JP7381605B2 - 構造が最適化されたシリコン粒子を有するトリクロロシランの製造方法 - Google Patents
構造が最適化されたシリコン粒子を有するトリクロロシランの製造方法 Download PDFInfo
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- 238000004519 manufacturing process Methods 0.000 title claims description 15
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 title claims description 4
- 239000005052 trichlorosilane Substances 0.000 title claims description 4
- 239000011856 silicon-based particle Substances 0.000 title description 7
- 239000002245 particle Substances 0.000 claims description 79
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 29
- 239000000203 mixture Substances 0.000 claims description 28
- 229910052710 silicon Inorganic materials 0.000 claims description 28
- 239000010703 silicon Substances 0.000 claims description 28
- 239000008187 granular material Substances 0.000 claims description 25
- 238000005469 granulation Methods 0.000 claims description 22
- 230000003179 granulation Effects 0.000 claims description 22
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical class Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims description 20
- 239000005046 Chlorosilane Substances 0.000 claims description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 16
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 14
- 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 claims description 11
- 239000012495 reaction gas Substances 0.000 claims description 11
- 239000005049 silicon tetrachloride Substances 0.000 claims description 11
- 239000001257 hydrogen Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 230000005484 gravity Effects 0.000 claims description 5
- 238000012856 packing Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 description 19
- 238000006243 chemical reaction Methods 0.000 description 18
- 239000003054 catalyst Substances 0.000 description 14
- 239000007789 gas Substances 0.000 description 12
- 238000009826 distribution Methods 0.000 description 10
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 239000006227 byproduct Substances 0.000 description 6
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000000428 dust Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 238000004817 gas chromatography Methods 0.000 description 3
- 238000007038 hydrochlorination reaction Methods 0.000 description 3
- 238000010191 image analysis Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 229910052718 tin Inorganic materials 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 2
- 229910003902 SiCl 4 Inorganic materials 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910052787 antimony Inorganic materials 0.000 description 2
- 229910052785 arsenic Inorganic materials 0.000 description 2
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 239000013590 bulk material Substances 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 2
- 229910052732 germanium Inorganic materials 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910052711 selenium Inorganic materials 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052714 tellurium Inorganic materials 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- GCAXGCSCRRVVLF-UHFFFAOYSA-N 3,3,4,4-tetrachlorothiolane 1,1-dioxide Chemical compound ClC1(Cl)CS(=O)(=O)CC1(Cl)Cl GCAXGCSCRRVVLF-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 1
- 229910021592 Copper(II) chloride Inorganic materials 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 230000002902 bimodal effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 150000002366 halogen compounds Chemical class 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 150000001367 organochlorosilanes Chemical class 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00584—Controlling the density
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00654—Controlling the process by measures relating to the particulate material
- B01J2208/00672—Particle size selection
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1809—Controlling processes
Description
(1)Si+3HCl→SiHCl3+H2+副生成物
(2)Si+3SiCl4+2H2→4SiHCl3+副生成物
(3)SiCl4+H2→SiHCl3+HCl+副生成物
HnSiCl4-n (1)
(式中、nは1~3である。)
のクロロシランを流動床反応器中において製造するための方法であって、
水素及び四塩化シリコンを含有する反応ガスを、シリコンを含有する粒状接触剤と350℃~800℃の温度で反応させ、流動床反応器に導入された、造粒物又は造粒混合物の意味として理解される操作造粒物(operating granulation)が、構造パラメータSにより表されるシリコン含有粒子Sを少なくとも1質量%含有し、
Sが、少なくとも0の値を有し、下記式:
φSは対称性-加重真球度係数であり、
ρSDは充填密度[g/cm3]であり、
ρFは平均粒子固体密度[g/cm3]である。)
により算出されるものである、方法を提供する。
・TCS選択性が一層高くなる。
・シリコン利用率が一層高くなる(粉塵の排出による損失が一層小さくなる)。
・接触剤の粒径分布が一層均質になり、それに伴い流動床の流体力学的特性が改善する。
・微粉化粒子又は粉塵画分(粒径70μm未満の粒子)が凝集し、工場の一部が封鎖及び/又は閉塞することが減少する。
・粒子混合物の搬送性が改善する。
・摩耗の減少によって反応器の運転可能時間が延びる(工場の利用可能性が一層高くなる)。
- 記載の方法によりTCSを製造する工程。
- 半導体品質のTCSを提供するために、製造したTCSを精製する工程。
- 好ましくはシーメンス法により、又は造粒物として、多結晶シリコンを堆積させる工程。
- 得られた多結晶シリコンを更に加工する工程。
製造過程で発生する超高純度のシリコン粉塵をリサイクルする工程/更に多結晶シリコンを加工する工程。
Claims (6)
- 一般式1
HnSiCl4-n (1)
(式中、nは1~3である。)
のクロロシランを流動床反応器中において製造するための方法であって、
水素及び四塩化シリコンを含有する反応ガスを、シリコンを含有する操作造粒物と350℃~800℃の温度で反応させ、流動床反応器に導入された、造粒物又は造粒混合物の意味として理解される前記操作造粒物が、構造パラメータSにより表されるシリコン含有粒子Sを少なくとも1質量%含有し、
Sが、少なくとも0の値を有し、下記式:
φSは、対称性係数と球形度との積である対称性加重球形度係数であり、
ここで、前記対称性係数は、粒子画像の重心を通る端から端までの経路を描いたときに得られる2つの経路区間の割合(重心から一方の端までの距離/重心からもう一方の端までの距離)の最小値を表し、
前記球形度は、粒子画像の外周の長さに対する、該粒子画像の面積と同じ面積を有する円の外周の長さの割合を表し、
ρSDは充填密度[g/cm3]であり、
ρFは平均粒子固体密度[g/cm3]であり、
前記対称性加重球形度係数φ S が0.70~1である。)
により算出されるものである、
方法。 - 構造パラメータS≧0を有する前記粒子の前記平均粒子固体密度ρFが2.20~2.70g/cm3であり、同定をDIN 66137-2:2019-03に従って実施する、請求項1に記載の方法。
- 前記操作造粒物が70~1500μmの粒径パラメータd50を有し、前記粒径パラメータをDIN ISO 9276-2に従って同定する、請求項1又は2に記載の方法。
- 前記反応器への導入の前に、前記反応ガスが少なくとも10体積%の水素及び四塩化シリコンを有する、請求項1~3のいずれか一項に記載の方法。
- 水素と四塩化シリコンとのモル比が1:1~10:1である、請求項1~4のいずれか一項に記載の方法。
- 製造される前記一般式1のクロロシランがトリクロロシラン(TCS)である、請求項1~5のいずれか一項に記載の方法。
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PCT/EP2019/060941 WO2020221421A1 (de) | 2019-04-29 | 2019-04-29 | Verfahren zur herstellung von trichlorsilan mit struktur-optimierten silicium-partikeln |
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JP2022533018A JP2022533018A (ja) | 2022-07-21 |
JPWO2020221421A5 JPWO2020221421A5 (ja) | 2023-03-10 |
JP7381605B2 true JP7381605B2 (ja) | 2023-11-15 |
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US (1) | US20220212938A1 (ja) |
EP (1) | EP3962861A1 (ja) |
JP (1) | JP7381605B2 (ja) |
KR (1) | KR20210138711A (ja) |
CN (1) | CN113795462A (ja) |
TW (1) | TWI724830B (ja) |
WO (1) | WO2020221421A1 (ja) |
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WO2019068335A1 (de) | 2017-10-05 | 2019-04-11 | Wacker Chemie Ag | Verfahren zur herstellung von chlorsilanen |
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2019
- 2019-04-29 JP JP2021564378A patent/JP7381605B2/ja active Active
- 2019-04-29 KR KR1020217033504A patent/KR20210138711A/ko active IP Right Grant
- 2019-04-29 EP EP19721256.6A patent/EP3962861A1/de active Pending
- 2019-04-29 WO PCT/EP2019/060941 patent/WO2020221421A1/de unknown
- 2019-04-29 CN CN201980095900.XA patent/CN113795462A/zh active Pending
- 2019-04-29 US US17/607,859 patent/US20220212938A1/en active Pending
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2020
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US20040047793A1 (en) | 2000-12-14 | 2004-03-11 | Leslaw Mleczko | Method for producing trichlorosilane |
WO2012152434A1 (en) | 2011-05-08 | 2012-11-15 | Centrotherm Photovoltaics Ag | A method for treating metallurgical silicon |
WO2018074269A1 (ja) | 2016-10-19 | 2018-04-26 | 株式会社トクヤマ | 固形分濃度管理方法及びトリクロロシランの製造方法 |
WO2019068335A1 (de) | 2017-10-05 | 2019-04-11 | Wacker Chemie Ag | Verfahren zur herstellung von chlorsilanen |
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WO2020221421A1 (de) | 2020-11-05 |
TW202039366A (zh) | 2020-11-01 |
EP3962861A1 (de) | 2022-03-09 |
TWI724830B (zh) | 2021-04-11 |
US20220212938A1 (en) | 2022-07-07 |
CN113795462A (zh) | 2021-12-14 |
JP2022533018A (ja) | 2022-07-21 |
KR20210138711A (ko) | 2021-11-19 |
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