JP6179624B2 - 結晶成長方法および発光素子の製造方法 - Google Patents
結晶成長方法および発光素子の製造方法 Download PDFInfo
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- 238000002109 crystal growth method Methods 0.000 title claims description 27
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 239000007789 gas Substances 0.000 claims description 382
- 150000004767 nitrides Chemical class 0.000 claims description 305
- 239000004065 semiconductor Substances 0.000 claims description 272
- 239000000758 substrate Substances 0.000 claims description 246
- 238000000034 method Methods 0.000 claims description 121
- 239000013078 crystal Substances 0.000 claims description 73
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 62
- 239000012298 atmosphere Substances 0.000 claims description 51
- 239000002019 doping agent Substances 0.000 claims description 45
- 239000000463 material Substances 0.000 claims description 43
- 239000011261 inert gas Substances 0.000 claims description 40
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 27
- 239000002994 raw material Substances 0.000 claims description 27
- 229910021529 ammonia Inorganic materials 0.000 claims description 13
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 238000001947 vapour-phase growth Methods 0.000 claims description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- 238000005229 chemical vapour deposition Methods 0.000 claims description 6
- 229910002601 GaN Inorganic materials 0.000 description 176
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 107
- 230000008569 process Effects 0.000 description 89
- 239000012159 carrier gas Substances 0.000 description 58
- 229910052739 hydrogen Inorganic materials 0.000 description 53
- 239000001257 hydrogen Substances 0.000 description 51
- 229910052757 nitrogen Inorganic materials 0.000 description 48
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 45
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 36
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- 239000010980 sapphire Substances 0.000 description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 17
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- 229910052738 indium Inorganic materials 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
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- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- -1 atomic hydrogen radicals Chemical class 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000007865 diluting Methods 0.000 description 3
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- 238000010438 heat treatment Methods 0.000 description 3
- 238000010348 incorporation Methods 0.000 description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical group [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 3
- 230000004807 localization Effects 0.000 description 3
- 125000004433 nitrogen atom Chemical group N* 0.000 description 3
- RHUYHJGZWVXEHW-UHFFFAOYSA-N 1,1-Dimethyhydrazine Chemical compound CN(C)N RHUYHJGZWVXEHW-UHFFFAOYSA-N 0.000 description 2
- 229910016455 AlBN Inorganic materials 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- YZCKVEUIGOORGS-UHFFFAOYSA-N Hydrogen atom Chemical compound [H] YZCKVEUIGOORGS-UHFFFAOYSA-N 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 229910052785 arsenic Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
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- 238000005215 recombination Methods 0.000 description 2
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- 239000000126 substance Substances 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- 238000000927 vapour-phase epitaxy Methods 0.000 description 2
- IIFFFBSAXDNJHX-UHFFFAOYSA-N 2-methyl-n,n-bis(2-methylpropyl)propan-1-amine Chemical compound CC(C)CN(CC(C)C)CC(C)C IIFFFBSAXDNJHX-UHFFFAOYSA-N 0.000 description 1
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000001540 azides Chemical class 0.000 description 1
- DQGZQAJIHKWEIU-UHFFFAOYSA-N azido(diethyl)alumane Chemical compound [N-]=[N+]=[N-].CC[Al+]CC DQGZQAJIHKWEIU-UHFFFAOYSA-N 0.000 description 1
- XBCDPKPGCRPSHQ-UHFFFAOYSA-N azido(diethyl)gallane Chemical compound CC[Ga](CC)N=[N+]=[N-] XBCDPKPGCRPSHQ-UHFFFAOYSA-N 0.000 description 1
- JUOJXNAVZADLAJ-UHFFFAOYSA-N bis(2-methylpropyl)diazene Chemical compound CC(C)CN=NCC(C)C JUOJXNAVZADLAJ-UHFFFAOYSA-N 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000005136 cathodoluminescence Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
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- 230000001419 dependent effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
- UCSVJZQSZZAKLD-UHFFFAOYSA-N ethyl azide Chemical compound CCN=[N+]=[N-] UCSVJZQSZZAKLD-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- QHGSGZLLHBKSAH-UHFFFAOYSA-N hydridosilicon Chemical compound [SiH] QHGSGZLLHBKSAH-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910052743 krypton Inorganic materials 0.000 description 1
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- PBTHJVDBCFJQGG-UHFFFAOYSA-N methyl azide Chemical compound CN=[N+]=[N-] PBTHJVDBCFJQGG-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- ZUSRFDBQZSPBDV-UHFFFAOYSA-N n-[bis(dimethylamino)stibanyl]-n-methylmethanamine Chemical compound CN(C)[Sb](N(C)C)N(C)C ZUSRFDBQZSPBDV-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- CTRLRINCMYICJO-UHFFFAOYSA-N phenyl azide Chemical compound [N-]=[N+]=NC1=CC=CC=C1 CTRLRINCMYICJO-UHFFFAOYSA-N 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 230000000644 propagated effect Effects 0.000 description 1
- 230000001902 propagating effect Effects 0.000 description 1
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- 229910052711 selenium Inorganic materials 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000000992 sputter etching Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
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- 229910052714 tellurium Inorganic materials 0.000 description 1
- 230000026683 transduction Effects 0.000 description 1
- 238000010361 transduction Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- VPYJNCGUESNPMV-UHFFFAOYSA-N triallylamine Chemical compound C=CCN(CC=C)CC=C VPYJNCGUESNPMV-UHFFFAOYSA-N 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- 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
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- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02634—Homoepitaxy
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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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
-
- 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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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
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- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02436—Intermediate layers between substrates and deposited layers
- H01L21/02439—Materials
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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- General Chemical & Material Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Led Devices (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Chemical Vapour Deposition (AREA)
Description
度の自然放冷、あるいは、温度制御をしながらの除冷、供給ガスによる冷却等による基体温度の下降を開始させる。降温工程においてはN2を継続供給するか或いは不活性ガスを供給するか若しくはN2の継続供給に加えて他の不活性ガスも供給するかする。かつ、成長工程においてH2を供給していた場合には、これを十分に低減、もしくは遮断し、NH3流量を成長時よりは低減させ、その後適切な温度までNH3を供給する。その後は、N2ガスのみ、或いは不活性ガスのみ、或いはN2ガスと不活性ガスの混合ガスのみによって、さらに基板温度を低下させる。
[比較例1]
[比較例2]
[比較例3]
[参考例1]
[参考例2]
2 サセプタ
3 基体
4 ステンレス製チャンバ
10 GaN基板 または、サファイア基板上GaNテンプレート
11 意図的にはSiをドーピングしていないGaN層
12 意図的にSiドープを実施したn型GaN層
13 InGaN/GaN多重量子井戸活性層構造
14 MgドープAlGaN層
15 MgドープGaN層
Claims (9)
- GaN自立基板の窒化物主面上に窒化物半導体を結晶成長させる方法であって、
前記GaN自立基板を、有機金属気相成長装置内にて、室温から700℃以上で1350℃以下である所定の昇温到達温度TAまで昇温する工程であって、前記窒化物主面をアンモニアを含み水素ガスを含まない雰囲気に暴露した状態で該基体を550℃以下の温度から前記昇温到達温度TAまで昇温する期間tAを含む昇温工程と、
前記有機金属気相成長装置内にて、前記GaN自立基板の窒化物主面をアンモニアを含む雰囲気に暴露した状態で該GaN自立基板の窒化物主面上にシリコン(Si)原料を意図的に供給することなく第1の窒化物半導体層を700℃以上で1350℃以下であるエピタキシャル成長温度Tg1でエピタキシャル成長させる第1の成長工程と、
前記有機金属気相成長装置内にて、前記第1の窒化物半導体層表面をアンモニアを含む雰囲気に暴露した状態で該第1の窒化物半導体層上にn型ドーパント原料を供給しながら第2の窒化物半導体層をエピタキシャル成長させる第2の成長工程とを備えている結晶成長方法。 - GaN自立基板の窒化物主面上に窒化物半導体を結晶成長させる方法であって、
前記GaN自立基板を、有機金属気相成長装置内にて、室温から700℃以上で1350℃以下である所定の昇温到達温度TAまで昇温する工程であって、アンモニアを含み水素ガスを含まないメインフローを構成した雰囲気中で前記基体を550℃以下の温度から前記昇温到達温度TAまで昇温する期間tAを含む昇温工程と、
前記有機金属気相成長装置内にて、アンモニアを含んでメインフローを構成した雰囲気中で前記GaN自立基板の窒化物主面上にシリコン(Si)原料を意図的に供給することなく第1の窒化物半導体層を700℃以上で1350℃以下であるエピタキシャル成長温度Tg1でエピタキシャル成長させる第1の成長工程と、
前記有機金属気相成長装置内にて、アンモニアを含んでメインフローを構成した雰囲気中で前記第1の窒化物半導体層上にn型ドーパント原料を供給しながら第2の窒化物半導体層をエピタキシャル成長させる第2の成長工程とを備えている結晶成長方法。 - 前記昇温工程における全ガスに対する不活性ガスの成分比は流量比で0.5以上1.0以下である、請求項1または2に記載の結晶成長方法。
- 前記第1の成長工程における全ガスに対する活性ガスの成分比は流量比で0.5以上1.0以下である、請求項1乃至3のいずれか1項に記載の結晶成長方法。
- 前記昇温工程における全ガスに対する不活性ガスの成分比は流量比で0.5以上1.0以下であり、
前記第1の成長工程における全ガスに対する活性ガスの成分比は流量比で0.5以上1.0以下である、請求項1または2に記載の結晶成長方法。 - 前記GaN自立基板の窒化物主面は(0001)面(c+面)±5度以下の結晶面である請求項1乃至5の何れか1項に記載の結晶成長方法。
- 前記第2の成長工程におけるn型ドーパント原料の供給は前記第2の窒化物半導体層中のシリコン濃度が1×1017cm-3以上で6×1019cm-3以下となるように実行される請求項1乃至6の何れか1項に記載の結晶成長方法。
- 前記第2の窒化物半導体層の上に活性層を含む積層構造体をエピタキシャル成長させる第3の工程を更に備えている請求項1乃至7の何れか1項に記載の結晶成長方法。
- 請求項1乃至8の何れか1項に記載の結晶成長方法を用いて窒化物半導体を結晶成長させる工程を含む、発光素子の製造方法。
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