CN106048728B - A kind of method of growing high quality silicon carbide whisker - Google Patents
A kind of method of growing high quality silicon carbide whisker Download PDFInfo
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- CN106048728B CN106048728B CN201610482192.3A CN201610482192A CN106048728B CN 106048728 B CN106048728 B CN 106048728B CN 201610482192 A CN201610482192 A CN 201610482192A CN 106048728 B CN106048728 B CN 106048728B
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- whisker
- silicon carbide
- graphite crucible
- stick
- collecting board
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
-
- 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
- C30B9/00—Single-crystal growth from melt solutions using molten solvents
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- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention belongs to silicon carbide solwution method technical fields, a kind of more particularly to method of growing high quality silicon carbide whisker, it employs and is realized with a kind of grower, by the way that whisker collection stick and collecting board are immersed in the silicon carbide solution in graphite crucible, by adjusting synthesising position and synthesis temperature, controllable growth whisker.Using the present invention provides a kind of methods for producing high-quality SiC whisker, production process is simple, and strong operability, production cost is low, can mass growth controlled dimensions high-quality silicon carbide whisker.
Description
Technical field
The invention belongs to silicon carbide solwution method technical field more particularly to a kind of sides of growing high quality silicon carbide whisker
Method.
Background technology
Silicon carbide (SiC) is the Typical Representative in half semiconductor material with wide forbidden band of the third generation, compared to traditional material silicon
（Si）It has apparent advantage in energy gap, thermal conductivity, critical breakdown strength, saturated electrons drift speed etc..Carbon
SiClx whisker has many advantages, such as high-melting-point, high intensity, low thermal expansion, corrosion-resistant, and ceramic base and Metal Substrate etc. can be used as multiple
The activeness and quietness agent of condensation material, can as ceramic mechanism, high grade refractory, refractory coating material, be widely used in machinery,
The fields such as electronics and aviation.
The method of growth silicon carbide whisker conventional at present, mainly by adding after simply silicon and carbon are mixed
It is generated after heat, heat preservation, natural cooling.The silicon carbide whisker of these methods generation, impurity content is high, and crystal form is more, and yield is small, together
When whisker length it is uncontrollable, it is impossible to as a kind of growth pattern of industrialization.And the silicon carbide whisker that these methods are synthesized
It must, it is also necessary to which the purification process after coming out of the stove needs to carry out the chemical treatments purifying such as decarburization, de- silica, deferrization.Growth technique
Complexity, and the whisker synthesized is unstable.
Therefore, mass grows the high-quality silicon carbide whisker of controlled dimensions, is current industrialization growth silicon carbide whisker
The key of palpus.
Invention content
The present invention provides a kind of method of growing high quality silicon carbide whisker to solve existing issue, and the present invention is simple easy
Operation, it is highly practical, it can be mass high-quality whisker.
To realize the purpose of foregoing invention, specific technical solution scheme of the present invention is as follows：
A kind of method of growing high quality silicon carbide whisker is realized, the structure of the grower using a kind of grower
It is as follows：
Whisker including that can accommodate the graphite crucible of silicon carbide solution and can stretch into inside graphite crucible collects stick, described
Whisker collects stick and is provided with collecting board；The top open part of the graphite crucible is provided with crucible cover；The graphite crucible
Outside be enclosed with thermal insulation board.
The graphite crucible, for storing raw material polysilicon（Polysilicon of the present invention can be block or powder, it is pure
It spends for more than 6N）And the solution after fusing；Graphite crucible be both hold solution container and crystal growth carbon source is provided.It is more
The Si of melting is formed after crystal silicon fusing, corrodes graphite crucible, forms silicon carbide solution.
The method of the growing high quality silicon carbide whisker, the specific steps are：First by the stone equipped with polycrystalline silicon raw material
Black crucible is put into vacuum drying oven, and vacuum furnace chamber then is evacuated to 0Pa, then to filling with inert gas in vacuum furnace chamber,
Such as helium or argon gas, 0.5-1atm is charged to, then graphite crucible is heated, be to slowly warm up to 1420 DEG C, until polycrystalline
Silicon melts；1500-2300 DEG C is continuously heating to, keeps the temperature 30min, the silicon of melting is made to corrode graphite crucible, so as to obtain silicon carbide
Solution；Then whisker is collected into stick and collecting board is immersed in the silicon carbide solution in graphite crucible, then rotated whisker and collect
Plate stirs silicon carbide solution, promotes the uniformity of solute Distribution, ensures the consistency of whisker growth environment, and rotation is finished, closed
Into position be that height of the collecting board apart from liquid level is at 0.2-5cm, generated time is kept for 1-20 hours, can obtain predetermined length
Silicon carbide whisker；After synthesis terminates, carbon whisker is collected into stick and collecting board lifts out solution, natural cooling is collected and obtained
Silicon carbide whisker.
The position and generated time that the length of heretofore described silicon carbide whisker is synthesized by it determine that length can be
1mm-5cm；
The crystal form of heretofore described silicon carbide whisker is determined that crystal form can be by synthesis temperature
3C-SiC, 4H-SiC, 6H-SiC and 15R-SiC etc.；
Heretofore described graphite crucible, polysilicon, whisker are collected stick and collecting board and can be reused, and reduce system
The cost of standby whisker.
The present invention also protects a kind of growth cell configuration as follows：
Whisker including that can accommodate the graphite crucible of silicon carbide solution and can stretch into inside graphite crucible collects stick, described
Whisker collects stick and is provided with collecting board；The top open part of the graphite crucible is provided with crucible cover；The graphite crucible
Outside be enclosed with thermal insulation board.
The mode of heating of heretofore described vacuum drying oven can be resistance-type heating or induction type heating.
In conclusion using the present invention provides a kind of methods for producing high-quality SiC whisker, production process is simple, behaviour
The property made is strong, and production cost is low, can mass growth controlled dimensions high-quality silicon carbide whisker.
Description of the drawings
Fig. 1 is growth cell configuration schematic diagram of the present invention；
1 is thermal insulation board in figure, and 2 be crucible cover, and 3 be graphite crucible, and 4 be silicon carbide solution, and 5 be collecting board, and 6 receive for whisker
Collect stick.
Specific embodiment
Embodiment 1
The graphite crucible equipped with polycrystalline silicon raw material is put into vacuum drying oven first, is then evacuated to vacuum furnace chamber
0Pa then to argon gas is filled in burner hearth, is charged to 0.5atm, then graphite crucible is heated, is to slowly warm up to 1420 DEG C,
Until polysilicon melts.1500 DEG C are continuously heating to, keeps the temperature 30 minutes, the silicon of melting is made to corrode graphite crucible, so as to obtain carbon
SiClx solution.Then silicon carbide whisker is collected into stick and collecting board is immersed in the silicon carbide solution in graphite crucible, collecting board
Apart from liquid level 3cm, kept for 3 hours, can obtain a diameter of 500 μm, the 3C-SiC whiskers of a length of 2cm.
Embodiment 2
The graphite crucible equipped with polycrystalline silicon raw material is put into vacuum drying oven first, is then evacuated to vacuum furnace chamber
0Pa then to argon gas is filled in burner hearth, is charged to 1atm, then graphite crucible is heated, is to slowly warm up to 1420 DEG C, directly
Melt to polysilicon.1500 DEG C are continuously heating to, keeps the temperature 30 minutes, the silicon of melting is made to corrode graphite crucible, so as to be carbonized
Silicon solution.Then silicon carbide whisker is collected stick and collecting board to be immersed in the silicon carbide solution in graphite crucible, collecting board away from
Chaotropic face 3cm is kept for 6 hours, can obtain a diameter of 500 μm, the 3C-SiC whiskers of a length of 4cm.
Embodiment 3
The graphite crucible equipped with polycrystalline silicon raw material is put into vacuum drying oven first, is then evacuated to vacuum furnace chamber
0Pa then to helium is filled in burner hearth, is charged to 0.7atm, then graphite crucible is heated, is to slowly warm up to 1420 DEG C,
Until polysilicon melts.1700 DEG C are continuously heating to, keeps the temperature 30 minutes, the silicon of melting is made to corrode graphite crucible, so as to obtain carbon
SiClx solution.Then silicon carbide whisker is collected into stick and collecting board is immersed in the silicon carbide solution in graphite crucible, collecting board
Apart from liquid level 1cm, kept for 3 hours, can obtain a diameter of 600 μm, the 4H-SiC whiskers of a length of 3cm.
Embodiment 4
The graphite crucible equipped with polycrystalline silicon raw material is put into vacuum drying oven first, is then evacuated to vacuum furnace chamber
0Pa then to helium is filled in burner hearth, is charged to 0.7atm, then graphite crucible is heated, is to slowly warm up to 1420 DEG C,
Until polysilicon melts.2200 DEG C are continuously heating to, keeps the temperature 30 minutes, the silicon of melting is made to corrode graphite crucible, so as to obtain carbon
SiClx solution.Then silicon carbide whisker is collected into stick and collecting board is immersed in the silicon carbide solution in graphite crucible, collecting board
Apart from liquid level 1cm, kept for 3 hours, can obtain a diameter of 550 μm, the 6H-SiC whiskers of a length of 4cm.
Embodiment 5
The graphite crucible equipped with polycrystalline silicon raw material is put into vacuum drying oven first, is then evacuated to vacuum furnace chamber
0Pa then to argon gas is filled in burner hearth, is charged to 1atm, then graphite crucible is heated, is to slowly warm up to 1420 DEG C, directly
Melt to polysilicon.1900 DEG C are continuously heating to, keeps the temperature 30 minutes, the silicon of melting is made to corrode graphite crucible, so as to be carbonized
Silicon solution.Then silicon carbide whisker is collected stick and collecting board to be immersed in the silicon carbide solution in graphite crucible, collecting board away from
Chaotropic face 5cm is kept for 20 hours, can obtain a diameter of 700 μm, the 4H-SiC whiskers of a length of 8cm.
Embodiment 6
Realize that the growth cell configuration of above-described embodiment 1-5 is as follows：
Whisker including that can accommodate the graphite crucible of silicon carbide solution and can stretch into inside graphite crucible collects stick, described
Whisker collects stick and is provided with collecting board；The top open part of the graphite crucible is provided with crucible cover；The graphite crucible
Outside be enclosed with thermal insulation board.
Claims (2)
- A kind of 1. method of growing high quality silicon carbide whisker, it is characterised in that：The structure of the grower is as follows：Including silicon carbide solution can be accommodated（4）Graphite crucible（3）With can stretch into graphite crucible（3）Internal whisker collects stick （6）, the whisker collects stick（6）It is provided with collecting board（5）；The graphite crucible（3）Top open part be provided with earthenware Crucible lid（2）；The graphite crucible（3）Outside be enclosed with thermal insulation board（1）；The method of the growing high quality silicon carbide whisker, the specific steps are：The graphite crucible equipped with polycrystalline silicon raw material is put into vacuum drying oven first, vacuum furnace chamber is then evacuated to 0Pa, with Filling with inert gas in backward vacuum furnace chamber, is charged to 0.5-1atm, then graphite crucible is heated, be to slowly warm up to 1420 DEG C, until polysilicon melts；1500-2300 DEG C is continuously heating to, keeps the temperature 30min, the silicon of melting is made to corrode graphite crucible, so as to Obtain silicon carbide solution；Then silicon carbide whisker is collected into stick and collecting board is immersed in the silicon carbide solution in graphite crucible, Then whisker collecting board is rotated, stirs silicon carbide solution, promotes the uniformity of solute Distribution, ensures the consistent of whisker growth environment Property, rotation finishes, and be height of the collecting board apart from liquid level in the position of synthesis is at 0.2-5cm, and generated time keeps 1-20 small When, it can obtain the silicon carbide whisker of predetermined length；After synthesis terminates, carbon whisker is collected into stick and collecting board lifts out solution, Natural cooling collects the silicon carbide whisker of acquisition.
- 2. realize the grower of the method for growing high quality silicon carbide whisker described in claim 1, it is characterised in that：Specific knot Structure is as follows：Including silicon carbide solution can be accommodated（4）Graphite crucible（3）With can stretch into graphite crucible（3）Internal whisker is collected Stick（6）, the whisker collects stick（6）It is provided with collecting board（5）；The graphite crucible（3）Top open part be provided with Crucible cover（2）；The graphite crucible（3）Outside be enclosed with thermal insulation board（1）.
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| CN116288717A (en) * | 2017-08-12 | 2023-06-23 | 天水佳吉化工有限公司 | Production method of nano-micron silicon carbide whisker |
| CN114481325A (en) * | 2022-01-29 | 2022-05-13 | 北京青禾晶元半导体科技有限责任公司 | Device and method for manufacturing silicon carbide polycrystal |
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| US4702901A (en) * | 1986-03-12 | 1987-10-27 | The United States Of America As Represented By The United States Department Of Energy | Process for growing silicon carbide whiskers by undercooling |
| CN100415951C (en) * | 2006-01-17 | 2008-09-03 | 浙江大学 | Method for SiC whisker growth |
| CN101402455B (en) * | 2008-09-22 | 2011-04-06 | 新疆天科合达蓝光半导体有限公司 | Method for producing silicon carbide nano-stick with sublimation |
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Address after: No.99, Tianyue South Road, Huaiyin District, Jinan City, Shandong Province Patentee after: Shandong Tianyue advanced technology Co., Ltd Address before: 250100 Shandong city of Ji'nan province high tech Zone Xinyu Road on the west side of century wealth center AB block 1106-6-01 Patentee before: Shandong Tianyue Advanced Materials Technology Co.,Ltd. |