CN105970286A - Method for multi-crucible LPE (liquid phase epitaxy) of SiC crystals - Google Patents
Method for multi-crucible LPE (liquid phase epitaxy) of SiC crystals Download PDFInfo
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- CN105970286A CN105970286A CN201610463988.4A CN201610463988A CN105970286A CN 105970286 A CN105970286 A CN 105970286A CN 201610463988 A CN201610463988 A CN 201610463988A CN 105970286 A CN105970286 A CN 105970286A
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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
- C30B19/00—Liquid-phase epitaxial-layer growth
- C30B19/06—Reaction chambers; Boats for supporting the melt; Substrate holders
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- Crystallography & Structural Chemistry (AREA)
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Abstract
The invention belongs to the technical field of novel material processing, and provides a method for multi-crucible LPE (liquid phase epitaxy) of SiC crystals. According to the method, a multi-crucible carrying device is adopted, and SiC seed crystals are fixed at bottoms of crucibles under the restriction of graphite ropes and are soaked in melt liquid to grow, therefore, a relatively stable growing environment is provided for the growth of the SiC crystals, C is easily supplied to parts near the SiC seed crystals at the bottom through flowing of the melt liquid, the multi-crucible growth is performed at the same time to improve the production efficiency, and a series of problems about unstable growing environment, low growing speeds and the like existing in a solution method are solved.
Description
Technical field
The invention belongs to new material field of crystal processing, be specifically related to a kind of many crucibles liquid phase epitaxy SiC brilliant
The method of body.
Background technology
Carborundum (SiC) has bigger band gap compared with silicon (Si), and the former possesses more excellent thing
Rationality energy.As the new generation of semiconductor material the most gradually risen, the manufacturer of high-quality SiC monocrystalline
Method causes this skilled person more and more to pay close attention to.The method of growth SiC single crystal is broadly divided at present
Vapor phase method and liquid phase method.Compared with vapor phase method, the speed of growth of liquid phase method is low, but produces height for pursuit
The SiC single crystal of quality, this method is worthy to be popularized.It is controlled that liquid phase method has relatively high polytype
Property also can efficiently reduce the crystal defects such as micro-pipe, fault, can obtain the high-quality SiC that crystallinity is good
Monocrystalline.It is a kind of method being conducive to and generating bulk high-purity SiC single crystal, and avoids vapor phase method
The FAQs such as micro-pipe of middle growth gained crystal existence and fault.Therefore, the expert in this field in recent years
Have been carried out multinomial research (see the open 2004-2173 of Japanese patent application (JP-A-2004-2173),
The open 2000-264790 (JP-A-2000-264790) of Japanese patent application, Japanese patent application disclosure
2007-76986 (JP-A-2007-76986)), attempt utilizing the method for rheotaxial growth SiC crystal
Improve growth rate.
In typical liquid phase method, being, by heating, the Si in graphite crucible is reached molten condition, this melts
Melt Si and there is thermograde, inside melt of si to surface temperature decline, keep inside melt of si to
The thermograde of melt of si surface cooling.C in graphite crucible melts at crucible bottom high-temperature area and melts
Enter in Si fused solution, mainly by the convection action of Si fused solution, the rising of C fused solution is arrived Si subsequently
The low-temperature space of fused solution near surface, so that the supersaturation in low-temperature space of C fused solution.To be fixed on
The SiC seed crystal of graphite rod end is held close on fused solution surface by the stretching of graphite rod, in the meantime,
Oversaturated C, by SiC seed crystal Epitaxial growth, thus obtains SiC single crystal.
But following situation can be there is according to the liquid phase method of this quasi-tradition: past on the aufwuchsplate of SiC crystal
Toward can relatively easily produce hillock.If generation hillock, monocrystalline can be grown individually by hillock,
Thus cause polycrystallization.Even if there being slight growth conditions to change, such as melting at crystal growing surface
In liquid, the slight change of C concentration and temperature can cause the polycrystallization of multiple independent growth hill, hinders formation tool
There is the homogeneous single crystal of flat growth surface, there is the problem being difficult to the smooth crystalline growth face of stable maintenance.
Liquid phase method is thermal balance process, is easier to control growth conditions compared with sublimed method in theory, but for understanding
Certainly stably maintain smooth this problem of crystalline growth face, it is necessary to the most strictly control fused solution convection current,
The parameters such as thermograde, bring great difficulty to concrete operations.
Summary of the invention
The deficiency existed according to prior art and blank, the present inventor provides a kind of many crucibles liquid
The method of phase epitaxy SiC crystal, which employs the bogey of a kind of many crucibles, by leading of graphite rope
System allows SiC seed crystal be fixed on crucible bottom and is immersed in fused solution growth, thus can give SiC crystal
Growth provides metastable growing environment, is prone to C to bottom SiC seed by the flowing of fused solution
Part supply near brilliant, carries out again the growth of many crucibles simultaneously and improves production efficiency, solve in solwution method and deposit
Growing environment is unstable, a series of difficult problems such as growth rate is low.
The concrete technical scheme of the present invention is as follows:
A kind of method of many crucibles liquid phase epitaxy SiC crystal, uses the bogey of a kind of many crucibles to realize,
The bogey structure of these many crucibles is as follows:
Including cavity, being provided with several crucibles in described cavity, connecting outside described crucible bottom has stone
Mo Sheng, described crucible bottom connects SiC seed crystal；Described crucible is graphite crucible；
The method of described many crucibles liquid phase epitaxy SiC crystal, concretely comprises the following steps:
SiC seed crystal is fixed on crucible bottom, and Si raw material is placed in crucible, afterwards that crucible is uniform
It is placed in cavity, and the graphite rope each crucible bottom connected flocks together and is placed in outside cavity, it
Rear airtight cavity, and cavity is placed in conventional liquid phase method in conventional crystalline grower, according to existing liquid
The method of phase epitaxy growth SiC crystal adjusts parameter；
After SiC crystal growth terminates, pulling graphite rope, make every crucible be inverted, SiC crystal inverts
Separate to top thus realization with fused solution.
The present invention also protects the bogey of a kind of many crucibles, and concrete structure includes cavity, described cavity
Inside being provided with several crucibles, connecting outside described crucible bottom has graphite rope, and described crucible bottom is even
It is connected to SiC seed crystal.
General when determining crucible quantity, can be adjusted according to producing needs, guarantee adjacent crucible simultaneously
Will not influence each other when the later stage inverts and be as the criterion；Crucible described in Tong Shi is arranged along the cincture of chamber outer wall surrounding,
So may insure that its later stage is heated evenly.Why the present invention selects graphite rope simultaneously, is owing to it is
Being made up of single C element, will not introduce other miscellaneous elements, graphite itself is resistant to high temperature simultaneously, can
To guarantee not rupture.
In order to reach more preferable effect, cavity bottom can be provided with rotating shaft, by this rotating shaft, whole cavity
Can rotate in crystal course of reaction, by this rotation, the rotation of crucible in chamber can be driven,
And can be accelerated according to the needs of crystal growth or slow down, thus the fused solution in crucible is along with rotation
And flow, it is easy to melted C is supplied near the SiC seed crystal of bottom.
Use the apparatus and method that the present invention provides, can be directly according to existing rheotaxial growth SiC crystal
Method (prior art as pointed out in background technology) adjusts parameter and produces, and such as mode of heating, adds
Heat time, growth atmosphere, heating rate and cooldown rate etc., inventor does not repeats them here；
Time specifically used after guaranteeing above-mentioned condition, by the high-temperature heating of prior art so that at graphite
Crucible is internally generated Si, C fused solution, and graphite crucible provides C source for system, constantly defeated in Si liquation
Send, now in order to reach more preferable effect, cavity and graphite rope can be made according to appointment by controlling rotating shaft
Direction fixed speed uniform rotation, is thus prone to keep equably the temperature of C, Si liquid in crucible, raw
Become SiC fused solution.The one of the present invention big feature is exactly that SiC seed crystal is arranged on crucible bottom, so simultaneously
SiC seed crystal can be immersed in generated SiC fused solution completely, and the C that graphite crucible is generated is the most not
Cut-off is given around SiC seed crystal.Because SiC seed crystal contacts with Si, C fused solution, so at SiC seed
The brilliant temperature temperature than other fused solution parts around creating thermograde and SiC crystal seed neighboring area
Low, make the fused solution of SiC seed crystal neighboring area be in hypersaturated state, thus the upper surface at seed crystal is opened
Begin growth SiC single crystal.In the growth crystallization process of said method, can suitable viscous according to fused solution
Degree judges the rough idea of crystal growth or directly uses other existing means to judge.
After growth terminates, by pulling graphite rope, every crucible can be inverted, now SiC crystal reversion
After be positioned at crucible top, thus separate with fused solution, it is simple to taking out, this process is without using traditional method
In graphite bars regulate and control, simple and direct effectively obtained SiC crystal, this is the present invention and prior art
Another different part, owing to present invention achieves many crucibles rheotaxial growth SiC crystal, productivity
High, it is simple to enterprise's industrialized production, its effect is much better than existing conventional liquid phase method production technology.
In sum, a kind of method inventor providing many crucibles liquid phase epitaxy SiC crystal, which employs
The bogey of a kind of many crucibles, allows SiC seed crystal be fixed on crucible bottom dipping by pining down of graphite rope
Fused solution grows, provides metastable growing environment thus can to the growth of SiC crystal,
It is prone to, by C part supply near the SiC seed crystal of bottom, carry out again many earthenwares by the flowing of fused solution simultaneously
Crucible growth improves production efficiency, solves that growing environment present in solwution method is unstable, growth rate is low
Etc. a series of difficult problems.
Accompanying drawing explanation
Fig. 1 is the bogey structural representation of many crucibles of the present invention；
Fig. 2 is the structure sectional view of A-A in Fig. 1；
Fig. 3 is the structural representation of the used crucible of the present invention；
In figure, 1 is cavity, and 2 is crucible, and 3 is graphite rope, and 4 is SiC seed crystal.
Detailed description of the invention
The present invention is further illustrated below by concrete preparation embodiment, it should be understood, however, that, this
A little embodiments are only used for specifically describing in more detail being used, and are not to be construed as in any form
Limit the present invention.
Embodiment 1
A kind of method of many crucibles liquid phase epitaxy SiC crystal, uses the bogey of a kind of many crucibles to realize,
The bogey structure of these many crucibles is as follows:
Including cavity 1, being provided with several crucibles 2 in described cavity 1, described crucible 2 bottom outside is even
Being connected to graphite rope 3, connecting bottom described crucible 2 has SiC seed crystal 4；Described crucible 2 is graphite crucible；
The method of described many crucibles liquid phase epitaxy SiC crystal, concretely comprises the following steps:
SiC seed crystal is fixed on crucible bottom, and Si raw material is placed in crucible, afterwards that crucible is uniform
It is placed in cavity, and the graphite rope each crucible bottom connected flocks together and is placed in outside cavity, it
Rear airtight cavity, and cavity is placed in conventional liquid phase method in conventional crystalline grower, according to existing liquid
The method of phase epitaxy growth SiC crystal adjusts parameter；
After SiC crystal growth terminates, pulling graphite rope, make every crucible be inverted, SiC crystal inverts
Separate to top thus realization with fused solution.
Embodiment 2
The bogey of a kind of many crucibles, concrete structure includes cavity 1, is provided with some in described cavity 1
Individual crucible 2, described crucible 2 bottom outside connects graphite rope 3, and connecting bottom described crucible 2 has
SiC seed crystal 4；Described crucible 2 is graphite crucible；
It is provided with rotating shaft bottom described cavity 1.
Claims (3)
1. the method for the SiC crystal of crucible liquid phase epitaxy more than one kind, it is characterised in that: use a kind of many crucibles
Bogey realize, the bogey structure of these many crucibles is as follows:
Including cavity (1), in described cavity (1), it is provided with several crucibles (2), described crucible (2)
Bottom outside connects graphite rope (3), and described crucible (2) bottom connects SiC seed crystal (4), institute
Stating crucible is graphite crucible；
The method of described many crucibles liquid phase epitaxy SiC crystal, concretely comprises the following steps:
SiC seed crystal is fixed on crucible bottom, and Si raw material is placed in crucible, afterwards that crucible is uniform
It is placed in cavity, and the graphite rope each crucible bottom connected flocks together and is placed in outside cavity, it
Rear airtight cavity, and cavity is placed in conventional liquid phase method in conventional crystalline grower, according to existing liquid
The method of phase epitaxy growth SiC crystal adjusts parameter；
After SiC crystal growth terminates, pulling graphite rope, make every crucible be inverted, SiC crystal is inverted to
Top thus realize separate with fused solution.
2. realizing the bogey of many crucibles liquid phase epitaxy SiC crystal method described in claim 1, it is special
Levy and be: concrete structure is as follows:
Including cavity (1), in described cavity (1), it is provided with several crucibles (2), described crucible (2)
Bottom outside connects graphite rope (3), and described crucible (2) bottom connects SiC seed crystal (4), institute
Stating crucible is graphite crucible.
Bogey the most according to claim 2, it is characterised in that: described cavity (1) bottom
It is provided with rotating shaft.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610463988.4A CN105970286B (en) | 2016-06-23 | 2016-06-23 | A kind of method of more crucible liquid phase epitaxy SiC crystals |
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| CN201610463988.4A CN105970286B (en) | 2016-06-23 | 2016-06-23 | A kind of method of more crucible liquid phase epitaxy SiC crystals |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115074820A (en) * | 2022-06-17 | 2022-09-20 | 哈尔滨工业大学 | Double-crucible liquid phase epitaxy preparation method of single crystal RIG thick film |
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| JP2000264790A (en) * | 1999-03-17 | 2000-09-26 | Hitachi Ltd | Production of silicon carbide single crystal |
| JP2004002173A (en) * | 2002-04-15 | 2004-01-08 | Sumitomo Metal Ind Ltd | Silicon carbide single crystal and its manufacturing method |
| JP2012036035A (en) * | 2010-08-05 | 2012-02-23 | Bridgestone Corp | Method for manufacturing silicon carbide single crystal |
| CN102534797A (en) * | 2010-11-26 | 2012-07-04 | 信越化学工业株式会社 | Method of producing sic single crystal |
| CN102925967A (en) * | 2011-08-10 | 2013-02-13 | 李汶军 | Method for growing silicon carbide mono-crystals through multi-crucible physical vapor transport technology, and device thereof |
| CN203613305U (en) * | 2013-11-27 | 2014-05-28 | 河北同光晶体有限公司 | Carbonized silicon single crystal production device |
| CN205907390U (en) * | 2016-06-23 | 2017-01-25 | 山东天岳先进材料科技有限公司 | Many crucibles liquid phase epitaxy siC crystal bear device |
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2016
- 2016-06-23 CN CN201610463988.4A patent/CN105970286B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2000264790A (en) * | 1999-03-17 | 2000-09-26 | Hitachi Ltd | Production of silicon carbide single crystal |
| JP2004002173A (en) * | 2002-04-15 | 2004-01-08 | Sumitomo Metal Ind Ltd | Silicon carbide single crystal and its manufacturing method |
| JP2012036035A (en) * | 2010-08-05 | 2012-02-23 | Bridgestone Corp | Method for manufacturing silicon carbide single crystal |
| CN102534797A (en) * | 2010-11-26 | 2012-07-04 | 信越化学工业株式会社 | Method of producing sic single crystal |
| CN102925967A (en) * | 2011-08-10 | 2013-02-13 | 李汶军 | Method for growing silicon carbide mono-crystals through multi-crucible physical vapor transport technology, and device thereof |
| CN203613305U (en) * | 2013-11-27 | 2014-05-28 | 河北同光晶体有限公司 | Carbonized silicon single crystal production device |
| CN205907390U (en) * | 2016-06-23 | 2017-01-25 | 山东天岳先进材料科技有限公司 | Many crucibles liquid phase epitaxy siC crystal bear device |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115074820A (en) * | 2022-06-17 | 2022-09-20 | 哈尔滨工业大学 | Double-crucible liquid phase epitaxy preparation method of single crystal RIG thick film |
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