JP4813313B2 - シリコン単結晶引上げ装置及び該装置に使用される黒鉛部材並びに黒鉛部材の劣化防止方法 - Google Patents
シリコン単結晶引上げ装置及び該装置に使用される黒鉛部材並びに黒鉛部材の劣化防止方法 Download PDFInfo
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- JP4813313B2 JP4813313B2 JP2006268028A JP2006268028A JP4813313B2 JP 4813313 B2 JP4813313 B2 JP 4813313B2 JP 2006268028 A JP2006268028 A JP 2006268028A JP 2006268028 A JP2006268028 A JP 2006268028A JP 4813313 B2 JP4813313 B2 JP 4813313B2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 126
- 229910002804 graphite Inorganic materials 0.000 title claims description 123
- 239000010439 graphite Substances 0.000 title claims description 123
- 239000013078 crystal Substances 0.000 title claims description 53
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims description 32
- 229910052710 silicon Inorganic materials 0.000 title claims description 32
- 239000010703 silicon Substances 0.000 title claims description 32
- 230000006866 deterioration Effects 0.000 title description 25
- 238000000034 method Methods 0.000 title description 15
- 230000003405 preventing effect Effects 0.000 title description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 3
- 239000007789 gas Substances 0.000 description 61
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 38
- 238000012545 processing Methods 0.000 description 18
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 16
- 229910010271 silicon carbide Inorganic materials 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000010453 quartz Substances 0.000 description 8
- 239000002344 surface layer Substances 0.000 description 8
- 239000000155 melt Substances 0.000 description 6
- 239000010410 layer Substances 0.000 description 5
- 238000005498 polishing Methods 0.000 description 4
- 238000010926 purge Methods 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 239000002019 doping agent Substances 0.000 description 3
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000035882 stress Effects 0.000 description 3
- 230000008646 thermal stress Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910052787 antimony Inorganic materials 0.000 description 2
- 229910052785 arsenic Inorganic materials 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000012634 fragment Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 230000020169 heat generation Effects 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 229910003465 moissanite Inorganic materials 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910020781 SixOy Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012800 visualization Methods 0.000 description 1
Images
Classifications
-
- 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
-
- 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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/003—Heating or cooling of the melt or the crystallised material
-
- 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/14—Heating of the melt or the crystallised materials
-
- 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
- C30B29/02—Elements
- C30B29/06—Silicon
-
- 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
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
- Y10T117/1032—Seed pulling
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
- Y10T117/1032—Seed pulling
- Y10T117/1068—Seed pulling including heating or cooling details [e.g., shield configuration]
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Description
t/8≦r≦t/4
の関係を満足することを特徴とする上記(1)記載の引上げ装置用黒鉛部材を提供できる。
SiO + C(黒鉛) → Si + CO↑ ・・・・・(C)
XO + C(黒鉛) → X + CO↑ ・・・・・(D)
X + C(黒鉛) → XC ・・・・・(E)
ここで、X=As、P、Sb ・・・・・(F)
図1は、CZ法による単結晶引き上げ装置を模式的に示した断面図である。図1では、シードチャック1、シリコン種結晶2、シリコン単結晶3、石英ルツボ4、シリコン融液5、断熱材6、黒鉛ヒータ7、黒鉛ルツボ8、ロアーリング9、排気口10、インナーシールド11、アッパーリング12、チャンバー13、ルツボ受け14、上部シールド15、支持棒16を示している。この装置では、パージガス(例えばアルゴン)がシリコン単結晶3の上方より流され、シリコン融液5の開放面から発生する反応性ガスと共に、排気口10へと下側へと導かれていく。図2は、黒鉛ヒータ7の一例を示した斜視図であり、図3は図2に示す黒鉛ヒータ7のA−A断面図である。
実施形態1では黒鉛ヒータについて説明したが、本実施形態では黒鉛ヒータ以外の黒鉛部材を用いる単結晶引き上げ装置の炉内の部品について説明する。単結晶引き上げ装置の構成は図1を用いる。図5に、炉体を流れる反応性ガスの経路の一例を示す。図5は図1の単結晶引き上げ装置の一部分を拡大した図に炉内のガスの主要な流路を点線の矢印で示したものである。主にルツボ8内の融液から発生した反応性ガスは、ガスの主要流路に沿って黒鉛ルツボ8の縁を超えて、黒鉛ヒータ7の上端部を通過し、インナーシールド11の内周面に沿って下方に流れていく。黒鉛ヒータ7の下方部には、やはり角部が存在するが、反応性ガスの流路に配置されていないため、この角部はR加工を施さなくてもよいが、流路が想定外に変化することを見越してR加工しておくことがより好ましい。
幅tが20mm、曲率半径rを4mmとして上端部7aをR面取りした黒鉛ヒータ7を用いて、シリコン単結晶の引き上げを繰り返し、黒鉛ヒータ7の上端部7aにクラックの発生、破片の発生とが何回目の引き上げで発生するかを調べた。シリコン単結晶の引き上げ条件により、クラックの発生のし易さが変化するため、同じ引上げ条件で、比較例として上端部をC2面取りした黒鉛ヒータを用いた試験を行った。クラック発生の検査は、黒鉛ヒータの外観を目視検査することにより実施した。表1に検査結果を示す。
2 シリコン種結晶
3 シリコン単結晶
4 石英ルツボ
5 シリコン融液
6 断熱材
7 黒鉛ヒータ
8 黒鉛ルツボ
9 ロアーリング
10 排気口
11 インナーシールド
12 アッパーリング
13 チャンバー
14 ルツボ受け
15 上部シールド
16 支持棒
Claims (5)
- シリコン単結晶引上げ装置に用いられる黒鉛部材において、
前記黒鉛部材は、黒鉛ヒータを構成し、
該黒鉛ヒータの反応性ガスにさらされる部分の角部がR加工されていることを特徴とする引上げ装置用黒鉛部材。 - 前記反応性ガスにさらされる部分は、厚み方向のサイズtが他のサイズに比べて小さい板状部分を含み、
前記R加工される角部の曲率半径rは、
t/8≦r≦t/4
の関係を満足することを特徴とする請求項1記載の引上げ装置用黒鉛部材。 - 前記反応性ガスは、シリコン酸化物を含むことを特徴とする請求項1又は2記載の引上げ装置用黒鉛部材。
- 前記黒鉛部材は、円筒形の黒鉛ヒータを構成し、その上端部の角部がR加工されていることを特徴とする請求項1から3のいずれか記載の引上げ装置用黒鉛部材。
- 請求項1から4いずれか記載の引上げ装置用黒鉛部材を備えるシリコン単結晶引上げ装置。
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JP2006268028A JP4813313B2 (ja) | 2006-09-29 | 2006-09-29 | シリコン単結晶引上げ装置及び該装置に使用される黒鉛部材並びに黒鉛部材の劣化防止方法 |
US11/863,894 US9212431B2 (en) | 2006-09-29 | 2007-09-28 | Silicon single crystal pulling device and graphite member used therein |
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JP2006268028A JP4813313B2 (ja) | 2006-09-29 | 2006-09-29 | シリコン単結晶引上げ装置及び該装置に使用される黒鉛部材並びに黒鉛部材の劣化防止方法 |
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JP2008087997A JP2008087997A (ja) | 2008-04-17 |
JP4813313B2 true JP4813313B2 (ja) | 2011-11-09 |
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Families Citing this family (7)
Publication number | Priority date | Publication date | Assignee | Title |
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JP5118386B2 (ja) * | 2007-05-10 | 2013-01-16 | Sumco Techxiv株式会社 | 単結晶の製造方法 |
JP5904079B2 (ja) * | 2012-10-03 | 2016-04-13 | 信越半導体株式会社 | シリコン単結晶育成装置及びシリコン単結晶育成方法 |
JP6029492B2 (ja) * | 2013-02-26 | 2016-11-24 | 信越半導体株式会社 | 炭化珪素の製造方法 |
JP6405122B2 (ja) * | 2014-06-03 | 2018-10-17 | イビデン株式会社 | カーボンヒータ、ヒータユニット、焼成炉及び珪素含有多孔質セラミック焼成体の製造方法 |
JP2018058711A (ja) * | 2016-10-03 | 2018-04-12 | 新日鐵住金株式会社 | 炭化珪素単結晶インゴット製造用の黒鉛坩堝 |
DE112018001044T5 (de) * | 2017-02-28 | 2019-11-28 | Sumco Corporation | Verfahren zum Herstellen von Silizium-Einkristallbarren, und Silizium-Einkristall-Barren |
JP6805886B2 (ja) * | 2017-02-28 | 2020-12-23 | 住友金属鉱山株式会社 | 結晶育成装置 |
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JP2008087997A (ja) | 2008-04-17 |
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