CN207193434U - A kind of growth crucible for improving single-crystal silicon carbide quality - Google Patents
A kind of growth crucible for improving single-crystal silicon carbide quality Download PDFInfo
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- CN207193434U CN207193434U CN201720574147.0U CN201720574147U CN207193434U CN 207193434 U CN207193434 U CN 207193434U CN 201720574147 U CN201720574147 U CN 201720574147U CN 207193434 U CN207193434 U CN 207193434U
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Abstract
It the utility model is related to a kind of growth crucible for improving single-crystal silicon carbide quality, it includes outer crucible, outer crucible port is provided with the crucible cover of sealing outer crucible, it is characterized in that, interior crucible is provided with outer crucible, described interior crucible includes bottom wall and side wall, side wall is double side walls, double side walls include inner and outer wall, the aperture of inwall is provided through on inwall, bottom wall is arranged on the bottom between inwall and outer wall, and the chamber that inwall surrounds is upper and lower hollow structure, and double side walls upper port is provided with the annular end cap of interlayer between sealing inwall and outer wall.The crucible structure is simple, the SiC powders being easily carbonized in high temperature location are closed in the interlayer between the inwall and outer wall of interior crucible by the crucible structure, prevent the small carbon particle after powder carbonization from being transported to seed crystal face, greatly reduce the carbon inclusion enclave in SiC single crystal, improve single-crystal silicon carbide quality.
Description
Technical field
A kind of growth crucible for improving single-crystal silicon carbide quality is the utility model is related to, belongs to crystal growth equipment technology neck
Domain.
Background technology
For carborundum (SiC) crystal compared with other many semiconductor single crystal materials, it has hardness is high (to be only second to Buddha's warrior attendant
Stone), thermal conductivity high (4.9W/cmK), low (3.1-4.5 × 10 of thermal coefficient of expansion-6/ K), the big (2.40- of energy gap
3.26eV), high (2.0-2.5 × 10 of saturation drift velocity7Cm/s), critical breakdown strength big (2~3 × 106V/cm), chemistry is steady
The qualitative high, excellent properties such as capability of resistance to radiation is strong.These excellent performances enable SiC semiconductor device in high temperature, high pressure, strong spoke
The extreme environment work penetrated, has broad application prospects, and future semiconductor is produced in photoelectron and field of power electronics
The development of industry produces material impact.
The main method of growth SiC single crystal has physical vapor transport, high temperature chemical vapor deposition method, liquid phase method.Wherein,
Physical vapor transport (Physical Vapor Transport-PVT) is the main stream approach of current growth SiC crystal, will
SiC seed crystals are bonded in graphite crucible and covered, and graphite crucible is controlled in growth course built with the SiC powder as growth raw material
For seed temperature between 2100 DEG C to 2200 DEG C, growth raw material resolves into after gaseous component the axial temperature ladder inside graphite crucible
Crystalline growth SiC crystal at seed crystal is transported under the driving of degree.
At present, SiC single crystal substrate has been used to prepare high power semiconductor illumination LED, HEMT, Xiao
The semiconductor devices such as special based diode, metal oxide semiconductor field effect tube, but the stability of device and permanent worker
The reliability of work nevertheless suffers from the influence of fault of construction in SiC single crystal backing material.Structural flaws typical bag in SiC single crystal
Include：Extraneous polytype structure, carbon inclusion enclave, dislocation, micro-pipe.How fault of construction in SiC single crystal is reduced, and acquisition has high structure
The SiC single crystal of integrality, it is a stern challenge for crystal growth work, while is also one long-term and arduous
Research topic.
Certainly for different faults of construction, it is necessary to be eliminated using corresponding Crystal Growth Technique means.It is mono- in SiC
In brilliant fault of construction, carbon inclusion enclave is the fault of construction that a kind of comparison is difficult to eliminate.Carbon inclusion enclave once produces in monocrystalline,
The formation of micropipe defects is usually associated with follow-up crystal growing process, this use to device has fatal influence.
Formation mechenism of the carbon inclusion enclave in single-crystal silicon carbide：At high temperature, SiC powders main decomposition is Si, Si2C and
SiC2Three kinds of gas phase species, wherein Si vapour pressure highest, this causes in gas phase Si/C ratios more than 1：1, i.e., Si original in gas phase
Subnumber is higher than C atomicity.Although at crystal growth initial stage, the Si/C in SiC powders is than keeping balancing, with the heat time
Extend, Si loss will be gradually serious, and powder will gradually be carbonized.Therefore, the carbon in the middle and later periods of SiC single crystal growth, powder
Particle can move to growth front, be attached to single-crystal surface, and stay in crystal with crystal growth with carrier gas or by diffusion
The position of different-thickness.In general, it is more higher to crystal growth later stage, carbon parcel volume density.
During the SiC single crystal of physical vapor transport growth at present, using Frequency Induction Heating SiC powders, therefore SiC
The temperature difference of diverse location is very big in powder, generally proximate to sidewall of crucible and close to the powder temperature highest at crucible bottom, from
Powder temperature at the more remote and close surface of sidewall of crucible is minimum.Therefore, current crucible is hinder SiC crystal Quality advance one
Hang-up.
Utility model content
In view of the shortcomings of the prior art, the utility model provides a kind of growth crucible for improving single-crystal silicon carbide quality, should
Crucible structure is simple, during silicon carbide monocrystal growth, because SiC powders are close to the portion temperature highest of sidewall of crucible, carbonization
The most serious, the SiC powders being easily carbonized in high temperature location are closed in the inwall of interior crucible by interior crucible of the present utility model
In interlayer between outer wall, the small carbon particle after powder carbonization is seted to greatly reduce from being transported to seed crystal face in SiC single crystal
Carbon inclusion enclave, improve single-crystal silicon carbide quality.
The technical solution of the utility model is as follows：
A kind of growth crucible for improving single-crystal silicon carbide quality, including outer crucible, outer crucible port are provided with the outer earthenware of sealing
The crucible cover of crucible, it is characterised in that interior crucible is provided with outer crucible, described interior crucible includes bottom wall and side wall, side wall
For double side walls, double side walls include inner and outer wall, are provided through the aperture of inwall on inwall, bottom wall be arranged on inwall with
Bottom between outer wall, the chamber that inwall surrounds are upper and lower hollow structure, double side walls upper port be provided with sealing inwall with it is outer
The annular end cap of interlayer between wall.
Preferable according to the utility model, the height of interior crucible is the 1/2-2/3 of outer crucible inner chamber vertical height, preferably
, the height of interior crucible is the 2/3 of outer crucible inner chamber vertical height.
Preferable according to the utility model, the outer wall of interior crucible is close to the madial wall of outer crucible, is smaller than 0.5mm；
It is close to the bottom of outer crucible the bottom of interior crucible.
Preferable according to the utility model, a diameter of 8-12mm of aperture on inwall, the spacing between aperture is 20-
35mm；Preferably, on inwall aperture a diameter of 10-12mm, the spacing between aperture is 20-30mm.
Preferable according to the utility model, described inwall, outer wall are in cylinder, between described inwall and outer wall
Spacing is 15-25mm, it is preferred that the spacing between inwall and outer wall is 18-22mm.
Preferable according to the utility model, outer wall is in cylinder, and inwall in the form of a truncated cone, justify by the lower end of conical butt
Diameter is more than upper end circular diameter, and the cone angle of conical butt is 40-50 °, it is preferred that the cone angle of conical butt is 45 °；Inwall
Interlayer between outer wall is more than the conical butt of lower end diameter for upper end diameter.
Preferable according to the utility model, described outer crucible lid includes the cover plate and boss being fixedly connected, and cover plate is circle
Plate shape, boss are inverted round stage.Preferably, the cone angle of inverted round stage is 30-60 °, and the height of inverted round stage is 5-10mm, inverted round stage lower end
The matching of round area and seed crystal.
During silicon carbide monocrystal growth, seed crystal is adhered on the table top of inverted round stage, and the cover plate and boss being fixedly connected make monocrystalline
There is a difference in height with polycrystalline, be advantageous to crystal growth and terminate rear monocrystalline to separate with polycrystalline.
Preferable according to the utility model, the chamber that inwall surrounds is interior crucible interior, interior crucible interior upper port and outer earthenware
The boss of crucible lid is relative, and interior crucible interior upper port diameter is less than or equal to boss lower end diameter of a circle.
It is further preferred that interior crucible interior upper port diameter is smaller 1-5mm than boss lower end diameter of a circle.
Preferable according to the utility model, outer crucible port top side wall is evenly distributed with screw, outer crucible cover with
Screw identical distribution spacing is evenly arranged with manhole, and graphite screws pass through the manhole and screw of crucible cover, realize
Sealed connection between crucible body and crucible cover；Preferably, the quantity of screw is 6, manhole and screw quantity Matching.
It is preferable according to the utility model, annular end cap and the connected mode and outer crucible and outer earthenware of double side walls upper port
The connected mode of crucible lid is identical.
It is preferable according to the utility model, it is fixed with silicon carbide seed in the boss surface of outer crucible lid.
Preferable according to the utility model, interior crucible, outer crucible are graphite crucible, and annular end cap, outer crucible lid are stone
Inky cap.
The structure setting of crucible, relative position greatly reduce carbon inclusion enclave in obtained monocrystalline in the utility model,
Under high temperature, the pyrolysis of SiC powders in interior crucible interlayer and inner chamber is gaseous component, and the gaseous component decomposed in inner chamber is to upload
It is defeated, it is transported to seed crystal face；Aperture of the gaseous component decomposed in interlayer along interior crucible internal walls arrives by inner chamber SiC powder carries
Seed crystal face, finally grow into monocrystalline；During silicon carbide monocrystal growth, interior crucible of the present utility model will be in high-temperature position
Put the SiC powders being easily carbonized to be sealed in the interlayer between the inwall and outer wall of interior crucible, the small carbon after powder carbonization
Grain can not be transported to seed crystal face, while the powder in inner chamber plays a role in filtering to the gas phase being pyrolyzed in interlayer, avoids carbon
Pellet transportation is to SiC single crystal surface, so as to greatly reduce the carbon inclusion enclave in SiC single crystal.
Preferable according to the utility model, the silicon carbide seed is 6H-SiC or 4H-SiC.
Preferable according to the utility model, when silicon carbide seed is 6H-SiC, silicon face is aufwuchsplate, works as silicon carbide seed
For 4H-SiC when, carbon face is aufwuchsplate.
Preferable according to the utility model, the sic powder particle diameter is 0.5-1mm.Sic powder is existing skill
Art, it is made using conventional method, preparation method reference " influence that temperature synthesizes to sic powder ", Tian Mu, xuwei etc.,《Electricity
Sub- technology》3rd 182-185 pages of the phase in 2012.
Growth crucible of the present utility model can be by the interior chamber size of crucible in adjustment, the gas phase decomposed to SiC powders
The transmission of component is regulated and controled.
The method for using growth crucible of the present utility model grow high quality SiC single crystal, workflow are as follows：
(1) silicon carbide seed is fixed on the inverted round stage end face of outer crucible lid, and carries out carbonization treatment；Carbonization treatment is true
Reciprocal of duty cycle is 10-2~10-3Pa, carburizing temperature are 500 DEG C, and the time is 2 hours；
(2) by SiC powders be filled in interior crucible inner chamber and inwall and outer wall between interlayer in, it is close using annular end cap
Binder layer upper port；
(3) the outer crucible lid for the fixation seed crystal for obtaining step (1) is placed in the upper port of outer crucible, and will with graphite screws
Outer crucible lid is tightly connected with outer crucible；
(4) crucible is integrally placed to the center of monocrystal growing furnace growth room, growth room is vacuumized, reaches vacuum
To 10-5Pa~10-2Pa；
(5) to crystal growth stove heat, temperature in crucible is reached 2273K~2773K, be passed through inert gas regulation growth
Pressure is 50-80mbar, carries out crystal growth；
(6) after crystal growth terminates, adjustment growth room pressure is 1000mbar, is cooled to room temperature, obtains high quality SiC
Monocrystalline.
Use the crucible to grow to obtain thickness for the carbon-free inclusion enclave generation of 20mm SiC single crystal, and grown with common crucible
Obtain thickness be 10mm monocrystalline with regard to carbon inclusion enclave can be observed.
The growth crucible provided by the utility model for improving single-crystal silicon carbide quality, the crucible phase with common growth carborundum
Than having advantages below：
1st, the SiC powders being easily carbonized in high temperature location are closed in the inwall of interior crucible by interior crucible of the present utility model
In interlayer between outer wall, the small carbon particle after powder carbonization can not be transported to seed crystal and show, while the powder in inner chamber
The gas phase being pyrolyzed in interlayer is played a role in filtering, carbon particle is avoided and is transferred to SiC single crystal surface, so as to greatly reduce SiC
Carbon inclusion enclave in monocrystalline, growth obtain the carbon-free inclusion enclave generation of SiC single crystal that thickness is 20mm.
2nd, the setting of interior crucible of the present utility model, interlayer can make SiC powders point between the inwall and outer wall of interior crucible
The gaseous component of solution is transferred to SiC single crystal surface, ensures the utilization rate of powder, the utilization rate of SiC powders is compared with common crucible
It is kept essentially constant, plays a part of small carbon particle after closing carbonization again.
3rd, in the utility model crucible setting, change conventional crucibles close to sidewall of crucible carbonization critical regions SiC powder
The path that the gaseous component that material decomposes transmits upwards, but along the aperture of interior crucible internal walls by inner chamber SiC powder carries to seed
Brilliant surface, due to nearby being transmitted upwards without direct gaseous component close to sidewall of crucible, correspondence position on crucible cover can be reduced
The polycrystalline growth speed at place, be advantageous to monocrystalline and polycrystalline separation.
4th, crucible structure of the present utility model is simple, and only interior crucible and outer crucible, cost is low, utilization easy to spread.
Brief description of the drawings
Fig. 1 is the structural representation of the growth crucible of raising single-crystal silicon carbide quality of the present utility model；
Fig. 2 is another structural representation of the growth crucible of raising single-crystal silicon carbide quality of the present utility model；
Wherein, 1, outer crucible lid, 2, outer crucible, 3, seed crystal, 4, annular end cap, 5, inwall, 6, powder, 7, boss, 8, folder
Layer, 9, aperture, 10, outer wall.
Embodiment
In order that the purpose of this utility model, technical scheme and advantage are more clear and it can be readily appreciated that below in conjunction with accompanying drawing
And embodiment, the utility model is further elaborated.It should be appreciated that specific embodiment described herein is only used
To explain the utility model, it is not used to limit the utility model.In addition, each embodiment party of the utility model disclosed below
As long as involved technical characteristic does not form conflict can and is mutually combined each other in formula.
Embodiment 1
The growth crucible of inclusion enclave in a kind of reduction single-crystal silicon carbide, structure is as shown in figure 1, including outer crucible 2, outer crucible
Port is provided with the crucible cover 1 of sealing outer crucible, interior crucible is provided with outer crucible 2, interior crucible includes bottom wall and side wall, side
Wall is double side walls, and double side walls include inwall 5 and outer wall, and the aperture 9 of inwall, the diameter of aperture are provided through on inwall 5
For 10mm, the spacing between aperture is 25mm, and bottom wall is arranged on the bottom between inwall and outer wall, and the chamber that inwall surrounds is upper
Lower hollow structure, double side walls upper port are provided with the annular end cap 4 of interlayer between sealing inwall and outer wall.Interior crucible, outer earthenware
Crucible is graphite crucible, and annular end cap, outer crucible lid are graphite cover.The outer wall of interior crucible is close to the madial wall of outer crucible 2,
Away from less than 0.5mm；It is close to the bottom of outer crucible the bottom of interior crucible.The height of interior crucible is the inner chamber vertical height of outer crucible 2
2/3.
In cylinder, the spacing between inwall 5 and outer wall is 20mm for inwall 5, outer wall.Outer crucible lid 1 includes fixed connect
The cover plate and boss 7 connect, cover plate are circular plate type, and boss 7 is inverted round stage, and the cone angle of inverted round stage is 45 °, and the height of inverted round stage is
10mm, the matching of the area and seed crystal of inverted round stage lower end circle.Silicon carbide seed 3 is fixed with the table top of boss 7 of outer crucible lid.Carbon
During SiClx crystal growth, seed crystal is adhered on the table top of inverted round stage, and the cover plate and boss being fixedly connected make monocrystalline and polycrystalline have one
Difference in height, is advantageous to crystal growth and terminates rear monocrystalline to separate with polycrystalline.
The chamber that inwall surrounds is interior crucible interior, and interior crucible interior upper port is relative with the boss 7 of outer crucible lid, interior crucible
Inner chamber upper port diameter is smaller 2mm than boss lower end diameter of a circle.
The port top side wall of outer crucible 2 is evenly distributed with screw, and outer crucible is covered with equal with screw identical distribution spacing
Even to be provided with manhole, graphite screws pass through the manhole and screw of crucible cover, realized between crucible body and crucible cover
It is tightly connected；Preferably, the quantity of screw is 6, manhole and screw quantity Matching.Annular end cap 4 is double-deck with interior crucible
The connected mode of sidewall upper mouth is identical with the connected mode of outer crucible and outer crucible lid.
Embodiment 2
The growth crucible of inclusion enclave in a kind of reduction single-crystal silicon carbide, as described in Example 1, except that：
A diameter of 10mm of aperture, the spacing between aperture are 25mm, and the height of interior crucible is vertically high for the inner chamber of outer crucible 2
The 1/2 of degree.In cylinder, the spacing between inwall 5 and outer wall is 20mm for inwall 5, outer wall.Outer crucible lid 1 includes fixed connect
The cover plate and boss 7 connect, cover plate are circular plate type, and boss 7 is inverted round stage, and the cone angle of inverted round stage is 45 °, and the height of inverted round stage is
10mm, the matching of the area and seed crystal of inverted round stage lower end circle.
Embodiment 3
The growth crucible of inclusion enclave in a kind of reduction single-crystal silicon carbide, structure as the utility model as shown in Fig. 2 implement
A kind of mode of texturing of example 1, as described in Example 1, except that：
Outer wall 10 is in cylinder, and in the form of a truncated cone, the lower end circular diameter of conical butt is more than upper end circular diameter to inwall,
The cone angle of conical butt is 45 °；Interlayer between inwall and outer wall is more than the conical butt of lower end diameter for upper end diameter.
Claims (9)
1. a kind of growth crucible for improving single-crystal silicon carbide quality, including outer crucible, outer crucible port are provided with sealing outer crucible
Crucible cover, it is characterised in that interior crucible is provided with outer crucible, described interior crucible includes bottom wall and side wall, and side wall is
Double side walls, double side walls include inner and outer wall, are provided through the aperture of inwall on inwall, bottom wall be arranged on inwall with it is outer
Bottom between wall, the chamber that inwall surrounds are upper and lower hollow structure, and double side walls upper port is provided with sealing inwall and outer wall
Between interlayer annular end cap.
2. the growth crucible according to claim 1 for improving single-crystal silicon carbide quality, it is characterised in that the height of interior crucible
For the 1/2-2/3 of outer crucible inner chamber vertical height；The outer wall of interior crucible is close to the madial wall of outer crucible, is smaller than 0.5mm；
It is close to the bottom of outer crucible the bottom of interior crucible.
3. the growth crucible according to claim 1 for improving single-crystal silicon carbide quality, it is characterised in that aperture on inwall
A diameter of 8-12mm, the spacing between aperture is 20-35mm.
4. the growth crucible according to claim 1 for improving single-crystal silicon carbide quality, it is characterised in that described inwall,
Outer wall is in cylindrical, and the spacing between described inwall and outer wall is 15~25mm.
5. the growth crucible according to claim 1 for improving single-crystal silicon carbide quality, it is characterised in that outer wall is in cylinder
Shape, in the form of a truncated cone, the lower end circular diameter of conical butt is more than upper end circular diameter to inwall, and the cone angle of conical butt is
40-50 °, the interlayer between inwall and outer wall is more than the conical butt of lower end diameter for upper end diameter.
6. the growth crucible according to claim 1 for improving single-crystal silicon carbide quality, it is characterised in that described outer crucible
Lid includes the cover plate and boss being fixedly connected, and cover plate is circular plate type, and boss is inverted round stage, and the cone angle of inverted round stage is 30-60 °, is fallen
The height of round platform is 5-10mm, the matching of area and seed crystal that inverted round stage lower end is justified.
7. the growth crucible according to claim 1 for improving single-crystal silicon carbide quality, it is characterised in that the chamber that inwall surrounds
For interior crucible interior, interior crucible interior upper port is relative with the boss of outer crucible lid, and interior crucible interior upper port diameter compares boss
The small 1-5mm of lower end diameter of a circle.
8. the growth crucible according to claim 1 for improving single-crystal silicon carbide quality, it is characterised in that outer crucible port side
Screw is evenly distributed with the top of wall, outer crucible is covered to be evenly arranged with manhole, graphite with screw identical distribution spacing
Screw passes through the manhole and screw of crucible cover, and the quantity of screw is 6, manhole and screw quantity Matching；Annular end
Lid is identical with the connected mode of outer crucible and outer crucible lid with the connected mode of double side walls upper port.
9. it is according to claim 1 improve single-crystal silicon carbide quality growth crucible, it is characterised in that outer crucible lid it is convex
Silicon carbide seed is fixed with platform table top；Interior crucible, outer crucible are graphite crucible, and annular end cap, outer crucible lid are graphite cover.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109402731A (en) * | 2018-10-17 | 2019-03-01 | 福建北电新材料科技有限公司 | A kind of high-purity semi-insulating silicon carbide crystalloid grower and its method |
| CN110498686A (en) * | 2019-09-02 | 2019-11-26 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of interlayer silicon carbide microwave heat structure crucible and preparation method thereof |
| CN110565167A (en) * | 2019-08-19 | 2019-12-13 | 河北同光晶体有限公司 | Charging device and charging method for growing SiC single crystal by PVT method |
| CN111575795A (en) * | 2020-05-15 | 2020-08-25 | 南通大学 | Preparation method of blue morusite |
| CN112831841A (en) * | 2020-12-31 | 2021-05-25 | 湖南三安半导体有限责任公司 | Silicon carbide single crystal growth device and growth method thereof |
| CN112981523A (en) * | 2021-03-18 | 2021-06-18 | 哈尔滨化兴软控科技有限公司 | Method and device capable of effectively improving quality of SiC single crystal |
| CN115676833A (en) * | 2021-07-28 | 2023-02-03 | 北京北方华创微电子装备有限公司 | Method for improving synthesis efficiency of silicon carbide powder |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109402731A (en) * | 2018-10-17 | 2019-03-01 | 福建北电新材料科技有限公司 | A kind of high-purity semi-insulating silicon carbide crystalloid grower and its method |
| US11851784B2 (en) | 2018-10-17 | 2023-12-26 | Fujian Beidian Material Technologies Co., Ltd. | Apparatus and method for growing high-purity semi-insulating silicon carbide crystal |
| CN110565167A (en) * | 2019-08-19 | 2019-12-13 | 河北同光晶体有限公司 | Charging device and charging method for growing SiC single crystal by PVT method |
| CN110498686A (en) * | 2019-09-02 | 2019-11-26 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of interlayer silicon carbide microwave heat structure crucible and preparation method thereof |
| CN110498686B (en) * | 2019-09-02 | 2021-08-20 | 中建材蚌埠玻璃工业设计研究院有限公司 | Interlayer silicon carbide crucible with microwave thermal structure and preparation method thereof |
| CN111575795A (en) * | 2020-05-15 | 2020-08-25 | 南通大学 | Preparation method of blue morusite |
| CN112831841A (en) * | 2020-12-31 | 2021-05-25 | 湖南三安半导体有限责任公司 | Silicon carbide single crystal growth device and growth method thereof |
| CN112981523A (en) * | 2021-03-18 | 2021-06-18 | 哈尔滨化兴软控科技有限公司 | Method and device capable of effectively improving quality of SiC single crystal |
| CN115676833A (en) * | 2021-07-28 | 2023-02-03 | 北京北方华创微电子装备有限公司 | Method for improving synthesis efficiency of silicon carbide powder |
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Effective date of registration: 20190327 Address after: 511458 Nansha District, Guangzhou City, Guangdong Province, No. 7 Nanjiang Second Road, Zhujiang Street, self-compiled 2 buildings and 2 floors Patentee after: Guangzhou Nansha Wafer Semiconductor Technology Co., Ltd. Address before: No. 27, mountain Dana Road, Ji'nan City, Shandong, Shandong Patentee before: Shandong University |
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