JP5231599B2 - 窒化物単結晶の製造装置 - Google Patents
窒化物単結晶の製造装置 Download PDFInfo
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- JP5231599B2 JP5231599B2 JP2011099016A JP2011099016A JP5231599B2 JP 5231599 B2 JP5231599 B2 JP 5231599B2 JP 2011099016 A JP2011099016 A JP 2011099016A JP 2011099016 A JP2011099016 A JP 2011099016A JP 5231599 B2 JP5231599 B2 JP 5231599B2
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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
- 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
- C30B19/06—Reaction chambers; Boats for supporting the melt; Substrate holders
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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
- C30B29/406—Gallium nitride
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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
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
- C30B35/002—Crucibles or containers
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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
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10S117/90—Apparatus characterized by composition or treatment thereof, e.g. surface finish, surface coating
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/1016—Apparatus with means for treating single-crystal [e.g., heat treating]
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
- Y10T117/1032—Seed pulling
- Y10T117/1064—Seed pulling including a fully-sealed or vacuum-maintained crystallization chamber [e.g., ampoule]
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
- Y10T117/1096—Apparatus for crystallization from liquid or supercritical state including pressurized crystallization means [e.g., hydrothermal]
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- Crystals, And After-Treatments Of Crystals (AREA)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
Description
前記溶液を収容するための坩堝、
前記坩堝を収容する内側容器、
前記内側容器を収容する加熱容器であって、発熱体、この発熱体が設けられている容器本体、およびこの容器本体と組み合わされる蓋を備えている加熱容器、
前記加熱容器を収容し、少なくとも窒素ガスを含む雰囲気を充填するための圧力容器、および
前記容器本体上に前記内側容器を支持する支持部材を備えており、支持部材、加熱容器および内側容器によって閉空間が形成されており、少なくとも一つの発熱体が閉空間に面していることを特徴とする。
圧力容器30は、本体4と蓋2とからなる。容器30の内側空間5には、加熱容器31が設置されている。加熱容器31は蓋21と容器本体22とからなる。本例では、容器本体22の内側面に面するように一連の発熱体14が設けられている。また容器本体13の底板部20には発熱体19が設けられている。
また、閉空間は完全に容器内空間15に対して密閉されている必要はなく、ほぼ閉空間になっていればよい。例えば、支持部材17には、切り欠きや貫通孔が形成されていてもよい。
SUS310S、インコネル、タンタル、モリブデン、タングステン
セラミックスファイバー、セラミックスウール、グラファイトウール、スチールウール
本発明においては、窒素を含有する雰囲気下で単結晶の育成を行う。窒素含有雰囲気は、窒素のみからなっていてよいが、窒素以外の非酸化性ガス、例えば、アルゴンなどの不活性ガスや還元性ガスを含有していてよい。
カリウム、ルビジウム、セシウム、マグネシウム、ストロンチウム、バリウム、錫
GaN、AlN、InN、これらの混晶(AlGaInN)、BN
(窒化ガリウム単結晶の育成例)
本発明を利用し、少なくともナトリウム金属を含むフラックスを使用して窒化ガリウム単結晶を育成できる。このフラックスには、ガリウム原料物質を混合する。ガリウム原料物質としては、ガリウム単体金属、ガリウム合金、ガリウム化合物を適用できるが、ガリウム単体金属が取扱いの上からも好適である。
本発明は、少なくともアルミニウムとアルカリ土類を含むフラックスを含む融液を特定の条件下で窒素含有雰囲気中で加圧することによって、AlN単結晶を育成する場合にも有効であることが確認できた。
図1に模式的に示す装置を使用し、前述したようにして窒化ガリウム単結晶を育成した。
具体的には、支持部材17は円筒形状とし、材質はSUS310Sとし、直径φ155cm、高さ10cmとした。円筒状の支持部材17の側面には、直径3cmの穴を6カ所均等に設けた。
図2に示すような装置を作製した。ただし、支持部材27はアルミナパイプとし、4本設置した。付勢手段3、断熱部材11は設けていない。この結果、加熱容器内部の温度分布は、上部ほど高温となり、温度勾配は、上下方向で見て高さ10cm当たり50℃となった。
Claims (2)
- フラックスおよび原料を含む溶液を使用して窒化物単結晶を育成する装置であって、
前記溶液を収容するための坩堝、
前記坩堝を収容する内側容器、
前記内側容器を収容する加熱容器であって、発熱体、この発熱体が設けられている容器本体、およびこの容器本体と組み合わされる蓋を備えている加熱容器、
前記加熱容器を収容し、少なくとも窒素ガスを含む雰囲気を充填するための圧力容器、および
前記容器本体上に前記内側容器を支持する支持部材を備えており、
前記支持部材、前記加熱容器および前記内側容器によって実質的に閉空間が形成されており、少なくとも一つの前記発熱体が前記閉空間下に設けられていることを特徴とする、窒化物単結晶の製造装置。 - 前記蓋を前記容器本体へと向かって前記圧力容器から付勢する付勢手段を備えていることを特徴とする、請求項1記載の装置。
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JP2011099017A Active JP5337195B2 (ja) | 2006-03-23 | 2011-04-27 | 窒化物単結晶の製造装置 |
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US (1) | US9017479B2 (ja) |
JP (3) | JP4766620B2 (ja) |
CN (1) | CN101405439B (ja) |
WO (1) | WO2007108498A1 (ja) |
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WO2007094126A1 (ja) * | 2006-02-13 | 2007-08-23 | Ngk Insulators, Ltd. | フラックスからナトリウム金属を回収する方法 |
WO2007122865A1 (ja) * | 2006-03-24 | 2007-11-01 | Ngk Insulators, Ltd. | 窒化物単結晶の製造方法 |
WO2010143748A1 (ja) | 2009-06-11 | 2010-12-16 | 日本碍子株式会社 | Iii族金属窒化物単結晶の育成方法およびこれに用いる反応容器 |
JP2012214331A (ja) * | 2011-03-31 | 2012-11-08 | Mitsubishi Chemicals Corp | 第13族窒化物結晶の製造方法 |
JP6841191B2 (ja) * | 2016-09-06 | 2021-03-10 | 豊田合成株式会社 | Iii族窒化物半導体の製造方法 |
CN109930202A (zh) * | 2019-04-02 | 2019-06-25 | 四川航空工业川西机器有限责任公司 | 一种适合氨热法生成氮化镓单晶制品的热等静压装置 |
CN116536758B (zh) * | 2023-05-04 | 2024-01-23 | 山东晶升电子科技有限公司 | 一种氮化镓晶体高压助熔剂外延生长的设备及方法 |
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AU2003272882A1 (en) * | 2002-09-19 | 2004-04-08 | Showa Denko K.K. | Silicon carbide single crystal and method and apparatus for producing the same |
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JP5177557B2 (ja) * | 2006-03-23 | 2013-04-03 | 日本碍子株式会社 | 窒化物単結晶の製造装置 |
JP5187846B2 (ja) * | 2006-03-23 | 2013-04-24 | 日本碍子株式会社 | 窒化物単結晶の製造方法および装置 |
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CN101405439B (zh) | 2012-04-04 |
US20080282971A1 (en) | 2008-11-20 |
JP2011153073A (ja) | 2011-08-11 |
JPWO2007108498A1 (ja) | 2009-08-06 |
JP4766620B2 (ja) | 2011-09-07 |
US9017479B2 (en) | 2015-04-28 |
CN101405439A (zh) | 2009-04-08 |
JP2011173792A (ja) | 2011-09-08 |
WO2007108498A1 (ja) | 2007-09-27 |
JP5337195B2 (ja) | 2013-11-06 |
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