beam epitaxy source material |
| CN112410732B (en) * | 2020-11-20 | 2022-08-26 | 湖南烁科晶磊半导体科技有限公司 | In-situ pretreatment method for molecular beam epitaxy source material |
| CN113151900A (en) * | 2021-04-30 | 2021-07-23 | 山东天岳先进科技股份有限公司 | Silicon carbide crystal and preparation method thereof |
| CN113388888A (en) * | 2021-06-22 | 2021-09-14 | 山东天岳先进科技股份有限公司 | Silicon carbide crystal, seed crystal used by same and preparation method of seed crystal |
| WO2024050843A1 (en) * | 2022-09-09 | 2024-03-14 | 眉山博雅新材料股份有限公司 | Crystal growth method and apparatus |
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