JP6517355B2 - 多結晶シリコンの製造方法 - Google Patents
多結晶シリコンの製造方法 Download PDFInfo
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- JP6517355B2 JP6517355B2 JP2017541336A JP2017541336A JP6517355B2 JP 6517355 B2 JP6517355 B2 JP 6517355B2 JP 2017541336 A JP2017541336 A JP 2017541336A JP 2017541336 A JP2017541336 A JP 2017541336A JP 6517355 B2 JP6517355 B2 JP 6517355B2
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims description 69
- 238000004519 manufacturing process Methods 0.000 title description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 141
- 239000010703 silicon Substances 0.000 claims description 138
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 137
- 238000000034 method Methods 0.000 claims description 53
- 238000000576 coating method Methods 0.000 claims description 31
- 239000011248 coating agent Substances 0.000 claims description 28
- 235000012431 wafers Nutrition 0.000 claims description 17
- 239000003638 chemical reducing agent Substances 0.000 claims description 11
- 230000008018 melting Effects 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- 229910052736 halogen Inorganic materials 0.000 claims description 7
- 150000002367 halogens Chemical class 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 5
- 229910052801 chlorine Inorganic materials 0.000 claims description 5
- 239000000460 chlorine Substances 0.000 claims description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 229920005591 polysilicon Polymers 0.000 claims 1
- 230000006911 nucleation Effects 0.000 description 26
- 238000010899 nucleation Methods 0.000 description 26
- 239000002245 particle Substances 0.000 description 18
- 239000013078 crystal Substances 0.000 description 17
- 238000009736 wetting Methods 0.000 description 15
- 230000001737 promoting effect Effects 0.000 description 9
- 238000007711 solidification Methods 0.000 description 9
- 230000008023 solidification Effects 0.000 description 9
- 239000002667 nucleating agent Substances 0.000 description 8
- 239000011856 silicon-based particle Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 229910021419 crystalline silicon Inorganic materials 0.000 description 6
- 230000007547 defect Effects 0.000 description 6
- 239000002210 silicon-based material Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000012495 reaction gas Substances 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 4
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 4
- 239000005052 trichlorosilane Substances 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000013058 crude material Substances 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 239000005046 Chlorosilane Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical group Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000005243 fluidization Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000001404 mediated effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910003822 SiHCl3 Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 150000001553 barium compounds Chemical class 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000003947 neutron activation analysis Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- -1 oxides Chemical class 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
- SBEQWOXEGHQIMW-UHFFFAOYSA-N silicon Chemical compound [Si].[Si] SBEQWOXEGHQIMW-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
- 238000004857 zone melting Methods 0.000 description 1
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- 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
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- C30—CRYSTAL GROWTH
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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Description
− シリコン融液を受け入れるための容器を提供する工程であって、前記容器は底部および内面を有する工程、
− 容器内にシリコン融液を提供する工程、
− 容器の底部から熱を除去してシリコン融液を冷却する工程
を含み、
− 不均一な温度分布が、底部の領域における容器の内面に少なくとも一時的に確立されるように熱が除去されるシリコンブロックの製造方法を開示する。温度分布は、好ましくは、少なくとも0.1K、より具体的には少なくとも1K、より具体的には少なくとも5Kで50K以下、より具体的には10K以下の温度範囲を含む。底部の領域における0.1から50ケルビンの温度差は、核形成、ひいてはバルク結晶化に影響を及ぼす可能性がある。
− シリコン融液を受け入れるための容器を提供する工程、
− 前記容器内に細粒シリコン層を配置する工程、
− 前記細粒シリコン層に接触して前記容器内にシリコン融液を配置する工程、
− 前記細粒シリコン層から出発して前記シリコン融液を一方向凝固させる工程
を含む該方法を請求する。
(a) 最初に、核形成促進層を金型の底部に加え、金型自体が垂直方向を画定する工程;
(b) 金型内の核形成促進層上にシリコン源を提供する工程;
(c) シリコン源が完全に溶融してシリコン融液が得られるまで金型を加熱する工程;
(d) 複数のシリコン粒子が核形成促進層上に配置されたシリコン融液から核形成し、垂直方向に成長することができるように、シリコン融液に関する少なくとも1つの熱制御パラメータを連続的に制御する工程;および
(e) シリコン融液全体が凝固して結晶質シリコンブロックが得られるまで、シリコン粒子が垂直方向に連続的に成長できるように、該少なくとも1つの熱制御パラメータを連続的に制御する工程
を含む結晶シリコンブロックを製造する方法を開示する。
− シリコン融液を受け入れるための容器を提供する工程、
− 容器内のシリコン融液の温度を制御するために温度制御装置を提供する工程、
− シリコン融液中の不均一核形成を促進するために、シリコンおよび少なくとも1つの核形成剤を含む粗製材料を容器内に配置する工程、および
− この方法の特定の段階の間に、粗製材料が容器内に方法の次の段階で方向性凝固されるシリコン融液として存在するように容器内の温度を制御する工程
を含み、
− 核形成剤はナノ粒子を含む
シリコンインゴットの製造方法が開示されている。
− 少なくとも1つの容器壁の内面の少なくとも一部上の核形成抑制表面と、核形成阻害表面が設けられた内表面上の少なくとも1つの核形成部位とを含むシリコン融液を受け入れる容器を提供する工程、
− 液体シリコンを注ぐことによって、または固体シリコンを溶融することによって容器内にシリコン融液を配置する工程、
− 核形成抑制表面を有する少なくとも1つの容器壁を冷却してシリコン融液を結晶化させる工程を含むシリコンブロックの製造方法が記載されている。
− 底部および内面を含む、シリコン融液を受け入れるためのるつぼを提供する工程であって、るつぼの少なくとも底部は、Si3N4、酸化Si3N4およびSiO2からなる群から選択される1つ以上の化合物を含むコーティングを有する工程、
− るつぼの底部のコーティングと接触して、るつぼ内にシリコン層を配置する工程、
− シリコン層と接触して、るつぼ内に多結晶シリコンを配置する工程、
− 多結晶シリコンおよびシリコン層が完全に融解してシリコン融液を得るまで、るつぼを加熱する工程、
− シリコン融液を一方向凝固させて多結晶シリコンブロックを形成する工程、
を含み、
シリコン層は、るつぼの加熱中および/またはシリコン層の融解中に還元剤を放出する該方法によって達成される。
本発明の方法Aは、トリクロロシランを使用し、0から4000μmの結晶粒径および35ppmwを超える塩素含量を有する、流動床に堆積した粒状多結晶シリコンを初期充填することを含む。
標準的な方法Bは、シーメンス法によって製造され、0から15mmの結晶粒径および1ppmw未満の塩素含量を有するチャンク状の多結晶シリコンをるつぼの底部に初期充填することを含む。
2 多結晶シリコン(チャンクまたは粒状)
3 るつぼ
4 るつぼコーティング
Claims (14)
- 多結晶シリコンを製造する方法であって、
− 底部および内面を含む、シリコン融液を受け入れるためのるつぼを提供する工程であって、るつぼの少なくとも底部は、Si3N4、酸化Si3N4およびSiO2からなる群から選択される1つ以上の化合物を含むコーティングを有する工程、
− るつぼの底部のコーティングと接触して、るつぼ内にシリコン層を配置する工程、
− シリコン層と接触して、るつぼ内に多結晶シリコンを配置する工程、
− 多結晶シリコンおよびシリコン層が完全に融解してシリコン融液を得るまで、るつぼを加熱する工程、
− シリコン融液を一方向凝固させて多結晶シリコンブロックを形成する工程、
を含み、
シリコン層が多結晶シリコンを含み、シリコン層のハロゲン含量は3から90ppmwであり、シリコン層が、るつぼの加熱中および/またはシリコン層の融解中に還元剤を放出する該方法。 - シリコン層が、0.5から40ppmwの水素含量を有する多結晶シリコンを含む請求項1に記載の方法。
- ハロゲンが塩素である請求項1又は2に記載の方法。
- 多結晶シリコンブロックは、3%未満の電気的再結合−活性面積率を有する請求項1から3のいずれか一項に記載の方法。
- 初期充填シリコン層は、50から4000μmの結晶粒径を有する粒状多結晶シリコンを含む請求項1から4のいずれか一項に記載の方法。
- るつぼ内のシリコン層は、それがるつぼの底部の面積の少なくとも30%を覆うように配置される請求項1から5のいずれか一項に記載の方法。
- シリコン層は、50μmから100cmの高さを有する請求項1から5のいずれか一項に記載の方法。
- シリコン層は、るつぼの内面と直接接触しない請求項1から7のいずれか一項に記載の方法。
- シリコン層とるつぼの内面との間の距離は少なくとも1mmである請求項1から8のいずれか一項に記載の方法。
- 多結晶シリコンブロックは、多結晶シリコンブロックの底部領域において12.5mm2未満の平均結晶粒径を有し、底部領域は、シリコンブロックの底部から、シリコンブロックの高さ5cm(底部から0から5cmの領域)まで伸びる請求項1から9のいずれか一項に記載の方法。
- 多結晶シリコンブロックは、156×156mm2の面積で測定した12.5mm2の最大平均結晶粒径を有する請求項1から10のいずれか一項に記載の方法。
- 多結晶シリコンブロックは、3未満の変動係数を有する微細構造を有する請求項1から11のいずれか一項に記載の方法。
- 多結晶シリコンブロックは、さらなる工程で多結晶シリコンインゴットに切断される請求項1から12のいずれか一項に記載の方法。
- 多結晶シリコンインゴットは、さらなる工程で多結晶シリコンウェハに切断される請求項13に記載の方法。
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JPH02233514A (ja) | 1989-03-06 | 1990-09-17 | Osaka Titanium Co Ltd | 多結晶シリコンの製造方法 |
EP1820777A4 (en) * | 2004-11-30 | 2010-01-20 | Noritake Tcf Co Ltd | METHOD FOR PRODUCING A POLYCRYSTALLINE SILICON STAIN |
US20110177284A1 (en) * | 2009-07-16 | 2011-07-21 | Memc Singapore Pte Ltd. | Silicon wafers and ingots with reduced oxygen content and methods for producing them |
DE102010000687B4 (de) | 2010-01-05 | 2012-10-18 | Solarworld Innovations Gmbh | Tiegel und Verfahren zur Herstellung von Silizium-Blöcken |
DE102011003578A1 (de) | 2010-02-25 | 2011-08-25 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V., 80686 | Vorrichtung und Verfahren zur Herstellung von Silizium-Blöcken |
US20110239933A1 (en) | 2010-04-01 | 2011-10-06 | Bernhard Freudenberg | Device and method for the production of silicon blocks |
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DE102011002598B4 (de) * | 2011-01-12 | 2016-10-06 | Solarworld Innovations Gmbh | Verfahren zur Herstellung eines Silizium-Ingots |
TWI441962B (zh) * | 2011-10-14 | 2014-06-21 | Sino American Silicon Prod Inc | 矽晶鑄錠及其製造方法(一) |
CN103088418B (zh) * | 2011-11-01 | 2015-07-08 | 昆山中辰矽晶有限公司 | 硅晶铸锭及其制造方法 |
US9493357B2 (en) | 2011-11-28 | 2016-11-15 | Sino-American Silicon Products Inc. | Method of fabricating crystalline silicon ingot including nucleation promotion layer |
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US20130193559A1 (en) * | 2012-01-27 | 2013-08-01 | Memc Singapore Pte. Ltd. (Uen200614794D) | CAST SILICON ingot prepared BY DIRECTIONAL SOLIDIFICATION |
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DE102012206439A1 (de) * | 2012-04-19 | 2013-10-24 | Wacker Chemie Ag | Polykristallines Siliciumgranulat und seine Herstellung |
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CN107208308A (zh) | 2017-09-26 |
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