WO2013065232A1 - 単結晶の製造方法 - Google Patents
単結晶の製造方法 Download PDFInfo
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- WO2013065232A1 WO2013065232A1 PCT/JP2012/006288 JP2012006288W WO2013065232A1 WO 2013065232 A1 WO2013065232 A1 WO 2013065232A1 JP 2012006288 W JP2012006288 W JP 2012006288W WO 2013065232 A1 WO2013065232 A1 WO 2013065232A1
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- 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
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- 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
- C30B15/10—Crucibles or containers for supporting the melt
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- 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
- the present invention relates to a method for producing a single crystal by the Czochralski method (hereinafter referred to as CZ method).
- a CZ method is widely known in which a silicon polycrystal raw material is melted in a crucible and a seed crystal is brought into contact with the melt surface and pulled to raise the single crystal. .
- Patent Document 1 impurity content of the synthetic layer (Al, Fe, Ni, Cr, etc.) less synthetic quartz crucible used, minute defects manufactures 3 / cm 2 or less of a single crystal.
- the graphite parts in the furnace are generally ultra-high-purity graphite materials and high-purity graphite materials. Is used.
- the standards of these metal impurity concentrations (Fe, Al, Ni, Cr, etc.) were around 0.3 ppm (300 ppb) for ultra-high purity graphite material and around 0.5 ppm (500 ppb) for high-purity graphite material. Conventionally, if the graphite material satisfies these criteria, the impurities of the graphite material did not affect the single crystal.
- LPD Light Point Defect
- the present invention has been made in view of the above-described problems, and an object of the present invention is to provide a method capable of producing a single crystal free from LT reduction or LPD abnormality in the production of a single crystal by the CZ method.
- the Ni concentration of at least one graphite component used in a furnace for producing a single crystal is analyzed, and the analyzed Ni concentration is analyzed.
- the graphite component is preferably at least one of a graphite component that is in direct contact with the quartz crucible and a graphite component that is in direct contact with the quartz crucible through the graphite component in direct contact.
- the graphite component is preferably a graphite crucible.
- the graphite crucible is in direct contact with the quartz crucible containing the melt, it is possible to more effectively prevent single crystal LT degradation and LPD abnormality by setting the Ni concentration to 30 ppb or less.
- the graphite part is at least one of a crucible tray and a pedestal. Furthermore, by making such a graphite part to have a Ni concentration of 30 ppb or less, it is possible to reliably prevent LT degradation and LPD abnormality of the manufactured single crystal.
- the method for analyzing the Ni concentration is a high-sensitivity analysis method in which the graphite material of the graphite component is plasma ashed and acid-dissolved.
- the Ni concentration of the graphite material of the graphite component can be quantitatively analyzed to 30 ppb or less, so that it is possible to reliably prevent LT degradation and LPD abnormality of the manufactured single crystal. Can do.
- a high-quality single crystal that does not cause LT degradation or LPD abnormality can be produced with high yield.
- the present inventor paid attention to graphite parts that were previously considered not to be a cause for LT degradation and LPD anomalies that occurred in single crystals produced by the CZ method, and examined as follows. did.
- a single crystal is manufactured using a raw material polycrystal having a very low impurity content and a quartz crucible, and the single crystal is reduced in both cases where the LT of the single crystal is reduced or when an LPD abnormality has occurred or not.
- the graphite parts used at the time of manufacture were analyzed by a highly sensitive analysis method (Fe, Al, Ni, Cr, etc., the lower limit of quantification was 5 to 10 ppb) and compared.
- Fe, Al, Ni, Cr, etc. the lower limit of quantification was 5 to 10 ppb
- the process in which the metal impurities in the graphite part are taken into the single crystal will be described in the case of a graphite crucible.
- impurities contained in the graphite crucible impurities with a particularly large diffusion coefficient diffuse out of the base material of the graphite crucible during long-time single crystal production and diffuse into the quartz crucible in contact with the graphite crucible. Then, it passes through the quartz crucible and is then taken into the melt. Further, segregation from the melt into the growing single crystal results in LT degradation and LPD abnormality in the crystal quality of the produced single crystal.
- the production method of the present invention is suitable for multi-pooling in which a plurality of single crystals are pulled up from the same crucible while recharging the raw material.
- three or more single crystals are used for low-speed growth and four or more single crystals are used for high-speed growth. It is suitable for multi-pooling that is pulled up.
- Ni has a large diffusion coefficient in the graphite material and in the quartz material among the metal impurities in the graphite component, and since the concentration in the graphite material is relatively high, when a graphite component having a concentration exceeding 30 ppb is used, This will affect the crystal quality.
- FIG. 1 is a schematic view of a single crystal production apparatus that can be used in the production method of the present invention.
- a quartz crucible 5 for storing the melt 4 and a graphite crucible 6 for supporting the quartz crucible 5 are arranged in the main chamber 2.
- the crucibles 5 and 6 are supported by a support shaft 11 that can be rotated up and down by a rotation drive mechanism (not shown) attached to the lower part of the single crystal manufacturing apparatus 1.
- the support shaft 11 is usually made of metal.
- a graphite pedestal 8 serving as a base for the crucibles 5 and 6 is connected to the support shaft 11, and the crucibles 5 and 6 are supported by the pedestal 8 via a graphite crucible tray 7.
- a heater 9 that surrounds the crucibles 5 and 6 and heats the melt 4 and a heat insulating member 10 disposed between the heater 9 and the inner wall of the main chamber 2 are provided.
- a pulling shaft (wire or shaft or the like) 14 for pulling up the seed crystal 13 is provided above the crucibles 5 and 6, a pulling shaft (wire or shaft or the like) 14 for pulling up the seed crystal 13 is provided.
- the Ni concentration of at least one graphite part used in a furnace for manufacturing the single crystal is analyzed, and the analyzed Ni concentration A single crystal is produced using a graphite part of 30 ppb or less.
- a graphite part having a Ni concentration of more than 30 ppb is used, Ni is mixed as an impurity in the manufactured single crystal, resulting in LT degradation and LPD abnormality. Therefore, by using a graphite part that is analyzed in advance and has a Ni concentration of 30 ppb or less, a high-quality single crystal that does not cause LT degradation or LPD abnormality can be produced with high productivity.
- the graphite component used by analyzing the Ni concentration is not particularly limited and can be any graphite component, but this causes a problem in terms of cost.
- the graphite component used by analyzing the Ni concentration in the present invention is at least one of the graphite component that is in direct contact with the quartz crucible 5 and the graphite component that is in direct contact with the quartz crucible 5 through the graphite component in direct contact.
- One is preferable.
- Graphite crucibles, crucible pans, and pedestals are made of graphite material and are close to the quartz crucible containing the melt, and Ni is easily diffused and taken into the melt.
- Ni concentration 30 ppb or less By using a Ni concentration of 30 ppb or less, LT reduction and LPD abnormality can be more effectively prevented.
- the priority order that needs to be Ni concentration 30 ppb or less is the order of the graphite crucible, the crucible tray, and the pedestal.
- the graphite component analyzed in the present invention may be other than the graphite crucible 6, the crucible tray 7, and the pedestal 8. Even graphite parts other than graphite crucible 6, crucible tray 7 and pedestal 8 are used after being analyzed in the present invention, so that any graphite parts with a Ni concentration of 30 ppb or less are used reliably. Thus, it is possible to prevent parts contaminated with Ni from being used as in the conventional case where analysis has not been performed. Accordingly, it is possible to exert an effect of suppressing LT reduction and LPD abnormality. In particular, the effect can be achieved with a graphite part used immediately above the quartz crucible 5.
- the method for analyzing the Ni concentration is a high-sensitivity analysis method in which a graphite material of a graphite part is plasma ashed and acid-dissolved.
- a graphite material of a graphite part is plasma ashed and acid-dissolved.
- metal impurities Fe, Al, Ni, Cr, etc.
- the lower limit of quantification was 50 to 100 ppb, and a concentration of 50 to 100 ppb or less could not be measured.
- Such an analysis method is sufficient for the standard of metal impurity concentrations (Fe, Al, Ni, Cr, etc.) of conventional graphite parts (about 300 ppb for ultra-high-purity graphite material and about 500 ppb for high-purity graphite material). It was the lower limit of quantification. However, with such a conventional method, it is impossible to analyze a Ni concentration of 30 ppb or less at which LT reduction or LPD abnormality occurs. On the other hand, the lower limit of quantification of the Ni concentration in the high-sensitivity analysis method as described above is 5 ppb, and it can be accurately identified whether it is 30 ppb or less, and the production method of the present invention can be reliably carried out. However, any analytical method with a Ni concentration lower limit of 30 ppb or less can be used in the present invention and is not limited to the above method.
- a graphite part having a Ni concentration of 30 ppb or less can be obtained by processing a graphite material having a Ni concentration of 30 ppb or less to produce a graphite part.
- the Ni concentration may be set to 30 ppb or less by performing purification and the like. That is, the Ni concentration of the resulting graphite part may be 30 ppb or less.
- a single crystal is manufactured as follows.
- the polycrystalline raw material filled in the quartz crucible 5 is heated by a heater 9 to form a melt 4, a seed crystal 13 is immersed in the melt 4, and a single crystal ( Ingot) 12 is grown.
- the single crystal 12 can be grown while applying a magnetic field to the melt 4.
- a single crystal when performing multi-pooling, a single crystal can be similarly manufactured by pulling up a single crystal 12 and then recharging the polycrystalline raw material in the quartz crucible 5. Multi-pooling that repeatedly pulls up such a single crystal can produce a plurality of single crystals from a quartz crucible that can only be used once and cannot be reused, thereby improving the production yield and reducing the cost of the quartz crucible. .
- LT decreases even for single crystals after three pulls.
- Example 1-3 Impurity concentration is analyzed by a high-sensitivity analysis method, and multi-pooling (5-drawing) is performed in a single crystal manufacturing apparatus using a graphite crucible with Ni concentration of 15 ppb to 30 ppb, Fe concentration of 45 ppb to 131 ppb, and Cr concentration of 35 ppb to 118 ppb.
- the single crystal production according to) was carried out.
- the manufactured single crystal was inspected for LT and LPD, the LT value was not lowered for single crystals after three pulls, and no abnormality of LPD was observed. Tables 1 and 2 show the results.
- Example 4-6 The Ni concentration is analyzed by a high-sensitivity analysis method. This is a single crystal manufacturing apparatus using a graphite crucible with a Ni concentration of 19 ppb to 30 ppb, a crucible tray with a Ni concentration of 23 ppb to 29 ppb, and a pedestal with a Ni concentration of 22 ppb to 28 ppb. Single crystal production was performed by pooling (5-drawing). When the manufactured single crystal was inspected for LT and LPD, the LT value was not lowered for single crystals after three pulls, and no abnormality of LPD was observed. Tables 3 and 4 show the results.
- the LT decrease and the LPD abnormality depend on the Ni concentration in the graphite, and the LT decrease and the LPD abnormality are suppressed at a Ni concentration of 30 ppb or less. Even if the Ni concentration in the graphite crucible is set to 30 ppb or less, LT reduction and LPD abnormality are effectively suppressed. Moreover, as can be seen from Tables 3 and 4, if the graphite crucible, the crucible tray, and the pedestal are all made to have a Ni concentration of 30 ppb or less, LT reduction and LPD abnormality are further suppressed.
- the present invention is not limited to the above embodiment.
- the above-described embodiment is an exemplification, and the present invention has substantially the same configuration as the technical idea described in the claims of the present invention, and any device that exhibits the same function and effect is the present invention. It is included in the technical scope of the invention.
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Abstract
Description
従来においては、これらの基準を満たす黒鉛材であれば、黒鉛材の不純物が単結晶に影響することが無かった。しかし、近年、低速で成長させる低欠陥結晶のマルチプーリング(一つのルツボから原料をリチャージすることで、多数本の単結晶を引き上げる方法)等によって、単結晶を製造する製造時間が過去の2~3倍に長くなり、黒鉛材中に含まれる不純物の内、特に黒鉛、石英、及びシリコン中での拡散係数が大きい不純物が、黒鉛材から外方拡散し、その後、融液を収容する石英ルツボを拡散して通過し、融液中に取り込まれ、さらに単結晶中に偏析し、単結晶の結晶品質に影響するようになった。
ここで、LTとは、光減衰法により測定され、半導体結晶中の少数キャリアが光で励起されて移動する時間を示し、金属不純物濃度が高いほど値が低くなる。また、LPDとは、単結晶から得られたウェーハにエピタキシャル層を形成し、そのエピタキシャル層表面をパーティクルカウンターで測定すると、0.09μm以上の結晶欠陥が観察され、これらのレーザ光を用いたウェーハ表面検査装置で観察される輝点欠陥の総称をLPDと称する。
このような黒鉛部品をNi濃度が30ppb以下とすることで、石英ルツボ内の融液へのNiの拡散を効率的に防止でき、単結晶のLT低下やLPD異常をより効果的に防止することができる。
このように黒鉛ルツボは、融液を収容する石英ルツボに直接接触しているため、Ni濃度30ppb以下とすることで、より効果的に単結晶のLT低下やLPD異常を防止することができる。
さらに、このような黒鉛部品をNi濃度30ppb以下とすることで、製造される単結晶のLT低下やLPD異常を確実に防止することができる。
このような高感度分析方法であれば、黒鉛部品の黒鉛材のNi濃度を30ppb以下まで定量的に分析することができるため、製造される単結晶のLT低下やLPD異常を確実に防止することができる。
黒鉛ルツボ中に含まれる不純物の内、特に拡散係数が大きい不純物が、長時間の単結晶製造中に黒鉛ルツボの基材内部から外方拡散し、黒鉛ルツボと接する石英ルツボの石英中に拡散して、石英ルツボを通過し、その後、融液中に取り込まれていく。そして、さらに融液から成長中の単結晶中に偏析し、製造された単結晶の結晶品質にLT低下やLPD異常が発生することになる。
図1は、本発明の製造方法で用いることができる単結晶製造装置の概略図である。
ルツボ5,6の上方には、種結晶13を引き上げるための引き上げ軸(ワイヤー又はシャフト等)14が設けられている。
Ni濃度が30ppbを超える黒鉛部品を使用すると、製造される単結晶にNiが不純物として混入し、LT低下やLPD異常を発生させてしまう。従って、予め分析してNi濃度が30ppb以下である黒鉛部品を使用することで、LT低下やLPD異常が発生しない高品質の単結晶を生産性良く製造することができる。
黒鉛ルツボ、ルツボ受皿、及びペディスタルは、黒鉛材が用いられ、融液を収容する石英ルツボに近接しており、Niが拡散して融液に取り込まれやすいため、本発明のように、分析してNi濃度が30ppb以下のものを用いることで、LT低下やLPD異常をより効果的に防止できる。この場合、Ni濃度30ppb以下とする必要がある優先順位は、黒鉛ルツボ、ルツボ受皿、ペディスタルの順である。もちろん、LT低下やLPD異常をより確実に防止するためには、黒鉛ルツボ6、ルツボ受皿7、及びペディスタル8の全てについて、分析してNi濃度が30ppb以下のものを用いることがより好ましい。
従来の黒鉛部品の黒鉛材の分析方法は、黒鉛を燃焼灰化した後、これを酸処理して、その酸溶解物を分析していたため、金属不純物(Fe,Al,Ni,Cr等)の定量下限が50~100ppbであり、50~100ppb以下の濃度を測定できなかった。このような分析方法は、従来の黒鉛部品の金属不純物濃度(Fe,Al,Ni,Cr等)の規格(超高純度黒鉛材が300ppb前後、高純度黒鉛材が500ppb前後)にとっては、十分な定量下限であった。しかし、このような従来の方法では、LT低下やLPD異常が発生する30ppb以下のNi濃度を分析することは不可能である。
一方、上記のような高感度分析方法のNi濃度の定量下限は5ppbであり、30ppb以下であるかどうかを精度良く識別でき、本発明の製造方法を確実に実施可能である。ただし、Ni濃度の定量下限が30ppb以下である分析方法であれば、本発明に用いることができ、上記の方法に限定されない。
石英ルツボ5内に充填された多結晶原料をヒータ9で加熱して融液4とし、この融液4に種結晶13を浸漬させ、引き上げ軸14で引き上げながら種結晶13の下端に単結晶(インゴット)12を成長させる。この際、MCZ法の場合は、融液4に磁場を印加しながら、単結晶12を成長させることができる。
(実施例1-3)
高感度分析方法で不純物濃度を分析して、Ni濃度が15ppb~30ppb、Fe濃度が45ppb~131ppb、Cr濃度が35ppb~118ppbの黒鉛ルツボを使用した単結晶製造装置で、マルチプーリング(5本引き)による単結晶製造を実施した。
製造された単結晶についてLT、LPDの検査を行ったところ、3本引き以降の単結晶についてもLT値に低下は無く、また、LPDの異常も観察されなかった。表1,2にその結果を示す。
高感度分析方法で不純物濃度を分析して、Ni濃度が38ppb~48ppb、Fe濃度が18ppb~125ppb、Cr濃度が15ppb~133ppbの黒鉛ルツボを使用した単結晶製造装置で、マルチプーリング(5本引き)による単結晶製造を実施した。
製造された単結晶についてLT、LPDの検査を行ったところ、特に3本引き以降の単結晶について、LT値に低下が生じ、また、LPDの異常も観察された。表1,2にその結果を示す。
高感度分析方法でNi濃度を分析して、Ni濃度が19ppb~30ppbの黒鉛ルツボ、Ni濃度が23ppb~29ppbのルツボ受皿、Ni濃度が22ppb~28ppbのペディスタルを使用した単結晶製造装置で、マルチプーリング(5本引き)による単結晶製造を実施した。
製造された単結晶についてLT、LPDの検査を行ったところ、3本引き以降の単結晶についてもLT値に低下は無く、また、LPDの異常も観察されなかった。表3,4にその結果を示す。
Claims (5)
- CZ法による単結晶の製造方法において、単結晶を製造する炉内で使用する少なくとも一つの黒鉛部品のNi濃度を分析して、該分析したNi濃度が30ppb以下の黒鉛部品を使用して前記単結晶を製造することを特徴とする単結晶の製造方法。
- 前記黒鉛部品を、石英ルツボに直接に接する黒鉛部品及び該直接に接する黒鉛部品を介して前記石英ルツボと間接的に接する黒鉛部品のうちの少なくとも一つとすることを特徴とする請求項1に記載の単結晶の製造方法。
- 前記黒鉛部品を、黒鉛ルツボとすることを特徴とする請求項1又は請求項2に記載の単結晶の製造方法。
- 前記黒鉛部品を、さらにルツボ受皿及びペディスタルの少なくとも一つとすることを特徴とする請求項3に記載の単結晶の製造方法。
- 前記Ni濃度を分析する方法を、前記黒鉛部品の黒鉛材をプラズマ灰化し、酸溶解したものを分析する高感度分析方法とすることを特徴とする請求項1乃至請求項4のいずれか一項に記載の単結晶の製造方法。
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KR1020147011472A KR101917851B1 (ko) | 2011-11-01 | 2012-10-02 | 단결정의 제조 방법 |
CN201280051969.0A CN103890241B (zh) | 2011-11-01 | 2012-10-02 | 单晶的制造方法 |
US14/350,269 US9738988B2 (en) | 2011-11-01 | 2012-10-02 | Method for manufacturing single crystal using a graphite component having 30 ppb or less nickel |
DE112012004206.9T DE112012004206B4 (de) | 2011-11-01 | 2012-10-02 | Verfahren zum Herstellen eines Einkristalls |
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JPH07223895A (ja) * | 1994-02-09 | 1995-08-22 | Toyo Tanso Kk | シリコン単結晶引上げ装置用ヒートシールド |
JPH08337493A (ja) * | 1995-06-15 | 1996-12-24 | Sumitomo Metal Ind Ltd | 単結晶引上げ用高純度黒鉛部材およびその製造方法 |
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- 2012-10-02 KR KR1020147011472A patent/KR101917851B1/ko active IP Right Grant
- 2012-10-02 CN CN201280051969.0A patent/CN103890241B/zh active Active
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KR20140088117A (ko) | 2014-07-09 |
US20140238292A1 (en) | 2014-08-28 |
DE112012004206B4 (de) | 2022-11-10 |
US9738988B2 (en) | 2017-08-22 |
DE112012004206T5 (de) | 2014-09-11 |
KR101917851B1 (ko) | 2018-11-13 |
CN103890241B (zh) | 2016-10-05 |
JP5782996B2 (ja) | 2015-09-24 |
JP2013095636A (ja) | 2013-05-20 |
CN103890241A (zh) | 2014-06-25 |
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