JP5565070B2 - 炭化珪素結晶および炭化珪素結晶の製造方法 - Google Patents
炭化珪素結晶および炭化珪素結晶の製造方法 Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims description 220
- 229910010271 silicon carbide Inorganic materials 0.000 title claims description 220
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims description 216
- 238000004519 manufacturing process Methods 0.000 title claims description 35
- 239000002994 raw material Substances 0.000 claims description 129
- 239000002245 particle Substances 0.000 claims description 47
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 34
- 239000000758 substrate Substances 0.000 claims description 29
- 238000009826 distribution Methods 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 21
- 229910052782 aluminium Inorganic materials 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 17
- 229910052742 iron Inorganic materials 0.000 claims description 17
- 238000005498 polishing Methods 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 6
- 239000003929 acidic solution Substances 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 description 26
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 239000007789 gas Substances 0.000 description 9
- 230000006866 deterioration Effects 0.000 description 6
- 238000010298 pulverizing process Methods 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 101000878457 Macrocallista nimbosa FMRFamide Proteins 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000000859 sublimation Methods 0.000 description 3
- 230000008022 sublimation Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000001636 atomic emission spectroscopy Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000005092 sublimation method Methods 0.000 description 2
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
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Description
本発明例1では、基本的には上述した実施の形態におけるSiC結晶の製造方法にしたがってSiC結晶を製造した。
本発明例2のSiC結晶の製造方法は、基本的には本発明例1と同様に製造したが、第2の原料12を形成する工程において、最大粒度のピークCの中心が200μm以上3mm以下の第2の原料12を形成した点において異なっていた。
本発明例3のSiC結晶の製造方法は、基本的には本発明例1と同様に製造したが、第2の原料12を形成する工程において、最小粒度のピークAの中心が1μm以上100μm以下の第2の原料12を形成した点において異なっていた。
本発明例4のSiC結晶の製造方法は、基本的には本発明例1と同様に製造したが、第2の原料12を形成する工程において、最小粒度のピークAの中心が1μm以上100μm以下で、かつ最大粒度のピークCの中心が200μm以上3mm以下の第2の原料12を形成した点において異なっていた。
比較例1のSiC結晶の製造方法は、基本的には本発明例1と同様に製造したが、第1のSiC結晶11を粉砕して第2の原料を形成する工程を実施しなかった点において異なっていた。つまり、第1のSiC結晶11を比較例1のSiC結晶とした。
本発明例1〜4および比較例1のSiC結晶について、Alの濃度、Feの濃度、マイクロパイプ密度およびエッチピット密度を以下のように測定した。
表1に示すように、第1の原料17を用いて第1のSiC結晶11を成長し、第1のSiC結晶11を粉砕して第2の原料12を形成し、第2の原料12を用いて第2のSiC結晶14を成長した本発明例1〜4は、比較例1よりもAlおよびFeの濃度を低減することができた。また、このように製造することで、0.1ppm以下の濃度のFeと、100ppm以下の濃度のAlとを含むSiC結晶を実現できることがわかった。
Claims (6)
- 炭化珪素結晶において、
鉄の濃度が0.002ppm以上0.1ppm以下であり、かつアルミニウムの濃度が0.02ppm以上100ppm以下であり、マイクロパイプ密度が2個/cm2以下であり、
前記炭化珪素結晶は、種基板と、前記種基板上に成長する結晶成長部とを備え、前記種基板および前記結晶成長部の双方が4H−SiCであることを特徴とする、炭化珪素結晶。 - エッチピット密度が4100個/cm2以上5200個/cm2以下であることを特徴とする、請求項1に記載の炭化珪素結晶。
- 第1の原料として研磨用炭化珪素粉末を準備する工程と、
前記第1の原料を加熱することにより昇華して、炭化珪素の結晶を析出することにより、第1の炭化珪素結晶を成長する工程と、
前記第1の炭化珪素結晶を粉砕して、第2の原料を形成する工程と、
前記第2の原料を加熱することにより昇華して、炭化珪素の結晶を析出することにより、第2の炭化珪素結晶を成長する工程とを備え、
前記第2の原料を形成する工程では、1μm以上3mm以下の範囲に粒度分布のピークが複数あり、各々の前記粒度分布のピークの中心の粒径から±50%の粒径の範囲に95%以上の粒子が存在するように前記第2の原料を形成する、炭化珪素結晶の製造方法。 - 前記第2の原料を形成する工程では、鉄の濃度が0.002ppm以上0.1ppm以下であり、かつアルミニウムの濃度が0.02ppm以上100ppm以下である前記第2の原料を形成する、請求項3に記載の炭化珪素結晶の製造方法。
- 前記第2の原料を形成する工程は、粉砕した前記第1の炭化珪素結晶を酸性溶液で洗浄する工程を含む、請求項3または4に記載の炭化珪素結晶の製造方法。
- 前記第2の炭化珪素結晶を粉砕して、第3の原料を形成する工程と、
前記第3の原料を加熱することにより昇華して、炭化珪素の結晶を析出することにより、第3の炭化珪素結晶を成長する工程とをさらに備えた、請求項3〜5のいずれか1項に記載の炭化珪素結晶の製造方法。
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JP2010100891A JP5565070B2 (ja) | 2010-04-26 | 2010-04-26 | 炭化珪素結晶および炭化珪素結晶の製造方法 |
CN2011800043891A CN102597339A (zh) | 2010-04-26 | 2011-02-25 | 碳化硅晶体和制造碳化硅晶体的方法 |
EP11774697.4A EP2565301B1 (en) | 2010-04-26 | 2011-02-25 | Silicon carbide crystal and method for producing silicon carbide crystal |
US13/499,482 US8574529B2 (en) | 2010-04-26 | 2011-02-25 | Silicon carbide crystal and method of manufacturing silicon carbide crystal |
KR1020127009040A KR20120130318A (ko) | 2010-04-26 | 2011-02-25 | 탄화규소 결정 및 탄화규소 결정의 제조 방법 |
PCT/JP2011/054339 WO2011135913A1 (ja) | 2010-04-26 | 2011-02-25 | 炭化珪素結晶および炭化珪素結晶の製造方法 |
CA2775923A CA2775923A1 (en) | 2010-04-26 | 2011-02-25 | Silicon carbide crystal and method of manufacturing silicon carbide crystal |
TW100113266A TW201142092A (en) | 2010-04-26 | 2011-04-15 | Silicon carbide crystal and method for producing silicon carbide crystal |
US14/019,882 US20140004303A1 (en) | 2010-04-26 | 2013-09-06 | Silicon carbide crystal and method of manufacturing silicon carbide crystal |
US15/185,602 US9725823B2 (en) | 2010-04-26 | 2016-06-17 | Silicon carbide crystal and method of manufacturing silicon carbide crystal |
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JP5910393B2 (ja) | 2012-07-26 | 2016-04-27 | 住友電気工業株式会社 | 炭化珪素基板の製造方法 |
JP6028754B2 (ja) | 2014-03-11 | 2016-11-16 | トヨタ自動車株式会社 | SiC単結晶基板の製造方法 |
US10108798B1 (en) * | 2016-01-04 | 2018-10-23 | Smart Information Flow Technologies LLC | Methods and systems for defending against cyber-attacks |
CN105603530B (zh) * | 2016-01-12 | 2018-02-27 | 台州市一能科技有限公司 | 用于碳化硅晶体高速生长的原料及碳化硅晶体的生长方法 |
JP6086167B2 (ja) * | 2016-03-18 | 2017-03-01 | 住友電気工業株式会社 | 炭化珪素基板の製造方法 |
WO2018176302A1 (zh) * | 2017-03-30 | 2018-10-04 | 新疆天科合达蓝光半导体有限公司 | 用于生长SiC晶体的SiC原料的制备方法和制备装置 |
CN115704110A (zh) * | 2021-08-06 | 2023-02-17 | 株式会社电装 | 碳化硅晶体制造设备、其控制装置及生成学习模型和控制其的方法 |
KR102442730B1 (ko) * | 2021-12-23 | 2022-09-13 | 주식회사 쎄닉 | 탄화규소 분말, 이를 이용하여 탄화규소 잉곳을 제조하는 방법 및 탄화규소 웨이퍼 |
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US8574529B2 (en) | 2013-11-05 |
CN102597339A (zh) | 2012-07-18 |
US20140004303A1 (en) | 2014-01-02 |
US9725823B2 (en) | 2017-08-08 |
CA2775923A1 (en) | 2011-11-03 |
JP2011230941A (ja) | 2011-11-17 |
EP2565301A4 (en) | 2013-11-27 |
EP2565301B1 (en) | 2015-03-25 |
US20160289863A1 (en) | 2016-10-06 |
WO2011135913A1 (ja) | 2011-11-03 |
TW201142092A (en) | 2011-12-01 |
US20120183466A1 (en) | 2012-07-19 |
KR20120130318A (ko) | 2012-11-30 |
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