WO2018125958A1 - Methods for forming single crystal silicon ingots with improved resistivity control - Google Patents
Methods for forming single crystal silicon ingots with improved resistivity control Download PDFInfo
- Publication number
- WO2018125958A1 WO2018125958A1 PCT/US2017/068632 US2017068632W WO2018125958A1 WO 2018125958 A1 WO2018125958 A1 WO 2018125958A1 US 2017068632 W US2017068632 W US 2017068632W WO 2018125958 A1 WO2018125958 A1 WO 2018125958A1
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- WO
- WIPO (PCT)
- Prior art keywords
- ppma
- less
- gallium
- resistivity
- silicon
- 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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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
- C30B15/20—Controlling or regulating
-
- 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
- C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
- C30B15/04—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt adding doping materials, e.g. for n-p-junction
-
- 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
Definitions
- different impurities in the melt may segregate at different rates which causes their ratio to vary over its length which may cause a type change in the ingot. This causes a portion of the ingot to fall outside of product specifications which increases the "non-prime" portion of the ingot .
- Figure 2 is a binary phase diagram for silicon containing impurity "A" that has a segregation coefficient less than 1;
- concentration of impurity A in the solid can be represented as a function of the fraction solidified using the following:
- the resistivity is related to the concentration of the dopant element by
- Phosphorous has a segregation coefficient (0.35) that is less than boron (0.80) which causes phosphorous to
- a dopant such as gallium or indium which has a smaller segregation
- the first dopant that is added to the crucible is gallium.
- a relatively small amount of gallium is added to the
- indium may be used as the first dopant.
- concentration of indium in the melt after indium is added to the crucible may be less than about 0.5 ppma (as measured after addition of indium and before pulling of the sample ingot) or even less than about 0.1 ppma, less than 0.01 ppma or less than about 0.001 ppma indium.
- concentration of indium in the melt after indium addition is from about 0.00001 ppma to about 0.5 ppma or from about 0.0001 ppma to about 0.1 ppma.
- the amount of alloy that is added to the crucible may depend on the size of the charge and the amount of gallium incorporated therein. In some embodiments, about 0.5 grams to about 50 grams or about 1 gram to about 15 grams of gallium or indium alloy is added to the crucible.
- the first dopant i.e., gallium and/or indium
- the polysilicon material is melted down.
- the amount of second dopant used may be determined based on Equations 2-5 provided above .
- the melting temperature of the material is raised (e.g., from the 29.7°C melting temperature of pure gallium when gallium is used) which eases transfer into the crucible.
- the solid-phase alloy also stays as a solid until it is melted in the polysilicon charge, allowing for ease of handling without the need to keep the material (e.g., pure gallium) refrigerated or cooled to below its melting temperature.
- phosphorous impurity accumulation was modeled and is shown in Figure 5. As shown in Figure 5, type-change from P-type to N-type occurred at about 17% solidified fraction due to the accumulation of phosphorous relative to boron.
- phosphorous and with and without 3xl0 14 atoms/cm 3 gallium are shown in Figure 7. As shown in Figure 7, when gallium was not used the type change to N-type occurred at about 10% of the solidified fraction. Use of gallium allowed the ingot to remain P-type throughout the length of the body.
- a master gallium- silicon alloy was produced.
- the alloy had a gallium concentration in the range of 0.1 to 0.3 wt%. Amounts of silicon and gallium were weighed. The materials were melted and frozen in a quartz container in low gradient furnace. The alloy material was separated from the container and acid washed in HF. The alloy was then dried, crushed, sized and cleaned to less than 3 mm. The
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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)
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201780080972.8A CN110382748B (zh) | 2016-12-28 | 2017-12-28 | 形成具有经改善的电阻率控制的单晶硅晶锭的方法 |
| JP2019535251A JP7365900B2 (ja) | 2016-12-28 | 2017-12-28 | 改善された抵抗率制御により単結晶シリコンインゴットを形成する方法 |
| JP2022151550A JP2022180551A (ja) | 2016-12-28 | 2022-09-22 | 改善された抵抗率制御により単結晶シリコンインゴットを形成する方法 |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US201662439743P | 2016-12-28 | 2016-12-28 | |
| US62/439,743 | 2016-12-28 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2018125958A1 true WO2018125958A1 (en) | 2018-07-05 |
Family
ID=61007847
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/US2017/068632 Ceased WO2018125958A1 (en) | 2016-12-28 | 2017-12-28 | Methods for forming single crystal silicon ingots with improved resistivity control |
Country Status (5)
| Country | Link |
|---|---|
| US (2) | US10920337B2 (enExample) |
| JP (2) | JP7365900B2 (enExample) |
| CN (1) | CN110382748B (enExample) |
| TW (1) | TWI745520B (enExample) |
| WO (1) | WO2018125958A1 (enExample) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020005901A1 (en) * | 2018-06-27 | 2020-01-02 | Globalwafers Co., Ltd. | Sample rod growth and resistivity measurement during single crystal silicon ingot production |
| US10781532B2 (en) | 2018-06-27 | 2020-09-22 | Globalwafers Co., Ltd. | Methods for determining the resistivity of a polycrystalline silicon melt |
| US11739437B2 (en) | 2018-12-27 | 2023-08-29 | Globalwafers Co., Ltd. | Resistivity stabilization measurement of fat neck slabs for high resistivity and ultra-high resistivity single crystal silicon ingot growth |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020131458A1 (en) * | 2018-12-21 | 2020-06-25 | Globalwafers Co., Ltd. | Sample rod center slab resistivity measurement during single crystal silicon ingot production |
| US11585010B2 (en) | 2019-06-28 | 2023-02-21 | Globalwafers Co., Ltd. | Methods for producing a single crystal silicon ingot using boric acid as a dopant and ingot puller apparatus that use a solid-phase dopant |
| US20220359195A1 (en) * | 2021-05-05 | 2022-11-10 | Globalwafers Co., Ltd. | Methods for forming an epitaxial wafer |
| CN115341271A (zh) * | 2021-05-13 | 2022-11-15 | 内蒙古中环协鑫光伏材料有限公司 | 一种控制单晶电阻率轴向衰减速率的方法 |
| US20230112094A1 (en) * | 2021-10-11 | 2023-04-13 | Globalwafers Co., Ltd. | Modeling thermal donor formation and target resistivity for single crystal silicon ingot production |
| US12351938B2 (en) | 2022-02-10 | 2025-07-08 | Globalwafers Co., Ltd. | Methods for producing a product ingot having low oxygen content |
| CN114690643B (zh) * | 2022-05-31 | 2022-08-23 | 广东高景太阳能科技有限公司 | 基于掺镓单晶中镓含量的电阻率控制方法、系统及设备 |
| CN115233292A (zh) * | 2022-07-25 | 2022-10-25 | 北京麦竹吉科技有限公司 | 一种低电阻率硅单晶及其制备方法 |
Citations (6)
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| US20120056135A1 (en) * | 2010-09-03 | 2012-03-08 | Deluca John P | Silicon Single Crystal Doped with Gallium, Indium, or Aluminum |
| US8317919B2 (en) | 2003-11-03 | 2012-11-27 | Solaicx, Inc. | System for continuous growing of monocrystalline silicon |
| EP2584070A1 (en) * | 2011-10-17 | 2013-04-24 | Siltronic AG | P-type silicon single crystal and method of manufacturing the same |
| CN102260900B (zh) * | 2011-07-14 | 2013-11-27 | 西安华晶电子技术股份有限公司 | 提高单晶硅纵向电阻率一致性的装置及其处理工艺 |
| WO2014106080A1 (en) * | 2012-12-31 | 2014-07-03 | Memc Electronic Materials S.P.A. | Fabrication of indium-doped silicon by the czochralski method |
| CN105887194A (zh) * | 2016-05-30 | 2016-08-24 | 上海超硅半导体有限公司 | 一种n型单晶硅的生长方法 |
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| US2847544A (en) * | 1955-12-16 | 1958-08-12 | Gen Electric | Silicon semiconductive devices |
| DE3049376A1 (de) | 1980-12-29 | 1982-07-29 | Heliotronic Forschungs- und Entwicklungsgesellschaft für Solarzellen-Grundstoffe mbH, 8263 Burghausen | Verfahren zur herstellung vertikaler pn-uebergaenge beim ziehen von siliciumscheiben aus einer siliciumschmelze |
| JPH1029894A (ja) * | 1996-07-15 | 1998-02-03 | Hitachi Ltd | 単結晶シリコンの比抵抗調整方法および単結晶シリコン製造装置 |
| JP2002226295A (ja) * | 2001-01-31 | 2002-08-14 | Shin Etsu Handotai Co Ltd | チョクラルスキー法によるシリコン単結晶製造工程の管理方法及びチョクラルスキー法による高抵抗シリコン単結晶の製造方法並びにシリコン単結晶 |
| US8021483B2 (en) * | 2002-02-20 | 2011-09-20 | Hemlock Semiconductor Corporation | Flowable chips and methods for the preparation and use of same, and apparatus for use in the methods |
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| CN102181919B (zh) * | 2011-04-13 | 2012-12-26 | 天津市环欧半导体材料技术有限公司 | 一种控制直拉硅单晶头部电阻率的方法 |
| PH12013502137A1 (en) | 2011-04-14 | 2014-01-13 | Gtat Ip Holding Llc | Silicon ingot having uniform multiple dopants and method and apparatus for producing same |
| US20130047913A1 (en) * | 2011-08-29 | 2013-02-28 | Max Era, Inc. | Method and Apparatus for Doping by Lane in a Multi-Lane Sheet Wafer Furnace |
| JP6168011B2 (ja) | 2014-08-19 | 2017-07-26 | 信越半導体株式会社 | 単結晶育成装置及びその装置を用いた単結晶育成方法 |
| JP6222013B2 (ja) | 2014-08-29 | 2017-11-01 | 信越半導体株式会社 | 抵抗率制御方法 |
-
2017
- 2017-12-27 US US15/855,466 patent/US10920337B2/en active Active
- 2017-12-28 JP JP2019535251A patent/JP7365900B2/ja active Active
- 2017-12-28 CN CN201780080972.8A patent/CN110382748B/zh active Active
- 2017-12-28 TW TW106146322A patent/TWI745520B/zh active
- 2017-12-28 WO PCT/US2017/068632 patent/WO2018125958A1/en not_active Ceased
-
2020
- 2020-10-15 US US17/071,714 patent/US12024789B2/en active Active
-
2022
- 2022-09-22 JP JP2022151550A patent/JP2022180551A/ja not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8317919B2 (en) | 2003-11-03 | 2012-11-27 | Solaicx, Inc. | System for continuous growing of monocrystalline silicon |
| US20120056135A1 (en) * | 2010-09-03 | 2012-03-08 | Deluca John P | Silicon Single Crystal Doped with Gallium, Indium, or Aluminum |
| CN102260900B (zh) * | 2011-07-14 | 2013-11-27 | 西安华晶电子技术股份有限公司 | 提高单晶硅纵向电阻率一致性的装置及其处理工艺 |
| EP2584070A1 (en) * | 2011-10-17 | 2013-04-24 | Siltronic AG | P-type silicon single crystal and method of manufacturing the same |
| WO2014106080A1 (en) * | 2012-12-31 | 2014-07-03 | Memc Electronic Materials S.P.A. | Fabrication of indium-doped silicon by the czochralski method |
| CN105887194A (zh) * | 2016-05-30 | 2016-08-24 | 上海超硅半导体有限公司 | 一种n型单晶硅的生长方法 |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020005901A1 (en) * | 2018-06-27 | 2020-01-02 | Globalwafers Co., Ltd. | Sample rod growth and resistivity measurement during single crystal silicon ingot production |
| US10781532B2 (en) | 2018-06-27 | 2020-09-22 | Globalwafers Co., Ltd. | Methods for determining the resistivity of a polycrystalline silicon melt |
| US10793969B2 (en) | 2018-06-27 | 2020-10-06 | Globalwafers Co., Ltd. | Sample rod growth and resistivity measurement during single crystal silicon ingot production |
| EP4317546A3 (en) * | 2018-06-27 | 2024-03-20 | GlobalWafers Co., Ltd. | Sample rod resistivity measurement during single crystal silicon ingot production |
| US11739437B2 (en) | 2018-12-27 | 2023-08-29 | Globalwafers Co., Ltd. | Resistivity stabilization measurement of fat neck slabs for high resistivity and ultra-high resistivity single crystal silicon ingot growth |
Also Published As
| Publication number | Publication date |
|---|---|
| US20180179660A1 (en) | 2018-06-28 |
| JP2022180551A (ja) | 2022-12-06 |
| TWI745520B (zh) | 2021-11-11 |
| US20210071315A1 (en) | 2021-03-11 |
| TW201840918A (zh) | 2018-11-16 |
| US10920337B2 (en) | 2021-02-16 |
| CN110382748A (zh) | 2019-10-25 |
| JP2020503231A (ja) | 2020-01-30 |
| US12024789B2 (en) | 2024-07-02 |
| CN110382748B (zh) | 2021-07-02 |
| JP7365900B2 (ja) | 2023-10-20 |
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