JP4001170B2 - Iii族元素窒化物単結晶の製造方法およびそれにより得られたiii族元素窒化物透明単結晶 - Google Patents
Iii族元素窒化物単結晶の製造方法およびそれにより得られたiii族元素窒化物透明単結晶 Download PDFInfo
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- JP4001170B2 JP4001170B2 JP2005506077A JP2005506077A JP4001170B2 JP 4001170 B2 JP4001170 B2 JP 4001170B2 JP 2005506077 A JP2005506077 A JP 2005506077A JP 2005506077 A JP2005506077 A JP 2005506077A JP 4001170 B2 JP4001170 B2 JP 4001170B2
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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
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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
- 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
- C30B29/38—Nitrides
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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
- 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
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
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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
- 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
- C30B9/08—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
- C30B9/10—Metal solvents
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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
- 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
- C30B9/08—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
- C30B9/12—Salt solvents, e.g. flux growth
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Description
つぎに、本発明の実施例について比較例と併せて説明する。
育成温度:800℃
育成圧力(N2):30atm(3.04MPa)
育成時間:96時間
使用坩堝:BN坩堝
(配合割合)
ガリウム(Ga)1gに対し、以下の表の割合で、ナトリウム(Na)とカルシウム(Ca)と配合した。
窒化ガリウムの確認は、元素分析(EDX)、フォトルミネッセンス(PL)により行った。元素分析は、電子顕微鏡により試料の位置を確認しながら、加速電圧15kVの電子線照射により行った。フォトルミネッセンス測定は、常温でヘリウム‐カドミウムレーザー光照射により行った。
得られた結晶について体積を求め、体積から生成量を換算した。
育成温度:800℃
育成圧力:30atm(3.04MPa)
育成時間:24時間
Na:Ca=9:1(ガリウム1gに対するモル比)
図3において、(A)が、500倍のSEM写真であり、(B)が、6000倍のSEM写真である。図示のように、サファイア基板12の上に、窒化ガリウム単結晶11の成長が確認できた。
ガス:Ga(CH3)3、NH3、H2
成長温度:1100℃
成長膜厚:約2μm
前記MOVPE法により得られたGaN薄膜について、透過型電子顕微鏡(TEM)により、その断面を調べた。その結果、図18のTEM写真に示すように、Naフラックスで形成されたGaN単結晶の上に、前記MOVPE法によるGaN単結晶薄膜の存在が確認でき、前記両GaN単結晶の界面も確認できた。
Claims (15)
- III族元素窒化物単結晶の製造方法であって、
ナトリウム(Na)と、リチウム(Li)、カリウム(K)、ルビジウム(Rb)、セシウム(Cs)、フランシウム(Fr)、カルシウム(Ca)、ストロンチウム(Sr)、バリウム(Ba)およびラジウム(Ra)からなる群から選択される少なくとも一つの金属との混合フラックス(Flux)中において、ガリウム(Ga)、アルミニウム(Al)およびインジウム(In)からなる群から選択された少なくとも一つのIII族元素と窒素(N)とを反応させることによりIII族元素窒化物の単結晶を成長させる製造方法。 - 前記混合フラックスが、ナトリウム(Na)と、リチウム(Li)、カリウム(K)、ルビジウム(Rb)、セシウム(Cs)およびフランシウム(Fr)からなる群から選択される少なくとも一つとの混合フラックスである請求項1記載の製造方法。
- 前記混合フラックスが、ナトリウム(Na)とリチウム(Li)との混合フラックスである請求項1記載の製造方法。
- 前記混合フラックスが、ナトリウム(Na)、カルシウム(Ca)およびリチウム(Li)の混合フラックスである請求項1記載の製造方法。
- 前記混合フラックスが、ナトリウム(Na)とカルシウム(Ca)との混合フラックスであって、前記単結晶の育成を、圧力1.5〜3MPaで行う請求項1記載の製造方法。
- III族元素が、ガリウム(Ga)であり、III族元素窒化物単結晶が、窒化ガリウム(GaN)単結晶である請求項1〜5のいずれか一項に記載の製造方法。
- III族元素窒化物を予め準備し、これに前記混合フラックスを接触させ、前記III族元素窒化物を核にして新たなIII族元素窒化物単結晶を成長させる請求項1〜6のいずれか一項に記載の製造方法。
- 核となる III 族元素窒化物が、基板上に形成された薄膜状であり、単結晶または非晶質である請求項7記載の製造方法。
- 少なくとも反応初期において、窒化物を前記混合フラックス中に存在させておく請求項7又は8記載の製造方法。
- 前記混合フラックス中に、ドーピングしたい不純物を存在させる請求項1〜9のいずれか一項に記載の製造方法。
- 請求項1〜10のいずれか一項に記載の製造方法により得られる透明な III 族元素窒化物単結晶。
- 転位密度が、10 5 /cm 2 以下である請求項11記載の III 族元素窒化物単結晶。
- 最大径の長さが、2cm以上である請求項11又は12記載の III 族元素窒化物単結晶。
- 半導体層を含み、この半導体層が、請求項11〜13のいずれか一項に記載の III 族元素窒化物透明単結晶から形成されている半導体装置。
- 請求項11〜13のいずれか一項に記載の III 族元素窒化物透明単結晶を基板に用いて成長させた III 族元素窒化物薄膜を含む半導体装置。
Applications Claiming Priority (13)
Application Number | Priority Date | Filing Date | Title |
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JP2002223190 | 2002-07-31 | ||
JP2002223190 | 2002-07-31 | ||
JP2002339875 | 2002-11-22 | ||
JP2002339875 | 2002-11-22 | ||
JP2002382610 | 2002-12-27 | ||
JP2002382610 | 2002-12-27 | ||
JP2003027888 | 2003-02-05 | ||
JP2003027888 | 2003-02-05 | ||
JP2003078680 | 2003-03-20 | ||
JP2003078680 | 2003-03-20 | ||
JP2003088482 | 2003-03-27 | ||
JP2003088482 | 2003-03-27 | ||
PCT/JP2003/008258 WO2004013385A1 (ja) | 2002-07-31 | 2003-06-30 | Iii族元素窒化物単結晶の製造方法およびそれにより得られたiii族元素窒化物透明単結晶 |
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JPWO2004013385A1 JPWO2004013385A1 (ja) | 2006-09-21 |
JP4001170B2 true JP4001170B2 (ja) | 2007-10-31 |
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US (1) | US7507292B2 (ja) |
EP (1) | EP1548160A4 (ja) |
JP (1) | JP4001170B2 (ja) |
KR (1) | KR100989507B1 (ja) |
CN (1) | CN1327044C (ja) |
AU (1) | AU2003246117A1 (ja) |
TW (1) | TW200403361A (ja) |
WO (1) | WO2004013385A1 (ja) |
Cited By (3)
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US8507364B2 (en) | 2008-05-22 | 2013-08-13 | Toyoda Gosei Co., Ltd. | N-type group III nitride-based compound semiconductor and production method therefor |
US10734548B2 (en) | 2016-02-25 | 2020-08-04 | Ngk Insulators, Ltd. | Free-standing substrate comprising polycrystalline group 13 element nitride and light-emitting element using same |
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2003
- 2003-06-30 JP JP2005506077A patent/JP4001170B2/ja not_active Expired - Fee Related
- 2003-06-30 AU AU2003246117A patent/AU2003246117A1/en not_active Abandoned
- 2003-06-30 KR KR1020057001789A patent/KR100989507B1/ko not_active IP Right Cessation
- 2003-06-30 WO PCT/JP2003/008258 patent/WO2004013385A1/ja active Application Filing
- 2003-06-30 EP EP03738566A patent/EP1548160A4/en not_active Ceased
- 2003-06-30 CN CNB038183285A patent/CN1327044C/zh not_active Expired - Fee Related
- 2003-06-30 US US10/522,488 patent/US7507292B2/en not_active Expired - Fee Related
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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US8507364B2 (en) | 2008-05-22 | 2013-08-13 | Toyoda Gosei Co., Ltd. | N-type group III nitride-based compound semiconductor and production method therefor |
US8501141B2 (en) | 2009-03-30 | 2013-08-06 | Toyoda Gosei Co., Ltd. | Method for producing group III nitride semiconductor |
US10734548B2 (en) | 2016-02-25 | 2020-08-04 | Ngk Insulators, Ltd. | Free-standing substrate comprising polycrystalline group 13 element nitride and light-emitting element using same |
US10804432B2 (en) | 2016-02-25 | 2020-10-13 | Ngk Insulators, Ltd. | Free-standing substrate comprising polycrystalline group 13 element nitride and light-emitting element using same |
Also Published As
Publication number | Publication date |
---|---|
EP1548160A1 (en) | 2005-06-29 |
KR20050030644A (ko) | 2005-03-30 |
AU2003246117A1 (en) | 2004-02-23 |
CN1327044C (zh) | 2007-07-18 |
JPWO2004013385A1 (ja) | 2006-09-21 |
TWI322202B (ja) | 2010-03-21 |
EP1548160A4 (en) | 2009-04-29 |
TW200403361A (en) | 2004-03-01 |
KR100989507B1 (ko) | 2010-10-22 |
WO2004013385A1 (ja) | 2004-02-12 |
CN1671892A (zh) | 2005-09-21 |
US7507292B2 (en) | 2009-03-24 |
US20060051942A1 (en) | 2006-03-09 |
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