CN105970286B - A kind of method of more crucible liquid phase epitaxy SiC crystals - Google Patents
A kind of method of more crucible liquid phase epitaxy SiC crystals Download PDFInfo
- Publication number
- CN105970286B CN105970286B CN201610463988.4A CN201610463988A CN105970286B CN 105970286 B CN105970286 B CN 105970286B CN 201610463988 A CN201610463988 A CN 201610463988A CN 105970286 B CN105970286 B CN 105970286B
- Authority
- CN
- China
- Prior art keywords
- crucible
- sic
- cavity
- liquid phase
- graphite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention belongs to new material processing technique field, inventor provide a kind of method of more crucible liquid phase epitaxy SiC crystals, which employs a kind of bogey of more crucibles, allow SiC seed crystals to be fixed on crucible bottom and be immersed in fused solution to grow by pining down for graphite rope, thus metastable growing environment can be provided to the growth of SiC crystal, it is easy to bottom SiC seed crystals nearby partly supply C by the flowing of fused solution, carry out more crucible growths again simultaneously and improve production efficiency, it is unstable to solve growing environment present in solwution method, a series of problems such as growth rate is low.
Description
Technical field
The invention belongs to new material field of crystal processing, and in particular to a kind of method of more crucible liquid phase epitaxy SiC crystals.
Background technology
Carborundum (SiC) has bigger band gap compared with silicon (Si), and the former possesses more excellent physical property.As
The new generation of semiconductor material gradually risen, the manufacture method of high-quality SiC monocrystalline cause art personnel more next
More concerns.The method of growth SiC single crystal is broadly divided into vapor phase method and liquid phase method at present.Compared with vapor phase method, liquid phase method
The speed of growth is low, but the SiC single crystal of high quality is produced for pursuit, and this method is worthy to be popularized.Liquid phase method has relative
High polytype controllability simultaneously can efficiently reduce the crystal defects such as micro-pipe, fault, can obtain the good high quality SiC of crystallinity
Monocrystalline.It is a kind of method for being advantageous to generate bulk high-purity SiC single crystal, and avoids growth gained crystal in vapor phase method
The FAQs such as existing micro-pipe and fault.Therefore, multinomial research has been carried out (see Japan in the brainstrust in the field in recent years
Patent application publication 2004-2173 (JP-A-2004-2173), Japanese patent application disclose 2000-264790 (JP-A-2000-
264790), Japanese patent application discloses 2007-76986 (JP-A-2007-76986)), trial utilizes rheotaxial growth SiC
The method of crystal improves growth rate.
It is that the Si in graphite crucible is reached into molten condition by heating, the melt of si is present in typical liquid phase method
Thermograde, decline inside melt of si to surface temperature, keep inside melt of si to the temperature ladder of melt of si surface cooling
Degree.C in graphite crucible melts and is dissolved into Si fused solutions in crucible bottom high-temperature area, then mainly by Si fused solutions
C fused solutions are risen to the low-temperature space up to Si fused solution near surfaces by convection action, so that C fused solutions mistake in low-temperature space
Saturation.The SiC seed crystals for being fixed on graphite rod end are held close on fused solution surface by the stretching of graphite rod, in this phase
Between, oversaturated C is by SiC seed crystal Epitaxial growths, thus obtaining SiC single crystal.
But following situation can be had according to the liquid phase method of this quasi-tradition：It is often relative on the aufwuchsplate of SiC crystal
Easily produce hillock.If producing hillock, monocrystalline can be grown individually by hillock, so as to cause polycrystallization.Even if
There is slight growth conditions to change, such as the slight change of C concentration and temperature can trigger in the fused solution at crystal growing surface
The polycrystallization of multiple individually growth hills, hinders to form the homogeneous single crystal with flat growth surface, exists and is difficult to stably remain flat
The problem of smooth crystalline growth face.Liquid phase method is thermal balance process, is easier control growth conditions in theory compared with sublimed method,
But in order to solve flat this problem of crystalline growth face of stable maintenance, it is necessary to strictly control very much convection current, the temperature of fused solution
The parameters such as gradient are spent, great difficulty is brought to concrete operations.
The content of the invention
According to the shortcomings of the prior art and blank, the present inventor provides a kind of more crucible liquid phase epitaxies
The method of SiC crystal, which employs a kind of bogey of more crucibles, allows SiC seed crystals to be fixed on earthenware by pining down for graphite rope
Crucible bottom, which is immersed in fused solution, to be grown, and thus can be provided metastable growing environment to the growth of SiC crystal, be passed through
The flowing of fused solution is easy to C to the part supply nearby of bottom SiC seed crystals, while carries out more crucibles growths again and improve production effect
Rate, a series of problems such as growing environment is unstable, growth rate is low are solved present in solwution method.
The concrete technical scheme of the present invention is as follows：
A kind of method of more crucible liquid phase epitaxy SiC crystals, realized using a kind of bogey of more crucibles, more crucibles
Bogey structure it is as follows：
Including cavity, several crucibles are provided with the cavity, graphite rope is connected with the outside of the crucible bottom, it is described
Crucible bottom be connected with SiC seed crystals；The crucible is graphite crucible；
The method of more crucible liquid phase epitaxy SiC crystals, is concretely comprised the following steps：
SiC seed crystals are fixed on crucible bottom, and Si raw materials are placed in crucible, crucible is uniformly placed on cavity afterwards
It is interior, and the graphite rope that each crucible bottom connects is flocked together and is placed in outside cavity, airtight cavity, and cavity is placed in afterwards
In conventional liquid phase method in conventional crystalline grower, according to the method adjusting parameter of existing rheotaxial growth SiC crystal；
After SiC crystal growth terminates, graphite rope is pulled, is inverted every crucible, SiC crystal is inverted to top so as to real
Now with the separation of fused solution.
The present invention also protects a kind of bogey of more crucibles, and concrete structure includes cavity, is provided with the cavity
Several crucibles, the crucible bottom outside are connected with graphite rope, and described crucible bottom is connected with SiC seed crystals.
Typically it is determined that during crucible quantity, can be adjusted according to production needs, while ensure that adjacent crucible is anti-in the later stage
It will not influence each other and be defined when turning；Described crucible so may insure its later stage along chamber outer wall surrounding around setting simultaneously
It is heated evenly.Why the present invention selects graphite rope simultaneously, is due to that it is made up of single C element, it is miscellaneous will not to introduce other
Element, while graphite is resistant to high temperature in itself, it can be ensured that it is not broken in process of production.
In order to reach more preferable effect, cavity bottom can be provided with rotating shaft, by the rotating shaft, whole cavity can be in crystal
Rotated in course of reaction, by this rotation, the rotation of crucible in chamber can be driven, and can be according to the needs of crystal growth
To carry out acceleration or deceleration, thus the fused solution in crucible flows with rotation, is easy to that melting C is attached to bottom SiC seed crystals
Nearly supply.
Using apparatus and method provided by the invention, can directly according to existing rheotaxial growth SiC crystal method (such as
The prior art pointed out in background technology) adjusting parameter produced, such as mode of heating, heat time, growth atmosphere, heating speed
Rate and cooldown rate etc., inventor will not be repeated here；
When specifically used after above-mentioned condition is ensured, pass through the high-temperature heating of prior art so that in graphite crucible
Portion generates Si, C fused solution, and graphite crucible provides C sources for system, constantly conveyed into Si liquations, now in order to reach more preferable
Effect, can be by controlling rotating shaft cavity and graphite rope is so made it easy to according to assigned direction fixed speed uniform rotation
The temperature of C, Si liquid in crucible is kept evenly, generates SiC fused solutions.The big feature of the present invention is exactly that SiC seed crystals are set simultaneously
In crucible bottom, such SiC seed crystals can be immersed in generated SiC fused solutions completely, and the C that graphite crucible is generated is in a steady stream not
Cut-off is given around SiC seed crystals.Because SiC seed crystals contact with Si, C fused solution, temperature ladder is generated around SiC seed crystals
The temperature of degree and SiC crystal seeds neighboring area is lower than the temperature of other fused solution parts, at the fused solution for making SiC seed crystals neighboring area
In hypersaturated state, thus start to grow SiC single crystal in the upper surface of seed crystal., can in the growth crystallization process of the above method
To judge the rough idea of crystal growth suitably according to the viscosity of fused solution or directly be judged using other existing means.
After growth terminates, you can by pulling graphite rope to be inverted every crucible, be located at earthenware after now SiC crystal reversion
At the top of crucible, so as to separate with fused solution, it is easy to take out, this process with the graphite bars in conventional method without being regulated and controled, letter
Victory has effectively obtained SiC crystal, and this is the present invention and the another different part of prior art, due to the present invention realize it is more
Crucible rheotaxial growth SiC crystal, yield is high, is easy to enterprise's industrialized production, its effect is much better than existing conventional liquid phase
Method production technology.
In summary, a kind of method of more crucible liquid phase epitaxy SiC crystals is inventor provided, which employs a kind of more earthenwares
The bogey of crucible, allow SiC seed crystals to be fixed on crucible bottom and be immersed in fused solution to grow by pining down for graphite rope, thus both
Metastable growing environment can be provided to the growth of SiC crystal, be easy to by the flowing of fused solution by C to bottom SiC seeds
Brilliant part nearby supplies, while carries out more crucible growths again and improve production efficiency, solves growing environment present in solwution method
A series of unstable, problems such as growth rate is low.
Brief description of the drawings
Fig. 1 is the bogey structural representation of more crucibles of the present invention；
Fig. 2 is the structure sectional view of A-A in Fig. 1；
Fig. 3 uses the structural representation of crucible for the present invention；
1 is cavity in figure, and 2 be crucible, and 3 be graphite rope, and 4 be SiC seed crystals.
Embodiment
The present invention is further illustrated below by the specific embodiment for preparing, it should be understood, however, that, these embodiments are only
It is only for specifically describing in more detail and is used, and is not to be construed as limiting the present invention in any form.
Embodiment 1
A kind of method of more crucible liquid phase epitaxy SiC crystals, realized using a kind of bogey of more crucibles, more crucibles
Bogey structure it is as follows：
Including cavity 1, several crucibles 2 are provided with the cavity 1, the bottom outside of crucible 2 is connected with graphite rope
3, the described bottom of crucible 2 is connected with SiC seed crystals 4；The crucible 2 is graphite crucible；
The method of more crucible liquid phase epitaxy SiC crystals, is concretely comprised the following steps：
SiC seed crystals are fixed on crucible bottom, and Si raw materials are placed in crucible, crucible is uniformly placed on cavity afterwards
It is interior, and the graphite rope that each crucible bottom connects is flocked together and is placed in outside cavity, airtight cavity, and cavity is placed in afterwards
In conventional liquid phase method in conventional crystalline grower, according to the method adjusting parameter of existing rheotaxial growth SiC crystal；
After SiC crystal growth terminates, graphite rope is pulled, is inverted every crucible, SiC crystal is inverted to top so as to real
Now with the separation of fused solution.
Embodiment 2
A kind of bogey of more crucibles, concrete structure include cavity 1, several crucibles 2 are provided with the cavity 1,
The bottom outside of crucible 2 is connected with graphite rope 3, and the described bottom of crucible 2 is connected with SiC seed crystals 4；The crucible 2 is graphite
Crucible；
The bottom of cavity 1 is provided with rotating shaft.
Claims (3)
- A kind of 1. method of more crucible liquid phase epitaxy SiC crystals, it is characterised in that：It is real using a kind of bogey of more crucibles Existing, the bogey structure of more crucibles is as follows：Including cavity (1), several crucibles (2) are provided with the cavity (1), crucible (2) bottom outside is connected with stone Ink rope (3), described crucible (2) bottom are connected with SiC seed crystals (4), and the crucible is graphite crucible；The method of more crucible liquid phase epitaxy SiC crystals, is concretely comprised the following steps：SiC seed crystals are fixed on crucible bottom, and Si raw materials are placed in crucible, are afterwards uniformly placed on crucible in cavity, And the graphite rope that each crucible bottom connects flocks together and is placed in outside cavity, airtight cavity, and cavity is placed in often afterwards Advise in liquid phase method in conventional crystalline grower, according to the method adjusting parameter of existing rheotaxial growth SiC crystal；After SiC crystal growth terminates, pull graphite rope, be inverted every crucible, SiC crystal be inverted to top so as to realize with The separation of fused solution.
- 2. realize the bogey of more crucible liquid phase epitaxy SiC crystal methods described in claim 1, it is characterised in that：Specific knot Structure is as follows：Including cavity (1), several crucibles (2) are provided with the cavity (1), crucible (2) bottom outside is connected with stone Ink rope (3), described crucible (2) bottom are connected with SiC seed crystals (4), and the crucible is graphite crucible.
- 3. bogey according to claim 2, it is characterised in that：Described cavity (1) bottom is provided with rotating shaft.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610463988.4A CN105970286B (en) | 2016-06-23 | 2016-06-23 | A kind of method of more crucible liquid phase epitaxy SiC crystals |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610463988.4A CN105970286B (en) | 2016-06-23 | 2016-06-23 | A kind of method of more crucible liquid phase epitaxy SiC crystals |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105970286A CN105970286A (en) | 2016-09-28 |
| CN105970286B true CN105970286B (en) | 2018-04-10 |
Family
ID=57022601
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610463988.4A Active CN105970286B (en) | 2016-06-23 | 2016-06-23 | A kind of method of more crucible liquid phase epitaxy SiC crystals |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105970286B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115074820B (en) * | 2022-06-17 | 2023-07-18 | 哈尔滨工业大学 | Double-crucible liquid phase epitaxy preparation method of single crystal RIG thick film |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000264790A (en) * | 1999-03-17 | 2000-09-26 | Hitachi Ltd | Production of silicon carbide single crystal |
| JP4100228B2 (en) * | 2002-04-15 | 2008-06-11 | 住友金属工業株式会社 | Silicon carbide single crystal and manufacturing method thereof |
| JP2012036035A (en) * | 2010-08-05 | 2012-02-23 | Bridgestone Corp | Method for manufacturing silicon carbide single crystal |
| US10167573B2 (en) * | 2010-11-26 | 2019-01-01 | Shin-Etsu Chemical Co., Ltd. | Method of producing SiC single crystal |
| 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 |
-
2016
- 2016-06-23 CN CN201610463988.4A patent/CN105970286B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN105970286A (en) | 2016-09-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR20120057536A (en) | Method of Producing SiC Single Crystal | |
| JP2008031019A (en) | Method of manufacturing sapphire single crystal | |
| CN105970286B (en) | A kind of method of more crucible liquid phase epitaxy SiC crystals | |
| CN205907390U (en) | Many crucibles liquid phase epitaxy siC crystal bear device | |
| CN107949665A (en) | Single-crystal manufacturing apparatus | |
| CN106012021B (en) | A kind of seed shaft and method of liquid growth silicon carbide | |
| CN206052208U (en) | A kind of seed shaft of scalable growth of silicon carbide thermograde | |
| KR100816764B1 (en) | Synthetic apparatus of semiconductor polycrystal compound and synthetic method of the same | |
| JP2531875B2 (en) | Method for producing compound semiconductor single crystal | |
| JP2758038B2 (en) | Single crystal manufacturing equipment | |
| CN113215660B (en) | Silicon carbide single crystal growth method capable of reducing heater loss | |
| CN105970294A (en) | Liquid-phase growing silicon carbide seed crystal shaft device | |
| JP2733898B2 (en) | Method for manufacturing compound semiconductor single crystal | |
| JPS63295498A (en) | Production of single-crystal of group iii-v compound semiconductor | |
| RU2626637C1 (en) | Method for growing high-temperature monocrystals by sinelnikov-dziov's method | |
| JP4576571B2 (en) | Method for producing solid solution | |
| KR101339151B1 (en) | Apparatus and method for growing monocrystalline silicon ingots | |
| JP2014156373A (en) | Manufacturing apparatus for sapphire single crystal | |
| JP2004338960A (en) | METHOD FOR MANUFACTURING InP SINGLE CRYSTAL | |
| JP2004250297A (en) | Method for manufacturing compound semiconductor single crystal | |
| JPH02229783A (en) | Method for growing single crystal of compound semiconductor by vertical type boat method | |
| CN113774489A (en) | Growth device and growth method of indium phosphide single crystal | |
| JPH09249479A (en) | Method for growing compound semiconductor single crystal | |
| JPS63215594A (en) | Growth of crystal by double crucible | |
| JP2004269328A (en) | Manufacturing apparatus of single crystal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: No.99, Tianyue South Road, Huaiyin District, Jinan City, Shandong Province Patentee after: Shandong Tianyue advanced technology Co., Ltd Address before: Room 1106-6-01, AB Block, Century Fortune Center, West Side of Xinyu Road, Jinan High-tech Zone, Shandong Province Patentee before: Shandong Tianyue Advanced Materials Technology Co.,Ltd. |