CN109234801B - A method of improving continuous growth single-crystal silicon carbide quality - Google Patents
A method of improving continuous growth single-crystal silicon carbide quality Download PDFInfo
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- CN109234801B CN109234801B CN201811303469.7A CN201811303469A CN109234801B CN 109234801 B CN109234801 B CN 109234801B CN 201811303469 A CN201811303469 A CN 201811303469A CN 109234801 B CN109234801 B CN 109234801B
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
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- 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
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Abstract
This application discloses a kind of methods of the continuous growth single-crystal silicon carbide quality of raising, belong to the preparation field of single-crystal silicon carbide.The method for continuously preparing single-crystal silicon carbide can be by simply adjusting the relative position of crucible and lantern ring, and the uniform single-crystal silicon carbide of convex rate can continuously be prepared by not needing replacement crucible；And specific thermal field can be targetedly designed, the gas phase transmission path inside crucible is changed, to realize efficiently and effectively thermal field and fluid control.In the method for the continuous growth single-crystal silicon carbide quality of the raising of the application, increase screw thread and matched bearing-ring device on the outside of crucible, it realizes being quickly converted for crucible hot zone, can quickly and easily realize the adjustment of thermal field, while substantially reducing the manufacturing cost of single-crystal silicon carbide.
Description
Technical field
This application involves a kind of methods of the continuous growth single-crystal silicon carbide quality of raising, belong to the preparation neck of single-crystal silicon carbide
Domain.
Background technique
ARTSemiconductor silicon carbide monocrystal material is after using silicon materials as first generation semiconductor material, GaAs and the phosphatization of representative
Indium etc. is the new generation of semiconductor monocrystal material after the second generation semiconductor material of representative.Its excellent physical property include compared with
Big forbidden bandwidth, high thermal conductivity coefficient, high critical breakdown strength and high saturated electrons mobility etc., are power electronic devices, micro-
The preferred substrate material of wave radio-frequency devices.
The excellent properties of single-crystal silicon carbide material are early just made known by scientist in the 1950s, but until 1978 years
After improveing the invention of Lely method, the preparation of electronic-grade semiconductor single-crystal silicon carbide is just graduallyd mature.Especially in U.S. CREE public affairs
The technology of department is led down, and the size of manufacturing silicon carbide semiconductor material is gradually developed to 6 inches and 8 inches, material from initial 2 inches
Quality is also continuously improved.However, compared to the excellent physical property of material itself and the urgent need in downstream application market, carbon
Increased quality and the cost reduction of SiClx single crystalline substrate still are apparent not enough.This is mainly due to prepare single-crystal silicon carbide semiconductor material
Physical method and technology limited.
Currently, physical carbon burdening (PVT) is the preparation method of manufacturing silicon carbide semiconductor monocrystalline mainstream.In PVT method, make
Magnetic field is formed with Medium frequency induction coil, the graphite crucible being placed in magnetic field forms silicon carbide monocrystal growth by induction heating
Thermal field.Powder needed for the growth single-crystal silicon carbide placed inside graphite crucible distils at high temperature releases Si, Si2C、SiC2
Equal gaseous components are simultaneously transmitted to crystallization at seed crystal.Since the silicon components inside graphite crucible can cause to invade to graphite crucible inner wall
Erosion, thus graphite crucible during reuse its be formed by thermal field and will necessarily change, to influence carbonization
The repeatability of crystal growth and the consistency of substrate quality.
In order to solve this problem, existing technology includes: progress crucible replacement after 1, each growth cycle, this is depended on
Whether quality is consistent, and graphite crucible is with high costs, is helpless to the reduction of single-crystal silicon carbide manufacturing cost.2, usually in carbon
SiClx will do it the fine tuning of thermal field and growth parameter(s) in the crystal growth period, be become with offsetting thermal field caused by graphite crucible is lost
Change, part adjusts thermal field by mobile crucible position in the prior art and patent CN107604439A passes through the mobile line of induction
The thermal field that circle carries out different growth periods is adjusted.However, techniques described above requires complicated scrap build and equipment control, no
Conducive to the reduction of single-crystal silicon carbide preparation cost.
Summary of the invention
It to solve the above-mentioned problems, should this application provides a kind of method of the continuous growth single-crystal silicon carbide quality of raising
Method increases screw thread and matched bearing-ring device using the outside of crucible, being quickly converted for crucible hot zone is realized, to improve
Thermal field repeatability and stability.The thermal field structure simply easily adjusted is formed compared to technology before, it can be quickly and easily real
The adjustment of existing thermal field, while substantially reducing the manufacturing cost of single-crystal silicon carbide and single-crystal silicon carbide and single crystalline substrate.
The method that the continuous growth of raising prepares the quality of single-crystal silicon carbide, the method include at least silicon carbide list
The first growth cycle and the second growth cycle of crystals growth, which is characterized in that the described method comprises the following steps:
First growth cycle: long brilliant raw material is placed in crucible, and at least one lantern ring is nested in the first of sidewall of crucible
On position, the first single-crystal silicon carbide is made in the first height in high-temperature region when long brilliant inside crucible；
Second growth cycle: long brilliant raw material is placed in crucible, and adjustment lantern ring is nested in the position on sidewall of crucible, so that the
The second single-crystal silicon carbide is made substantially in the first height in high-temperature region when the long crystalline substance of two growth cycles inside crucible.
Preferably, lantern ring is greater than or equal to lantern ring in the second growth cycle at a distance from seed crystal in first growth cycle
At a distance from seed crystal.
According to the sic powder distillation degree after period 1 crystal growth in the application, growth can be identified
The indoor high temperature zone position of chamber.
Optionally, first growth cycle includes: and long brilliant raw material is placed in crucible, and at least one lantern ring is nested
On the first position of sidewall of crucible, first single-crystal silicon carbide with the first convex rate is prepared；
Second growth cycle includes: the first convex rate according to the first growth cycle, and adjustment lantern ring is nested in sidewall of crucible
On position, long brilliant raw material is placed in crucible, the second single-crystal silicon carbide with the second convex rate is made.
Optionally, first single-crystal silicon carbide has the first convex rate, and the first convex rate is not more than 8mm；Described second
Single-crystal silicon carbide has the second convex rate, and the second convex rate is not more than 8mm.
Optionally, the time that the adjustment lantern ring is nested in the position on sidewall of crucible is the crucible weight of the first growth cycle
Or variable density；The adjustment lantern ring is nested in the position moving distance on sidewall of crucible according to the of first single-crystal silicon carbide
The changing value of one convex rate.
After a wheel crystal growth cycles, the graphite insulation quilt and graphite crucible for being used to form crystal growing thermal field all can
There is certain loss, while its physicochemical property can also drift about.Therefore, it is the crystal of repeated growth second period, needs
Under conditions of reusing a upper thermal field, simple and quick high-temperature region adjustment is carried out, method particularly includes: when period 1 grown junction
Whether Shu Hou judges high temperature zone position in chamber predeterminated position；If so, thermal field high-temperature region is passing through according to crystal growth rule
Cross one wheel crystal growth after can to seed crystal end drift about, in order to liquidate thermal field drift, by lantern ring accordingly to thermal field drift bearing into
Row movement.
As a kind of method for adjusting lantern ring, if crucible and insulation quilt density or weight change after crystal growth,
It then can be determined that thermal field can change, need to carry out thermal field adjustment in next period.Adjustment amount is true according to the convex rate of plane of crystal
It is fixed.If convex rate changes greatly, the corresponding position for adjusting lantern ring is larger, and such as convex rate then adjusts lantern ring and move up more than preset 1 times
20mm；In the range of crystal design, then adjustment amount can be smaller or even adjust convex rate.
Optionally, the preparation method of first single-crystal silicon carbide and/or the second single-crystal silicon carbide includes the following steps:
1) by sic powder and be used for crystal growth seed crystal be placed in inside graphite crucible and close graphite crucible after,
Lantern ring is nested in graphite crucible top region；
2) graphite crucible and graphite insulation quilt be placed in crystal growing furnace is intracavitary and after sealing, and setting single-crystal silicon carbide is raw
Long temperature is the crystal growth that 2100-2200 DEG C of pressure is the laggard behavior phase 100-200h of 5-50mbar；
3) after crystal growth, burner hearth is opened, after taking out graphite crucible, can get the single-crystal silicon carbide.
Optionally, by 4 inches of single crystalline substrate of first single-crystal silicon carbide and second single-crystal silicon carbide preparation
Curvature is 6-13 μm.
Optionally, the wall outer surface of the crucible and the inner surface of the lantern ring are connected through a screw thread.As a kind of reality
Mode is applied, makes external screw thread in crucible outer surface, making crucible cylinder is integrally in screw-rod structure；Prepare thimble structure, lantern ring internal diameter
Internal thread structure is equally prepared on the inside of and lantern ring equal with crucible outer diameter, making lantern ring integrally is in the nut knot to match with crucible
Structure.
Optionally, the screw pitch of the screw thread is 0.2-2mm.Further, the range of the changing value of the first distance
Lower limit be selected from 0.5mm, 0.7mm, 1.0mm, 1.3mm or 1.5mmm, the upper limit be selected from 0.5mm, 0.7mm, 1.0mm, 1.3mm,
1.5mmm or 1.7mm.The setting of the thread pitch of the application is so that the movement of lantern ring is accurate enough.Further, the screw thread
Screw pitch be 0.3-1.5mm.
Optionally, the standoff height of the lantern ring to the crucible is 5-15mm.Further, the height of the lantern ring
Lower limit is selected from 7mm, 10mm, 12mm or 14mm, and the upper limit is selected from 7mm, 10mm, 12mm or 14mm.Optionally, the height of the lantern ring
For 7-13mm.
Optionally, the lantern ring to the crucible standoff height and the crucible height ratio be 1:
5-20.Further, the lower limit of the height ratio of the height of the lantern ring and the crucible is selected from 1:7,1:10,1:
12,1:14 or 1:18, the upper limit are selected from 1:7,1:10,1:12,1:14 or 1:18.Further, the height of the lantern ring and institute
The height ratio for stating crucible is 1:7-18.The height of the lantern ring of the application makes lantern ring that can cover enough thermal fields when moving
Region meets thermal field adjustment demand.
Optionally, the lantern ring with a thickness of 5-25mm.Further, the lower limit of the thickness of the lantern ring be selected from 7mm,
10mm, 15mm, 20mm or 23mm, the upper limit are selected from 7mm, 10mm, 15mm, 20mm or 23mm.Further, the thickness of the lantern ring
Degree is 7-20mm.The thickness of the lantern ring of the application balance lantern ring itself because after kelvin effect fever heat blocking and heat transfer to earthenware
Efficiency in crucible.
Optionally, the crucible is graphite crucible, and the lantern ring is graphite lantern ring.
Optionally, the outer wall of the crucible has mark, and the mark can mark the position of lantern ring.Preferably, the mark
Knowing is scale mark.
As an implementation, scale mark can be carried out on the outside of graphite crucible, accurately to record lantern ring along graphite earthenware
The axial location of crucible
Optionally, the lantern ring that can be moved axially along crucible is at least arranged outside the crucible.
The lantern ring of the application is at least 1, can also be multiple when lantern ring is applied in combination.
Optionally, the heating device that the crucible uses is induction heating mode；Preferably, during the heating device includes
Frequency induction coil.As an implementation, single-crystal silicon carbide is prepared using PVT method, uses the coil-induced heating of Medium frequency induction
Graphite crucible.
Optionally, the crucible is graphite crucible, and the lantern ring is graphite lantern ring.
Optionally, the method for continuously preparing single-crystal silicon carbide includes the following steps:
1) by sic powder and be used for crystal growth seed crystal be placed in inside graphite crucible and close graphite crucible after,
Graphite lantern ring is nested in graphite crucible top region, scale mark can be carried out on the outside of graphite crucible, accurately to record stone
Black lantern ring is the location of axial along graphite crucible；
2) graphite crucible and graphite insulation quilt be placed in crystal growing furnace is intracavitary and after sealing, and setting single-crystal silicon carbide is raw
Long temperature is the crystal growth that 2100-2200 DEG C of pressure is the laggard behavior phase 100-200h of 5-50mbar；
3) after crystal growth, burner hearth is opened, can get single-crystal silicon carbide crystal ingot after taking out graphite crucible；
4) according to the convex rate of single-crystal silicon carbide is obtained, along graphite crucible axial-rotation graphite lantern ring certain distance, make graphite
After lantern ring is placed in graphite crucible specific position, powder and seed crystal are packed into graphite crucible again and carries out crystalline substance after being packaged in burner hearth
Body growth, repeats single-crystal silicon carbide step 2), without changing its growth parameter(s)；
5) after silicon carbide monocrystal growth, single-crystal silicon carbide, the single-crystal silicon carbide after being corrected, the first convex rate are taken out
Control is within 8mm；
6) it reuses the set graphite crucible and graphite insulation quilt carries out next heat silicon carbide monocrystal growth, root before growing
According to the convex rate data of upper furnace single-crystal silicon carbide and thermal field situation of change, after moving down graphite lantern ring certain position, by graphite crucible
It is encapsulated into burner hearth and by above-mentioned steps 2) growth parameter(s) progress crystal growth, the convex rate of available single-crystal silicon carbide second, second
Convex rate and the first convex rate are close to consistent single-crystal silicon carbide.
Optionally, graphite crucible overthe openings described in the carbonization single crystal seed.
In the application, PVT method refers to physical carbon burdening.
According to kelvin effect, there are when alternating electromagnetic field in conductor, internal current distribution is uneven is even to lead to electric current collection
In in crucible surface, crucible heating is concentrated mainly on surface and by inside heat transfer to crucible.With crystal growth cycles
It lengthens, is corroded and changed by silicon atmosphere inside crucible, influence the generation and conduction of crucible heat, and then lead to the change of thermal field
Change, the form of variation is usually expressed as the axial movement in crucible internal high temperature area.Generally for the thermal field to this variation into
Row correction, needing to improve equipment is adjusted the relative axial position of crucible and intermediate frequency coil, to change crucible in magnetic field
Axial position and fever center, to realize solidification to warm area position.
The method of the quality of the continuous growth single-crystal silicon carbide of the raising of the application, can be in the coil for not changing thermal field structure
In the case where bushing position, the adjustment and correction of thermal field are carried out by adjusting the position for the lantern ring being nested on the outside of crucible, in
The magnetic fields of frequency coil conduct heat to inside crucible after on outermost lantern ring, being arranged ring fever.Since lantern ring is embedding
It is placed on the outside of crucible, heat transmission is directly generated heat compared to sidewall of crucible and conducted to needing longer transmission distance inside crucible
From so that the thermal field of regional area is influenced by lantern ring and changed inside crucible, and then playing the role of adjusting thermal field.
In the application after crucible uses specific period, adjusts in the following manner: lantern ring is rotated to crucible certain bits
It sets, after crystal growth, thermal field change direction is determined according to the loss situation of crucible.If high-temperature region is moved axially upward,
Need to be corrected in next growth cycle, then by corresponding high-temperature region direction along axial-rotation graphite lantern ring to required temperature
Zone position, then high-temperature region regional temperature caused by a upper period can decline, so that thermal field be made to restore to the heat close to a upper period
Under field condition.
Outer divided by the upper thermal field adjustment for carrying out different growth periods, the application can also targetedly design specific thermal field.
Thermal field design method is as follows: the temperature if necessary to design seed crystal set-down location is lower, then rotates graphite lantern ring to seed crystal and place
Place, so as to reduce the temperature of seed crystal set-down location；It is reduced if necessary to the temperature between seed crystal and raw material, then by graphite lantern ring
Rotation is to the position between seed crystal and raw material, then the temperature in the region reduces accordingly.It is adjusted by these, it can be targetedly
Specific thermal field region is formed, the gas phase transmission path inside crucible is changed, to realize efficiently and effectively thermal field and fluid control
System.
High-temperature region in the application refers to the highest region of relative temperature in crystal growth enclosure, and heat is most in this area
Concentrate, sic powder distillation it is most abundant, in high-temperature area set powder be atmosphere needed for growing silicon carbice crystals mainly for
Ying Yuan；Low-temperature region is the crystal region and silicon carbide monocrystal growth area of sic powder in its corresponding chamber.
The beneficial effect of the application includes but is not limited to:
The method of the quality of the continuous growth single-crystal silicon carbide of the raising of the application increases screw thread and matched on the outside of crucible
Graphite bearing-ring device realizes being quickly converted for crucible hot zone, can quickly and easily realize the adjustment of thermal field, while dropping significantly
The manufacturing cost of low-carbon silicon single crystal.
The method of the quality of the continuous growth single-crystal silicon carbide of the raising of the application can not change load coil and
In the case where bushing position, the adjustment and correction of thermal field are carried out by adjusting the position for the lantern ring being nested on the outside of crucible.
Crucible in the method for the quality of the continuous growth single-crystal silicon carbide of the raising of the application passes through using after specific period
Following manner is adjusted: lantern ring being rotated to crucible specific position, after crystal growth, determines heat according to the loss situation of crucible
Field change direction.
The application can also targetedly design specific thermal field, can targetedly form specific thermal field region, change
Gas phase transmission path inside crucible, to realize efficiently and effectively thermal field and fluid control.
The method for continuously preparing single-crystal silicon carbide of the application is lower to equipment requirement, advantageously reduces single-crystal silicon carbide system
Cause this.
The method of the quality of the continuous growth single-crystal silicon carbide of the raising of the application is by simple adjustment graphite sleeve position
Thermal field can be achieved to adjust, it is convenient and efficient, thermal field repeatability is improved, is conducive to prepare quality stability and the high carbonization of consistency
Silicon single crystal.
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 is thermal field structure schematic diagram used in the continuous growth single-crystal silicon carbide method of the application.
Fig. 2 be this application involves the embodiment of the present application and comparative example continuous 6 single-crystal silicon carbides of growth the change of convex rate
Change figure.
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 " on ", "lower", "front", "rear", "left", "right",
The orientation or positional relationship of the instructions such as "inner", "outside", " axial direction ", " radial direction ", " circumferential direction " is orientation based on the figure or position
Relationship is set, description the application is merely for convenience of and simplifies description, rather than the device or element of indication or suggestion meaning are necessary
It with specific orientation, is constructed and operated in a specific orientation, therefore should not be understood as the limitation to the application.
In the description of the present application, the meaning of " plurality " is two or more, unless otherwise specifically defined.
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.
With reference to Fig. 1, embodiments herein discloses a kind of adjustable thermal field structure for continuously preparing single-crystal silicon carbide, should
Thermal field structure includes crucible 4 and heating device, and an adjustable lantern ring 3 is arranged outside crucible 4.
As an implementation, lantern ring 3 and crucible 4 are connected through a screw thread 5, and the outer wall whole region of crucible 4 has spiral shell
Line 5.Lantern ring 3 can be graphite cannula ring.In embodiment, screw pitch is set as 0.2-2mm, and graphite lantern ring height is set as 5-
15mm, graphite lantern ring with a thickness of 5-25mm.Further, in embodiment, screw pitch is set as 0.5mm, graphite lantern ring height
Be set as 10mm, graphite lantern ring with a thickness of 15mm.
In present embodiment, it can be to be used to prepare silicon carbide that crucible 4, which can be graphite crucible, but be not limited to graphite crucible
Any materials of monocrystalline.
As an implementation, insulation construction 1 is made of the material with insulation, such as keeps the temperature felt using graphite
At.
Further, for heating device by middle induction heating mode heating crucible 4, the outer of crucible 4 is arranged in insulation construction 1
The periphery of insulation construction 1 is arranged in portion, heating device.Growth single-crystal silicon carbide powder 6 is placed in crucible 4.
Further, there is seed crystal unit, seed crystal unit setting, should in 2 opening of graphite crucible in the thermal field structure
Seed crystal unit includes carbonization single crystal seed 2.
Presently filed embodiment, in the case where not changing coil and graphite crucible position, by adjusting stone is nested in
The position of graphite lantern ring on the outside of black crucible carries out the adjustment and correction of thermal field, and the magnetic fields of intermediate frequency coil are in outermost stone
On black lantern ring, conducted heat to inside graphite crucible after the fever of graphite lantern ring.Since graphite lantern ring is nested on the outside of crucible,
Heat transmission is directly generated heat compared to graphite crucible wall and is conducted to longer transmission range is needed inside graphite crucible, to make
The thermal field for obtaining regional area inside graphite crucible is influenced by graphite lantern ring and is changed, and then plays the role of adjusting thermal field.
It is adjusted in the following manner: after graphite crucible uses specific period by graphite as presently filed embodiment
Lantern ring is rotated to graphite crucible specific position, after silicon carbide monocrystal growth, determines heat according to the loss situation of graphite crucible
Field change direction.It if high-temperature region is moved axially upward, needs to be corrected in next growth cycle, then by corresponding height
Warm area direction along axial-rotation graphite lantern ring to required warm area position, then high-temperature region regional temperature caused by a upper period can under
Drop, so that thermal field be made to restore to the thermal field close to a upper period.
As a kind of method for adjusting lantern ring, if crucible and insulation quilt density or weight change after crystal growth,
It then can be determined that thermal field can change, need to carry out thermal field adjustment in next period.Adjustment amount is true according to the convex rate of plane of crystal
It is fixed.If convex rate changes greatly, the corresponding position for adjusting lantern ring is larger, and such as convex rate then adjusts lantern ring and move up more than preset 1 times
20mm；In the range of crystal design, then adjustment amount can be smaller or even adjust convex rate.
As presently filed embodiment, specific thermal field can also be targetedly designed.Thermal field design method is as follows: if
The temperature for needing to design seed crystal set-down location is lower, then rotates graphite lantern ring to seed crystal set-down location, put so as to reduce seed crystal
Set the temperature at place；It reduces, then rotates graphite lantern ring between seed crystal and raw material if necessary to the temperature between seed crystal and raw material
Position, then the temperature in the region reduces accordingly.It is adjusted by these, can targetedly form specific thermal field region,
Change the gas phase transmission path inside crucible, to realize efficiently and effectively thermal field and fluid control.
As other embodiments, multiple graphite lantern rings can be designed according to thermal field accordingly and be applied in combination.
Since silicon carbide monocrystal growth thermal field is radially in the feature that central temperature is low, lip temperature is high, silicon carbide
The edge thickness of monocrystalline is less than center thickness, and the difference (convex rate) of single-crystal silicon carbide center and edge thickness is 2-20mm.Convex rate is got over
Greatly, show that the radially even property of thermal field is poorer, corresponding single-crystal silicon carbide stress is poorer, and obtained single-crystal silicon carbide substrate is often
It is larger and other issues there are curvature and angularity；The uneven of thermal field leads to single-crystal silicon carbide inside impurity radially simultaneously
It is unevenly distributed, the resistivity inhomogeneities in single-crystal silicon carbide substrate face is caused to become larger.Therefore, the convex rate of reasonable single-crystal silicon carbide
It should control within 8mm, and be remained unchanged with the loss after graphite crucible and the reuse of graphite insulation quilt, to guarantee carbon
The consistency and stability of SiClx monocrystalline and substrate quality.Further, the convex rate of the single-crystal silicon carbide should control 5mm with
It is interior.
Single-crystal silicon carbide is prepared using the thermal field structure prepared in above-described embodiment, specific application method is as follows:
1) by sic powder and be used for crystal growth seed crystal be placed in inside graphite crucible and close graphite crucible after,
Graphite lantern ring is nested in graphite crucible top region, scale mark can be carried out on the outside of graphite crucible, accurately to record stone
Black lantern ring is the location of axial along graphite crucible；
2) graphite crucible and graphite insulation quilt be placed in crystal growing furnace is intracavitary and after sealing, and setting single-crystal silicon carbide is raw
Long temperature is the crystal growth that 2100-2200 DEG C of pressure is the laggard behavior phase 100-200h of 5-50mbar；
3) after crystal growth, burner hearth is opened, can get single-crystal silicon carbide crystal ingot after taking out graphite crucible；
4) according to the first convex rate of single-crystal silicon carbide is obtained, along graphite crucible axial-rotation graphite lantern ring certain distance, make
After graphite lantern ring is placed in graphite crucible specific position, powder and seed crystal are packed into graphite crucible again and to be packaged in burner hearth laggard
Row crystal growth repeats single-crystal silicon carbide step 2, without changing its growth parameter(s)；
5) after silicon carbide monocrystal growth, single-crystal silicon carbide, the single-crystal silicon carbide after being corrected, the second convex rate are taken out
Control is within 5mm；
6) it reuses the set graphite crucible and graphite insulation quilt carries out next heat silicon carbide monocrystal growth, root before growing
According to the convex rate data of upper furnace single-crystal silicon carbide and thermal field situation of change, after moving down graphite lantern ring certain position, by graphite crucible
It is encapsulated into burner hearth and carries out crystal growth by 2 growth parameter(s) of above-mentioned steps, the available convex rate of single-crystal silicon carbide is close to consistent
Single-crystal silicon carbide.
Fig. 2 is the convex rate variation diagram of 6 single-crystal silicon carbides of continuous growth of embodiment and comparative example (conventional method).It is conventional
Method are as follows: after the 4 inch silicon carbide silicon single crystal for continuously growing 6 rounds using same set of material in the same device, as graphite is protected
The loss thermal field of warm felt and graphite crucible will gradually change, and cause the convex rate of single-crystal silicon carbide to be gradually increased, single-crystal silicon carbide
Consistency and bad stability, such as the A line in Fig. 2；And use herein described thermal field structure and adjust thermal field method into
After the correction of row thermal field is adjusted, the convex rate of the 6 round crystal continuously grown can be consistent, to obtain consistency and stability
Excellent carborundum crystals and substrate, such as the B line in Fig. 2.
After single-crystal silicon carbide prepared by above-mentioned conventional method and the present processes is processed as substrate, conventional method is used
For the single-crystal silicon carbide substrate curvature Distribution value of preparation between 15-39 μm, numerical value is larger and discrete；Use the thermal field of the application
For the substrate curvature Distribution value of structures and methods preparation between 6-13 μm, single-crystal silicon carbide substrate face type quality is preferably and consistent
Property is higher.
The above, only embodiments herein, the protection scope of the application is not by these specific embodiments
Limitation, but determined by following claims.To those skilled in the art, the application can have various
Change and variation.All any modification, equivalent replacement, improvement and so within the technical idea and principle of the application, should all
Comprising within the scope of protection of this application.
Claims (15)
1. a kind of method of the continuous growth single-crystal silicon carbide quality of raising, the method includes at least the of silicon carbide monocrystal growth
One growth cycle and the second growth cycle, which is characterized in that the described method comprises the following steps:
First growth cycle: long brilliant raw material is placed in crucible, and at least one lantern ring is nested in the first position of sidewall of crucible
On, the first single-crystal silicon carbide is made in the first height in high-temperature region when long brilliant inside crucible；
Second growth cycle: long brilliant raw material is placed in crucible, and adjustment lantern ring is nested in the position on sidewall of crucible, so that second is raw
The second single-crystal silicon carbide is made substantially in the first height in high-temperature region when macrocyclic long brilliant inside crucible.
2. the method for the quality of the continuous growth single-crystal silicon carbide of raising according to claim 1, which is characterized in that
First growth cycle includes: long brilliant raw material to be placed in crucible, and at least one lantern ring is nested in sidewall of crucible
On first position, the first single-crystal silicon carbide with the first convex rate is made；
Second growth cycle includes: the first convex rate according to the first growth cycle, and adjustment lantern ring is nested on sidewall of crucible
Long brilliant raw material is placed in crucible, the second single-crystal silicon carbide with the second convex rate is made by position.
3. the method for the quality of the continuous growth single-crystal silicon carbide of raising according to claim 2, which is characterized in that described the
One convex rate is not more than 8mm, and the second convex rate is not more than 8mm.
4. the method for the quality of the continuous growth single-crystal silicon carbide of raising according to claim 1, which is characterized in that the tune
The time that a whole set of ring is nested in the position on sidewall of crucible is the crucible weight or variable density of the first growth cycle；The adjusting sleeve
Ring is nested in the position moving distance on sidewall of crucible according to the changing value of the first convex rate of first single-crystal silicon carbide.
5. the method for the quality of the continuous growth single-crystal silicon carbide of raising according to claim 2, which is characterized in that the tune
The time that a whole set of ring is nested in the position on sidewall of crucible is the crucible weight or variable density of the first growth cycle；The adjusting sleeve
Ring is nested in the position moving distance on sidewall of crucible according to the changing value of the first convex rate of first single-crystal silicon carbide.
6. the method for the quality of the continuous growth single-crystal silicon carbide of raising according to claim 3, which is characterized in that the tune
The time that a whole set of ring is nested in the position on sidewall of crucible is the crucible weight or variable density of the first growth cycle；The adjusting sleeve
Ring is nested in the position moving distance on sidewall of crucible according to the changing value of the first convex rate of first single-crystal silicon carbide.
7. the method for the quality of the continuous growth single-crystal silicon carbide of raising according to claim 1 to 6, feature
It is, the preparation method of first single-crystal silicon carbide and/or the second single-crystal silicon carbide includes the following steps:
1) by sic powder and be used for crystal growth seed crystal be placed in inside graphite crucible and close graphite crucible after, will cover
Ring is nested in graphite crucible top region；
2) by graphite crucible and graphite insulation quilt be placed in crystal growing furnace it is intracavitary and seal after, be arranged silicon carbide monocrystal growth temperature
Degree is the crystal growth that 100-200h is carried out after 2100-2200 DEG C of pressure is 5-50mbar；
3) after crystal growth, burner hearth is opened, after taking out graphite crucible, can get the single-crystal silicon carbide.
8. the method for the quality of the continuous growth single-crystal silicon carbide of raising according to claim 1 to 6, feature
It is, 4 inches of the single crystalline substrate curvature by first single-crystal silicon carbide and second single-crystal silicon carbide preparation is 6-
13μm。
9. the method for the quality of the continuous growth single-crystal silicon carbide of raising according to claim 1, which is characterized in that the earthenware
The wall outer surface of crucible and the inner surface of the lantern ring are connected through a screw thread.
10. the method for the quality of the continuous growth single-crystal silicon carbide of raising according to claim 9, the screw pitch of the screw thread are
0.2-2mm。
11. the method for the quality of the continuous growth single-crystal silicon carbide of raising according to claim 1, which is characterized in that described
The standoff height of lantern ring to the crucible is 5-15mm.
12. the method for the quality of the continuous growth single-crystal silicon carbide of raising according to claim 1, which is characterized in that described
Lantern ring to the crucible standoff height and the crucible height ratio be 1:5-20.
13. the method for the quality of the continuous growth single-crystal silicon carbide of raising according to claim 1, which is characterized in that described
Lantern ring with a thickness of 5-25mm.
14. the method for the quality of the continuous growth single-crystal silicon carbide of raising according to claim 1, which is characterized in that described
Lantern ring is graphite lantern ring.
15. the method for the quality of the continuous growth single-crystal silicon carbide of raising according to claim 14, which is characterized in that described
The outer wall of crucible has the mark of sign Case for holding ring position.
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| PCT/CN2018/123711 WO2020087718A1 (en) | 2018-11-02 | 2018-12-26 | Crucible for preparing single crystal of silicon carbide and use thereof |
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