JP2016056079A - SiC単結晶及びその製造方法 - Google Patents
SiC単結晶及びその製造方法 Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 235
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 246
- 229910018540 Si C Inorganic materials 0.000 claims abstract description 143
- 239000000758 substrate Substances 0.000 claims abstract description 56
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 22
- 230000007423 decrease Effects 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 description 164
- 238000000034 method Methods 0.000 description 28
- 239000002904 solvent Substances 0.000 description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 14
- 229910002804 graphite Inorganic materials 0.000 description 13
- 239000010439 graphite Substances 0.000 description 13
- 239000000203 mixture Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 7
- 239000000155 melt Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 230000005855 radiation Effects 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 230000005499 meniscus Effects 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 3
- 239000011810 insulating material Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 230000002093 peripheral effect Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- 229910000599 Cr alloy Inorganic materials 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000000879 optical micrograph Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011521 glass Substances 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
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- DECCZIUVGMLHKQ-UHFFFAOYSA-N rhenium tungsten Chemical compound [W].[Re] DECCZIUVGMLHKQ-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000005092 sublimation method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
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- 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
- C30B19/10—Controlling or regulating
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- C30B9/00—Single-crystal growth from melt solutions using molten solvents
- C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
- C30B9/06—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using as solvent a component of the crystal composition
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- C—CHEMISTRY; METALLURGY
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- 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
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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
- 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
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- C30—CRYSTAL GROWTH
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- C30B19/00—Liquid-phase epitaxial-layer growth
- C30B19/06—Reaction chambers; Boats for supporting the melt; Substrate holders
- C30B19/062—Vertical dipping system
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- C30B19/00—Liquid-phase epitaxial-layer growth
- C30B19/06—Reaction chambers; Boats for supporting the melt; Substrate holders
- C30B19/067—Boots or containers
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- 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
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- 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
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- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
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- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/16—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only elements of Group IV of the Periodic Table
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Abstract
【解決手段】内部から表面に向けて温度低下する温度勾配を有するSi−C溶液24にSiC種結晶基板14を接触させてSiC単結晶を成長させる、SiC単結晶の製造方法であって、Si−C溶液24として、Si、Cr、及びAlを含み、Alが、Si、Cr、及びAlの合計量を基準として3at%以上含まれるSi−C溶液24を用いること、並びにSi−C溶液24の表面領域の温度勾配y(℃/cm)を、式(1)を満たすようにすること、を含む、SiC単結晶の製造方法。y≧0.15789x+21.52632(1)(xはSi−C溶液中のAl含有量(at%))
【選択図】図1
Description
Si−C溶液として、Si、Cr、及びAlを含み、Alが、Si、Cr、及びAlの合計量を基準として3at%以上含まれるSi−C溶液を用いること、並びに
Si−C溶液の表面領域の温度勾配y(℃/cm)を、式(1):
y≧0.15789x+21.52632 (1)
(式中、xはSi−C溶液中のAl含有量(at%)を示す)
を満たすようにすること、
を含む、SiC単結晶の製造方法を対象とする。
Si−C溶液として、Si、Cr、及びAlを含み、Alが、Si、Cr、及びAlの合計量を基準として3at%以上含まれるSi−C溶液を用いること、並びにSi−C溶液の表面領域の温度勾配y(℃/cm)を、式(1):
y≧0.15789x+21.52632 (1)
(式中、xはSi−C溶液中のAl含有量(at%)を示す)
を満たすようにすること、を含む、SiC単結晶の製造方法を対象とする。
y≧0.15789x+21.52632 (1)
(式中、xはSi−C溶液中のAl含有量(at%)を示す)
を満たすようにすることによって、インクルージョンを含まない低抵抗p型SiC単結晶を成長させることができることが分かった。
y≧0.15789x+21.52632 (1)
(式中、xはSi−C溶液中のAl含有量(at%)を示す)
を満たす範囲である。上記のAl含有量を含むSi−C溶液の溶媒組成とともに、Si−C溶液の表面領域の温度勾配を上記の範囲にすることによって、インクルージョンを含まない低抵抗のp型SiC単結晶を含むことができる。Si−C溶液の表面領域の温度勾配は、好ましくはSi−C溶液中のAl含有量が3〜20(at%)の範囲で25℃/cm以上であり、より好ましくはSi−C溶液中のAl含有量が3〜41(at%)の範囲で28℃/cm以上であり、さらに好ましくはSi−C溶液中のAl含有量が3〜53.6(at%)の範囲で30℃/cm以上である。温度勾配の上限は、好ましくは55℃/cm以下であり、より好ましくは50℃/cm以下であり、さらに好ましくは42℃/cm以下である。温度勾配は、例えば25〜55℃/cm、28〜55℃/cm、または30〜42℃/cmであることができる。また、本開示の方法によれば、好ましくは600μm/h以上、より好ましくは800μm/h以上、さらに好ましくは1000μm/h以上の成長速度で低抵抗のp型SiC単結晶を成長させることができる。成長速度の上限は、好ましくは1000μm/h以下にすることができる。
温度勾配(℃/cm)=(B−A)/D
によって算出することができる。
直径が15mm、厚みが700μmの円盤状4H−SiC単結晶であって、下面が(000−1)面を有する昇華法により作製したn型SiC単結晶を用意して、種結晶基板として用いた。種結晶基板は20mΩ・cmの抵抗率を有していた。種結晶基板の上面を、円柱形状の黒鉛軸の端面の略中央部に、黒鉛の接着剤を用いて接着した。
Si−C溶液の溶媒組成(Si/Cr/Al)を54/36/10(at%)としたこと以外は、実施例1と同様の条件で結晶成長させた。
Si−C溶液の溶媒組成(Si/Cr/Al)を54/36/10(at%)とし、成長時間Si−C溶液の温度勾配を42℃/cmとし、成長時間を5時間にしたこと以外は、実施例1と同様の条件で結晶成長させた。
Si−C溶液の温度勾配を55℃/cmとし、成長時間を2時間にしたこと以外は、実施例1と同様の条件で結晶成長させた。
Si−C溶液の溶媒組成(Si/Cr/Al)を40.2/26.8/33(at%)とし、成長時間を5時間にしたこと以外は、実施例1と同様の条件で結晶成長させた。
Si−C溶液の温度勾配を22℃/cmとし、成長時間を5時間にしたこと以外は、実施例1と同様の条件で結晶成長させた。
Si−C溶液の溶媒組成(Si/Cr/Al)を48/32/20(at%)とし、Si−C溶液の温度勾配を25℃/cmとし、成長時間を5時間にしたこと以外は、実施例1と同様の条件で結晶成長させた。
Si−C溶液の溶媒組成(Si/Cr/Al)を35.4/23.6/41(at%)とし、Si−C溶液の温度勾配を28℃/cmとし、成長時間を5時間にしたこと以外は、実施例1と同様の条件で結晶成長させた。
Si−C溶液の溶媒組成を59.4/39.6/1(at%)とし、Si−C溶液の温度勾配を15℃/cmとしたこと以外は、実施例1と同様の条件で結晶成長させた。
Si−C溶液の温度勾配を15℃/cmとしたこと以外は、実施例1と同様の条件で結晶成長させた。
Si−C溶液の溶媒組成を54/36/10(at%)とし、Si−C溶液の温度勾配を15℃/cmとし、成長時間を20時間にしたこと以外は、実施例1と同様の条件で結晶成長させた。
Si−C溶液の溶媒組成(Si/Cr/Al)を35.4/23.6/41(at%)とし、Si−C溶液の温度勾配を20℃/cmとし、成長時間を5時間にしたこと以外は、実施例1と同様の条件で結晶成長させた。
10 坩堝
12 種結晶保持軸
14 種結晶基板
18 断熱材
22 高周波コイル
22A 上段高周波コイル
22B 下段高周波コイル
24 Si−C溶液
26 石英管
34 メニスカス
40 SiC成長結晶
42 切り出した成長結晶
Claims (3)
- 内部から表面に向けて温度低下する温度勾配を有するSi−C溶液にSiC種結晶基板を接触させてSiC単結晶を成長させる、SiC単結晶の製造方法であって、
前記Si−C溶液として、Si、Cr、及びAlを含み、前記Alが、前記Si、Cr、及びAlの合計量を基準として3at%以上含まれるSi−C溶液を用いること、並びに
前記Si−C溶液の表面領域の温度勾配y(℃/cm)を、式(1):
y≧0.15789x+21.52632 (1)
(式中、xは前記Si−C溶液中のAl含有量(at%)を示す)
を満たすようにすること、
を含む、SiC単結晶の製造方法。 - 前記Si−C溶液中のAl含有量が3〜41(at%)の範囲で、前記Si−C溶液の表面領域の温度勾配を28〜55℃/cmとすることを含む、請求項1に記載のSiC単結晶の製造方法。
- インクルージョンを含まず且つ35〜120mΩ・cmの抵抗率を有する、p型SiC単結晶。
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US14/824,811 US9732437B2 (en) | 2014-09-09 | 2015-08-12 | SiC single crystal and method for producing same |
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