CN108137411A - 外延生长用取向氧化铝基板 - Google Patents
外延生长用取向氧化铝基板 Download PDFInfo
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- CN108137411A CN108137411A CN201680050576.6A CN201680050576A CN108137411A CN 108137411 A CN108137411 A CN 108137411A CN 201680050576 A CN201680050576 A CN 201680050576A CN 108137411 A CN108137411 A CN 108137411A
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- Prior art keywords
- aluminum oxide
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- plate
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- 239000000758 substrate Substances 0.000 title claims abstract description 184
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title claims abstract description 133
- 239000013078 crystal Substances 0.000 claims abstract description 45
- 239000002245 particle Substances 0.000 claims abstract description 44
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910052749 magnesium 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
- 239000004065 semiconductor Substances 0.000 abstract description 48
- 239000000203 mixture Substances 0.000 abstract description 8
- 238000005530 etching Methods 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 133
- 239000000843 powder Substances 0.000 description 101
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 80
- 238000000034 method Methods 0.000 description 73
- 229910002601 GaN Inorganic materials 0.000 description 45
- 230000008569 process Effects 0.000 description 36
- 239000010408 film Substances 0.000 description 29
- 239000002346 layers by function Substances 0.000 description 18
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 17
- 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 16
- 229910052782 aluminium Inorganic materials 0.000 description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 15
- 239000000463 material Substances 0.000 description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 14
- 238000010304 firing Methods 0.000 description 13
- 239000002002 slurry Substances 0.000 description 13
- 238000010438 heat treatment Methods 0.000 description 11
- 238000000465 moulding Methods 0.000 description 11
- 238000012545 processing Methods 0.000 description 11
- 239000000126 substance Substances 0.000 description 11
- 238000000227 grinding Methods 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
- 230000008859 change Effects 0.000 description 9
- 239000010931 gold Substances 0.000 description 9
- 239000012299 nitrogen atmosphere Substances 0.000 description 9
- 229910052760 oxygen Inorganic materials 0.000 description 9
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- 239000012298 atmosphere Substances 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 239000010440 gypsum Substances 0.000 description 7
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- 239000000395 magnesium oxide Substances 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 238000001259 photo etching Methods 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 238000000151 deposition Methods 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
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- 239000004411 aluminium Substances 0.000 description 5
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- XQQWBPOEMYKKBY-UHFFFAOYSA-H trimagnesium;dicarbonate;dihydroxide Chemical compound [OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[O-]C([O-])=O.[O-]C([O-])=O XQQWBPOEMYKKBY-UHFFFAOYSA-H 0.000 description 5
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- 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
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- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
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- 208000037656 Respiratory Sounds Diseases 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
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- 229910052732 germanium Inorganic materials 0.000 description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 2
- 230000003760 hair shine Effects 0.000 description 2
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- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 229910001425 magnesium ion Inorganic materials 0.000 description 2
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- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 2
- 238000001451 molecular beam epitaxy Methods 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
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- 241000282994 Cervidae Species 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 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
- 238000001994 activation Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000004323 axial length Effects 0.000 description 1
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- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- 229910052731 fluorine Inorganic materials 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000010437 gem Substances 0.000 description 1
- 229910001751 gemstone Inorganic materials 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000001657 homoepitaxy Methods 0.000 description 1
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
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- 238000001746 injection moulding Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
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- 230000003287 optical effect Effects 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
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- 239000002994 raw material Substances 0.000 description 1
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- 102220043159 rs587780996 Human genes 0.000 description 1
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- 229910052717 sulfur Inorganic materials 0.000 description 1
- IEXRMSFAVATTJX-UHFFFAOYSA-N tetrachlorogermane Chemical compound Cl[Ge](Cl)(Cl)Cl IEXRMSFAVATTJX-UHFFFAOYSA-N 0.000 description 1
- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical compound CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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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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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
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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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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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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- 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
- 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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- 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
- 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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- 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
- 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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- 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
- 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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- 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
- 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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Abstract
作为本发明的一种实施方式的外延生长用取向氧化铝基板,其构成表面的晶体粒子的倾斜角为0.1°以上且小于1.0°,平均烧结粒径为10μm以上。这里,倾斜角是指X射线摆动曲线半高宽(XRC·FWHM)。平均烧结粒径是指:在对取向氧化铝基板的板面进行热蚀刻之后,利用由扫描电子显微镜拍摄到的图像进行测定所得的值。与以往相比,利用该外延生长用取向氧化铝基板制作的半导体器件的特性有所提高。
Description
技术领域
本发明涉及一种外延生长用取向氧化铝基板。
背景技术
作为发光二极管(LED)等发光元件或半导体器件用的外延生长用基板,使用蓝宝石(α-氧化铝单晶)基板,或者使用使GaN等的半导体层在蓝宝石基板上结晶生长而成的复合基板。具有在这样的外延生长用基板上按顺序依次层叠n型GaN层、多重量子阱层(MQW)以及p型GaN层而形成的结构的发光元件用基板实现了批量生产,其中,所述多重量子阱层是包括InGaN层的量子阱层与包括GaN层的势垒层交替层叠而成的。
然而,一般情况下,蓝宝石基板的面积小且价格昂贵。因此,本发明的发明人提出了使用取向氧化铝基板来代替蓝宝石基板的方案(参照专利文献1、2)。专利文献1中,利用MOCVD法在取向氧化铝基板上形成GaN晶种层,通过助熔剂法在该晶种层上形成GaN缓冲层,并在其上方形成发光功能层(按照n型GaN层c、多重量子阱层以及p型GaN层的顺序依次层叠而成的层)而制作发光元件用基板。在本说明书中,将这样在构成要素中包含取向氧化铝基板的类型的发光元件用基板称为元件用基板S1。另外,专利文献2中,利用MOCVD法在取向氧化铝基板上形成GaN晶种层,通过助熔剂法在该晶种层上形成Ge掺杂GaN层,然后通过基于砂轮的磨削加工而将取向氧化铝基板部除去,由此得到Ge掺杂GaN自立基板。然后,通过在该自立基板上形成发光功能层而制作发光元件用基板。在本说明书中,将这样包含半导体自立基板来代替取向氧化铝基板的类型的发光元件用基板称为元件用基板S2。
现有技术文献
专利文献
专利文献1:国际公开第2015/093335号小册子
专利文献2:日本专利第5770905号公报
发明内容
虽然使用这些元件用基板S1、S2制作的发光元件等半导体器件具有良好的特性,但期待进一步提高半导体器件的特性。
本发明是为了解决这样的课题而完成的,其主要目的在于使半导体器件的特性与以往相比进一步提高。
为了提高发光元件等半导体器件的特性,本发明的发明人进行了深入研究,结果发现:对于在制造半导体器件时所利用的外延生长用基板的构成表面的晶体粒子,通过将倾斜角设为0.1°以上且小于1.0°、并将平均烧结粒径设为10μm以上,使得半导体器件的特性显著提高,从而完成了本发明。
本发明的外延生长用取向氧化铝基板的构成表面的晶体粒子的倾斜角为0.1°以上且小于1.0°,平均烧结粒径为10μm以上。这里,倾斜角是指X射线摆动曲线半高宽(XRC·FWHM)。图1中示出了氧化铝晶体的倾斜角的示意性的说明图。平均烧结粒径是指:在对取向氧化铝基板的板面进行热蚀刻之后,利用由扫描电子显微镜拍摄到的图像进行测定所得的值。
如果利用本发明的外延生长用取向氧化铝基板制作上述的元件用基板S1、S2,并进一步利用这些元件用基板S1、S2制作半导体器件,则能得到与以往相比而特性有所提高的半导体器件。其理由尚不确定,但能推测出这是因为:构成发光功能层的半导体粒子略微倾斜而使得光提取效率等提高。此外,作为半导体器件,除了发光元件以外,可举出太阳能电池、功率器件等。在元件用基板S1、S2中,缓冲层或半导体层的形成方法并未特别限定,优选举例示出的MBE(分子束外延法)、HVPE(卤化物气相生长法)、溅射等气相法、Na助熔剂法、氨热法、水热法、溶胶-凝胶法等液相法、利用粉末的固相生长的粉末法、以及上述方法的组合。
本发明也可以如下理解为外延生长方法。即,也可以理解为:“使半导体晶体在构成表面的晶体粒子的倾斜角为0.1°以上且小于1.0°、平均烧结粒径为10μm以上的取向氧化铝基板的表面进行外延生长,由此形成薄膜的外延生长方法”。
附图说明
图1是氧化铝晶体的倾斜角的示意性的说明图。
图2是对层叠体1进行烧成而制作取向氧化铝基板7的工序的示意图。
图3是由发光元件用基板10制作发光元件30的工序的剖视图。
图4是由发光元件用基板20制作发光元件40的工序的剖视图。
图5是测定摆动曲线的说明图。
具体实施方式
[外延生长用取向氧化铝基板]
本发明的一个实施方式的外延生长用取向氧化铝基板是多晶氧化铝基板,构成表面的晶体粒子的倾斜角优选为0.1°以上且小于1.0°,平均烧结粒径优选为10μm以上。
当构成表面的晶体粒子的倾斜角小于0.1°时或达到1.0°以上时,最终得到的半导体器件的特性并未提高,因而并非为优选方式。其理由尚不明确,但能够想到这是因为:如果倾斜角小于0.1°,则外延生长时因取向氧化铝基板与外延生长膜的晶格失配而产生的晶格缺陷容易残留在外延生长膜中。另外,还能够想到这是因为:如果该倾斜角为1.0°以上,则来自外延生长膜的光提取效率等会降低。另外,能够想到:当将元件用基板S1用于发光元件时,取向氧化铝基板的光的透过性等也会降低。倾斜角的上限值优选小于1.0°,更优选为0.9°以下。倾斜角的下限值优选为0.1°以上,更优选为0.4°以上,进一步优选为0.6°以上,特别优选为0.8°以上。
只要平均烧结粒径为10μm以上就没有问题,但根据发光元件等的元件性能的观点,更优选为20μm以上。当平均烧结粒径小于10μm时,元件性能会降低,因而并非为优选方式。另一方面,如果平均烧结粒径过大,则强度降低,因而,根据操作性(handling)的观点,平均烧结粒径优选为300μm以下,更优选为150μm以下,进一步优选为100μm以下。平均烧结粒径的数值范围的上限和下限可以从这些数值中适当地选择并加以组合,但是,根据兼顾元件性能和操作性的观点,优选为10μm~300μm,更优选为20μm~150μm,进一步优选为20μm~100μm。
对于本实施方式的外延生长用取向氧化铝基板,通过Lotgering法求出的c面取向度优选为50%以上,更优选为70%以上,进一步优选为90%以上,特别优选为95%以上,最优选为100%。
优选地,本实施方式的外延生长用取向氧化铝基板的厚度为能独自立起的厚度,但是,若过厚,则根据制造成本的观点而并非为优选方式。因此,厚度优选为20μm以上,更优选为100μm以上,进一步优选为100~1000μm。另一方面,当使半导体晶体在该取向氧化铝基板生长时,因取向氧化铝基板与半导体晶体之间的热膨胀差所引起的应力而在基板整体产生翘曲,有时会对其后续的工序造成妨碍。作为抑制这样的翘曲的方法之一,可以使用较厚的取向氧化铝基板。
本实施方式的外延生长用取向氧化铝基板如果含有杂质,则在制作缓冲层、半导体层时,有时基板容易被侵蚀而断裂。特别是在Na、Mg、Si、P、Ca、Fe、Ti、Zn的含量多时,侵蚀较为明显,根据耐腐蚀性的观点,Na、Mg、Si、P、Ca、Fe、Ti、Zn各自的含量优选为1500ppm以下,更优选为1000ppm以下,更优选为500ppm以下,更优选为150ppm以下,更优选为100ppm以下,更优选为50ppm以下,更优选为10ppm以下,并不存在下限。另一方面,为了控制取向氧化铝基板的取向度、倾斜角、烧结粒径,有时加入MgO、SiO2、CaO等氧化物或氟化物作为烧结助剂。在控制烧结粒径的基础上,MgO抑制异常晶粒生长的效果也较高。特别是以高温进行烧成时,可以通过加入MgO而以良好的成品率制作不含有异常晶粒的取向氧化铝烧结体。因此,根据抑制异常晶粒生长的观点,优选含有15ppm以上的Mg(优选30ppm以上,更优选50ppm以上,进一步优选100ppm以上)。因此,作为兼顾耐腐蚀性和制造时的成品率的Mg的含量,优选为15~1500ppm,更优选为15~1000ppm,进一步优选为15~500ppm,特别优选为30~150ppm。
[外延生长用取向氧化铝基板的制法]
本实施方式的外延生长用取向氧化铝基板的制法并未特别限定,作为优选的制法,可举出包含(a)制作层叠体的工序、以及(b)对层叠体进行烧成的工序的制法,上述层叠体是微细氧化铝粉末层、与板状氧化铝粒子的板面以沿着微细氧化铝粉末层的表面的方式排列而成的板状氧化铝粉末层交替层叠而成的。
工序(a)中使用的微细氧化铝粉末层是微细氧化铝粒子的集合体的层。微细氧化铝粉末是平均粒径比板状氧化铝粉末的平均粒径小的粉末。微细氧化铝粉末层可以是对微细氧化铝粉末本身进行成型而成的层,也可以是对微细氧化铝粉末中加入有添加剂的物质进行成型而成的层。作为添加剂,例如可举出烧结助剂、石墨、粘合剂、增塑剂、分散剂、分散介质等。成型方法并未特别限定,例如可举出带成型、挤出成型、浇铸成型、注塑成型、单轴加压成型等。微细氧化铝粉末层的厚度优选为5~100μm,更优选为10~100μm,进一步优选为20~60μm。
工序(a)中使用的板状氧化铝粉末层为板状氧化铝粒子的集合体的层。根据高取向化、低倾斜化的观点,优选板状氧化铝粉末的长径比较大,从而优选为3以上,更优选为10以上,进一步优选为30以上。长径比为平均粒径/平均厚度。这里,平均粒径为粒子板面的长轴长度的平均值,平均厚度为粒子的短轴长度的平均值。利用扫描式电子显微镜(SEM)观察板状氧化铝粉末中任意的100个粒子而确定上述这些值。根据取向烧结体的高取向化、低倾斜化的观点,优选板状氧化铝粉末的平均粒径较大,从而优选为1.5μm以上,更优选为5μm以上,进一步优选为10μm以上,特别优选为15μm以上。但是,根据致密化的观点,优选板状氧化铝粉末的平均粒径较小,从而优选为30μm以下。因此,为了兼顾高取向和致密化,平均粒径优选为1.5~30μm。另外,根据高取向化、低倾斜化的观点,优选板状氧化铝粉末的平均厚度比微细氧化铝粉末的平均厚度厚。板状氧化铝粉末层可以是板状氧化铝粉末本身的层,也可以是在板状氧化铝粉末中加入有添加剂的物质的层。作为添加剂,例如可举出烧结助剂、石墨、粘合剂、增塑剂、分散剂、分散介质等。对于板状氧化铝粉末层,构成板状氧化铝粉末的板状氧化铝粒子的板面以沿着微细氧化铝粉末层的表面的方式排列。优选板状氧化铝粉末为单一粒子。在并非单一粒子的情况下,有时会使得取向度、倾斜角变差,根据低倾斜化的观点,这一点非常重要。为了使粒子变得单一,只要采用分级处理、碎解处理以及淘析处理中的至少1种处理即可,优选采用所有处理。优选在出现凝聚等时采用分级处理、碎解处理。作为分级处理,可举出气流分级等。作为碎解处理,可举出罐式碎解、湿式微粒化方式等。优选在混入有微粒粉时采用淘析处理。
通过工序(a)制作的层叠体是微细氧化铝粉末层与板状氧化铝粉末层交替层叠而成的。根据低倾斜化的观点,在制作层叠体时,优选地,制作利用板状氧化铝粉末层将微细氧化铝粉末的成型体的单面的整个面或一部分覆盖而成的单面加工体,并利用该单面加工体制作层叠体。或者,优选地,制作利用板状氧化铝粉末层将微细氧化铝粉末的成型体的双面的整个面或一部分覆盖而成的双面加工体,并利用该双面加工体和未加工的成型体制作层叠体。
可以在微细氧化铝粉末的成型体的单面或双面对与该成型体相比而厚度较薄的板状氧化铝粉末的成型体进行层叠,由此制作单面加工体或双面加工体。在该情况下,板状氧化铝粉末的成型体可以使用以沿着该成型体的表面的方式通过带成型或印刷等对板状氧化铝粒子的板面施加剪切力而成型的成型体。或者,可以通过在微细氧化铝粉末的成型体的单面或双面对板状氧化铝粉末的分散液进行印刷、喷涂、旋涂或浸涂而制作单面加工体或双面加工体。在喷涂、旋涂、浸涂中,即使不强制性地施加剪切力,板状氧化铝粒子的板面也以沿着其成型体的表面的方式排列。对于在成型体的表面排列的板状氧化铝粒子而言,几个板状氧化铝粒子可以重叠,但优选不与其它板状氧化铝粒子重叠。
在利用单面加工体时,只要以使得微细氧化铝粉末层与板状氧化铝粉末层交替层叠的方式对单面加工体进行层叠即可。在利用双面加工体时,只要使双面加工体与未加工的微细氧化铝粉末的成型体交替层叠即可。此外,可以利用单面加工体和双面加工体的双方来制作层叠体,也可以利用单面加工体、双面加工体以及未加工的成型体来制作层叠体。
工序(b)中,对层叠体进行烧成。在该情况下,烧成方法并未特别限定,优选对层叠体进行加压烧成。作为加压烧成,例如可举出热压烧成、HIP烧成等。此外,可以在加压烧成前进行常压预烧成。在进行HIP烧成时,还可以使用胶囊法。热压烧成时的压力优选为50kgf/cm2以上,更优选为200kgf/cm2以上。HIP烧成时的压力优选为1000kgf/cm2以上,更优选为2000kgf/cm2以上。烧成气氛并未特别限定,优选大气、氮、Ar等惰性气体、真空气氛下的任一种,特别优选处于氮、Ar气氛下,最优选氮气气氛。优选烧成温度(最高到达温度)在不产生异常晶粒生长或熔融的范围内较高,从而优选为1700~2050℃,更优选为1800~2000℃,进一步优选为1900~2000℃。图2是对层叠体1进行烧成而制作取向氧化铝基板7的工序的示意图。如图2所示,层叠体1是作为微细氧化铝粒子3a的集合体的层的微细氧化铝粉末层3、与板状氧化铝粒子5a的板面沿微细氧化铝粉末层3的表面排列而成的板状氧化铝粉末层5交替层叠而成的。如果对层叠体1进行烧成,则板状氧化铝粒子5a成为晶种(模板,template),微细氧化铝粒子3a成为基质(matrix),模板一边引入基质一边进行同质外延生长。因此,得到的烧结体成为取向度较高、且倾斜角较小的取向氧化铝基板7。除了取决于板状氧化铝粉末的粒径、长径比、板状氧化铝粉末的厚度与微细氧化铝粉末的粒径差、板状氧化铝粒子的凝聚状态、板状氧化铝粉末层中的板状氧化铝粒子的重叠状态、烧成条件以外,取向度和倾斜角还取决于板状氧化铝粉末将微细氧化铝粉末层的表面覆盖的覆盖率。可以通过适当地控制这些因素而得到取向度较高、倾斜角为0.1以上且小于1°的取向氧化铝基板。当该覆盖率为1~60%(优选为1~20%,更优选为3~20%)时,取向度升高,倾斜角减小。另外,对于取向度和倾斜角而言,当微细氧化铝粉末层的厚度为5~100μm(优选为10~100μm,更优选为20~60μm)时,取向度升高,倾斜角减小。这里,取向度是指:使用X射线衍射图谱并通过Lotgering法而求出的c面取向度。
[元件用基板S1以及使用该元件用基板S1的发光元件30]
元件用基板S1是构成要素中包含取向氧化铝基板的类型的发光元件用基板。图3的上段是作为元件用基板S1的一个例子的发光元件用基板10的剖视图。发光元件用基板10在形成于取向氧化铝基板12上的缓冲层16上形成有发光功能层14。发光功能层14是自缓冲层16侧开始层叠有n型层14c、活性层14b以及p型层14a的复合层。构成发光功能层14的各层由以半导体材料为主成分的材料构成。作为半导体材料,可举出GaN系材料、ZnO系材料以及AlN系材料等,其中,优选为GaN系材料。n型层14c在半导体材料中掺杂有n型掺杂剂,p型层14a在半导体材料中掺杂有p型掺杂剂。活性层14b是量子阱层与势垒层交替层叠而成的多重量子阱层,当使用GaN材料作为半导体材料时,可以将量子阱层设为InGaN层、且将势垒层设为GaN层。缓冲层16是用于减少因取向氧化铝基板12与发光功能层14的晶格失配所致的晶格缺陷而改善结晶性的层。优选地,缓冲层16是与发光功能层14的晶体结构相同或类似的、具有高结晶性的晶体结构,可以使用晶格常数相同或相近的晶体结构。缓冲层16具有模仿取向氧化铝基板12的结晶方位生长而成的结构。优选缓冲层16由以上述半导体材料为主成分的材料构成,也可以适当地含有用于控制成p型或n型的掺杂剂。
例如可以以如下方式制造发光元件用基板10。即,通过使GaN等半导体的晶体在取向氧化铝基板12上进行外延生长而形成半导体层(缓冲层16)。在该情况下,可以使半导体的晶体在取向氧化铝基板12上进行外延生长而形成半导体薄膜(晶种层),进一步使相同的半导体的晶体在该半导体薄膜上进行外延生长而形成比半导体薄膜厚的膜,并将这两个膜作为半导体层。此外,可以以气相、液相、固相中的任一方式进行外延生长。接下来,在缓冲层16上按照n型层14c、活性层14b以及p型层14a的顺序依次对它们进行层叠而形成发光功能层14。由此,得到发光元件用基板10。
可以以如下方式制造利用了发光元件用基板10的发光元件30。图3是制作发光元件30的工序的剖视图。首先,在发光元件用基板10的发光功能层14侧使n型层14c的一部分露出。接着,在n型层14c的露出的部分形成阴极电极17。另一方面,在p型层14a的上表面形成透光性阳极电极18,并进一步在其上方形成阳极电极焊盘19。最后,将电极形成后的发光元件用基板10切断而实现芯片化,并将其安装于引线框(lead frame)而得到横型结构的发光元件30。
此外,也可以利用发光元件用基板10而制作纵型结构的发光元件。例如,可以通过如下方式来制作:在发光元件用基板10的p型层14a的上表面形成阳极电极,使阳极电极与安装基板接合,通过激光剥离法将取向氧化铝基板12除去,并在露出的n型层14c的表面形成阴极电极。当通过激光剥离法将取向氧化铝基板12除去时,可以将缓冲层16也一并除去。
[元件用基板S2和使用该元件用基板S2的发光元件40]
元件用基板S2是构成要素中包含半导体自立基板以代替元件用基板S1的取向氧化铝基板的类型的发光元件用基板。图4的上段是作为元件用基板S2的一个例子的发光元件用基板20的剖视图。发光元件用基板20在半导体自立基板22上形成有发光功能层24。发光功能层24是层叠有n型层24c、活性层24b以及p型层24a的复合层,但基本上与上述的发光功能层14相同,因此省略其说明。图4中的半导体自立基板22是掺杂有n型掺杂剂的半导体材料,但也可以为非掺杂的半导体材料。由通过n型掺杂剂的导入而具有导电性的氮化镓制成基板,由此能够实现纵型结构的发光元件。
例如可以以如下方式制造发光元件用基板20。即,通过使GaN等半导体的晶体在取向氧化铝基板上进行外延生长而形成半导体层。在该情况下,可以使半导体的晶体在取向氧化铝基板上进行外延生长而形成半导体薄膜(晶种层),进一步使相同的半导体的晶体在该半导体薄膜上进行外延生长而形成比半导体薄膜厚的膜,并将这两个膜作为半导体层。此外,可以以气相、液相、固相中的任一方式而进行外延生长。接下来,通过磨削加工等方法将取向氧化铝基板除去,由此得到半导体层的单体、即半导体自立基板22。在该半导体自立基板22上按照n型层24c、活性层24b以及p型层24a的顺序依次对它们进行层叠而形成发光功能层24。由此,得到发光元件用基板20。
利用发光元件用基板20的发光元件40可以通过如下方式制造。图4是制作发光元件40的工序的剖视图。首先,在发光元件用基板20的半导体自立基板22侧形成阴极电极27。另一方面,在p型层24a的上表面形成透光性阳极电极28,进一步在其上方形成阳极电极焊盘29。最后,将电极形成后的发光元件用基板20切断而实现芯片化,并将其安装于引线框,由此得到纵型结构的发光元件40。
此外,本发明未受到上述实施方式的任何限定,只要属于本发明的技术范围,当然可以以各种方式而实施。
【实施例】
以下说明的实验例A1~A6为外延取向氧化铝基板的制作例,实验例B1~B6为元件用基板S1和使用该元件用基板S1的发光元件的制作例,实验例C1~C6为元件用基板S2和使用该元件用基板S2的发光元件的制作例。
[实验例A1]
(1)取向氧化铝基板的制作
(1a)层叠体的制作
相对于微细氧化铝粉末(大明化学工业株式会社制,等级为TM-DAR)的100质量份,加入0.0125质量份(125质量ppm)的氧化镁(500A,宇部Material制)、7.8质量份的作为粘合剂的聚乙烯醇缩丁醛(型号为BM-2,积水化学工业制)、3.9质量份的作为增塑剂的邻苯二甲酸二(2-乙基己基)酯(黑金化成制)、2质量份的作为分散剂的失水山梨糖醇三油酸酯(RHEODOL SP-O30,花王制)、以及作为分散介质的2-乙基己醇进行混合。分散介质的量调整成使得浆料粘度达到20000cP。通过刮刀法(doctor brade method)使这样制备的浆料在PET膜上成型为片状,并使其干燥后的厚度达到40μm,由此制成微细氧化铝粉末层。
对于市场贩卖的板状氧化铝粉末(KINSEI MATEC制,等级为YFA10030),利用气流分级机(日清工程制的TC-15N)将切割点设定为3μm而进行分级,接下来,利用罐式碎解机并借助φ0.3mm的球石进行20小时的碎解,最后通过淘析而将微粒粉末除去。相对于得到的板状氧化铝粉末的100质量份,加入500质量份的作为分散介质的异丙醇。利用超声波分散机对得到的分散液(板状氧化铝浆料)进行5分钟的分散,然后,利用喷枪(TAMIYA制的Spray-Work HG Airbrush Wide)以0.2MPa的喷雾压力、20cm的喷射距离对上述微细氧化铝粉末层的单面进行喷雾,由此得到单面加工体。此时,板状氧化铝粉末将微细氧化铝粉末层的表面覆盖的覆盖率为1%。此外,以如下方式对单面加工体的覆盖率进行计算。即,利用光学显微镜观察微细氧化铝粉末层表面,通过图像处理将该观察照片分割为板状氧化铝粉末的部分和除此以外的部分,并将观察照片中的板状氧化铝粉末的面积相对于微细氧化铝粉末层表面的面积的比例设为覆盖率。
将得到的单面加工体切断成直径为50mm的圆形,然后,使其从PET膜剥离,以不使喷雾后的加工面重叠的方式层叠65层,并将其载置于厚度为10mm的Al板的上方,然后,装入袋中并将内部抽成真空而制成真空包装。在85℃的温水中以100kgf/cm2的压力对该真空包装进行静水压力加压,由此得到层叠体。
(1b)层叠体的烧成
将得到的层叠体配置于脱脂炉中,以600℃、10小时的条件进行了脱脂。使用石墨制的模具,通过热压的方式在氮中以1975℃的烧成温度(最高到达温度)、4小时、200kgf/cm2的表面压力的条件对得到的脱脂体进行烧成,由此得到氧化铝烧结体。此外,当从烧成温度开始降温时,直至1200℃为止而维持加压压力,在小于1200℃的温度区域将加压压力释放为零。
(1c)取向氧化铝基板的制作
将这样得到的烧结体固定于陶瓷平板(surface plate),使用磨石磨削至#2000而使板面变得平坦。接着,通过使用金刚石研磨粒子的研磨加工,使板面实现平滑化,作为取向氧化铝基板而得到直径为50mm、厚度为0.5mm的取向氧化铝烧结体。使得研磨粒子的尺寸从3μm阶梯式地减小到0.5μm,并提高了平坦性。加工后的平均粗糙度Ra为4nm。
(2)取向氧化铝基板的特性
(2a)c面取向度
为了确认得到的取向氧化铝基板的取向度,以与取向氧化铝基板的上表面平行的方式进行研磨加工,然后,对其研磨面照射X射线而测定c面取向度。使用XRD装置(理学制,RINT-TTR III),在2θ=20~70°的范围内对XRD图谱进行了测定。具体而言,使用CuKα射线以50kV的电压、300mA的电流的条件进行了测定。通过Lotgering法对c面取向度进行了计算。具体而言,通过下式进行了计算。式中,P是根据取向氧化铝基板的XRD而得到的值,P0是根据标准α-氧化铝(JCPDS Cards No.46-1212)而计算出的值。实验例1的取向氧化铝基板的c面取向度为100%。
[数学式1]
(Io(h k l)、Is(h k l)分别为ICDD No.461212以及试样中的(h k l)面的衍射强度的积分值(2θ=20~70°))
(2b)倾斜角
倾斜角是结晶轴的斜率分布,且是对氧化铝的结晶方位相对于c轴以何种程度的频率倾斜进行评价的参数。这里,由X射线摆动曲线半高宽(XRC·FWHM)来表示倾斜角。对于XRC·FWHM,像图5那样使X射线源与检测器联动而对取向氧化铝基板的板面(与c面取向度的测定相同的面)进行扫描,并对所得到的曲线的半高宽进行了测定。将这样使得2θ(检测器与入射X射线所成的角度)的值固定为其衍射峰值位置、且仅对ω(试样基板面与入射X射线所成的角度)进行扫描的测定方法称为摆动曲线测定。对于装置,使用理学制的RINT-TTRIII,利用CuKα射线以50kV的电压、300mA的电流的条件而使得ω的扫描范围变为3.8°~38.8°。实验例1的取向氧化铝基板的XRC·FWHM为0.9°。
(2c)取向氧化铝基板的粒径评价
对于取向氧化铝基板的烧结体粒子,通过以下方法对板面的平均烧结粒径进行了测定。对得到的取向氧化铝基板以1550℃的温度进行了45分钟的热蚀刻,然后,利用扫描电子显微镜拍摄了图像。在对得到的图像的对角线引出直线的情况下,使得引出的任意直线均穿过10个~30个粒子,将可引出上述直线的范围作为视野范围。对得到的图像的对角线引出的2条直线中,对于直线所穿过的全部粒子而求出各粒子的内侧的线段的长度的平均值,并将该平均值乘以1.5而得的值设为板面的平均烧结粒径。其结果,板面的平均烧结粒径为66μm。
(2d)取向氧化铝基板的杂质量
利用纯度为99.9质量%的氧化铝研钵将氧化铝烧结体粉碎,然后,通过下述方法进行了定量分析。然后,求出氧化铝烧结体中的Na、Mg、Si、P、Ca、Fe、Ti、Zn的质量比例(ppm)。实验例1的氧化铝烧结体中除了Mg以外的杂质元素均为检测边界值以下,并且检测出了62ppm的Mg。
杂质定量方法:通过基于JISR1649的加压硫酸分解法而将板状氧化铝粉末溶解,使用ICP(感应耦合等离子体)发光分析装置(日立高新技术制的PS3520UV-DD)进行了分析。
表1中对实验例A1的烧成方法、烧成温度以及取向氧化铝基板的特性进行了总结。
[表1]
[实验例A2]
在实验例A1中,作为板状氧化铝粉末,使用本公司制的板状氧化铝粉末,除此以外,与实验例A1同样地制作了取向氧化铝基板,并对其特性进行了测定。表1中示出了取向氧化铝基板的特性。
以如下方式制作本公司制的板状氧化铝粉末。对于96质量份的高纯度γ-氧化铝(TM-300D,大明化学制)、4质量份的高纯度AlF3(关东化学制,鹿特级)、以及0.17质量份的作为晶种的高纯度α-氧化铝(TM-DAR,大明化学制,D50=1μm),利用罐式磨料机(pot mill)并借助φ2mm的氧化铝球(alumina ball)以IPA(异丙醇)为溶剂而进行了5小时的混合。得到的混合粉末中除了F、H、C、S以外的杂质元素的质量比例的合计值为1000ppm以下。将得到的300g的混合原料粉末装入纯度为99.5质量%的高纯度氧化铝制的烧盆(容积为750cm3),并盖上纯度为99.5质量%的高纯度氧化铝制的盖,由此在电炉内的气流中以900℃的温度进行了3小时的热处理。空气的流量设为25000cc/min。在大气中以1150℃的温度对热处理后的粉末进行了40小时的退火处理,然后,利用φ2mm的氧化铝球进行了4小时的粉碎,由此得到平均粒径为2μm、平均厚度为0.2μm、长径比为10的板状氧化铝粉末。利用扫描式电子显微镜(SEM)观察了板状氧化铝粉末中任意的100个粒子,由此确定粒子的平均粒径、平均厚度。平均粒径是粒子的长轴长的平均值,平均厚度是粒子的短轴长的平均值,长径比是平均粒径/平均厚度。所得到的板状氧化铝粉末为α-氧化铝。
[实验例A3]
在实验例A3中,除了将烧成温度设为1900℃以外,与实验例A1同样地制作取向氧化铝基板,并对其特性进行了测定。表1中示出了取向氧化铝基板的特性。
[实验例A4]
相对于微细氧化铝粉末(大明化学工业株式会社制,等级为TM-DAR)的100质量份,加入0.0125质量份(125质量ppm)的氧化镁(500A,宇部Material制)、7.8质量份的作为粘合剂的聚乙烯醇缩丁醛(型号为BM-2,积水化学工业制)、3.9质量份的作为增塑剂的邻苯二甲酸二(2-乙基己基)酯(黑金化成制)、2质量份的作为分散剂的失水山梨糖醇三油酸酯(RHEODOL SP-O30,花王制)、以及作为分散介质的2-乙基己醇进行了混合。分散介质的量调整成使得浆料粘度达到20000cP。通过刮刀法使这样制备的浆料在PET膜上成型为片状,且使得干燥后的厚度达到40μm,由此制成微细氧化铝粉末层。
相对于市场贩卖的板状氧化铝粉末(KINSEI MATEC制,等级为YFA10030),KINSEIMATEC制)的100质量份,加入50质量份的作为粘合剂的聚乙烯醇缩丁醛(型号为BM-2,积水化学工业制)、25质量份的作为增塑剂的邻苯二甲酸二(2-乙基己基)酯(黑金化成制)、2质量份的作为分散剂的失水山梨糖醇三油酸酯(RHEODOL SP-O30,花王制)、以及作为分散介质的二甲苯和1-丁醇的混合熔液(混合比率1:1)而进行了混合。分散介质的量调整成使得浆料粘度达到5000cP。通过反向刮刀法使这样制备的浆料在PET膜上成型为片状,且使得干燥后的厚度达到3μm,由此制成板状氧化铝粉末层。
将微细氧化铝粉末层和板状氧化铝粉末层分别切断成直径为50mm的圆形,然后,使它们从PET膜剥离,使50层的微细氧化铝粉末层和50层的板状氧化铝粉末层交替层叠并将它们载置于厚度为10mm的Al板上,然后,将它们装入袋中且将内部抽成真空而制成真空包装。在85℃的温水中以100kgf/cm2的压力对该真空包装进行静水压力加压,由此得到层叠体。此时,板状氧化铝粉末层将微细氧化铝粉末层的表面覆盖的覆盖率为60%。
通过与实验例A1相同的方法对得到的层叠体进行脱脂、烧成、加工而制作取向氧化铝基板,并对其特性进行了测定。表1中示出了取向氧化铝基板的特性。
[实验例A5]
对99.8质量份的微细氧化铝粉末(大明化学工业株式会社制,等级为TM-DAR)、0.2质量份的氧化钇粉末(信越化学工业株式会社制,等级为UU)进行混合,相对于100g的混合粉末以50cc的比例添加作为溶剂的水,利用球磨机(ball mill)进行了40小时的混合粉碎而实现了浆料化。将得到的浆料注入至内径为50mm的石膏模具,并在12T的磁场中载置3小时而进行了浇铸成型。使成型体从石膏中脱模,在室温下进行干燥之后,使用石墨制的模具,通过热压的方式在氮中以1400℃、4小时、200kgf/cm2的表面压力的条件进行了烧成。与实验例A1同样地对得到的烧结体进行加工而制作取向氧化铝基板,并对其特性进行了测定。表1中示出了取向氧化铝基板的特性。
[实验例A6]
对于市场贩卖的板状氧化铝粉末(KINSEI MATEC制,等级为YFA10030),利用气流分级机(日清工程制的TC-15N)将切割点设定为3μm而进行了分级,接下来,利用罐式碎解机且借助φ0.3mm的球石进行了20小时的碎解,最后通过淘析而将微粒粉末除去。对得到的0.5质量份的板状氧化铝粉末与99.5质量份的微细氧化铝粉末(大明化学工业株式会社制,等级为TM-DAR)进行了混合。进一步相对于混合粉末的100质量份而混合了0.0125质量份(125质量ppm)的氧化镁(500A,宇部Material制),由此得到调配粉末。相对于调配粉末的100g以50cc的比例添加作为溶剂的水,并利用球磨机进行40小时的混合粉碎而使其实现浆料化。将得到的浆料注入至内径为50mm的石膏模具中,并在12T的磁场中载置3小时而进行了浇铸成型。使成型体从石膏中脱模,在室温下进行干燥之后,使用石墨制的模具,通过热压的方式在氮中以1975℃、4小时、200kgf/cm2的表面压力的条件进行了烧成。与实验例A1同样地对得到的烧结体进行加工而制作取向氧化铝基板,并对其特性进行了测定。表1中示出了取向氧化铝基板的特性。
[实验例A7]
相对于微细氧化铝粉末(住友化学制,等级AKP-3000)的100质量份而混合了0.0125质量份(125质量ppm)的氧化镁(500A,宇部Material制),相对于100g的混合粉末以50cc的比例而添加了作为溶剂的水,并利用球磨机进行40小时的混合粉碎而实现了浆料化。将得到的浆料注入至内径为50mm的石膏模具中,并在10T的磁场中载置3小时而进行了浇铸成型。使得成型体从石膏中脱模,在室温下进行干燥之后,使用石墨制的模具,通过热压的方式在氮中以1975℃、4小时、200kgf/cm2的表面压力的条件进行了烧成。与实验例A1同样地对得到的烧结体进行加工而制作取向氧化铝基板,并对其特性进行了测定。表1中示出了取向氧化铝基板的特性。
[实验例A8]
将浆料注入到内径为50mm的石膏模具中,除了在12T的磁场中载置8小时而进行浇铸成型以外,与实验例A7同样地制作了氧化铝烧结体。与实验例A1同样地对得到的烧结体进行加工而制作取向氧化铝基板,并对其特性进行了测定。表1中示出了取向氧化铝基板的特性。
[实验例A9]
在实验例A1中,除了以如下方式对单面加工体的制作方法进行变更以外,与实验例A4同样地制作了氧化铝烧结体。
在实验例A9中,以如下方式制作单面加工体。对于市场贩卖的板状氧化铝粉末(KINSEI MATEC制,等级为YFA10030),利用气流分级机(日清工程制TC-15N)将切割点设定为3μm而进行了分级,接下来,利用罐式碎解机且借助φ0.3mm的球石进行了20小时的碎解,最后通过淘析将微粒粉末除去。相对于得到的板状氧化铝粉末的100质量份,加入100质量份的作为粘合剂的聚乙烯醇缩丁醛(型号为BLS,积水化学工业制)和3500质量份的作为分散剂的松油醇而进行了混合,由此得到印刷浆糊。利用带有乳剂的制版(ST640网,乳剂厚度:5μm)将该印刷浆糊印刷于微细氧化铝粉末层的单面而得到单面加工体。此时的板状氧化铝粉末层的厚度为0.5μm。与实验例A1同样地对得到的烧结体进行加工而制作取向氧化铝基板,并对其特性进行了测定。表1中示出了取向氧化铝基板的特性。
[实验例B1]
(1)发光元件用基板(元件用基板S1)的制作
(1a)晶种层的成膜
利用MOCVD法在实验例A1中制作的取向氧化铝基板的上方形成晶种层。具体而言,在530℃的温度下堆积40nm的低温GaN层,然后,以1050℃的温度对厚度为3μm的GaN膜进行层叠而得到晶种基板。
(1b)基于Na助熔剂法的GaN缓冲层的成膜
将通过上述工序制作的晶种基板设置于内径为80mm、高度为45mm的圆筒平底的氧化铝坩埚的底部,接下来,在杂物箱(glove box)内将熔液组合物填充到坩埚内。熔液组合物的组成如下。
·金属Ga:60g
·金属Na:60g
将该氧化铝坩埚放入耐热金属制的容器进行密闭,然后,将其设置于晶体培育炉的能够旋转的工作台上。在氮气气氛中升温加压至870℃、4.0MPa,然后保持10小时、且使熔液旋转,由此一边搅拌、一边使氮化镓晶体生长为缓冲层。在结晶生长结束之后,花费3小时逐渐冷却至室温,并从晶体培育炉中将培育容器取出。使用乙醇将残留于坩埚内的熔液组合物除去,并对氮化镓晶体生长后的试样进行了回收。对于得到的试样而言,氮化镓晶体在50mm的晶种基板的整个面上生长,晶体的厚度约为0.1mm。并未确认到裂纹。
将这样得到的取向氧化铝基板上的氮化镓晶体连同基板一起固定于陶瓷平板,利用#600和#2000的磨石对氮化镓晶体的板面进行磨削而使板面变得平坦。接着,通过使用金刚石研磨粒子的研磨加工,使氮化镓晶体的板面实现了平滑化。此时,使得研磨粒子的尺寸从3μm阶梯式地减小到0.1μm,并提高了平坦性。氮化镓晶体板面的加工后的平均粗糙度Ra为0.2nm。这样,得到在取向氧化铝基板上形成有厚度约为50μm的氮化镓晶体层的基板。此外,虽然在本例中为了提高后述的发光功能层的结晶性而形成这样的氮化镓缓冲层,但也可以根据目标特性或用途而将缓冲层本身省略。另外,也可以形成为在氮化镓缓冲层中掺杂有锗、硅、氧等而具有导电性的结构。
(1c)基于MOCVD法的发光功能层的成膜
使用MOCVD法,作为n型层,在基板上以1050℃的温度堆积3μm的n-GaN层,该n-GaN层掺杂成使得Si原子浓度达到5×1018/cm3。接下来,作为活性层,以750℃的温度而堆积多重量子阱层。具体而言,对5层由InGaN构成的2.5nm的阱层、6层由GaN构成的10nm的势垒层交替地进行层叠。接下来,作为p型层,以950℃的温度堆积200nm的p-GaN,上述p-GaN掺杂成使得Mg原子浓度达到1×1019/cm3。然后,将其从MOCVD装置中取出,作为p型层的Mg离子的活化处理,在氮气气氛中进行10分钟的800℃的热处理,由此得到发光元件用基板。
(2)横型发光元件的制作
在已制作的发光元件用基板的发光功能层侧,利用光刻工艺和RIE法,使n型层的一部分露出。继而,利用光刻工艺和真空蒸镀法,在n型层的露出部分分别以15nm、70nm、12nm、60nm的厚度使作为阴极电极的Ti/Al/Ni/Au膜形成图案。然后,为了使欧姆接触特性变得良好,在氮气气氛中进行30秒的700℃的热处理。进而,利用光刻工艺和真空蒸镀法,在p型层分别以6nm、12nm的厚度使作为透光性阳极电极的Ni/Au膜形成图案。然后,为了使欧姆接触特性变得良好,在氮气气氛中进行30秒的500℃的热处理。进而,利用光刻工艺和真空蒸镀法,在作为透光性阳极电极的Ni/Au膜的上表面的一部分区域分别以5nm、60nm的厚度使作为阳极电极焊盘的Ni/Au膜形成图案。将这样得到的晶片切断而实现芯片化,并进一步将其安装于引线框而得到横型结构的发光元件。
[实验例B2~B9]
使用实验例A2~A9的取向氧化铝基板,通过与实验例B1相同的方法制作了发光元件用基板。另外,通过与实验例B1相同的方法制作了横型结构的发光元件。
[发光元件的评价]
针对实验例B1~B9中制作的横型发光元件,对阴极电极与阳极电极之间通电而进行I-V测定,其结果,对于任何试样都确认到整流性。另外,流过使正向电流流通,均确认到波长为450nm的光。对于发光亮度,实验例B1、B2、B9的元件明显为高亮度。使用实验例B3、B7的基板的元件也为高亮度,但与实验例B1、B2、B9相比而亮度略低。使用实验例B8的基板的元件也为高亮度,但与实验例B3、B7相比略低。实验例B4的元件与实验例B8相比而亮度大幅降低。实验例B5、B6的元件与实验例B4相比而亮度进一步降低。
[实验例C1]
(1)发光元件用基板(元件用基板S2)的制作
(1a)晶种层的成膜
利用MOCVD法在实验例A1中制作的取向氧化铝基板的上方形成晶种层。具体而言,作为缓冲层,以530℃的衬托器(susceptor)温度在氢气气氛中堆积30nm的低温GaN层,然后,在氮气、氢气气氛中升温至1050℃的衬托器温度而对厚度为3μm的GaN膜进行层叠,由此得到晶种基板。
(1b)基于Na助熔剂法的Ge掺杂GaN层的成膜
将通过上述工序制作的晶种基板设置于内径为80mm、高度为45mm的圆筒平底的氧化铝坩埚的底部,接下来,在杂物箱内将熔液组合物填充到坩埚内。熔液组合物的组成如下。
·金属Ga:60g
·金属Na:60g
·四氯化锗:1.85g
在将该氧化铝坩埚放入耐热金属制的容器中进行密闭之后,将其设置于晶体培育炉的能够旋转的工作台上。在氮气气氛中升温加压至870℃、3.5MPa,然后保持100小时、并使熔液旋转,由此一边进行搅拌、一边使氮化镓晶体生长。在结晶生长结束后,花费3小时而逐渐冷却至室温,并从晶体培育炉中取出培育容器。使用乙醇而将残留于坩埚内的熔液组合物除去,并对氮化镓晶体生长后的试样进行了回收。在得到的试样中,Ge掺杂氮化镓晶体在50mm的晶种基板的整个面上生长,晶体的厚度约为1.4mm。并未确认到裂纹。通过基于磨石的磨削加工而将这样得到的试样的取向氧化铝基板部除去,由此得到Ge掺杂氮化镓的单体。对该Ge掺杂氮化镓晶体的板面进行研磨而使板面变得平坦。进而,利用研磨加工和CMP使板面实现平滑化,由此作为发光元件用基板而得到厚度约为500μm的Ge掺杂多晶氮化镓自立基板。多晶氮化镓自立基板面的加工后的平均粗糙度Ra为0.2nm。
此外,虽然在本例中掺杂锗而制作n型半导体,但也可以根据用途、结构而掺杂不同的元素或者不掺杂元素。
(2)发光元件的制作
利用MOCVD法,在实验例C1中制作的各Ge掺杂多晶氮化镓自立基板上以1050℃的温度堆积1μm的n-GaN层作为n型层,该n-GaN层掺杂成Si原子浓度为5×1018/cm3。接下来,作为发光层,以750℃的温度而堆积多重量子阱层。具体而言,对5层由InGaN构成的2.5nm的阱层、以及6层由GaN构成的10nm的势垒层交替地进行层叠。接下来,作为p型层,以950℃的温度堆积200nm的p-GaN,该p-GaN掺杂成Mg原子浓度为1×1019/cm3。然后,将其从MOCVD装置中取出,进行p型层的Mg离子的活化处理,并在氮气气氛中以800℃的温度进行10分钟的热处理。
接下来,利用光刻和真空蒸镀法,在多晶氮化镓自立基板的相对于n-GaN层以及p-GaN层的相反侧的面,分别以15nm、70nm、12nm、60nm的厚度使作为阴极电极的Ti/Al/Ni/Au膜形成图案。然后,为了使欧姆接触特性变得良好,在氮气气氛中以700℃的温度进行30秒的热处理。进而,利用光刻和真空蒸镀法,在p型层分别以6nm、12nm的厚度使作为透光性阳极电极的Ni/Au膜形成图案。然后,为了得到良好的欧姆接触特性,在氮气气氛中以500℃的温度进行30秒的热处理。进而,利用光刻和真空蒸镀法,在作为透光性阳极电极的Ni/Au膜的上表面的一部分区域分别以5nm、60nm的厚度使作为阳极电极焊盘的Ni/Au膜形成图案。将这样得到的晶片切断而实现芯片化,并将其进一步安装于引线框,由此得到纵型结构的发光元件。
[实验例C2~C9]
在实验例C2~C9中,使用实验例A2~A9的取向氧化铝基板,并通过与实验例C1相同的方法制作发光元件用基板,进一步利用与实验例C1相同的方法制作了纵型结构的发光元件。
[发光元件的评价]
针对实验例C1~C9中制作的纵型发光元件,对阴极电极与阳极电极间通电而进行I-V测定,其结果,对于任意试料都确认到整流性。另外,通过使正向电流流通时,均确认到了波长为450nm的光。对于发光亮度,实验例C1、C2、C9的元件明显为高亮度。使用实验例C3、C7的基板的元件也为高亮度,但与实验例C1、C2、C9相比而亮度略低。使用实验例C8的基板的元件也为高亮度,但与实验例C3、C7相比略低。实验例C4的元件与实验例C8相比而亮度大幅降低。实验例C5、C6的元件与实验例C4相比而亮度进一步降低。
在以上说明的实验例中,实验例A1~A3、A7~A9相当于本发明的实验例,实验例A4~A6相当于比较例。此外,本发明未受到上述实施例的任何限定,只要属于本发明的技术范围,当然也可以以各种方式来实施。
本申请以2016年7月14日申请的日本专利申请第2016-139508号、2016年3月29日申请的日本专利申请第2016-66431号、2016年2月25申请的日本专利申请第2016-34005号,2016年1月25日申请的日本专利申请第2016-11190号,2015年11月16日申请的日本国日本专利申请第2015-224164号,2015年9月30日申请的日本专利申请第2015-193943号以及2015年9月30日申请的日本专利申请第2015-193944号为主张优先权的基础,通过引用而将它们的所有内容包含于本说明书中。
产业上的可利用性
例如在制造半导体器件时利用本发明的外延生长用基板。
附图标记说明
1…层叠体;3…微细氧化铝粉末层;3a…微细氧化铝粒子;5…板状氧化铝粉末层;5a…板状氧化铝粒子;7…取向氧化铝基板;10…发光元件用基板;12…取向氧化铝基板;14…发光功能层;14a…p型层;14b…活性层;14c…n型层;16…缓冲层;17…阴极电极;18…透光性阳极电极;19…阳极电极焊盘;20…发光元件用基板;22…半导体自立基板;24…发光功能层;24a…p型层;24b…活性层;24c…n型层;27…阴极电极;28…透光性阳极电极;29…阳极电极焊盘;30…发光元件;40…发光元件;S1…元件用基板;S2…元件用基板。
Claims (4)
1.一种外延生长用取向氧化铝基板,其特征在于,
构成表面的晶体粒子的倾斜角为0.1°以上且小于1.0°,
平均烧结粒径为10μm以上。
2.根据权利要求1所述的外延生长用取向氧化铝基板,其特征在于,
构成表面的晶体粒子的平均烧结粒径为20μm以上。
3.根据权利要求1或2所述的外延生长用取向氧化铝基板,其特征在于,
Na、Mg、Si、P、Ca、Fe、Ti、Zn各自的含量为1500ppm以下。
4.根据权利要求1~3中任一项所述的外延生长用取向氧化铝基板,其特征在于,
Mg的含量为15ppm以上。
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CN115536369B (zh) * | 2022-10-18 | 2023-09-26 | 湖北晶耐新材料有限公司 | 一种自增韧氧化铝陶瓷材料的制备方法 |
CN115925399A (zh) * | 2022-11-01 | 2023-04-07 | 南充三环电子有限公司 | 一种抗热震陶瓷基板及其制备方法 |
CN115925399B (zh) * | 2022-11-01 | 2023-12-12 | 南充三环电子有限公司 | 一种抗热震陶瓷基板及其制备方法 |
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