JP7228467B2 - Iii族化合物基板の製造方法及びiii族化合物基板 - Google Patents
Iii族化合物基板の製造方法及びiii族化合物基板 Download PDFInfo
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- 239000000758 substrate Substances 0.000 title claims description 72
- 150000001875 compounds Chemical class 0.000 title claims description 50
- 238000004519 manufacturing process Methods 0.000 title claims description 28
- 239000013078 crystal Substances 0.000 claims description 166
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 claims description 91
- 238000000034 method Methods 0.000 claims description 32
- 239000000126 substance Substances 0.000 claims description 29
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical group N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 23
- 238000003776 cleavage reaction Methods 0.000 claims description 14
- 230000007017 scission Effects 0.000 claims description 14
- 238000004645 scanning capacitance microscopy Methods 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 238000000927 vapour-phase epitaxy Methods 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 4
- 230000008719 thickening Effects 0.000 claims 1
- 229910002601 GaN Inorganic materials 0.000 description 69
- 238000006243 chemical reaction Methods 0.000 description 15
- 239000010410 layer Substances 0.000 description 11
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- 238000002248 hydride vapour-phase epitaxy Methods 0.000 description 9
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- XOYLJNJLGBYDTH-UHFFFAOYSA-M chlorogallium Chemical compound [Ga]Cl XOYLJNJLGBYDTH-UHFFFAOYSA-M 0.000 description 6
- 230000007547 defect Effects 0.000 description 6
- 239000010408 film Substances 0.000 description 6
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- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
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- 229910052594 sapphire Inorganic materials 0.000 description 5
- 239000010980 sapphire Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000011109 contamination Methods 0.000 description 4
- 230000032798 delamination Effects 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910017083 AlN Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 3
- 229910052582 BN Inorganic materials 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- -1 crystalline AlN Chemical class 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
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- 238000010438 heat treatment Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910005267 GaCl3 Inorganic materials 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- UPWPDUACHOATKO-UHFFFAOYSA-K gallium trichloride Chemical compound Cl[Ga](Cl)Cl UPWPDUACHOATKO-UHFFFAOYSA-K 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229920000592 inorganic polymer Polymers 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
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- 239000012808 vapor phase Substances 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
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- 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
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- C30B29/406—Gallium nitride
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Description
例えばGaN基板について見ると、一般的に液体アンモニア若しくはNaフラックス等の液中でGaN結晶を成長させたバルクGaN基板は比較的高品質だが、大口径化が難しい。これに対し、気相で結晶成長する有機金属気相成長法(MOCVD法)やハイドライド気相成長法(HVPE法、THVPE法等)では、サファイア基板、GaAs基板、AlN基板等の基板上にGaNをヘテロエピタキシャル成長させる事に依り、大口径のGaN薄膜が得られる。しかし、ヘテロエピタキシャル成長法では、高品質な基板を得ようと膜厚を厚くすると、格子欠陥、反り、割れが生じやすい。
(1)サセプターに載置され、固定された種結晶に、気相成長法により、III族化合物の結晶を成長させるIII族化合物基板の製造方法であって、前記サセプター及び前記種結晶の少なくとも一方の部材に剥離可能な劈開性を有する物質を用いることを特徴とするIII族化合物基板の製造方法。
(2)前記サセプターは、少なくとも前記種結晶を載置している面が前記剥離可能な劈開性を有する物質で構成され、前記剥離可能な劈開性を有する物質が熱分解窒化ホウ素(PBN)であることを特徴とする上記(1)に記載のIII族化合物基板の製造方法。
(3)前記剥離可能な劈開性を有する物質が熱分解窒化ホウ素(PBN)及び炭素の複合体であることを特徴とする上記(1)または(2)に記載のIII族化合物基板の製造方法。
(4)前記種結晶が前記剥離可能な劈開性を有する物質で構成され、
前記剥離可能な劈開性を有する物質がSCAM(ScAlMgO4)結晶であることを特徴とする上記(1)~(3)のいずれか1つに記載のIII族化合物基板の製造方法。
(5)第1の結晶速度で前記種結晶にIII族化合物の結晶を成長させる第1の結晶成長工程、及び前記第1の結晶成長工程の後に、前記第1の結晶速度よりも結晶速度が低い第2の結晶速度で、前記種結晶にIII族化合物の結晶を成長させる第2の結晶成長工程を含むことを特徴とする上記(1)~(4)のいずれか1つに記載のIII族化合物基板の製造方法。
(6)前記第1の結晶成長工程及び前記第2の結晶工程の間に、第3の結晶速度で前記種結晶にIII族化合物の結晶を成長させる第3の結晶工程を含み、前記第3の結晶工程では、前記第3の結晶速度は、前記第1の結晶速度から前記第2の結晶速度へ、段階的に及び/又は連続的に変わることを特徴とする上記(5)に記載のIII族化合物基板の製造方法。
(7)前記III族化合物が窒化ガリウム(GaN)であることを特徴とする上記(1)~(6)のいずれか1つに記載のIII族化合物基板の製造方法。
(8)上記(1)~(7)のいずれか1つに記載のIII族化合物基板の製造方法により製造されることを特徴とするIII族化合物基板。
これにより、気相成長法の特長である、高成膜速度の特長を生かしつつ、より高品質な大型GaN結晶基板が低コストで得られる。即ち、大口径でバラツキの無い、極めて厚物のGaN結晶基板が作成出来る為、基板の結晶特性にも優れ且つ、低コストの大口径GaN基板が容易に得られる。
なお、「剥離可能な劈開性を有する物質」とは、III族化合物基板及び種結晶を割ったり傷付けたりしない程度の機械的衝撃で劈開する物質、または、III族化合物基板及び種結晶の間の熱膨張率の差異による生ずる熱応力で劈開する物質である。
水冷ジャケットと排気口を有する内径1500mm×高さ1800mmのステンレス製反応装置(内面は予め極薄くジルコニアを溶射し、コーテングした)にアルミナのマット状の断熱材を入れ、その内側に円筒状にロッド状のSiCヒーターを持つ加熱装置(内径1000mm×高さ1300mm)とガス供給管(図2の符号6参照)(上記の反応装置と同材質で中心管61;内径φ30mm、2番目の管62;内径φ40mm、最外管63;内径φ50mm)を備えた。一方、φ170mmの層間剥離性が容易なPBN(PBN製造時に炉内圧をパルス的に変動させ製造した物)製の3枚のサセプター(図2の符号2参照)を120°間隔に配置収納するφ520mmのPBNコート・グラファイトのサセプター公転冶具(図2の符号5参照)を準備した。このサセプター面に2インチのSCAM結晶から種基板(図2の符号3参照)としてタイル状に加工し、裏面にアルミナ系接着材(図1の符号4参照)を付け6インチの円盤状に接着した後、加熱ヒーターで1380℃に加熱しつつ、同時にサセプター公転冶具5は10rpmで回転してサセプター2を公転させ、その公転歯車の力を用いて3枚の各サセプター2は30rpmで自転させ温度、回転が安定を確認した後、反応装置内部に3重管の中心管61からGaCl3ガスを、最外管63からNH3ガスを、中心管と最外管との間の管62からN2ガスを供給しTHVPE反応を開始した。
実施例1で種結晶をSCAM結晶から、剥離可能な劈開性を有さないNaフラックスで製造した2インチのGaN基板に、サセプターを剥離可能な劈開性を有さないコランダムのセラミックス製に変えた以外は全く同じ条件で結晶成長を行った。その結果、THVPE反応後、冷却して内部の生成物を取り出そうとしたがGaNとサセプターとが融着して、生成GaNと貴重な種基板は粉々に割れていずれも回収不可能であった。
実施例1のSCAMの種基板を剥離可能な劈開性を有さないNaフラックスで製造した2インチのGaN基板に変え、反応ガスをGaCl3ガスからGaClに変えてTHVPEからHVPE法にした以外は同一条件で結晶成長反応を行った。尚、反応はGa分換算で実施例1と同一線速となる様にした。冷却後、得られたGaN結晶は種結晶と一体になった形でGaN結晶は層状のPBN製サセプターから容易に引き剥がす事が出来た。心配した冷却時の熱応力は層間剥離で吸収し、クラック発生も無く、又、殆ど反りも発生しなかった。実施例1と同様に製品化したGaN基板の(100)面のX線ロッキングカーブのFWHM(Full Width at Half Maximum)は面内の任意の3点が平均25arcsec、バラツキが3arcsecであった。金属不純物の分析値は測定限界以下であった。又、積層欠陥を単色Cathode Luminescence像で観察した結果、GaNの表面層には殆ど見られなかった。上記の測定と観察から、得られたGaN結晶は極めてバラツキの無い均一で良好な結晶基板である事を示している。
実施例1で最初のから低速度の約100μm/hで結晶成長を50時間行なった事とサセプターに劈開性を有するが剥離することが難しい熱分解グラファイト(PG)製を使用した事、以外は全く同一条件で結晶成長を行った。得られたGaN結晶は容易に種結晶のSCAM及びPG製サセプターから剥離出来、SCAMは回収し再使用が可能であった。剥離したGaN結晶は層状のPG製サセプターの層間剥離性が弱かった為、GaN結晶の熱応力を充分に吸収出来ず数ミリの反りが発生した。しかし割れは起こらなかった。多少、矯正しながら円筒研削でφ6インチに加工した。
2 サセプター
3 種結晶
4 接着剤
5 サセプター公転治具
6 ガス供給管
11 ベース(ハンドル)基板部分
12 GaN結晶本体部分
13 結晶成長速度遷移部分
Claims (6)
- サセプターに載置され、固定された種結晶に、気相成長法により、III族化合物の結晶を成長させるIII族化合物基板の製造方法であって、
前記サセプターに剥離可能な劈開性を有する物質を用い、
前記サセプターに前記種結晶を固定した状態で前記III族化合物の結晶を厚膜化し、
前記種結晶がSCAM(ScAlMgO 4 )結晶で構成されることを特徴とするIII族化合物基板の製造方法。 - 前記サセプターは、少なくとも前記種結晶を載置している面が前記剥離可能な劈開性を有する物質で構成され、
前記剥離可能な劈開性を有する物質が熱分解窒化ホウ素(PBN)であることを特徴とする請求項1に記載のIII族化合物基板の製造方法。 - 前記剥離可能な劈開性を有する物質が熱分解窒化ホウ素(PBN)及び炭素の複合体であることを特徴とする請求項1または2に記載のIII族化合物基板の製造方法。
- 第1の結晶速度で前記種結晶にIII族化合物の結晶を成長させる第1の結晶成長工程、及び
前記第1の結晶成長工程の後に、前記第1の結晶速度よりも結晶速度が低い第2の結晶速度で、前記種結晶にIII族化合物の結晶を成長させる第2の結晶成長工程を含むことを特徴とする請求項1~3のいずれか1項に記載のIII族化合物基板の製造方法。 - 前記第1の結晶成長工程及び前記第2の結晶成長工程の間に、第3の結晶速度で前記種結晶にIII族化合物の結晶を成長させる第3の結晶成長工程を含み、
前記第3の結晶成長工程では、前記第3の結晶速度は、前記第1の結晶速度から前記第2の結晶速度へ、段階的に及び/又は連続的に変わることを特徴とする請求項4に記載のIII族化合物基板の製造方法。 - 前記III族化合物が窒化ガリウム(GaN)であることを特徴とする請求項1~5のいずれか1項に記載のIII族化合物基板の製造方法。
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