JP2001064098A5 - - Google Patents
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- JP2001064098A5 JP2001064098A5 JP1999237195A JP23719599A JP2001064098A5 JP 2001064098 A5 JP2001064098 A5 JP 2001064098A5 JP 1999237195 A JP1999237195 A JP 1999237195A JP 23719599 A JP23719599 A JP 23719599A JP 2001064098 A5 JP2001064098 A5 JP 2001064098A5
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- Prior art keywords
- crystal
- group iii
- iii nitride
- melt
- flux
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 36
- TWXTWZIUMCFMSG-UHFFFAOYSA-N nitride(3-) Chemical compound [N-3] TWXTWZIUMCFMSG-UHFFFAOYSA-N 0.000 description 34
- 239000000155 melt Substances 0.000 description 26
- 238000004519 manufacturing process Methods 0.000 description 22
- 230000004907 flux Effects 0.000 description 20
- 229910052757 nitrogen Inorganic materials 0.000 description 18
- 239000002184 metal Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 230000001629 suppression Effects 0.000 description 3
- 238000002109 crystal growth method Methods 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 210000004940 Nucleus Anatomy 0.000 description 1
Description
【特許請求の範囲】
【請求項1】 反応容器内で、少なくともIII族金属を含む融液とフラックスと窒素原料とが接する領域から、種結晶を用いてIII族窒化物結晶を成長させることを特徴とする結晶成長方法。
【請求項2】 反応容器内で、少なくともIII族金属を含む融液とフラックスと窒素原料からIII族窒化物結晶を成長させる結晶成長装置において、III族窒化物の種結晶を保持する種結晶保持手段と、フラックス蒸気圧を制御可能にフラックスを供給するフラックス供給手段と、窒素圧力を制御可能に窒素原料を供給する窒素供給手段とを具備しており、前記種結晶保持手段を移動させることで、種結晶と前記融液と窒素原料が接することができる領域を移動可能となっていることを特徴とする結晶成長装置。
【請求項3】 請求項2記載の結晶成長装置において、種結晶と融液とフラックスと窒素原料とが接する領域を限定する限定手段がさらに設けられていることを特徴とする結晶成長装置。
【請求項4】 請求項2記載の結晶成長装置において、前記フラックス供給手段は、III族窒化物の種結晶を保持している周辺からフラックスを供給する機能を有していることを特徴とする結晶成長装置。
【請求項5】 請求項2乃至請求項4のいずれか一項に記載の結晶成長装置において、フラックスとしてNaが用いられ、前記フラックス供給手段は、フラックスとしてのNaの蒸気圧を制御する機能を有していることを特徴とする結晶成長装置。
【請求項6】 請求項2乃至請求項5のいずれか一項に記載の結晶成長装置において、反応容器の内壁のうち、前記融液が接する領域が窒化物で形成されていることを特徴とする結晶成長装置。
【請求項7】 請求項2または請求項3記載の結晶成長装置において、前記種結晶保持手段を融液がある側とは反対側の上方に移動させて種結晶を引き上げ可能となっていることを特徴とする結晶成長装置。
【請求項8】 請求項2記載の結晶成長装置において、種結晶を融液中に沈ませながら移動させるよう、前記種結晶保持手段を移動可能となっていることを特徴とする結晶成長装置。
【請求項9】 請求項2乃至請求項8のいずれか一項に記載の結晶成長装置において、種結晶は、気液界面と概ね平行な面の一辺が長く、かつ結晶成長初期において、気液界面と概ね平行な面が気液界面に接しているか、もしくは種結晶が融液中に浸っている形状となっていることを特徴とする結晶成長装置。
【請求項10】 請求項3記載の結晶成長装置において、前記限定手段は、所定の大きさに制御可能な開口部を有していることを特徴とする結晶成長装置。
【請求項11】 請求項2乃至請求項10のいずれか一項に記載の結晶成長装置を用いてIII族窒化物結晶を結晶成長させることを特徴とする結晶成長方法。
【請求項12】 請求項1記載の結晶成長方法を用いて結晶成長させたIII族窒化物結晶。
【請求項13】
少なくともIII族金属を含む融液と窒素原料とを含む反応容器内にフラックスを供給してIII族窒化物結晶を製造するIII族窒化物結晶の製造方法。
【請求項14】
少なくともIII族金属を含む融液とフラックスと窒素原料とを含む反応容器内で種結晶を用いてIII族窒化物結晶を製造するIII族窒化物結晶の製造方法。
【請求項15】
前記III族金属は、Gaであり、
前記フラックスは、Naである、請求項14に記載のIII族窒化物結晶の製造方法。
【請求項16】
前記種結晶を移動させながら前記III族窒化物結晶を製造する、請求項14または請求項15に記載のIII族窒化物結晶の製造方法。
【請求項17】
前記種結晶を前記融液から遠ざけながら前記III族窒化物結晶を製造する、請求項14または請求項15に記載のIII族窒化物結晶の製造方法。
【請求項18】
前記種結晶を気液界面から遠ざけながら前記III族窒化物結晶を製造する、請求項17に記載のIII族窒化物結晶の製造方法。
【請求項19】
前記種結晶以外の核発生を抑制して前記III族窒化物結晶を製造する、請求項14から請求項18のいずれか1項に記載のIII族窒化物結晶の製造方法。
【請求項20】
前記窒素原料を前記融液に供給する領域を制限して前記III族窒化物結晶を製造する、請求項19に記載のIII族窒化物結晶の製造方法。
【請求項21】
前記フラックスを前記融液に供給しながら前記III族窒化物結晶を製造する、請求項14から請求項20のいずれか1項に記載のIII族窒化物結晶の製造方法。
【請求項22】
前記種結晶は、棒形状からなる、請求項13から請求項21のいずれか1項に記載のIII族窒化物結晶の製造方法。
【請求項23】
前記窒素原料を気液界面から前記融液に供給して前記III族窒化物結晶を製造する、請求項13から請求項22のいずれか1項に記載のIII族窒化物結晶の製造方法。
【請求項24】
種結晶を含むIII族窒化物結晶。
【請求項25】
サイズが前記種結晶よりも大きい、請求項24に記載のIII族窒化物結晶。
【請求項26】
Gaと窒素との比が一定である、請求項24または請求項25に記載のIII族窒化物結晶。
【請求項27】
サイズが種結晶よりも大きいIII族窒化物結晶基板。
【請求項28】
Gaと窒素との比が一定であるIII族窒化物結晶基板。
【請求項29】
結晶方位が制御されたバルクIII族窒化物結晶。
【請求項30】
少なくともIII族金属を含む融液と窒素原料とを含む反応容器と、
前記反応容器内にフラックスを供給する手段とを備える結晶製造装置。
【請求項31】
少なくともIII族金属を含む融液とフラックスと窒素原料とを含む反応容器と、
種結晶が前記融液に接するように、または前記種結晶が前記融液に浸漬するように前記種結晶を保持する保持手段とを備える結晶製造装置。
【請求項32】
前記種結晶を前記融液から遠ざける手段をさらに備える、請求項31に記載の結晶製造装置。
【請求項33】
前記遠ざける手段は、前記種結晶を移動させることにより前記種結晶を前記融液から遠ざける、請求項32に記載の結晶製造装置。
【請求項34】
前記遠ざける手段は、前記融液を移動させることにより前記種結晶を前記融液から遠ざける、請求項32に記載の結晶製造装置。
【請求項35】
前記種結晶以外の核発生を抑制する手段をさらに備える、請求項31から請求項34のいずれか1項に記載の結晶製造装置。
【請求項36】
前記抑制する手段は、前記窒素原料を前記融液に供給する領域を制限することにより前記核発生を抑制する、請求項35に記載の結晶製造装置。
【請求項37】
前記フラックスを前記融液に供給する手段をさらに備える、請求項31から請求項36のいずれか1項に記載の結晶製造装置。
【請求項38】
前記種結晶は、棒形状である、請求項31から請求項37のいずれか1項に記載の結晶製造装置。
【請求項39】
前記反応容器は、
前記フラックスおよび前記窒素原料を保持する第1の反応容器と、
前記第1の反応容器の内部に配置され、前記融液を保持する第2の反応容器とを含む、請求項31から請求項38のいずれか1項に記載の結晶製造装置。
【請求項40】
前記反応容器の前記融液が接する領域は、窒化物からなる、請求項31から請求項39のいずれか1項に記載の結晶製造装置。
【請求項41】
前記窒素原料を気液界面から前記融液へ供給する手段をさらに備える、請求項31から請求項40のいずれか1項に記載の結晶製造装置。
[Claims]
1. A method for growing a group III nitride crystal using a seed crystal from a region where a flux containing at least a group III metal, a flux and a nitrogen source are in contact with each other in a reaction vessel. .
2. A seed crystal holding apparatus for holding a group III nitride seed crystal in a crystal growth apparatus for growing a group III nitride crystal from a melt containing at least a group III metal, a flux and a nitrogen source in a reaction vessel. Means, a flux supply means for supplying a flux so that the flux vapor pressure can be controlled, and a nitrogen supply means for supplying a nitrogen raw material so that the nitrogen pressure can be controlled, by moving the seed crystal holding means. A crystal growth apparatus capable of moving a region where the seed crystal, the melt and the nitrogen source can come into contact with each other.
3. The crystal growth apparatus according to claim 2, further comprising a limiting means for limiting an area where the seed crystal, the melt, the flux, and the nitrogen source are in contact with each other.
4. The crystal growth apparatus according to claim 2, wherein said flux supply means has a function of supplying a flux from a periphery holding a group III nitride seed crystal. Crystal growth equipment.
5. The crystal growth apparatus according to claim 2, wherein Na is used as a flux, and said flux supply means has a function of controlling a vapor pressure of Na as a flux. A crystal growth apparatus, comprising:
6. The crystal growth apparatus according to claim 2, wherein a region of the inner wall of the reaction vessel in contact with the melt is formed of nitride. Crystal growth equipment.
7. The crystal growth apparatus according to claim 2, wherein the seed crystal holding means can be moved upward on the side opposite to the side where the melt is located, so that the seed crystal can be pulled up. A crystal growth apparatus characterized by the above-mentioned.
8. The crystal growth apparatus according to claim 2, wherein said seed crystal holding means is movable so as to move the seed crystal while sinking in the melt.
9. The crystal growth apparatus according to claim 2, wherein the seed crystal has a long side substantially parallel to a gas-liquid interface, and has a gas-liquid A crystal growth apparatus characterized in that a plane substantially parallel to the interface is in contact with the gas-liquid interface or a seed crystal is immersed in the melt.
10. The crystal growth apparatus according to claim 3, wherein said limiting means has an opening which can be controlled to a predetermined size.
11. A crystal growth method, wherein a group III nitride crystal is grown using the crystal growth apparatus according to any one of claims 2 to 10.
12. A group III nitride crystal grown using the crystal growth method according to claim 1.
Claim 13
A method for producing a group III nitride crystal, comprising supplying a flux into a reaction vessel containing a melt containing at least a group III metal and a nitrogen source to produce a group III nitride crystal.
14.
A method for producing a group III nitride crystal, wherein a group III nitride crystal is produced using a seed crystal in a reaction vessel containing a melt containing at least a group III metal, a flux and a nitrogen source.
15.
The Group III metal is Ga,
The method for producing a group III nitride crystal according to claim 14, wherein the flux is Na.
16.
The method for producing a group III nitride crystal according to claim 14 or claim 15, wherein the group III nitride crystal is produced while moving the seed crystal.
17.
16. The method for producing a group III nitride crystal according to claim 14, wherein the group III nitride crystal is produced while keeping the seed crystal away from the melt.
18.
The method for producing a group III nitride crystal according to claim 17, wherein the group III nitride crystal is produced while keeping the seed crystal away from a gas-liquid interface.
(19)
The method for producing a group III nitride crystal according to any one of claims 14 to 18, wherein the group III nitride crystal is produced by suppressing nucleation other than the seed crystal.
20.
20. The method for producing a group III nitride crystal according to claim 19, wherein the group III nitride crystal is produced by limiting a region where the nitrogen source is supplied to the melt.
21.
The method for producing a group III nitride crystal according to any one of claims 14 to 20, wherein the group III nitride crystal is produced while supplying the flux to the melt.
22.
22. The method for producing a group III nitride crystal according to claim 13, wherein the seed crystal has a rod shape.
23.
The method for producing a group III nitride crystal according to any one of claims 13 to 22, wherein the nitrogen source is supplied to the melt from a gas-liquid interface to produce the group III nitride crystal.
24.
Group III nitride crystals including seed crystals.
25.
25. The group III nitride crystal according to claim 24, wherein the size is larger than the seed crystal.
26.
26. The group III nitride crystal according to claim 24, wherein the ratio of Ga to nitrogen is constant.
27.
A group III nitride crystal substrate having a size larger than a seed crystal.
28.
A group III nitride crystal substrate having a constant ratio of Ga to nitrogen.
29.
A bulk group III nitride crystal having a controlled crystal orientation.
30.
A reaction vessel containing at least a melt containing a Group III metal and a nitrogen raw material;
Means for supplying a flux into the reaction vessel.
31.
A reaction vessel containing a melt containing at least a Group III metal, a flux, and a nitrogen source;
A crystal manufacturing apparatus comprising: holding means for holding the seed crystal such that the seed crystal is in contact with the melt or the seed crystal is immersed in the melt.
32.
The crystal manufacturing apparatus according to claim 31, further comprising a unit that keeps the seed crystal away from the melt.
33.
33. The crystal manufacturing apparatus according to claim 32, wherein the means for moving away moves the seed crystal away from the melt by moving the seed crystal.
34.
33. The crystal manufacturing apparatus according to claim 32, wherein the separating means moves the seed crystal away from the melt by moving the melt.
35.
The crystal manufacturing apparatus according to any one of claims 31 to 34, further comprising means for suppressing generation of nuclei other than the seed crystal.
36.
36. The crystal manufacturing apparatus according to claim 35, wherein the suppressing unit suppresses the nucleation by restricting a region where the nitrogen source is supplied to the melt.
37.
37. The crystal manufacturing apparatus according to claim 31, further comprising a unit configured to supply the flux to the melt.
38.
The crystal manufacturing apparatus according to any one of claims 31 to 37, wherein the seed crystal has a rod shape.
39.
The reaction vessel,
A first reaction vessel holding the flux and the nitrogen source,
The crystal production apparatus according to any one of claims 31 to 38, further comprising: a second reaction container disposed inside the first reaction container and holding the melt.
40.
The crystal production apparatus according to any one of claims 31 to 39, wherein a region of the reaction vessel in contact with the melt is made of a nitride.
41.
The crystal manufacturing apparatus according to any one of claims 31 to 40, further comprising a unit configured to supply the nitrogen source from the gas-liquid interface to the melt.
Priority Applications (7)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP23719599A JP4094780B2 (en) | 1999-08-24 | 1999-08-24 | Crystal growth method, crystal growth apparatus, group III nitride crystal production method, and crystal production apparatus |
US09/590,063 US6592663B1 (en) | 1999-06-09 | 2000-06-08 | Production of a GaN bulk crystal substrate and a semiconductor device formed on a GaN bulk crystal substrate |
US10/601,301 US7250640B2 (en) | 1999-06-09 | 2003-06-13 | Production of a GaN bulk crystal substrate and a semiconductor device formed on a GaN bulk crystal substrate |
US11/408,656 US7508003B2 (en) | 1999-06-09 | 2006-04-20 | Production of a GaN bulk crystal substrate and a semiconductor device formed thereon |
US12/367,013 US8591647B2 (en) | 1999-06-09 | 2009-02-06 | Production of a GaN bulk crystal substrate and a semiconductor device formed thereon |
US14/057,690 US20140044970A1 (en) | 1999-06-09 | 2013-10-18 | PRODUCTION OF A GaN BULK CRYSTAL SUBSTRATE AND A SEMICONDUCTOR DEVICE FORMED ON A GaN BULK CRYSTAL SUBSTRATE |
US14/619,237 US9869033B2 (en) | 1999-06-09 | 2015-02-11 | Production of a GaN bulk crystal substrate and a semiconductor device formed on a GaN bulk crystal substrate |
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JP23719599A JP4094780B2 (en) | 1999-08-24 | 1999-08-24 | Crystal growth method, crystal growth apparatus, group III nitride crystal production method, and crystal production apparatus |
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JP2007022916A Division JP2007191390A (en) | 2007-02-01 | 2007-02-01 | Group iii nitride crystal and group iii nitride crystal substrate |
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US8545626B2 (en) | 2008-03-03 | 2013-10-01 | Mitsubishi Chemical Corporation | Nitride semiconductor crystal and its production method |
JP5115413B2 (en) * | 2008-09-09 | 2013-01-09 | トヨタ自動車株式会社 | Silicon carbide single crystal manufacturing apparatus and manufacturing method |
JP4956515B2 (en) * | 2008-09-26 | 2012-06-20 | 株式会社リコー | Method for producing group III nitride crystal |
JP5093924B2 (en) * | 2009-01-09 | 2012-12-12 | 住友電気工業株式会社 | Etching method of seed crystal surface |
JP5911478B2 (en) | 2010-05-31 | 2016-04-27 | インターナショナル・ビジネス・マシーンズ・コーポレーションInternational Business Machines Corporation | Method and device for the production of single crystal sheets |
JP2014520752A (en) * | 2011-07-13 | 2014-08-25 | ザ リージェンツ オブ ザ ユニバーシティ オブ カリフォルニア | Growth of bulk group III nitride crystals |
JP5589997B2 (en) * | 2011-09-12 | 2014-09-17 | 株式会社リコー | Crystal manufacturing equipment |
JP5621870B2 (en) * | 2013-03-22 | 2014-11-12 | 株式会社リコー | Method for producing group III nitride crystal |
CN115819791A (en) * | 2022-12-16 | 2023-03-21 | 烟台大学 | Method for regulating MOF morphology by controlling protective gas pressure |
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