CN1544715A - Method and apparatus for growing silicon carbide single crystal by physical vapor transportation - Google Patents
Method and apparatus for growing silicon carbide single crystal by physical vapor transportation Download PDFInfo
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- CN1544715A CN1544715A CNA2003101135239A CN200310113523A CN1544715A CN 1544715 A CN1544715 A CN 1544715A CN A2003101135239 A CNA2003101135239 A CN A2003101135239A CN 200310113523 A CN200310113523 A CN 200310113523A CN 1544715 A CN1544715 A CN 1544715A
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- crucible
- crystal
- lid
- silicon carbide
- physical vapor
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- 239000013078 crystal Substances 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 24
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims description 27
- 229910010271 silicon carbide Inorganic materials 0.000 title claims description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 239000010439 graphite Substances 0.000 claims description 12
- 230000005540 biological transmission Effects 0.000 claims description 9
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 238000012423 maintenance Methods 0.000 claims description 3
- 230000000295 complement effect Effects 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 14
- 241000209456 Plumbago Species 0.000 description 8
- 239000002245 particle Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 4
- 238000012856 packing Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method of growing SiC by physical gas-phase transportation, and its step: 1, keeping the state parameters and control modes of existing techniques; 2, during the growth of crystal, in the state that crucible cover reliably covers the crucible all along, by changing the positions in the temperature fields where they exist respectively, keeping the temperature difference between the crystal growth surface and the material surface in the crucible. Where the step 2 can also be: during the growth of crystal, in the state that crucible cover reliably covers the crucible all along, by changing their relative positions, keeping the distance between the crystal growth surface and the material surface in the crucible. By this method, the crystal growth is in an optimum driving force state all along, and it is simple to construct and convenient to operate. In addition, the crystal quality is ensured.
Description
Technical field
The present invention relates to a kind of method and device thereof of physical vapor transmission growing silicon carbide single crystal.
Background technology
In the method for conventional at present physical vapor transmission growing silicon carbide single crystal, silicon carbide material source and seed crystal place the two ends up and down of same close crucible, leave certain clearance therebetween.General situation is: material source is placed on crucible bottom, seed crystal places on the crucible interior surface, puts in the stove with suitable temperature field distribution after crucible fixedly assembles with lid and grows, and consults U.S. Pat 6,261,363B1 and " Journal of Inorganic Materials " the 17th volume the 4th phase 685-690 page or leaf July in 2002.In process of growth, crucible (comprising crucible and lid) is an integral body, does not have artificial controlled relative movement between silicon carbide material source wherein and the seed crystal.Like this, along with crystal is constantly long thick, the temperature head between charge level and the crystal growth face must be among the continuous variation, and one of stable key factor that guarantees the good growth of single-crystal silicon carbide exactly of this temperature head.
During physical vapor transmission growing silicon carbide single crystal, material source should be in the high-temperature zone, and seed crystal (or rather, being the solid-aerosphere face of crystal growth) should be in cold zone, and the temperature head between the two is exactly the motivating force source of growing silicon carbice crystals.From the crystal aspect: along with crystal is long gradually thick, himself is incubated and becomes better and better, the temperature on the growth interface will be more and more higher, causes the growth motivating force more and more littler.From the material source aspect: along with the carrying out of growing silicon carbice crystals, raw material constantly consumes, and the temperature distribution in charge level and the material source can change thereupon, and this also is unfavorable for keeping the temperature head between charge level and the crystal growth face constant.
Summary of the invention
Problem at the prior art existence, the present invention proposes a kind of new physical vapor and transmit the method for growing silicon carbide single crystal, this method is in the growing silicon carbice crystals process, can keep the temperature head between charge level and the crystal growth face constant or stable as far as possible, thereby provide reliable motivating force for crystal growth.
Another object of the present invention provides a kind of special copple used in aforesaid method and crucible lid thereof.
The present invention is achieved in that
1. keep constant with same state parameter and the control mode of prior art;
2. in crystal growing process, be in all the time under the state of reliable fastening with crucible at the crucible lid,
By changing the position in crucible lid and the crucible temperature of living in separately field, cover crystal to keep crucible
Temperature head in aufwuchsplate and the crucible between the charge level is constant.
The another kind of mode that realizes the object of the invention is:
1. keep constant with same state parameter and the control mode of prior art;
2. in crystal growing process, be in all the time under the state of reliable fastening with crucible at the crucible lid, by changing the mutual alignment between crucible lid and the crucible, constant to keep crucible to cover in crystal growth face and the crucible distance between the charge level.
Further, the mutual alignment between described change crucible lid and the crucible, promptly control crucible lid and crucible vertically by suitable speed mutually near or mutually away from.
Further, described suitable speed equal or the crystal growth face of being approximately equal to and charge level between away from or approaching speed.
A kind of special copple that aforesaid method is used and crucible lid, wherein crucible lid is the column that is complementary with the crucible section form or the tubular of an end opening one end sealing, crucible covers spiral-lock or is inserted on the crucible and also is slidingly matched with it, the two has suitable overlap length, keeping under the constant situation of buckling state with crucible to guarantee the crucible lid, can slide mutually vertically within the specific limits, described crucible and crucible lid are made by graphite.
After adopting the inventive method, the crystalline growth is in optimal drive power state all the time, thereby has overcome can not growing than the limitation of macrocrystal that prior art exists, and in implementation process, easy and simple to handle.In addition, because of crystal is grown under the ambient conditions of stable and consistent always, so its quality is well ensured.
Embodiment
Embodiment 1
With external diameter 100
-0.1The plumbago crucible of mm, high 70mm, internal diameter 90mm, dark 65mm, the dark 1mm particle diameter sic raw material of dress 55mm; Plumbago crucible lid external diameter 110mm, high 100mm, internal diameter 100
+ 0.1Mm, dark 95mm, the silicon carbide seed of sticking a slice diameter 80mm, thickness 1mm of bottom center within it.Cover at last, crucible descending in the coaxial induction furnace of packing into, control the position that it is suitable that crucible and pot cover move up and down respectively, and the initial total height that makes lid overlap crucible is 106mm.Intensification makes 2400 ℃ of charge level temperatures, 2300 ℃ of seed temperatures, vacuum tightness is adjusted to 1000Pa by filling Ar, handles crucible (material source) then, it is moved upward (near crystal) with the speed of 10mm per hour, grow the carborundum crystals of diameter 80mm, thickness 20mm after 2 hours.
Embodiment 2
With external diameter 100
-0.1The plumbago crucible of mm, high 70mm, internal diameter 90mm, dark 65mm, the dark 1mm particle diameter sic raw material of dress 55mm; Plumbago crucible lid external diameter 110mm, high 100mm, internal diameter 100
+ 0.1Mm, dark 95mm, the silicon carbide seed of sticking a slice diameter 80mm, thickness 1mm of bottom center within it.Cover at last, crucible descending in the coaxial induction furnace of packing into, control the position that it is suitable that crucible and pot cover move up and down respectively, and the initial total height that makes lid overlap crucible is 106mm.Intensification makes 2400 ℃ of charge level temperatures, 2300 ℃ of seed temperatures, and vacuum tightness is adjusted to 1000Pa by filling Ar, keeps growing after 2 hours the carborundum crystals of diameter 80mm, thickness 10mm.
Embodiment 3
With the plumbago crucible of external diameter 80mm, high 80mm, internal diameter 70mm, dark 75mm, the 0.05mm particle diameter silicon carbide micro-powder that interior dress 65mm is dark; Plumbago crucible lid external diameter 90mm, high 80mm, internal diameter 81mm, dark 75mm, the silicon carbide seed of sticking a slice diameter 60mm, thickness 2mm of bottom center within it.Cover at last, crucible descending in the coaxial graphite heating resistance furnace of packing into, control the position that it is suitable that crucible and pot cover move up and down respectively, and the initial total height that makes lid overlap crucible is 86mm.Intensification makes 2200 ℃ of charge level temperatures, 2150 ℃ of seed temperatures, vacuum tightness is adjusted to 5000Pa by filling Ar, handles crucible lid (seed crystal) then, it is moved upward (leaving material source) with the speed of 0.1mm per hour, grow the single-crystal silicon carbide of diameter 60mm, thickness 10mm after 100 hours.
Embodiment 4
With the plumbago crucible of external diameter 80mm, high 80mm, internal diameter 70mm, dark 75mm, the 0.05mm particle diameter silicon carbide micro-powder that interior dress 65mm is dark; Plumbago crucible lid external diameter 90mm, high 80mm, internal diameter 81mm, dark 75mm, the silicon carbide seed of sticking a slice diameter 60mm, thickness 2mm of bottom center within it.Cover at last, crucible descending in the coaxial graphite heating resistance furnace of packing into, control the position that it is suitable that crucible and pot cover move up and down respectively, and the initial total height that makes lid overlap crucible is 86mm.Intensification makes 2200 ℃ of charge level temperatures, 2150 ℃ of seed temperatures, and vacuum tightness is adjusted to 5000Pa by filling Ar, handles crucible lid (seed crystal) then, keeps growing after 100 hours the single-crystal silicon carbide of diameter 60mm, thickness 5mm.
Among the embodiment 1, because material source is a 1mm particle diameter sic raw material, raw material is piled up more open, along with crystalline is constantly grown, charge level reduction amount much larger than with the increment of crystal growth face, the ratio of the two was approximately equal to 2: 1, like this, in the case must crucible and crucible lid is approaching mutually by the speed identical with crystalline growth velocity, could keep the distance between charge level and the crystal growth face constant, and make two temperature heads between the face keep constant substantially thus.
Compare with embodiment 1, the data presentation of embodiment 2, under equal conditions, and under the situation that mobile crucible or crucible lid is not constant with the distance between maintenance crystal growth face and the charge level, half when crystal growth thickness only is mobile.
Among the embodiment 3, because material source is a 0.05mm particle diameter silicon carbide micro-powder, raw material is piled up dense.Because of element silicon than the easier consumption of silicon carbide, thereby when silicon carbide is consumed, on charge level, also produce the greying phenomenon simultaneously, cause the charge level position constant substantially, silicon carbide then constantly moves to the charge level distillation from lower floor, and at this moment the distance between crystal growth face and the charge level constantly shortens along with crystal growth, in the case, for two distances between the face are remained unchanged, just must with crucible and crucible lid by the speed identical with crystalline growth velocity mutually away from.
Identical with the situation of embodiment 2, the condition of embodiment 4 is identical with embodiment 3, under the situation that mobile crucible or crucible lid is not constant with the distance between maintenance crystal growth face and the charge level, and half when crystal growth thickness only is mobile.
In actual mechanical process, make actually material source relative with crystal near or leave, depend on the two position in the temperature field and the characteristic of material source (as granularity, charging density, greying situation etc.), final purpose all is in order to keep the temperature head between charge level and the crystal growth interface constant, make growing silicon carbice crystals continue under the constant condition to carry out stablizing, thus the high-quality of growing, large-sized single-crystal silicon carbide.
Claims (5)
1. the method for physical vapor transmission growing silicon carbide single crystal, its step is as follows:
1. keep constant with same state parameter and the control mode of prior art;
2. in crystal growing process, be in all the time under the state of reliable fastening with crucible at the crucible lid, by changing the position in crucible lid and the crucible temperature of living in separately field, it is constant to cover in crystal growth face and the crucible temperature head between the charge level with the maintenance crucible.
2. the method for physical vapor transmission growing silicon carbide single crystal, its step is as follows:
1. keep constant with same state parameter and the control mode of prior art;
2. in crystal growing process, be in all the time under the state of reliable fastening with crucible at the crucible lid, by changing the mutual alignment between crucible lid and the crucible, constant to keep crucible to cover in crystal growth face and the crucible distance between the charge level.
3. the method for physical vapor as claimed in claim 2 transmission growing silicon carbide single crystal is characterized in that, the mutual alignment between described change crucible lid and the crucible, promptly control crucible lid and crucible vertically by suitable speed mutually near or mutually away from.
4. the method for physical vapor as claimed in claim 3 transmission growing silicon carbide single crystal is characterized in that, described suitable speed equal or the crystal growth face of being approximately equal to and charge level between away from or approaching speed.
5. realize a kind of special copple and crucible lid used in the method for claim 1 or 2 described physical vapor transmission growing silicon carbide single crystals, comprise crucible, crucible lid, it is characterized in that, described crucible lid is the column that is complementary with the crucible section form or the tubular of an end opening one end sealing, crucible covers spiral-lock or is inserted on the crucible and also is slidingly matched with it, the two has suitable overlap length, keeping under the constant situation of buckling state with crucible to guarantee the crucible lid, can slide mutually vertically within the specific limits, described crucible and crucible lid are made by graphite.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200310113523 CN1261622C (en) | 2003-11-14 | 2003-11-14 | Method and apparatus for growing silicon carbide single crystal by physical vapor transportation |
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|---|---|---|---|
| CN 200310113523 CN1261622C (en) | 2003-11-14 | 2003-11-14 | Method and apparatus for growing silicon carbide single crystal by physical vapor transportation |
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| CN1544715A true CN1544715A (en) | 2004-11-10 |
| CN1261622C CN1261622C (en) | 2006-06-28 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100523315C (en) * | 2007-09-28 | 2009-08-05 | 中国科学院物理研究所 | Split type tantalum crucible and manufacturing method thereof |
| CN102021653A (en) * | 2010-12-30 | 2011-04-20 | 北京华进创威电子有限公司 | Method for growing silicon carbide single crystal by using high-density material block |
| CN102586858A (en) * | 2012-04-01 | 2012-07-18 | 北京华进创威电子有限公司 | Double-crucible device for growing single crystals through induction heating physical vapor phase transfer |
| CN104120493A (en) * | 2013-04-24 | 2014-10-29 | 梅咬清 | Method for synthesizing monocrystal silicon carbide by utilizing resistance furnace |
| CN104213195A (en) * | 2014-09-24 | 2014-12-17 | 中国电子科技集团公司第四十六研究所 | Low-temperature PVT method for controlling single crystal growth wrappage defect |
| CN107201546A (en) * | 2016-09-01 | 2017-09-26 | 梅咬清 | Resistance furnace synthetic single crystal carbonization silicon preparation method |
| US11408089B2 (en) | 2020-05-06 | 2022-08-09 | Meishan Boya Advanced Materials Co., Ltd. | Devices and methods for growing crystals |
-
2003
- 2003-11-14 CN CN 200310113523 patent/CN1261622C/en not_active Expired - Lifetime
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100523315C (en) * | 2007-09-28 | 2009-08-05 | 中国科学院物理研究所 | Split type tantalum crucible and manufacturing method thereof |
| CN102021653A (en) * | 2010-12-30 | 2011-04-20 | 北京华进创威电子有限公司 | Method for growing silicon carbide single crystal by using high-density material block |
| CN102021653B (en) * | 2010-12-30 | 2013-06-12 | 北京华进创威电子有限公司 | Method for growing silicon carbide single crystal by using high-density material block |
| CN102586858A (en) * | 2012-04-01 | 2012-07-18 | 北京华进创威电子有限公司 | Double-crucible device for growing single crystals through induction heating physical vapor phase transfer |
| CN104120493A (en) * | 2013-04-24 | 2014-10-29 | 梅咬清 | Method for synthesizing monocrystal silicon carbide by utilizing resistance furnace |
| CN104213195A (en) * | 2014-09-24 | 2014-12-17 | 中国电子科技集团公司第四十六研究所 | Low-temperature PVT method for controlling single crystal growth wrappage defect |
| CN104213195B (en) * | 2014-09-24 | 2016-08-24 | 中国电子科技集团公司第四十六研究所 | A kind of low temperature PVT controls the method for crystal growth wrappage defect |
| CN107201546A (en) * | 2016-09-01 | 2017-09-26 | 梅咬清 | Resistance furnace synthetic single crystal carbonization silicon preparation method |
| US11408089B2 (en) | 2020-05-06 | 2022-08-09 | Meishan Boya Advanced Materials Co., Ltd. | Devices and methods for growing crystals |
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| Publication number | Publication date |
|---|---|
| CN1261622C (en) | 2006-06-28 |
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Owner name: BEIJING TIANKEHEDA BLUE LIGHT SEMICONDUCTOR CO., Free format text: FORMER OWNER: INST. OF PHYSICS, CAS Effective date: 20080509 |
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Address after: 100190, room 1, building 66, No. 2005 East Zhongguancun Road, Beijing, Haidian District Patentee after: TANKEBLUE SEMICONDUCTOR Co.,Ltd. Patentee after: INSTITUTE OF PHYSICS, CHINESE ACADEMY OF SCIENCES Address before: 100080 B, block 66, East Zhongguancun Road, Beijing, Haidian District, 910 Patentee before: TANKEBLUE SEMICONDUCTOR Co.,Ltd. Patentee before: INSTITUTE OF PHYSICS, CHINESE ACADEMY OF SCIENCES |
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Effective date of registration: 20190918 Address after: Room 301, Building 9, Tianrong Street, Daxing Biomedical Industry Base, Zhongguancun Science and Technology Park, Daxing District, Beijing 102600 Patentee after: TANKEBLUE SEMICONDUCTOR Co.,Ltd. Address before: 100190, room 1, building 66, No. 2005 East Zhongguancun Road, Beijing, Haidian District Co-patentee before: INSTITUTE OF PHYSICS, CHINESE ACADEMY OF SCIENCES Patentee before: TANKEBLUE SEMICONDUCTOR Co.,Ltd. |
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Application publication date: 20041110 Assignee: Shenzhen Reinvested Tianke Semiconductor Co.,Ltd. Assignor: TANKEBLUE SEMICONDUCTOR Co.,Ltd. Contract record no.: X2023990000684 Denomination of invention: Method and device for growing silicon carbide single crystals through physical vapor transport Granted publication date: 20060628 License type: Common License Record date: 20230725 |
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