JP6465114B2 - アルミナ基板 - Google Patents
アルミナ基板 Download PDFInfo
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- JP6465114B2 JP6465114B2 JP2016542549A JP2016542549A JP6465114B2 JP 6465114 B2 JP6465114 B2 JP 6465114B2 JP 2016542549 A JP2016542549 A JP 2016542549A JP 2016542549 A JP2016542549 A JP 2016542549A JP 6465114 B2 JP6465114 B2 JP 6465114B2
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- 239000000758 substrate Substances 0.000 title claims description 169
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims description 100
- 239000013078 crystal Substances 0.000 claims description 112
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 99
- 150000002910 rare earth metals Chemical class 0.000 claims description 85
- 229910052594 sapphire Inorganic materials 0.000 claims description 30
- 239000010980 sapphire Substances 0.000 claims description 30
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 140
- 239000010410 layer Substances 0.000 description 123
- 238000000034 method Methods 0.000 description 23
- 238000005121 nitriding Methods 0.000 description 21
- 238000010438 heat treatment Methods 0.000 description 19
- 239000000463 material Substances 0.000 description 17
- 239000000243 solution Substances 0.000 description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 14
- 229910052799 carbon Inorganic materials 0.000 description 14
- 239000004065 semiconductor Substances 0.000 description 14
- 238000005259 measurement Methods 0.000 description 11
- 239000007789 gas Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000010409 thin film Substances 0.000 description 8
- 229910002704 AlGaN Inorganic materials 0.000 description 7
- 239000004570 mortar (masonry) Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 230000007547 defect Effects 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- 238000004528 spin coating Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 238000003384 imaging method Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- OKTJSMMVPCPJKN-BJUDXGSMSA-N carbon-11 Chemical compound [11C] OKTJSMMVPCPJKN-BJUDXGSMSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000007716 flux method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000004453 electron probe microanalysis Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000007740 vapor deposition Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910002601 GaN Inorganic materials 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- HQFCOGRKGVGYBB-UHFFFAOYSA-N ethanol;nitric acid Chemical compound CCO.O[N+]([O-])=O HQFCOGRKGVGYBB-UHFFFAOYSA-N 0.000 description 2
- 238000004299 exfoliation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 230000002269 spontaneous effect Effects 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 238000005092 sublimation method Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- 238000001947 vapour-phase growth Methods 0.000 description 2
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-IGMARMGPSA-N Carbon-12 Chemical compound [12C] OKTJSMMVPCPJKN-IGMARMGPSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910021386 carbon form Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002602 lanthanoids Chemical group 0.000 description 1
- 239000002346 layers by function Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- GZIAUVGSMHERLN-UHFFFAOYSA-N neodymium(3+);trinitrate;hydrate Chemical compound O.[Nd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GZIAUVGSMHERLN-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000010897 surface acoustic wave method Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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- 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
- C30B29/38—Nitrides
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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
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- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
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- C30B1/00—Single-crystal growth directly from the solid state
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- C30B19/00—Liquid-phase epitaxial-layer growth
- C30B19/02—Liquid-phase epitaxial-layer growth using molten solvents, e.g. flux
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- C30B19/00—Liquid-phase epitaxial-layer growth
- C30B19/08—Heating of the reaction chamber or the substrate
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- C30B19/00—Liquid-phase epitaxial-layer growth
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- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
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- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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- C30B5/00—Single-crystal growth from gels
- C30B5/02—Single-crystal growth from gels with addition of doping materials
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- 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
- C30B9/12—Salt solvents, e.g. flux growth
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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
- H01L21/20—Deposition of semiconductor materials on a substrate, e.g. epitaxial growth solid phase epitaxy
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- Crystals, And After-Treatments Of Crystals (AREA)
Description
本発明の望ましい態様としては、希土類含有領域の形状は、アルミナ基板表面に対し垂直な方向よりも平行な方向に長い形状であることが好ましい。応力集中が顕著となるためである。
本発明の望ましい態様としては、希土類含有層および希土類含有領域は、アルミナ基板表面に対し平行な方向に分布していることが好ましい。AlN結晶育成と自然剥離による自立化を行う場合、クラックの伝搬方向を基板表面に対し平行な方向に誘導し、自然剥離の際にAlN結晶へのクラック伝搬を抑止できるためである。
なお照射位置431を起点とした照射位置432の変位ベクトルと結像位置441を起点とした結像位置442の変位ベクトルが平行であれば凸、反平行であれば凹となっている。
2インチφのサイズをもつc面サファイア基板に濃度2wt%の希土類元素としてYを含有するMOD溶液を、2000rpmで20秒間スピンコートにより塗布した。塗布後、150℃のホットプレート上で10分間乾燥させた後、空気中にて600℃、2時間熱処理した。熱処理後、100mm角のアルミナ板13に載せ、更に図5に示すように基板10の周囲4か所に20mgづつ総量80mgの粉末状カーボン11を配置した。これを図4に示すように、75mm角、高さ30mmのアルミナ匣鉢12で全体を覆ったうえで、試料設置台20に設置した。窒化処理炉はカーボンをヒーターとする抵抗加熱型の電気炉である。加熱前に回転ポンプと拡散ポンプを用いて0.03Paまで脱気し、次いで100kPa(大気圧)になるまで窒素ガスを流した後、窒素ガスのフローを停止した。窒化処理の処理温度を1750℃、処理時間を4時間、昇降温速度を600℃/時間とした。室温まで冷却後、処理基板を取り出し評価した。処理基板は概ね透明であったが、外周部から約1mm内側の領域にかけて白濁が認められた。また顕微鏡観察によると、透明部でもヒロックが形成されている箇所が認められた。
実施例1で切り出した10mm角の試料中、外周部付近の試料を用いて実施例1と同様にXRD測定、曲率半径測定、蛍光X線分析、およびSEM観察を行った。XRD測定では実施例1と同様、AlN(002)の回折線が認められ、サファイア(006)回折線に対するAlN(002)回折線の強度比は48%であった。(112)面を利用した極図測定では6回軸対象のピークが6本出現しており、単結晶であることを確認できた。しかし外周部近傍の白濁が認められた領域ではAlN(002)に加えAlN(101)も出現しており、単結晶ではなくボウル状となっていた。曲率半径は120mであり、また蛍光X線分析ではAl原子数に対し180ppmのY原子が検出された。実施例1と比較すると、希土類含有量が増えると曲率半径が大きくなる、即ちソリが小さくなっていることがわかる。
c面サファイアを10mm角に切り出し窒化処理用の基板10を準備した。硝酸ネオジム水和物をエタノールに溶かし、濃度2wt%とした後、若干界面活性剤を加え、塗布溶液を作成した。スピンコートは3000rpmで20秒間行った。250℃のホットプレート上で10分間乾燥させた後、空気中にて800℃、2時間熱処理した。窒化処理は実施例3と同様に行った。ただし処理温度は1750℃とした。
窒化処理時間12時間、アルミナ匣鉢12として直径60mm、高さ50mmの円筒状アルミナルツボを用いた以外は実施例3と同様な処理を行ったところ、サファイア(006)回折線に対するAlN(002)回折線の強度比は18%、第一の結晶50の厚さは0.17μmと実施例3とほぼ同様であった。一方、曲率半径は15m、またNdは検出されなかった。実施例3と比較例1との比較から、希土類を含有することにより、本実施形態のアルミナ基板の曲率半径が大きくなる、即ちソリが小さくなっていることがわかる。
c面サファイアを10mm角に切り出し窒化処理用の基板10を準備した。濃度2wt%の希土類元素としてEuを含有するMOD溶液を、2000rpmで20秒間スピンコートにより塗布した。塗布後、150℃のホットプレート上で10分間乾燥させた後、空気中にて600℃、2時間熱処理した。窒化処理は実施例3と同様に行った。ただし処理温度は1650℃とした。
多結晶アルミナ基板を10mm角に切り出し、窒化処理用の基板10を準備した。実施例4と同様の塗布、乾燥、空気中熱処理、および窒化処理を行った。ただし窒化処理温度は1550℃とした。
実施例1にて中心部付近から切り出した10mm角の試料の中の1つを基板とし、フラックス法にてAlN単結晶育成を行った。フラックス法は以下の条件である。イットリア安定化ジルコニア製ルツボに材料(組成:Si35.7wt%、C2.3wt%、Al62.0wt% 重量:150g)を入れて、高周波加熱炉の加熱領域に置いた。材料直上には窒化処理したサファイア基板を固定したイットリア安定化ジルコニア製の撹拌治具を配置した。窒素雰囲気中で材料温度を1600℃まで上げて溶融させた後、撹拌羽根で溶液を撹拌しながら5時間保持して溶液を窒素で飽和させた。その後窒化処理したサファイア基板を溶液表面に接触させて100rpmで回転させながら、材料温度を徐々に下げてサファイア基板上にAlN単結晶を20時間かけて成長させた。結晶成長が終了した後、サファイア基板を溶液から離し材料を室温まで冷やした。冷却終了後炉内から試料を取り出したところ、アルミナ基板が横方向に剥離し、AlN単結晶板がサファイア基板の部分から分離していた。AlN結晶の育成中に希土類含有層が格子不整合による応力を集中して受けた結果、自然剥離したと思われる。AlN単結晶板の厚さは250μmであった。
11 カーボン
12 アルミナ匣鉢
13 アルミナ板
20 試料設置台
22 カーボンヒーター
23 チャンバー
24 ガス排気口
25 ガス導入口
30 AlN層
31 希土類含有層
32 希土類含有領域
33 アルミナ基板
41 可視のLD、またはLED光源
42 スクリーン
431 本実施形態のアルミナ基板10のAlN層が形成されている側の任意の一点における光の照射位置
432 本実施形態のアルミナ基板10をスクリーン42と平行に移動した後の光の照射位置
441 光の照射位置431に対応してスクリーン上に結像した反射光の結像位置
442 光の照射位置432に対応してスクリーン上に結像した反射光の結像位置
50 第一の結晶
51 白く光る層
52 白く光る領域
53 第二の結晶
Claims (7)
- アルミナ基板であって、前記アルミナ基板表面にはAlN層が形成されており、かつ前記AlN層と前記アルミナ基板との界面に希土類含有層および/または希土類含有領域が形成されていることを特徴とするアルミナ基板。
- 希土類元素の含有量がAl元素比で1〜10000ppmであることを特徴とする請求項1に記載のアルミナ基板。
- 前記AlN層の厚さが0.02μmから100μmであることを特徴とする請求項1又は2に記載のアルミナ基板。
- 前記アルミナ基板はサファイアであることを特徴とする請求項1〜3のいずれか一項に記載のアルミナ基板。
- 前記AlN層は主として単結晶であることを特徴とする請求項4に記載のアルミナ基板。
- 前記希土類含有領域の形状は、前記アルミナ基板表面に対し垂直な方向よりも平行な方向に長い形状であることを特徴とする、請求項1〜5のいずれか一項に記載のアルミナ基板。
- 前記希土類含有層および前記希土類含有領域は、前記アルミナ基板表面に対し平行な方向に分布していることを特徴とする、請求項1〜6のいずれか一項に記載のアルミナ基板。
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