JP7085833B2 - 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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- 239000013078 crystal Substances 0.000 title claims description 112
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims description 112
- 229910010271 silicon carbide Inorganic materials 0.000 title claims description 111
- 238000004519 manufacturing process Methods 0.000 title claims description 26
- 238000000034 method Methods 0.000 title description 16
- 238000010438 heat treatment Methods 0.000 claims description 36
- 238000001816 cooling Methods 0.000 claims description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 238000005092 sublimation method Methods 0.000 claims description 9
- 230000007547 defect Effects 0.000 description 16
- 239000000758 substrate Substances 0.000 description 13
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000006698 induction Effects 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 239000003507 refrigerant Substances 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 230000035882 stress Effects 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
-
- 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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/002—Controlling or regulating
-
- 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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
- C30B23/06—Heating of the deposition chamber, the substrate or the materials to be evaporated
- C30B23/063—Heating of the substrate
-
- 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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
- C30B23/06—Heating of the deposition chamber, the substrate or the materials to be evaporated
- C30B23/066—Heating of the material to be evaporated
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/0237—Materials
- H01L21/02373—Group 14 semiconducting materials
- H01L21/02378—Silicon carbide
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- Crystallography & Structural Chemistry (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
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- Crystals, And After-Treatments Of Crystals (AREA)
- Physical Vapour Deposition (AREA)
- Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
Description
予備加熱工程では、坩堝100内を室温から2000[℃]以上2500[℃]以下の温度になるまで昇温し、この温度を一定時間維持して炭化珪素種結晶102の加熱を行う。昇温速度は、50[℃/分]以上1200[℃/分]以下とすることが好ましい。昇温時間を除いた加熱時間、すなわち一定温度で加熱する時間は、30[分]以上90[分]以下とすることが好ましい。
続く冷却工程では、坩堝100内を室温になるまで降温し、室温を一定時間維持して炭化珪素種結晶102の冷却を行う。降温速度は、50[℃/分]以上400[℃/分]以下とすることが好ましい。
次に、炭化珪素種結晶102上に、炭化珪素単結晶を成長させるための本加熱工程について説明する。図1(b)は、昇華法による本加熱を行って、予備加熱工程、冷却工程を経た炭化珪素種結晶102上に、炭化珪素単結晶105を成長させている状態を示している。炭化珪素種結晶102とその台座101については、冷却工程を経た状態のままで継続して用いる。炭化珪素種結晶102、台座101以外の構成要素(坩堝100内の雰囲気、炭化珪素原料103、周辺部材等)については、冷却工程と本加熱工程との間に入れ替えを行ってもよい。
上記実施形態の製造方法において、本加熱工程まで経て炭化珪素単結晶のインゴットを作製した。全工程にわたり、坩堝内の圧力を140[Torr]とした。
上記実施形態の製造方法において、本加熱工程のみを経た炭化珪素単結晶基板のインゴットを3つ作製し、各インゴットから1枚ずつ、炭化珪素単結晶基板を切り出して取得した。予備加熱工程および冷却工程を経ていない点以外の製造条件については、実施例1と同様とした。
101・・・台座
102・・・炭化珪素種結晶
103・・・炭化珪素原料
104・・・炭化膜
105・・・炭化珪素単結晶
Claims (4)
- 昇華法を用いた炭化珪素単結晶の製造方法であって、
坩堝内の一方の側に配置された黒鉛部材上に炭化珪素種結晶を貼り付け、他方の側に炭化珪素原料を配置した状態で、前記炭化珪素種結晶上に炭化珪素単結晶を成長させる前に、
前記炭化珪素種結晶を、2000[℃]以上の温度になるように加熱する予備加熱工程と、
前記炭化珪素種結晶を、室温になるように冷却する冷却工程と、本加熱工程と、を順に有し、
前記予備加熱工程における昇温時間を除いた加熱時間は、30[分]以上90[分]以下であり、
前記本加熱工程では、前記炭化珪素種結晶と前記黒鉛部材とを、前記冷却工程を経た状態のままで継続して用いることを特徴とする炭化珪素単結晶の製造方法。 - 前記予備加熱工程、前記冷却工程において、前記坩堝内の圧力を150[Torr]以下とすることを特徴とする請求項1に記載の炭化珪素単結晶の製造方法。
- 前記予備加熱工程における昇温速度を、50[℃/分]以上1200[℃/分]以下とすることを特徴とする請求項1または2のいずれかに記載の炭化珪素単結晶の製造方法。
- 前記冷却工程における降温速度を、50[℃/分]以上400[℃/分]以下とすることを特徴とする請求項1~3のいずれか一項に記載の炭化珪素単結晶の製造方法。
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JP2017248349A JP7085833B2 (ja) | 2017-12-25 | 2017-12-25 | 炭化珪素単結晶の製造方法 |
CN201811548672.0A CN109957841A (zh) | 2017-12-25 | 2018-12-18 | 碳化硅单晶的制造方法 |
US16/225,967 US20190194818A1 (en) | 2017-12-25 | 2018-12-19 | Method of producing silicon carbide single crystal |
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JP6737488B1 (ja) * | 2019-06-17 | 2020-08-12 | 株式会社エクサウィザーズ | 情報処理装置、情報処理方法、プログラム及び学習済みモデル |
CN114423889A (zh) | 2019-09-27 | 2022-04-29 | 学校法人关西学院 | SiC单晶的制造方法、SiC单晶的制造装置以及SiC单晶晶片 |
CN114540954B (zh) * | 2020-11-25 | 2022-12-09 | 北京天科合达半导体股份有限公司 | 碳化硅单晶片、晶体及制备方法、半导体器件 |
CN115467016B (zh) * | 2021-06-11 | 2023-11-07 | 中电化合物半导体有限公司 | 可释放碳化硅单晶生长应力的生长组件、设备及方法 |
CN114264652A (zh) * | 2021-12-09 | 2022-04-01 | 浙江大学杭州国际科创中心 | 碳化硅中位错产生及演变的逆向分析方法 |
Citations (3)
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JP2001158695A (ja) | 1999-11-29 | 2001-06-12 | Denso Corp | 炭化珪素単結晶の製造方法 |
JP2005179155A (ja) | 2003-12-22 | 2005-07-07 | Toyota Central Res & Dev Lab Inc | SiC単結晶の製造方法 |
JP2014034504A (ja) | 2012-08-10 | 2014-02-24 | Toyota Central R&D Labs Inc | 昇華性単結晶の製造方法 |
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US6780243B1 (en) * | 2001-11-01 | 2004-08-24 | Dow Corning Enterprises, Inc. | Method of silicon carbide monocrystalline boule growth |
US8591714B2 (en) * | 2007-04-17 | 2013-11-26 | National Tank Company | High velocity electrostatic coalescing oil/water separator |
US8163086B2 (en) * | 2007-08-29 | 2012-04-24 | Cree, Inc. | Halogen assisted physical vapor transport method for silicon carbide growth |
CN102597337A (zh) * | 2009-08-27 | 2012-07-18 | 住友金属工业株式会社 | SiC 单晶晶片及其制造方法 |
CN102560671B (zh) * | 2010-12-31 | 2015-05-27 | 中国科学院物理研究所 | 半绝缘碳化硅单晶 |
CN103160928A (zh) * | 2011-12-13 | 2013-06-19 | 北京有色金属研究总院 | 一种生长高质量SiC单晶的籽晶处理方法 |
CN103628141A (zh) * | 2013-12-11 | 2014-03-12 | 中国电子科技集团公司第二研究所 | 一种SiC单晶晶体质量均匀化方法 |
CN105780107A (zh) * | 2014-12-18 | 2016-07-20 | 中国科学院物理研究所 | 提高碳化硅晶体生长质量的籽晶处理方法以及用于碳化硅晶体生长的方法 |
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JP2001158695A (ja) | 1999-11-29 | 2001-06-12 | Denso Corp | 炭化珪素単結晶の製造方法 |
JP2005179155A (ja) | 2003-12-22 | 2005-07-07 | Toyota Central Res & Dev Lab Inc | SiC単結晶の製造方法 |
JP2014034504A (ja) | 2012-08-10 | 2014-02-24 | Toyota Central R&D Labs Inc | 昇華性単結晶の製造方法 |
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