JP4225296B2 - 炭化珪素単結晶の製造方法 - Google Patents
炭化珪素単結晶の製造方法 Download PDFInfo
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- JP4225296B2 JP4225296B2 JP2005179412A JP2005179412A JP4225296B2 JP 4225296 B2 JP4225296 B2 JP 4225296B2 JP 2005179412 A JP2005179412 A JP 2005179412A JP 2005179412 A JP2005179412 A JP 2005179412A JP 4225296 B2 JP4225296 B2 JP 4225296B2
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- crystal
- single crystal
- silicon carbide
- melt
- carbide single
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- 239000013078 crystal Substances 0.000 title claims description 150
- 229910010271 silicon carbide Inorganic materials 0.000 title claims description 49
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims description 25
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 238000000034 method Methods 0.000 claims description 32
- 239000000155 melt Substances 0.000 claims description 28
- 239000000758 substrate Substances 0.000 claims description 25
- 239000002994 raw material Substances 0.000 claims description 21
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 2
- 230000007547 defect Effects 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 230000009466 transformation Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005092 sublimation method Methods 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000003475 lamination Methods 0.000 description 3
- 230000035882 stress Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000001947 vapour-phase growth Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 238000001835 Lely method Methods 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000011856 silicon-based particle Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
Images
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
- 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
- C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method
-
- 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
-
- 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
- C30B19/02—Liquid-phase epitaxial-layer growth using molten solvents, e.g. flux
- C30B19/04—Liquid-phase epitaxial-layer growth using molten solvents, e.g. flux the solvent being a component of the crystal composition
Description
a)前記種結晶基板を前記融液表面と接触させて単結晶を成長させた後に、この種結晶基板を前記融液表面から離して単結晶の成長を中断させる工程、及び
b)再び前記種結晶基板を前記融液表面と接触させて単結晶を成長させる工程
からなるサイクルを少なくとも1回以上行うことを含み、前記種結晶が6H−炭化珪素単結晶又は15R−炭化珪素単結晶であり、得られる単結晶が4H−炭化珪素単結晶であることを特徴とする。
a)前記種結晶基板を前記融液表面と接触させて単結晶を成長させた後に、この種結晶基板を前記融液表面から離して単結晶の成長を中断させる工程、及び
b)再び前記種結晶基板を前記融液表面と接触させて単結晶を成長させる工程
からなるサイクルを少なくとも1回以上行い、結晶成長の中断を1回もしくは複数回行うことを特徴としている。
図1に示す装置を用い、黒鉛製るつぼに珪素粒子と各種添加元素を所定量添加し、表1に示す条件において炭化珪素単結晶を成長させた。結果を以下の表1に示す。
実施例の方法に準じ、ただし結晶成長の過程においてこの成長を中断させることなく連続的に結晶成長を行った。条件及び結果を以下の表2に示す。
2 るつぼ
3 加熱装置
4 原料
5 種結晶
6 引き上げ棒
Claims (6)
- SiとCを含む原料を融解した融液に単結晶の炭化珪素種結晶基板を接触させ、前記基板上に炭化珪素単結晶を成長させることを含む炭化珪素単結晶の製造方法であって、下記工程a)及びb)
a)前記種結晶基板を前記融液表面と接触させて単結晶を成長させた後に、この種結晶基板を前記融液表面から離して単結晶の成長を中断させる工程、及び
b)再び前記種結晶基板を前記融液表面と接触させて単結晶を成長させる工程
からなるサイクルを少なくとも1回以上行うことを含み、前記種結晶が6H−炭化珪素単結晶又は15R−炭化珪素単結晶であり、得られる単結晶が4H−炭化珪素単結晶であることを特徴とする方法。 - 前記原料がAlを3〜45at%含む、請求項1記載の方法。
- 前記原料がSnを1〜20at%含む、請求項1記載の方法。
- 前記原料がGeを1〜30at%含む、請求項1記載の方法。
- 前記融液の温度が、前記原料の融点以上、2300℃以下である、請求項1〜4のいずれか1項に記載の方法。
- 前記融液が、その内部から種結晶と接触する表面に向かって10〜45℃/cmの温度勾配を形成して温度が低下する、請求項1〜5のいずれか1項に記載の方法。
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2005179412A JP4225296B2 (ja) | 2005-06-20 | 2005-06-20 | 炭化珪素単結晶の製造方法 |
PCT/JP2006/312553 WO2006137500A1 (ja) | 2005-06-20 | 2006-06-16 | 炭化珪素単結晶の製造方法 |
KR1020077029431A KR100897312B1 (ko) | 2005-06-20 | 2006-06-16 | 탄화규소단결정의 제조방법 |
US11/921,463 US8052793B2 (en) | 2005-06-20 | 2006-06-16 | Method for producing silicon carbide single crystal |
CN2006800222602A CN101203635B (zh) | 2005-06-20 | 2006-06-16 | 制备碳化硅单晶的方法 |
EP06767203.0A EP1895031B1 (en) | 2005-06-20 | 2006-06-16 | Process for producing silicon carbide single crystal |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2005179412A JP4225296B2 (ja) | 2005-06-20 | 2005-06-20 | 炭化珪素単結晶の製造方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2006347852A JP2006347852A (ja) | 2006-12-28 |
JP4225296B2 true JP4225296B2 (ja) | 2009-02-18 |
Family
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2005179412A Expired - Fee Related JP4225296B2 (ja) | 2005-06-20 | 2005-06-20 | 炭化珪素単結晶の製造方法 |
Country Status (6)
Country | Link |
---|---|
US (1) | US8052793B2 (ja) |
EP (1) | EP1895031B1 (ja) |
JP (1) | JP4225296B2 (ja) |
KR (1) | KR100897312B1 (ja) |
CN (1) | CN101203635B (ja) |
WO (1) | WO2006137500A1 (ja) |
Families Citing this family (29)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4811354B2 (ja) * | 2007-06-11 | 2011-11-09 | トヨタ自動車株式会社 | SiC単結晶の製造方法 |
JP4450074B2 (ja) * | 2008-01-15 | 2010-04-14 | トヨタ自動車株式会社 | 炭化珪素単結晶の成長方法 |
JP4586857B2 (ja) | 2008-02-06 | 2010-11-24 | トヨタ自動車株式会社 | p型SiC半導体単結晶の製造方法 |
JP4888432B2 (ja) * | 2008-04-01 | 2012-02-29 | トヨタ自動車株式会社 | 4H−SiC単結晶の製造方法 |
TW201011814A (en) * | 2008-09-08 | 2010-03-16 | Kinik Co | Method for growing epitaxy |
JP5115413B2 (ja) * | 2008-09-09 | 2013-01-09 | トヨタ自動車株式会社 | 炭化珪素単結晶の製造装置および製造方法 |
CN101649491A (zh) * | 2009-07-17 | 2010-02-17 | 宁波工程学院 | 一种定向生长SiC单晶纳米线阵列的方法 |
JP5218431B2 (ja) * | 2009-07-21 | 2013-06-26 | トヨタ自動車株式会社 | 溶液法による単結晶成長用種結晶軸 |
EP2484815B1 (en) * | 2009-09-29 | 2014-12-24 | Fuji Electric Co., Ltd. | METHOD FOR PRODUCING SiC SINGLE CRYSTAL |
JP5355533B2 (ja) * | 2010-11-09 | 2013-11-27 | 新日鐵住金株式会社 | n型SiC単結晶の製造方法 |
JP5287840B2 (ja) * | 2010-12-16 | 2013-09-11 | 株式会社デンソー | 炭化珪素単結晶の製造装置 |
JP5656623B2 (ja) * | 2010-12-28 | 2015-01-21 | トヨタ自動車株式会社 | SiC単結晶の製造装置および製造方法 |
CN102021653B (zh) * | 2010-12-30 | 2013-06-12 | 北京华进创威电子有限公司 | 一种用高密度料块生长碳化硅单晶的方法 |
JP5758986B2 (ja) * | 2011-03-23 | 2015-08-05 | トヨタ自動車株式会社 | SiC単結晶の製造方法および製造装置 |
KR20120135739A (ko) * | 2011-06-07 | 2012-12-17 | 엘지이노텍 주식회사 | 잉곳 제조 장치 및 잉곳 제조 방법 |
KR20130002616A (ko) * | 2011-06-29 | 2013-01-08 | 에스케이이노베이션 주식회사 | 탄화규소 단결정 성장 장치 및 그 방법 |
KR20130007109A (ko) * | 2011-06-29 | 2013-01-18 | 에스케이이노베이션 주식회사 | 탄화규소 단결정 성장 장치 및 그 방법 |
EP2775015B1 (en) * | 2011-10-31 | 2017-06-21 | Toyota Jidosha Kabushiki Kaisha | SiC SINGLE CRYSTAL MANUFACTURING METHOD |
JP5801730B2 (ja) * | 2012-01-20 | 2015-10-28 | トヨタ自動車株式会社 | 単結晶の製造装置に用いられる種結晶保持軸及び単結晶の製造方法 |
JP5876390B2 (ja) * | 2012-08-30 | 2016-03-02 | トヨタ自動車株式会社 | SiC単結晶の製造方法 |
JP2014122133A (ja) * | 2012-12-21 | 2014-07-03 | Kyocera Corp | 結晶の製造方法 |
CN105264126A (zh) * | 2013-04-09 | 2016-01-20 | 新日铁住金株式会社 | SiC单晶的制造方法 |
JP5854013B2 (ja) * | 2013-09-13 | 2016-02-09 | トヨタ自動車株式会社 | SiC単結晶の製造方法 |
KR101801867B1 (ko) * | 2014-02-12 | 2017-11-28 | 도요타지도샤가부시키가이샤 | SiC 단결정의 제조 방법 |
US9732437B2 (en) | 2014-09-09 | 2017-08-15 | Toyota Jidosha Kabushiki Kaisha | SiC single crystal and method for producing same |
JP6259053B2 (ja) * | 2016-11-29 | 2018-01-10 | 京セラ株式会社 | 結晶の製造方法 |
KR102136320B1 (ko) * | 2017-06-20 | 2020-07-21 | 주식회사 엘지화학 | 결정 형성 장치 및 이를 이용한 실리콘카바이드 단결정의 형성 방법 |
KR102153519B1 (ko) * | 2017-06-23 | 2020-09-08 | 주식회사 엘지화학 | 실리콘카바이드 단결정의 제조 장치 |
JP2018035069A (ja) * | 2017-12-07 | 2018-03-08 | 京セラ株式会社 | 結晶の製造方法 |
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US3053635A (en) * | 1960-09-26 | 1962-09-11 | Clevite Corp | Method of growing silicon carbide crystals |
JP3128179B2 (ja) | 1992-11-24 | 2001-01-29 | シャープ株式会社 | n型炭化珪素単結晶の製造方法 |
JPH07172998A (ja) | 1993-12-21 | 1995-07-11 | Toshiba Corp | 炭化ケイ素単結晶の製造方法 |
JP2000264790A (ja) * | 1999-03-17 | 2000-09-26 | Hitachi Ltd | 炭化珪素単結晶の製造方法 |
JP2001010896A (ja) | 1999-06-23 | 2001-01-16 | Toshiba Ceramics Co Ltd | シリコン単結晶引上げ装置およびこれを用いたシリコン単結晶の引上げ方法 |
JP4561000B2 (ja) | 2001-05-31 | 2010-10-13 | 住友金属工業株式会社 | 炭化珪素(SiC)単結晶の製造方法 |
JP4673528B2 (ja) | 2001-09-28 | 2011-04-20 | 新日本製鐵株式会社 | 炭化珪素単結晶インゴットおよびその製造方法 |
JP4196791B2 (ja) | 2003-09-08 | 2008-12-17 | トヨタ自動車株式会社 | SiC単結晶の製造方法 |
CN1282770C (zh) * | 2003-12-24 | 2006-11-01 | 山东大学 | 一种生长具有半导体特性的大直径6H-SiC单晶的装置和方法 |
-
2005
- 2005-06-20 JP JP2005179412A patent/JP4225296B2/ja not_active Expired - Fee Related
-
2006
- 2006-06-16 EP EP06767203.0A patent/EP1895031B1/en not_active Expired - Fee Related
- 2006-06-16 CN CN2006800222602A patent/CN101203635B/zh not_active Expired - Fee Related
- 2006-06-16 US US11/921,463 patent/US8052793B2/en not_active Expired - Fee Related
- 2006-06-16 WO PCT/JP2006/312553 patent/WO2006137500A1/ja active Application Filing
- 2006-06-16 KR KR1020077029431A patent/KR100897312B1/ko active IP Right Grant
Also Published As
Publication number | Publication date |
---|---|
WO2006137500A1 (ja) | 2006-12-28 |
KR20080009333A (ko) | 2008-01-28 |
EP1895031B1 (en) | 2015-06-03 |
EP1895031A1 (en) | 2008-03-05 |
EP1895031A4 (en) | 2014-05-21 |
US20090101062A1 (en) | 2009-04-23 |
CN101203635B (zh) | 2011-09-28 |
CN101203635A (zh) | 2008-06-18 |
KR100897312B1 (ko) | 2009-05-14 |
JP2006347852A (ja) | 2006-12-28 |
US8052793B2 (en) | 2011-11-08 |
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