JP7182262B2 - Ramo4基板およびその製造方法、ならびにiii族窒化物半導体 - Google Patents
Ramo4基板およびその製造方法、ならびにiii族窒化物半導体 Download PDFInfo
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- JP7182262B2 JP7182262B2 JP2018230734A JP2018230734A JP7182262B2 JP 7182262 B2 JP7182262 B2 JP 7182262B2 JP 2018230734 A JP2018230734 A JP 2018230734A JP 2018230734 A JP2018230734 A JP 2018230734A JP 7182262 B2 JP7182262 B2 JP 7182262B2
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- group iii
- iii nitride
- ramo4
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- 239000000758 substrate Substances 0.000 title claims description 116
- 150000004767 nitrides Chemical class 0.000 title claims description 64
- 239000004065 semiconductor Substances 0.000 title claims description 28
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 239000013078 crystal Substances 0.000 claims description 212
- 238000010438 heat treatment Methods 0.000 claims description 50
- 239000000155 melt Substances 0.000 claims description 47
- 238000000034 method Methods 0.000 claims description 44
- 239000002994 raw material Substances 0.000 claims description 38
- 229910052733 gallium Inorganic materials 0.000 claims description 8
- 229910052738 indium Inorganic materials 0.000 claims description 8
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 229910052706 scandium Inorganic materials 0.000 claims description 6
- 238000001228 spectrum Methods 0.000 claims description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 5
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 5
- 229910052793 cadmium Inorganic materials 0.000 claims description 5
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 5
- 150000002602 lanthanoids Chemical class 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 229910052748 manganese Inorganic materials 0.000 claims description 5
- 229910052727 yttrium Inorganic materials 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
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- 230000000052 comparative effect Effects 0.000 description 24
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- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 11
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- 238000003776 cleavage reaction Methods 0.000 description 6
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- 230000008018 melting Effects 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical class O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
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- 239000011261 inert gas Substances 0.000 description 3
- 229910052741 iridium Inorganic materials 0.000 description 3
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 241000894007 species Species 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
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- 239000010937 tungsten Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 206010021143 Hypoxia Diseases 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
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- 239000002019 doping agent Substances 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
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- 238000011160 research Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 229910052716 thallium Inorganic materials 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 2
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000004033 diameter control Methods 0.000 description 1
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 229910001195 gallium oxide Inorganic materials 0.000 description 1
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 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
- 230000010354 integration Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- PVADDRMAFCOOPC-UHFFFAOYSA-N oxogermanium Chemical compound [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- 238000000927 vapour-phase epitaxy Methods 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
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/26—Complex oxides with formula BMe2O4, wherein B is Mg, Ni, Co, Al, Zn, or Cd and Me is Fe, Ga, Sc, Cr, Co, or Al
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- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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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
- C30B29/403—AIII-nitrides
- C30B29/406—Gallium nitride
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- Chemical Kinetics & Catalysis (AREA)
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- Crystals, And After-Treatments Of Crystals (AREA)
- Chemical Vapour Deposition (AREA)
Description
本開示の一実施の形態に係るRAMO4基板を構成するRAMO4単結晶体は、チョクラルスキー法(以下、「CZ法」とも称する)による結晶引き上げ装置で作製することができる。本実施の形態の結晶育成工程で用いる結晶引き上げ装置には、抵抗加熱方式炉または高周波加熱方式炉が含まれる。図1は、抵抗加熱方式炉100の構成を示す模式図であり、図2は、高周波加熱方式炉200の構成を示す模式図である。以下、抵抗加熱方式または高周波加熱方式により、RAMO4単結晶体の一つであるScAlMgO4単結晶体を製造する場合を例に、RAMO4単結晶体(RAMO4基板)の製造方法を説明する。ただし、本開示に適用可能なRAMO4単結晶体(RAMO4基板)は、ScAlMgO4単結晶体(ScAlMgO4基板)に限定されない。
加熱コイル240は、銅製であり、断熱材230を取り囲むように配置され、銅管の内部には冷却水が循環している。加熱コイル240に高周波電流を流すと高周波磁束が発生する。高周波磁束によりルツボ120に渦電流が発生し、ルツボ120の表面が発熱する。これにより、ルツボ120内の原料110が加熱される。
結晶育成工程後、冷却されたScAlMgO4単結晶体は取り出され、劈開や表面加工等を経て、ScAlMgO4基板とされる。このとき、ScAlMgO4基板の一方の面は、エピタキシャル成長面とされる。ScAlMgO4基板のエピタキシャル成長面にそろえて新たな結晶を配列させる(エピタキシャル成長を行う)ことで、高品質なIII族窒化物半導体を得ることができる。エピタキシャル成長では、有機金属気相成長法(Metal Organic Chemical Vapor Deposition:以下、MOCVD法)や、ハイドライド気相成長法(Hydride Vaper Phase Epitaxy:以下、HVPE法)、酸化ガリウム法(Oxide Vaper Phase Epitaxy:以下、OVPE法)等を用いて、III族窒化物などの化合物半導体の結晶を成長させる。
上述のScAlMgO4基板301を用いたIII族窒化物半導体について、以下、より詳しく説明する。
前述のように、一般的なScAlMgO4基板では、III族窒化物結晶303を形成後の冷却工程において、ScAlMgO4基板301とIII族窒化物結晶303との格子不整合および熱膨張係数差に起因してScAlMgO4基板301が反ることがある。そして、応力が集中する箇所でScAlMgO4基板301に割れやすく、製品の歩留りに多大な悪影響を与えるという問題があった。
ω=aX+b ・・・(式1)
最小二乗法を用いて求められる回帰直線の傾きaと切片bは、それぞれ式2および式3で表される。
実施の形態で示した図1の抵抗加熱方式炉100あるいは図2の高周波加熱方式炉200を用いて、ScAlMgO4単結晶体を育成した。結晶育成を新規で行う際の原料は、Sc2O3:Al2O3:MgO=27.5%:26.5%:46.0%(atom%)となる配合比率で混合した混合物とした。そして、当該混合物を焼結した後、イリジウム製のルツボ120に充填し、加熱溶融により融液状の原料110を得た。原料110の融液に種結晶152を接触させた後、結晶引上げ軸150を回転させながら生成した結晶を引き上げて、外径φ65mmのScAlMgO4単結晶体を育成した。結晶引上げ軸150の引き上げ速度450と回転速度460、および融液面の位置検出器160を用いて一定に保持した融液面430と熱源上端(ヒータ140または加熱コイル240の上端)との垂直距離480は、表1に示す実施例1~8の各条件に設定した。
融液面の位置検出器160を用いない従来の構成で、原料110の融液面430と熱源上端(ヒータ140または加熱コイル240の上端)との垂直距離480の調整は行わずに、結晶引上げ軸150の引き上げ速度450と回転速度460を設定し、それ以外は、実施例と同一の方法にてScAlMgO4単結晶体を育成した。
次に、融液面の位置検出器160を用いた実施例と同様に、原料110の融液面430と熱源上端(ヒータ140または加熱コイル240の上端)との垂直距離480を一定に保持しながら、結晶引上げ軸150の引き上げ速度450を実施例よりも高く設定した。なお、それ以外の事項は、実施例と同一の方法とし、ScAlMgO4単結晶体を育成した。結晶引上げ軸150の引き上げ速度450と回転速度460、および融液面の位置検出器160を用いて測定した融液面430と熱源上端(ヒータ140または加熱コイル240の上端)との垂直距離480は、表5に示す比較例8~9の各条件に設定した。
110 原料
120 ルツボ
121 ルツボ支持軸
122 耐火材
130 断熱材
140 ヒータ
150 結晶引き上げ軸
151 シードホルダ
152 種結晶
160 融液面の位置検出器
200 高周波加熱方式炉
230 断熱材
240 加熱コイル
300 III族窒化物半導体
301 ScAlMgO4基板
302 バッファ層
303 III族窒化物結晶
410 結晶
420 結晶成長界面
430 融液面
440 温度勾配
450 引き上げ速度
460 回転速度
470 融液の対流
480 融液面と熱源上端との垂直距離
Claims (10)
- 一般式RAMO4で表される単結晶体(一般式において、Rは、Sc、In、Y、およびランタノイド系元素からなる群から選択される一つまたは複数の三価の元素を表し、Aは、Fe(III)、Ga、及びAlからなる群から選択される一つまたは複数の三価の元素を表し、Mは、Mg、Mn、Fe(II)、Co、Cu、Zn、およびCdからなる群から選択される一つまたは複数の二価の元素を表す)からなるRAMO4基板であり、
前記RAMO4基板の中心を通る直線上の複数の位置Xi(i=1,2,3,・・・,n)でX線ロッキングカーブを測定して、各位置XiにおけるX線ロッキングカーブの回折スペクトルのX線ピーク位置ωiを特定し、
X線ピーク位置ωiと位置Xiとの関係から得られる回帰直線に基づき、結晶面の曲率半径rの絶対値を算出し、さらに
X線ピーク位置ωiと位置Xiとに基づき、下記式で算出される相関係数ρの2乗を算出した場合に、
RAMO4基板。 - 前記一般式RAMO4における前記RはSc、前記AはAl、前記MはMgである、
請求項1に記載のRAMO4基板。 - 厚さが100μm~1000μmの範囲である、
請求項1または2に記載のRAMO4基板。 - 直径が25mm~200mmの範囲である、
請求項1~3のいずれか一項に記載のRAMO4基板。 - 請求項1~5のいずれか一項に記載のRAMO4基板と、
前記RAMO4基板の一方の面に形成されたエピタキシャル成長面上に配置されたバッファ層と、
前記バッファ層上に配置された、III族窒化物結晶を有する、
III族窒化物半導体。 - 前記バッファ層はInAlGaNで表される化合物からなる、アモルファス、単結晶、または多結晶の層である、
請求項6に記載のIII族窒化物半導体。 - 前記III族窒化物結晶はGaNまたはAlNである、
請求項6または7に記載のIII族窒化物半導体。 - 一般式RAMO4で表される単結晶体(一般式において、Rは、Sc、In、Y、およびランタノイド系元素からなる群から選択される一つまたは複数の三価の元素を表し、Aは、Fe(III)、Ga、及びAlからなる群から選択される一つまたは複数の三価の元素を表し、Mは、Mg、Mn、Fe(II)、Co、Cu、Zn、およびCdからなる群から選択される一つまたは複数の二価の元素を表す)からなるRAMO4基板の製造方法であって、
前記RAMO4で表される単結晶体の原料の融液に種結晶を接触させて結晶を生じさせ、前記結晶を引き上げることで単結晶体を育成する結晶育成工程を有し、
前記結晶育成工程における前記結晶の引き上げ速度が0.3mm/h以上0.7mm/h以下であり、
前記結晶引き上げ時の融液の表面と前記融液を加熱するヒータの上端との距離が19mm以上29mm以下である、
RAMO4基板の製造方法。
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