JP6684815B2 - エピタキシャル成長用配向アルミナ基板 - Google Patents
エピタキシャル成長用配向アルミナ基板 Download PDFInfo
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- JP6684815B2 JP6684815B2 JP2017543254A JP2017543254A JP6684815B2 JP 6684815 B2 JP6684815 B2 JP 6684815B2 JP 2017543254 A JP2017543254 A JP 2017543254A JP 2017543254 A JP2017543254 A JP 2017543254A JP 6684815 B2 JP6684815 B2 JP 6684815B2
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- alumina
- light emitting
- plate
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- 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 216
- 239000000758 substrate Substances 0.000 title claims description 183
- 239000013078 crystal Substances 0.000 claims description 59
- 239000002245 particle Substances 0.000 claims description 51
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 239000010410 layer Substances 0.000 description 158
- 239000000843 powder Substances 0.000 description 96
- 239000004065 semiconductor Substances 0.000 description 53
- 229910002601 GaN Inorganic materials 0.000 description 51
- 238000000034 method Methods 0.000 description 44
- 238000004519 manufacturing process Methods 0.000 description 24
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 20
- 238000010304 firing Methods 0.000 description 20
- 239000010408 film Substances 0.000 description 19
- 239000002346 layers by function Substances 0.000 description 19
- 239000000463 material Substances 0.000 description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- IUVCFHHAEHNCFT-INIZCTEOSA-N 2-[(1s)-1-[4-amino-3-(3-fluoro-4-propan-2-yloxyphenyl)pyrazolo[3,4-d]pyrimidin-1-yl]ethyl]-6-fluoro-3-(3-fluorophenyl)chromen-4-one Chemical compound C1=C(F)C(OC(C)C)=CC=C1C(C1=C(N)N=CN=C11)=NN1[C@@H](C)C1=C(C=2C=C(F)C=CC=2)C(=O)C2=CC(F)=CC=C2O1 IUVCFHHAEHNCFT-INIZCTEOSA-N 0.000 description 14
- 239000002002 slurry Substances 0.000 description 13
- 238000011282 treatment Methods 0.000 description 11
- 230000008569 process Effects 0.000 description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 9
- 239000002612 dispersion medium Substances 0.000 description 9
- 239000011777 magnesium Substances 0.000 description 9
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- 239000012299 nitrogen atmosphere Substances 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 7
- 239000000395 magnesium oxide Substances 0.000 description 7
- 238000000465 moulding Methods 0.000 description 7
- 238000000206 photolithography Methods 0.000 description 7
- 239000010409 thin film Substances 0.000 description 7
- 239000002270 dispersing agent Substances 0.000 description 6
- 239000010440 gypsum Substances 0.000 description 6
- 229910052602 gypsum Inorganic materials 0.000 description 6
- 239000000155 melt Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000001771 vacuum deposition Methods 0.000 description 6
- 229920002799 BoPET Polymers 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 5
- 230000004888 barrier function Effects 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 5
- 239000002019 doping agent Substances 0.000 description 5
- 238000007716 flux method Methods 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 239000004014 plasticizer Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 230000002159 abnormal effect Effects 0.000 description 4
- 239000006061 abrasive grain Substances 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
- 239000011812 mixed powder Substances 0.000 description 4
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 4
- 238000007639 printing Methods 0.000 description 4
- 229910052594 sapphire Inorganic materials 0.000 description 4
- 239000010980 sapphire Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 239000004147 Sorbitan trioleate Substances 0.000 description 3
- PRXRUNOAOLTIEF-ADSICKODSA-N Sorbitan trioleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCC\C=C/CCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCC\C=C/CCCCCCCC PRXRUNOAOLTIEF-ADSICKODSA-N 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
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- 238000007606 doctor blade method Methods 0.000 description 3
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- 238000000227 grinding Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
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- 239000007790 solid phase Substances 0.000 description 3
- 229960000391 sorbitan trioleate Drugs 0.000 description 3
- 235000019337 sorbitan trioleate Nutrition 0.000 description 3
- 239000012808 vapor phase Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- -1 MgO Chemical class 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
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- 239000000919 ceramic Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 238000003618 dip coating Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 229910001425 magnesium ion Inorganic materials 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000001451 molecular beam epitaxy Methods 0.000 description 2
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- 238000005507 spraying Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910016569 AlF 3 Inorganic materials 0.000 description 1
- 241000282994 Cervidae Species 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229940116411 terpineol Drugs 0.000 description 1
- IEXRMSFAVATTJX-UHFFFAOYSA-N tetrachlorogermane Chemical compound Cl[Ge](Cl)(Cl)Cl IEXRMSFAVATTJX-UHFFFAOYSA-N 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000000927 vapour-phase epitaxy Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- 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
- C30B29/20—Aluminium oxides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
- C04B35/111—Fine ceramics
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/6342—Polyvinylacetals, e.g. polyvinylbutyral [PVB]
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/638—Removal thereof
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
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- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/12—Single-crystal growth directly from the solid state by pressure treatment during the growth
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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
- 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
- C30B19/12—Liquid-phase epitaxial-layer growth characterised by the substrate
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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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- 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
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/183—Epitaxial-layer growth characterised by the substrate being provided with a buffer layer, e.g. a lattice matching layer
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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
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/02—Production of homogeneous polycrystalline material with defined structure directly from the solid state
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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
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/02428—Structure
- H01L21/0243—Surface structure
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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Description
本発明の一実施形態のエピタキシャル成長用配向アルミナ基板は、多結晶アルミナ基板であって、表面を構成する結晶粒子のチルト角が0.1°以上1.0°未満であることが好ましく、平均焼結粒径が10μm以上であることが好ましい。
本実施形態のエピタキシャル成長用配向アルミナ基板の製法は特に限定がないが、好ましい製法としては、(a)微細アルミナ粉末層と、板状アルミナ粒子の板面が微細アルミナ粉末層の表面に沿うように配列された板状アルミナ粉末層とが、交互に積層された積層体を作製する工程と、(b)積層体を焼成する工程と、を含む製法が挙げられる。
素子用基板S1は、配向アルミナ基板を構成要素に含むタイプの発光素子用基板である。図3の上段は、素子用基板S1の一例である発光素子用基板10の断面図である。発光素子用基板10は、配向アルミナ基板12上に形成されたバッファ層16上に発光機能層14が形成されている。発光機能層14は、バッファ層16側からn型層14c、活性層14b及びp型層14aが積層された複合層である。発光機能層14を構成する各層は、半導体材料を主成分とする材料で構成されている。半導体材料としては、GaN系材料、ZnO系材料及びAlN系材料などが挙げられるが、このうちGaN系材料が好ましい。n型層14cは半導体材料にn型ドーパントがドープされ、p型層14aは半導体材料にp型ドーパントがドープされている。活性層14bは、量子井戸層と障壁層とが交互に積層された多重量子井戸層であり、半導体材料としてGaN材料を用いる場合、量子井戸層をInGaN層、障壁層をGaN層とすることができる。バッファ層16は、配向アルミナ基板12と発光機能層14の格子ミスマッチによる格子欠陥を低減し、結晶性を改善するための層である。バッファ層16は、発光機能層14の結晶構造と同じ又は類似した高い結晶性を有するものであることが好ましく、格子定数が同じ又は近いものを用いてもよい。バッファ層16は、配向アルミナ基板12の結晶方位に倣って成長した構造を有する。バッファ層16は、上述した半導体材料を主成分とする材料で構成されるのが好ましく、p型ないしn型に制御するためのドーパントを適宜含むものであってもよい。
素子用基板S2は、素子用基板S1の配向アルミナ基板の代わりに半導体自立基板を構成要素に含むタイプの発光素子用基板である。図4の上段は、素子用基板S2の一例である発光素子用基板20の断面図である。発光素子用基板20は、半導体自立基板22上に発光機能層24が形成されている。発光機能層24は、n型層24c、活性層24b及びp型層24aが積層された複合層であるが、基本的には上述した発光機能層14と同じであるため、説明を省略する。図4の半導体自立基板22は、n型ドーパントがドープされた半導体材料であるが、ノンドープの半導体材料でもよい。n型ドーパントの導入により導電性を持たせた窒化ガリウムを基板とすることで、縦型構造の発光素子を実現することができる。
(1)配向アルミナ基板の作製
(1a)積層体の作製
微細アルミナ粉末(大明化学工業株式会社製、グレードTM−DAR)100質量部に対し、酸化マグネシウム(500A、宇部マテリアルズ製)0.0125質量部(125質量ppm)と、バインダーとしてポリビニルブチラール(品番BM−2、積水化学工業製)7.8質量部と、可塑剤としてジ(2−エチルヘキシル)フタレート(黒金化成製)3.9質量部と、分散剤としてトリオレイン酸ソルビタン(レオドールSP−O30、花王製)2質量部と、分散媒として2−エチルヘキサノールとを加えて混合した。分散媒の量は、スラリー粘度が20000cPとなるように調整した。このようにして調製されたスラリーを、ドクターブレード法によってPETフィルムの上に乾燥後の厚みが40μmとなるようにシート状に成形し、微細アルミナ粉末層とした。
得られた積層体を脱脂炉中に配置し、600℃で10時間の条件で脱脂を行った。得られた脱脂体を黒鉛製の型を用い、ホットプレスにて窒素中、焼成温度(最高到達温度)1975℃で4時間、面圧200kgf/cm2の条件で焼成し、アルミナ焼結体を得た。なお、焼成温度から降温する際に1200℃までプレス圧を維持し、1200℃未満の温度域ではプレス圧をゼロに開放した
このようにして得た焼結体をセラミックスの定盤に固定し、砥石を用いて#2000まで研削して板面を平坦にした。次いで、ダイヤモンド砥粒を用いたラップ加工により、板面を平滑化し、直径50mm、厚さ0.5mmの配向アルミナ焼結体を配向アルミナ基板として得た。砥粒のサイズを3μmから0.5μmまで段階的に小さくしつつ、平坦性を高めた。加工後の平均粗さRaは4nmであった。
(2a)c面配向度
得られた配向アルミナ基板の配向度を確認するため、配向アルミナ基板の上面に対して平行になるように研磨加工した後、その研磨面に対してX線を照射しc面配向度を測定した。XRD装置(リガク製、RINT−TTR III)を用い、2θ=20〜70°の範囲でXRDプロファイルを測定した。具体的には、CuKα線を用いて電圧50kV、電流300mAという条件で測定した。c面配向度は、ロットゲーリング法によって算出した。具体的には、以下の式により算出した。式中、Pは配向アルミナ基板のXRDから得られた値であり、P0は標準α−アルミナ(JCPDSカードNo.46−1212)から算出された値である。実験例1の配向アルミナ基板のc面配向度は100%であった。
チルト角は、結晶軸の傾き分布であり、アルミナの結晶方位がc軸からどの程度の頻度で傾いているかを評価するパラメータである。ここでは、チルト角をX線ロッキングカーブ半値幅(XRC・FWHM)で表す。XRC・FWHMは、配向アルミナ基板の板面(c面配向度測定と同じ面)に対し、図5のようにX線源と検出器を連動させてスキャンし、得られたカーブの半値幅を測定した。このように2θ(検出器と入射X線とのなす角度)の値をその回折ピーク位置に固定し、ω(試料基板面と入射X線とのなす角度)のみ走査する測定方法をロッキングカーブ測定とよぶ。装置はリガク製、RINT−TTR IIIを用い、CuKα線を用いて電圧50kV、電流300mAという条件でωの走査範囲を3.8°〜38.8°とした。実験例1の配向アルミナ基板のXRC・FWHMは0.9°であった。
配向アルミナ基板の焼結体粒子について、板面の平均焼結粒径を以下の方法により測定した。得られた配向アルミナ基板を、1550℃で45分間サーマルエッチングを行った後、走査電子顕微鏡にて画像を撮影した。視野範囲は、得られる画像の対角線に直線を引いた場合に、いずれの直線も10個から30個の粒子と交わるような直線が引けるような視野範囲とした。得られた画像の対角線に引いた2本の直線において、直線が交わる全ての粒子に対し、個々の粒子の内側の線分の長さを平均したものに1.5を乗じた値を板面の平均焼結粒径とした。この結果、板面の平均焼結粒径は66μmであった。
アルミナ焼結体を純度99.9質量%のアルミナ乳鉢で粉砕した後、下記方法により定量分析した。そして、アルミナ焼結体中のNa、Mg、Si、P、Ca、Fe、Ti、Znの質量割合(ppm)を求めた。実験例1のアルミナ焼結体のMg以外の不純物元素は、いずれも検出限界以下であり、Mgが62ppm検出された。
不純物定量方法: JISR1649に準拠した加圧硫酸分解法にて板状アルミナ粉末を溶解し、ICP(誘導結合プラズマ)発光分析装置(日立ハイテクサイエンス製 PS3520UV−DD)にて分析した。
実験例A1において、板状アルミナ粉末として、自社製のものを用いた以外は、実験例A1と同様にして配向アルミナ基板を作製し、その特性を測定した。配向アルミナ基板の特性を表1に示す。
実験例A3において、焼成温度を1900℃とした以外は、実験例A1と同様にして配向アルミナ基板を作製し、その特性を測定した。配向アルミナ基板の特性を表1に示す。
微細アルミナ粉末(大明化学工業株式会社製、グレードTM−DAR)100質量部に対し、酸化マグネシウム(500A、宇部マテリアルズ製)0.0125質量部(125質量ppm)と、バインダーとしてポリビニルブチラール(品番BM−2、積水化学工業製)7.8質量部と、可塑剤としてジ(2−エチルヘキシル)フタレート(黒金化成製)3.9質量部と、分散剤としてトリオレイン酸ソルビタン(レオドールSP−O30、花王製)2質量部と、分散媒として2−エチルヘキサノールとを加えて混合した。分散媒の量は、スラリー粘度が20000cPとなるように調整した。このようにして調製されたスラリーを、ドクターブレード法によってPETフィルムの上に乾燥後の厚みが40μmとなるようにシート状に成形し、微細アルミナ粉末層とした。
微細アルミナ粉末(大明化学工業株式会社製、グレードTM−DAR)99.8質量部、イットリア粉末(信越化学工業株式会社製、グレードUU)0.2質量部を混合し、混合粉末100gに対して溶媒として水50ccの割合で添加し、ボールミルにて40時間混合粉砕し、スラリー化した。得られたスラリーを内径50mmの石膏型に注ぎ、12Tの磁場中で3時間戴置し、鋳込み成形を行った。成形体は石膏から脱型し、室温での乾燥後、黒鉛製の型を用い、ホットプレスにて窒素中1400℃で4時間、面圧200kgf/cm2の条件で焼成した。得られた焼結体を実験例A1と同様にして加工して配向アルミナ基板を作製し、その特性を測定した。配向アルミナ基板の特性を表1に示す。
市販の板状アルミナ粉末(キンセイマテック製、グレードYFA10030)を気流分級機(日清エンジニアリング製TC−15N)にてカット点を3μmに設定して分級し、次にポット解砕機にてφ0.3mmの玉石で20時間解砕し、最後に水簸にて微粒粉末を除去した。得られた板状アルミナ粉末0.5質量部と微細アルミナ粉末(大明化学工業株式会社製、グレードTM−DAR)99.5質量部を混合した。更に混合粉末100質量部に対し、酸化マグネシウム(500A、宇部マテリアルズ製)0.0125質量部(125質量ppm)を混合し、調合粉末を得た。調合粉末100gに対して溶媒として水50ccの割合で添加し、ボールミルにて40時間混合粉砕し、スラリー化した。得られたスラリーを内径50mmの石膏型に注ぎ、12Tの磁場中で3時間戴置し、鋳込み成形を行った。成形体は石膏から脱型し、室温での乾燥後、黒鉛製の型を用い、ホットプレスにて窒素中1975℃で4時間、面圧200kgf/cm2の条件で焼成した。得られた焼結体を実験例A1と同様にして加工して配向アルミナ基板を作製し、その特性を測定した。配向アルミナ基板の特性を表1に示す。
微細アルミナ粉末(住友化学製、グレードAKP−3000)100質量部に対し、酸化マグネシウム(500A、宇部マテリアルズ製)0.0125質量部(125質量ppm)を混合し、混合粉末100gに対して溶媒として水50ccの割合で添加し、ボールミルにて40時間混合粉砕し、スラリー化した。得られたスラリーを内径50mmの石膏型に注ぎ、10Tの磁場中で3時間戴置し、鋳込み成形を行った。成形体は石膏から脱型し、室温での乾燥後、黒鉛製の型を用い、ホットプレスにて窒素中1975℃で4時間、面圧200kgf/cm2の条件で焼成した。得られた焼結体を実験例A1と同様にして加工して配向アルミナ基板を作製し、その特性を測定した。配向アルミナ基板の特性を表1に示す。
スラリーを内径50mmの石膏型に注ぎ、12Tの磁場中で8時間載置し、鋳込み成形を行った以外は、実験例A7と同様にしてアルミナ焼結体を作製した。得られた焼結体を実験例A1と同様にして加工して配向アルミナ基板を作製し、その特性を測定した。配向アルミナ基板の特性を表1に示す。
実験例A1において、片面加工体の作製方法を以下のように変更した以外は、実験例A4と同様にしてアルミナ焼結体を作製した。
(1)発光素子用基板(素子用基板S1)の作製
(1a)種結晶層の成膜
実験例A1で作製した配向アルミナ基板の上に、MOCVD法を用いて、種結晶層を形成した。具体的には、530℃にて低温GaN層を40nm堆積させた後に、1050℃にて厚さ3μmのGaN膜を積層させて種結晶基板を得た。
上記工程で作製した種結晶基板を、内径80mm、高さ45mmの円筒平底のアルミナ坩堝の底部分に設置し、次いで融液組成物をグローブボックス内で坩堝内に充填した。融液組成物の組成は以下のとおりである。
・金属Ga:60g
・金属Na:60g
MOCVD法を用いて、基板上にn型層として1050℃でSi原子濃度が5×1018/cm3になるようにドーピングしたn−GaN層を3μm堆積した。次に活性層として750℃で多重量子井戸層を堆積した。具体的にはInGaNによる2.5nmの井戸層を5層、GaNによる10nmの障壁層を6層にて交互に積層した。次にp型層として950℃でMg原子濃度が1×1019/cm3になるようにドーピングしたp−GaNを200nm堆積した。その後、MOCVD装置から取り出し、p型層のMgイオンの活性化処理として、窒素雰囲気中で800℃の熱処理を10分間行い、発光素子用基板を得た。
作製した発光素子用基板の発光機能層側においてフォトリソグラフィープロセスとRIE法とを用い、n型層の一部を露出した。続いて、フォトリソグラフィープロセスと真空蒸着法とを用いて、n型層の露出部分に、カソード電極としてのTi/Al/Ni/Au膜をそれぞれ15nm、70nm、12nm、60nmの厚みでパターニングした。その後、オーム性接触特性を良好なものとするために、窒素雰囲気中での700℃の熱処理を30秒間行った。さらに、フォトリソグラフィープロセスと真空蒸着法とを用いて、p型層に透光性アノード電極としてNi/Au膜をそれぞれ6nm、12nmの厚みにパターニングした。その後、オーム性接触特性を良好なものとするために窒素雰囲気中で500℃の熱処理を30秒間行った。さらに、フォトリソグラフィープロセスと真空蒸着法とを用いて、透光性アノード電極としてのNi/Au膜の上面の一部領域に、アノード電極パッドとなるNi/Au膜をそれぞれ5nm、60nmの厚みにパターニングした。こうして得られたウェハーを切断してチップ化し、さらにリードフレームに実装して、横型構造の発光素子を得た。
実験例A2〜A9の配向アルミナ基板を用いて、実験例B1と同様の方法で発光素子用基板を作製した。また、実験例B1と同様の方法で横型構造の発光素子を作製した。
実験例B1〜B9で作製した横型発光素子に対し、カソード電極とアノード電極間に通電し、I−V測定を行ったところ、いずれの試料も整流性が確認された。また、順方向の電流を流したところ、いずれも波長450nmの発光が確認された。発光輝度は実験例B1、B2、B9の素子が著しく高輝度であった。実験例B3、B7の基板を用いた素子も高輝度であるが、実験例B1、B2、B9より輝度がわずかに低下した。実験例B8の基板を用いた素子も高輝度であったが、実験例B3、B7よりわずかに低下した。実験例B4の素子は実験例B8よりも大幅に輝度が低下した。実験例B5、B6の素子は実験例B4より更に輝度が低下した。
(1)発光素子用基板(素子用基板S2)の作製
(1a)種結晶層の成膜
実験例A1で作製した配向アルミナ基板の上に、MOCVD法を用いて種結晶層を形成した。具体的には、バッファ層としてサセプタ温度530℃、水素雰囲気中にて低温GaN層を30nm堆積させた後に、窒素・水素雰囲気にてサセプタ温度1050℃まで昇温し厚さ3μmのGaN膜を積層させて種結晶基板を得た。
上記工程で作製した種結晶基板を、内径80mm、高さ45mmの円筒平底のアルミナ坩堝の底部分に設置し、次いで融液組成物をグローブボックス内で坩堝内に充填した。融液組成物の組成は以下のとおりである。
・金属Ga:60g
・金属Na:60g
・四塩化ゲルマニウム:1.85g
MOCVD法を用いて、実験例C1で作製した各Geドープ多結晶窒化ガリウム自立基板上にn型層として1050℃でSi原子濃度が5×1018/cm3になるようにドーピングしたn−GaN層を1μm堆積した。次に発光層として750℃で多重量子井戸層を堆積した。具体的にはInGaNによる2.5nmの井戸層を5層、GaNによる10nmの障壁層を6層にて交互に積層した。次にp型層として950℃でMg原子濃度が1×1019/cm3になるようにドーピングしたp−GaNを200nm堆積した。その後、MOCVD装置から取り出し、p型層のMgイオンの活性化処理として、窒素雰囲気中で800℃の熱処理を10分間行った。
実験例C2〜C9では、実験例A2〜A9の配向アルミナ基板を用いて、実験例C1と同様の方法で発光素子用基板を作製し、更に実験例C1と同様の方法で縦型構造の発光素子を作製した。
実験例C1〜C9で作製した縦型発光素子に対し、カソード電極とアノード電極間に通電し、I−V測定を行ったところ、いずれの試料も整流性が確認された。また、順方向の電流を流したところ、いずれも波長450nmの発光が確認された。発光輝度は実験例C1、C2、C9の素子が著しく高輝度であった。実験例C3、C7の基板を用いた素子も高輝度であるが、実験例C1、C2、C9より輝度がわずかに低下した。実験例C8の基板を用いた素子も高輝度であったが、実験例C3、C7よりわずかに低下した。実験例C4の素子は実験例C8よりも大幅に輝度が低下した。実験例C5、C6の素子は実験例C4より更に輝度が低下した。
Claims (4)
- 表面を構成する結晶粒子のチルト角が0.1°以上1.0°未満であり、
平均焼結粒径が10μm以上である、
エピタキシャル成長用配向アルミナ基板。 - 表面を構成する結晶粒子の平均焼結粒径が20μm以上である、
請求項1記載のエピタキシャル成長用配向アルミナ基板。 - Na、Mg、Si、P、Ca、Fe、Ti、Znの各含有量が1500ppm以下であることを特徴とする、
請求項1又は2に記載のエピタキシャル成長用配向アルミナ基板。 - Mg含有量が15ppm以上であることを特徴とする、
請求項1〜3のいずれか1項に記載のエピタキシャル成長用配向アルミナ基板。
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JP6691132B2 (ja) * | 2015-09-30 | 2020-04-28 | 日本碍子株式会社 | アルミナ焼結体及び光学素子用下地基板 |
JP6681406B2 (ja) * | 2015-09-30 | 2020-04-15 | 日本碍子株式会社 | エピタキシャル成長用配向アルミナ基板 |
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