JP5767141B2 - 窒化ガリウム基板およびそれを用いた光デバイス - Google Patents
窒化ガリウム基板およびそれを用いた光デバイス Download PDFInfo
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- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 title claims description 132
- 239000000758 substrate Substances 0.000 title claims description 74
- 229910002601 GaN Inorganic materials 0.000 title claims description 63
- 230000003287 optical effect Effects 0.000 title claims description 25
- 238000000034 method Methods 0.000 claims description 30
- 230000001133 acceleration Effects 0.000 claims description 23
- WQZGKKKJIJFFOK-PHYPRBDBSA-N alpha-D-galactose Chemical compound OC[C@H]1O[C@H](O)[C@H](O)[C@@H](O)[C@H]1O WQZGKKKJIJFFOK-PHYPRBDBSA-N 0.000 claims description 16
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 claims description 16
- 238000004140 cleaning Methods 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 9
- 238000004125 X-ray microanalysis Methods 0.000 claims description 2
- 238000007517 polishing process Methods 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 35
- 229910052799 carbon Inorganic materials 0.000 description 35
- 239000013078 crystal Substances 0.000 description 29
- 239000007789 gas Substances 0.000 description 16
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 15
- 238000005530 etching Methods 0.000 description 13
- 238000005498 polishing Methods 0.000 description 13
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 description 11
- 239000011800 void material Substances 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 10
- 238000001039 wet etching Methods 0.000 description 10
- 229910003460 diamond Inorganic materials 0.000 description 9
- 239000010432 diamond Substances 0.000 description 9
- 230000035515 penetration Effects 0.000 description 8
- 239000012495 reaction gas Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 230000007423 decrease Effects 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 7
- XOYLJNJLGBYDTH-UHFFFAOYSA-M chlorogallium Chemical compound [Ga]Cl XOYLJNJLGBYDTH-UHFFFAOYSA-M 0.000 description 6
- 238000010894 electron beam technology Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000012159 carrier gas Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 229910052594 sapphire Inorganic materials 0.000 description 5
- 239000010980 sapphire Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 4
- 150000004767 nitrides Chemical class 0.000 description 4
- 238000005424 photoluminescence Methods 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 239000006061 abrasive grain Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000012459 cleaning agent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000004452 microanalysis Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 1
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0632—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with gallium, indium or thallium
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- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
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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
- 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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- G01N23/2252—Measuring emitted X-rays, e.g. electron probe microanalysis [EPMA]
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- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
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- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
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- H01S5/00—Semiconductor lasers
- H01S5/30—Structure or shape of the active region; Materials used for the active region
- H01S5/32—Structure or shape of the active region; Materials used for the active region comprising PN junctions, e.g. hetero- or double- heterostructures
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- H01S5/32341—Structure or shape of the active region; Materials used for the active region comprising PN junctions, e.g. hetero- or double- heterostructures in AIIIBV compounds, e.g. AlGaAs-laser, InP-based laser emitting light at a wavelength less than 900 nm blue laser based on GaN or GaP
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- H01L33/26—Materials of the light emitting region
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Description
GaN基板表面に埋め込まれて残存し、ダイアモンドのカーボン成分によりエピタキシャル成長層の結晶性が悪化することがわかった。また、研磨の際に用いるワックスが残存し、ワックスのカーボン成分により結晶性が悪化することがわかった。
り得られるEDXスペクトルのGaLα/CKαのピーク強度比が2以上の窒化ガリウム基板である。
るEDXスペクトルのGaLα/CKαのピーク強度比からカーボン量を測定した。そして、カーボン量が発光強度の増減に及ぼす影響を評価した。その結果、GaLα/CKαのピーク強度比が所定数値よりも大きくなり、GaN基板の表面付近に残存するカーボン量が減少すると、エピタキシャル成長層の結晶性が良好となり、光デバイスにおける発光強度も向上できることを見出し、本発明を創作するに至った。
本実施形態の窒化ガリウム基板(GaN基板)は、その表面に対する、走査型電子顕微鏡(SEM:Scanning Electron Microscope)の加速電圧を3kVとしたときのエネルギー分散型X線分析(EDX:Energy Dispersive X-ray microanalysis)において、ED
Xにより得られるEDXスペクトルのGaLα/CKαのピーク強度比が2以上となっている。
ークの高さ(ピーク強度)から、GaN基板を構成する元素のおおよその含有量が把握される。本実施形態においては、GaN基板表面に残存するカーボン量を評価するため、Gaに対するC(カーボン)量として、GaLα/CKαのピーク強度比を算出し、残存するカーボン量の増減を判断している。そして、本実施形態のGaN基板はGaLα/CKαのピーク強度比が2以上となっており、Gaに対してCが所定の比率以下となっている。
本実施形態においては、GaN基板の表面におけるカーボン量を評価するため、加速電圧を低くして走査することが好ましい。ただし、加速電圧を下げると、検出できる元素の特性X線の種類が減少し、また検出される特性X線の強度が下がり、測定時間が非常に長くなる。したがって、本実施形態においては、SEMの加速電圧を3kVとして、EDXによりGaN基板表面におけるカーボン量を評価している。
ない窒化ガリウム基板とすることができる。このため、この窒化ガリウム基板を下地基板として用いて結晶成長させた場合、得られるエピタキシャル成長層の結晶性を向上することができる。
上述した窒化ガリウム基板の製造方法は、窒化ガリウム基板(GaN基板)を形成する工程と、窒化ガリウム基板を研削・研磨する工程と、窒化ガリウム基板を所定の温度でボイル洗浄する工程と、窒化ガリウム基板を所定の温度でウェットエッチングする工程と、を有している。本実施形態においては、VAS法によりGaN基板を形成する。
るが、基板の表面にわずかに残存することになる。つまり、研削・研磨工程において、GaN基板表面にはカーボン成分が付着し残存する。
続いて、上記で得られたGaN基板を用いて、光デバイスを製造する光デバイスの製造方法について説明する。
本実施例では、VAS法により、GaN単結晶を成長させてGaN基板を製造した。
まず、ボイド形成基板を準備した。ボイド形成基板は、サファイア基板(直径3.5インチ)上にMOVPE法などで厚さ500nmのGaN下地層を形成し、この表面に厚さ30nmのTi層を蒸着し、その後、H2およびNH3の混合ガス中で30分間熱処理(温度1000℃)することで、Ti層を網目構造のTiNに変換しつつ、GaN層をボイド化することによって作製した。
、反応ガス導入管13により5×10−2atmのNH3ガスを、キャリアガスである6×10−1atmのN2ガスとともに導入し、反応ガス導入管15により5×10−3atmのGaClガスを、キャリアガスである2.0×10−latmN2ガスと1.0×10−1atmH2ガスとともに導入して、20分間結晶成長させた。
実施例2〜14、比較例1〜7では、実施例1における洗浄条件(洗浄実施温度)およびウェットエッチング条件(エッチング実施温度)を表1に示すように変更した以外は、実施例1と同様の条件でGaN基板を製造した。
2 GaNバッファ層
3 多重量子井戸層
4 GaNキャップ層
10 光デバイス
Claims (3)
- 研削・研磨工程及び洗浄工程がなされた窒化ガリウム基板であって、当該窒化ガリウム基板の表面に対する、走査型電子顕微鏡(SEM:Scanning Electron Microscope)の加速電圧を3kVとしたときのエネルギー分散型X線分析(EDX:Energy Dispersive X-ray microanalysis)において、前記EDXにより得られるEDXスペクトルのGaLα/CKαのピーク強度比が2以上であることを特徴とする窒化ガリウム基板。
- 請求項1に記載の窒化ガリウム基板において、前記EDXスペクトルの前記GaLα/CKαのピーク強度比が3以上であることを特徴とする窒化ガリウム基板。
- 請求項1または2に記載の窒化ガリウム基板上にデバイス構造を形成したことを特徴とする光デバイス。
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2012047203A JP5767141B2 (ja) | 2012-03-02 | 2012-03-02 | 窒化ガリウム基板およびそれを用いた光デバイス |
CN201310059764.3A CN103296171B (zh) | 2012-03-02 | 2013-02-26 | 氮化镓基板以及使用了该氮化镓基板的光设备 |
US13/781,568 US20130230447A1 (en) | 2012-03-02 | 2013-02-28 | Gallium nitride substrate and optical device using the same |
US15/012,459 US10381230B2 (en) | 2012-03-02 | 2016-02-01 | Gallium nitride substrate and optical device using the same |
Applications Claiming Priority (1)
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US20130230447A1 (en) | 2013-09-05 |
US10381230B2 (en) | 2019-08-13 |
US20160148817A1 (en) | 2016-05-26 |
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