JP3889409B2 - 高純度四塩化けい素とその製造方法 - Google Patents
高純度四塩化けい素とその製造方法 Download PDFInfo
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- JP3889409B2 JP3889409B2 JP2004124333A JP2004124333A JP3889409B2 JP 3889409 B2 JP3889409 B2 JP 3889409B2 JP 2004124333 A JP2004124333 A JP 2004124333A JP 2004124333 A JP2004124333 A JP 2004124333A JP 3889409 B2 JP3889409 B2 JP 3889409B2
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- Prior art keywords
- silicon tetrachloride
- trichlorosilane
- hcl
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- concentration
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 title claims description 85
- 239000005049 silicon tetrachloride Substances 0.000 title claims description 84
- 238000004519 manufacturing process Methods 0.000 title description 22
- 239000005052 trichlorosilane Substances 0.000 claims description 30
- 238000010992 reflux Methods 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 20
- 239000006227 byproduct Substances 0.000 claims description 19
- 239000012535 impurity Substances 0.000 claims description 18
- 239000002184 metal Substances 0.000 claims description 14
- 229910052751 metal Inorganic materials 0.000 claims description 14
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 13
- 238000011946 reduction process Methods 0.000 claims description 6
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims 1
- 238000004821 distillation Methods 0.000 description 42
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 30
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 30
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 30
- PPDADIYYMSXQJK-UHFFFAOYSA-N trichlorosilicon Chemical compound Cl[Si](Cl)Cl PPDADIYYMSXQJK-UHFFFAOYSA-N 0.000 description 30
- 239000007789 gas Substances 0.000 description 19
- 239000007788 liquid Substances 0.000 description 16
- 239000004065 semiconductor Substances 0.000 description 12
- 238000001704 evaporation Methods 0.000 description 11
- 230000008020 evaporation Effects 0.000 description 10
- 238000009825 accumulation Methods 0.000 description 9
- 238000009835 boiling Methods 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 9
- 239000002994 raw material Substances 0.000 description 9
- 238000006722 reduction reaction Methods 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 238000000926 separation method Methods 0.000 description 7
- 239000005046 Chlorosilane Substances 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000013307 optical fiber Substances 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000004508 fractional distillation Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
Images
Description
本発明の高純度四塩化けい素と、従来の四塩化けい素とを同一条件で使用したところ、これまでの残渣蓄積速度の評価実績としては、高純度四塩化けい素が相対値で1〜2と飛躍的に小さくなった。
シーメンス法による多結晶シリコンの還元工程から排出される副生ガスを、四塩化けい素とトリクロロシランを分離・回収する蒸留を還流比5.0で行い、回収された四塩化けい素に含まれるSi2HCl5の濃度を測定したところ1500〜2800ppmwであった。次に回収された四塩化けい素を再度蒸留した。このときの還流比は7.5および10の2水準で行い、得られた四塩化けい素は、Si2HCl5の濃度を測定したところ、ともに50ppmw未満であった。また、金属不純物のFe、Crの濃度はいずれも1ppbw未満であり、かつZnの濃度は0.5ppbw未満であった。この四塩化けい素を半導体用に使用したときの蒸発器における残渣蓄積速度は、基準100に対し、それぞれ2および1の速度であった。
本発明例と同様、副生ガスから四塩化けい素とトリクロロシランを分離・回収する蒸留を還流比5.0で行い、引き続き、回収された四塩化けい素を還流比5.0で再度蒸留したところSi2HCl5の濃度が200〜300ppmwに減少し、金属不純物のFe、Crの濃度はいずれも1ppbw未満であり、かつZnの濃度は0.5ppbw未満であったが、残渣蓄積速度は、基準100に対し、40〜60の速度であった。
1:金属けい素(Si)、 2:水素ガス、 3:蒸留設備Bからのフィードバック液
4:蒸留塔Dからのフィードバック液
5:トリクロロシランと四塩化けい素を主成分とするクロロシラン類
6:高純度のトリクロロシラン、 7:ヘビーエンド成分、 8:副生ガス
9:分離・回収された高純度のトリクロロシラン、 10:ポリマーなどの不純物
11:フィードバック液4から分岐した高純度四塩化けい素の原料
12:高純度四塩化けい素、 13:Si2HCl5
Claims (3)
- Si2HCl5の濃度が50ppmw未満であることを特徴とする高純度四塩化けい素。
- 金属不純物濃度が、Fe:2ppbw未満、Cr:1ppbw未満およびZn:0.5ppbw未満であることを特徴とする請求項1記載の高純度四塩化けい素。
- シーメンス法による多結晶シリコンの還元工程から排出される副生ガスを蒸留し、トリクロロシランと分離された四塩化けい素を、さらに還流比を7.5以上で蒸留することを特徴とする請求項1または請求項2記載の高純度四塩化けい素の製造方法。
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JP2005306645A JP2005306645A (ja) | 2005-11-04 |
JP3889409B2 true JP3889409B2 (ja) | 2007-03-07 |
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Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2007269679A (ja) * | 2006-03-31 | 2007-10-18 | Sumitomo Titanium Corp | 高純度アルキルシランの製造方法 |
DE102011003453A1 (de) * | 2011-02-01 | 2012-08-02 | Wacker Chemie Ag | Verfahren zur destillativen Reinigung von Chlorsilanen |
CN102530959B (zh) * | 2011-12-30 | 2013-11-06 | 湖北犇星化工有限责任公司 | 一种四氯化硅的提纯方法及其设备 |
JP7220847B2 (ja) | 2019-06-26 | 2023-02-13 | 住友金属鉱山株式会社 | 四塩化ケイ素の測定ユニット、四塩化ケイ素の品質評価方法、四塩化ケイ素の品質管理方法、炭化ケイ素基板の製造方法、および、炭化ケイ素基板製造装置 |
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