WO2013014831A1 - Procédé de fracturation d'une tige de silicium polycristallin - Google Patents

Procédé de fracturation d'une tige de silicium polycristallin Download PDF

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Publication number
WO2013014831A1
WO2013014831A1 PCT/JP2012/002691 JP2012002691W WO2013014831A1 WO 2013014831 A1 WO2013014831 A1 WO 2013014831A1 JP 2012002691 W JP2012002691 W JP 2012002691W WO 2013014831 A1 WO2013014831 A1 WO 2013014831A1
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Prior art keywords
polycrystalline silicon
silicon rod
impact force
crushing
central axis
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PCT/JP2012/002691
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English (en)
Japanese (ja)
Inventor
秀一 宮尾
岡田　淳一
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信越化学工業株式会社
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Publication of WO2013014831A1 publication Critical patent/WO2013014831A1/fr

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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
    • C01B33/02—Silicon

Definitions

  • the present invention relates to a method for crushing a polycrystalline silicon rod to obtain a polycrystalline silicon lump used for a nugget for charging a crucible for silicon single crystal growth by the CZ method.
  • Polycrystalline silicon having high purity is generally produced by a so-called Siemens method.
  • Siemens method a polycrystalline silicon rod (polycrystalline silicon rod) is obtained by growing (depositing) a silicon polycrystal on a heated silicon core wire by a CVD method.
  • Such polycrystalline silicon rods are currently over 100 mm in diameter and over 2000 mm in length.
  • Such a polycrystalline silicon rod is crushed into a polycrystalline silicon lump (crushed polycrystalline silicon), and is used, for example, as a nugget that is a raw material for silicon single crystal growth by the CZ method.
  • the polycrystalline silicon rod When processing a polycrystalline silicon rod into a raw material for silicon single crystal growth, etc., if the rod is crushed to a size that can be easily handled in advance, it is relatively easy to further crush it into a nugget size. It is.
  • the polycrystalline silicon rod has a large size of more than 100 mm in diameter and more than 2000 mm in length, and it is necessary to crush while preventing contamination in order to ensure the quality as a raw material for semiconductor manufacturing. Therefore, crushing work at an actual manufacturing site is not so easy.
  • Patent Document 1 Japanese Patent Application Laid-Open No. 7-618008
  • a rod is cracked by thermal shock by rapidly heating polycrystalline silicon deposited and grown in a rod shape by a thermal CVD method using a laser.
  • Patent Document 2 Japanese Patent Application Laid-Open No. 2011-46594 proposes a method in which a rod is cracked by causing local cooling after heating the rod.
  • Patent Document 3 Japanese Patent Application Laid-Open No. Hei 8-109903 describes that a manual hammer is used to crush the silicon lump as large as a fist.
  • any of the conventionally proposed methods for crushing polycrystalline silicon rods has room for improvement from the viewpoint of preventing contamination and productivity.
  • a method involving heating as disclosed in Patent Documents 1 and 2 requires a relatively large apparatus and complicated operations.
  • the method involving high-temperature heating as disclosed in Patent Document 2 is susceptible to contamination from the heating furnace.
  • the present invention has been made in view of the problems of such a conventional crushing method, and the object of the present invention is to provide a method for crushing a polycrystalline silicon rod that is easy to operate and hardly contaminates or contains foreign matter. It is to provide.
  • a polycrystalline silicon rod crushing method is a method for crushing a columnar polycrystalline silicon rod, wherein a mechanical component is provided in the central axis direction of the polycrystalline silicon rod. Applying an impact force of 1 to one end of the polycrystalline silicon rod to generate a first elastic wave, and crushing it into a polycrystalline silicon lump having a crushing surface that divides the central axis of the polycrystalline silicon rod; It is characterized by.
  • the method for crushing a polycrystalline silicon rod according to the present invention further includes applying a second impact force to the polycrystalline silicon rod within a time of less than 2 seconds before or after applying the first impact force.
  • a second impact force to the polycrystalline silicon rod within a time of less than 2 seconds before or after applying the first impact force.
  • the second impact force is applied to the other end which is the opposite end to the one end where the first impact force is applied to the polycrystalline silicon rod.
  • the application of the first impact force is performed in a state in which the other end which is the end opposite to the one end of the polycrystalline silicon rod is fixed.
  • the present invention provides a method for crushing a polycrystalline silicon rod that is easy to operate and hardly contaminates or contains foreign matter.
  • FIG. It is a figure for demonstrating the mode of crushing which gives the impact force of Example 3.
  • FIG. It is a figure for demonstrating a mode at the time of giving an impact on the single crystal silicon rod on the same conditions as Example 3 (comparative example 2).
  • FIG. It is a figure for demonstrating the mode of the crushing which gives the impact force of Example 4.
  • FIG. It is a figure for demonstrating the mode of crushing which gives the impact force of Example 5.
  • FIG. It is a figure for demonstrating the mode of crushing which gives the impact force of Example 6.
  • FIG. 1A is a cross-sectional view illustrating the most basic aspect of the polycrystalline silicon rod crushing method of the present invention.
  • reference numeral 10 is a columnar polycrystalline silicon rod
  • the axis indicated by C is the central axis (long axis) of the polycrystalline silicon rod 10.
  • silicon rods generally used have a length in the major axis direction of about 1500 to 2500 mm.
  • an impact force F 1 first impact force having a mechanical component in the direction of the central axis C is applied to one end portion of the polycrystalline silicon rod 10 by striking or the like. .
  • This impact force (striking force) F 1 generates an elastic wave (first elastic wave) inside the polycrystalline silicon rod 10 and divides the central axis C of the polycrystalline silicon rod 10 by this elastic wave. Crushing into a polycrystalline silicon lump having a crushing surface 1.
  • Examples of the method for applying the impact force include a manual hammer and an impact pulverizer.
  • the application of the first impact force is preferably performed in a state in which the other end, which is the end opposite to the one end of the polycrystalline silicon rod 10, is fixed.
  • the present inventors have fixed the end portion of the polycrystalline silicon rod 10 opposite to the end portion to which the first impact force is applied, so that the first impact force is fixed. It is considered that when the elastic wave generated by is reflected at the fixed end, the attenuation is suppressed and a strong standing wave-like elastic wave is formed.
  • the polycrystalline silicon rod 10 may be fixed, for example, by pressing the other end of the polycrystalline silicon rod 10 laid horizontally against a wall or a barrier provided on a jig on which the polycrystalline silicon rod 10 is placed. . There may be a method in which the polycrystalline silicon rod 10 is vertically set on the floor surface and an impact force is applied from above. However, since the polycrystalline silicon rod 10 is crushed in a manner that its long axis is divided, the safety aspect is increased. Is not preferable.
  • the impact force need not have a mechanical component only in the direction of the central axis C of the polycrystalline silicon rod 10 as shown in FIG. 1A.
  • the mechanical component F ′ 1 h in the direction of the central axis C of the polycrystalline silicon rod 10 and the mechanical component F ′ 1 v in the direction perpendicular to the central axis C are synthesized. It may be what was done.
  • the mechanical component F ′ 1h in the direction of the central axis C of the polycrystalline silicon rod 10 of the impact force is converted into the mechanical component in the direction perpendicular to the central axis C. It is preferable that it is larger than F ′ 1v . As shown in FIG. 1A, if an impact force is applied from the direction of the central axis C of the polycrystalline silicon rod 10 (a direction parallel to the center axis C), crushing can be most efficiently caused.
  • an impact force can be performed by a manual hammer, an impact pulverizer, or the like.
  • the impact force is sufficiently strong in order to prevent contamination from the jig to be used, mixing of foreign matters, and the like.
  • a jig made of a high strength material such as tungsten carbide or titanium can be exemplified.
  • the impact strength required for crushing depends on the crystal size and grain size distribution of the polycrystalline silicon rod, or the strain generated in the manufacturing process, so it is necessary to adjust the strength of the impact force when crushing. However, the adjustment is very easy.
  • the second impact force is applied to the polycrystalline silicon rod 10 within a period of less than 2 seconds before or after the application of the first impact force.
  • the elastic wave is generated. And it crushes into the polycrystal silicon lump which has the crushing surface which divides
  • Such a second impact force is preferably applied to the other end, which is the end opposite to the one end where the first impact force is applied to the polycrystalline silicon rod 10.
  • the second elastic wave only needs to be synthesized with the first elastic wave over the entire polycrystalline silicon rod 10. Moreover, since these two elastic waves should just be synthesize
  • the application of the first impact force and the application of the second impact force are not possible. If it is performed in less than 2 seconds, the effect of crushing by combining the first elastic wave and the second elastic wave can be sufficiently obtained.
  • the silicon rod is longer than the above, the time difference between applying the first and second impact forces is allowed to be larger. In this case, the first impact force may be applied first, or the second impact force may be applied first.
  • the first impact force is applied. It is preferable to apply a second impact force to one end (one end) of the polycrystalline silicon rod 10 on the opposite end (the other end) or in the vicinity thereof.
  • the second impact force is not limited as to the directionality as the first impact force.
  • the mechanical component in the direction perpendicular to the central axis C of the polycrystalline silicon rod 10 is used. It may have.
  • the mechanical component F ′ 2h in the direction of the central axis C of the polycrystalline silicon rod 10 having the second impact force is converted into the dynamic component F ′ in the direction perpendicular to the central axis C. It is preferable that it is larger than 2v . If the second impact force is applied from the direction of the central axis C of the polycrystalline silicon rod 10 (a direction parallel to the central axis C), crushing can be most efficiently caused.
  • Example 1 As shown in FIG. 2, the cylindrical polycrystalline silicon rod 10 is laid on the floor, and is on a vertical line passing through the central axis C, and the height from the floor is a quarter of the diameter D of the polycrystalline silicon rod 10. 3, the first and second impact forces (F 1 and F 2 ) having a dynamic component only in the direction of the central axis C are applied from one end and the other end, respectively, and the first and second elasticity A wave was generated. The magnitudes of the first and second impact forces were equal, and the strength was such that no crushing occurred alone, and the application was performed simultaneously.
  • a crushing surface 1 that divides the central axis C of the polycrystalline silicon rod 10 can be generated inside, and can be crushed into a polycrystalline silicon lump.
  • Example 2 As shown in FIG. 3, the cylindrical polycrystalline silicon rod 10 is laid on the floor, and is on a vertical line passing through the central axis C, and the height from the floor is half of the diameter D of the polycrystalline silicon rod 10.
  • the first and second impact forces (F 1 and F 2 ) having a dynamic component only in the direction of the central axis C are applied to the first point from one end and the other end, respectively.
  • a wave was generated.
  • the magnitudes of the first and second impact forces were equal, and the strength was such that no crushing occurred alone, and the application was performed simultaneously.
  • Example 3 As shown in FIG. 5, the cylindrical polycrystalline silicon rod 10 is laid on the floor and is on a perpendicular line passing through the central axis C, and the height from the floor is a quarter of the diameter D of the polycrystalline silicon rod 10.
  • the mechanical components (F 1h and F 2h ) in the direction of the central axis C of the polycrystalline silicon rod 10 and the mechanical components (F 1v and F 2v ) in the direction perpendicular to the central axis C are synthesized.
  • First and second impact forces (F 1 and F 2 ) were applied approximately symmetrically from one end and the other end to generate first and second elastic waves, respectively. The magnitudes of the first and second impact forces were equal, and the strength was such that no crushing occurred alone, and the application was performed simultaneously.
  • Example 4 As shown in FIG. 7, a cylindrical polycrystalline silicon rod 10 having a length in the major axis direction of about 2000 mm is laid on the floor, and is on a vertical line passing through the central axis C, and the height from the floor is polycrystalline.
  • a first impact force (F 1 ) having a mechanical component only in the direction of the central axis C is applied from one end to a third quarter of the diameter D of the silicon rod 10, and further, a second impact force (F 2 ) was added to the edge of the side surface in the vicinity of the other end to generate first and second elastic waves.
  • the magnitudes of the first and second impact forces were equal, and the strength was such that no crushing occurred alone, and the application was performed simultaneously.
  • a crushing surface 1 that divides the central axis C of the polycrystalline silicon rod 10 can be generated inside, and can be crushed into a polycrystalline silicon lump.
  • Example 5 As shown in FIG. 8, the cylindrical polycrystalline silicon rod 10 was laid on the floor of the fixing jig 2, and the other end of the polycrystalline silicon rod 10 was pressed against the barrier provided on the fixing jig 2. In the state, a first component having a mechanical component only in the direction of the central axis C at a point on a perpendicular line passing through the central axis C and having a height from the floor of 3 ⁇ 4 of the diameter D of the polycrystalline silicon rod 10. An impact force (F 1 ) was applied from one end to generate a first elastic wave.
  • a crushing surface 1 that divides the central axis C of the polycrystalline silicon rod 10 can be generated inside, and can be crushed into a polycrystalline silicon lump.
  • Example 6 As shown in FIG. 9, the cylindrical polycrystalline silicon rod 10 is laid on the floor and is on a perpendicular line passing through the central axis C, and the height from the floor is a quarter of the diameter D of the polycrystalline silicon rod 10.
  • F 1 first impact force
  • F 2 second impact force
  • a second elastic wave was generated from the other end. The magnitudes of the first and second impact forces are the same, and the strength is such that no single crushing occurs.
  • a crushing surface 1 that divides the central axis C of the polycrystalline silicon rod 10 can be generated inside, and can be crushed into a polycrystalline silicon lump.
  • the present invention provides a method for crushing a polycrystalline silicon rod that is easy to operate and hardly causes contamination or foreign matter.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

La présente invention concerne un procédé de fracturation d'une tige de silicium polycristallin. Selon l'invention, une force d'impact (F1) (première force d'impact) ayant un composant dynamique dans la direction d'un axe central (C) est appliquée à une extrémité d'une tige de silicium polycristallin (10). La force d'impact (force de frappe) (F1) génère une onde élastique (première onde élastique) dans la tige de silicium polycristallin (10) et, au moyen de cette onde élastique, la tige est fracturée en des morceaux de silicium polycristallin ayant une surface de fracture (1) qui fractionne l'axe central (C) de la tige de silicium polycristallin (10). La tige de silicium polycristallin est un ensemble de grains cristallins et il existe des variations localisées de résistance dans la tige. La force d'impact appliquée agit ainsi efficacement au niveau des zones de faiblesse de résistance localisée et il est possible de réaliser une fracturation sur l'ensemble de la longueur même si la tige de silicium polycristallin est longue.
PCT/JP2012/002691 2011-07-25 2012-04-18 Procédé de fracturation d'une tige de silicium polycristallin WO2013014831A1 (fr)

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JP2011162384A JP5689382B2 (ja) 2011-07-25 2011-07-25 多結晶シリコンロッドの破砕方法
JP2011-162384 2011-07-25

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Publication number Priority date Publication date Assignee Title
JP5984741B2 (ja) * 2013-05-28 2016-09-06 信越化学工業株式会社 多結晶シリコン棒の選択方法、および、ｆｚ単結晶シリコンの製造方法
DE102014201096A1 (de) * 2014-01-22 2015-07-23 Wacker Chemie Ag Verfahren zur Herstellung von polykristallinem Silicium
KR20220017394A (ko) * 2019-06-06 2022-02-11 가부시끼가이샤 도꾸야마 다결정 실리콘 로드의 절단 방법, 다결정 실리콘 로드의 컷 로드의 제조 방법, 다결정 실리콘 로드의 너깃의 제조 방법, 및 다결정 실리콘 로드의 절단 장치

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JPH01249618A (ja) * 1988-02-18 1989-10-04 Union Carbide Corp シリコン棒材から予め大きさを定めた粒子を形成する方法
JPH06271309A (ja) * 1993-03-22 1994-09-27 Sumitomo Sitix Corp 多結晶シリコンの破砕方法
JPH0761808A (ja) * 1993-08-26 1995-03-07 Koujiyundo Silicon Kk 多結晶シリコンの破砕方法
JPH08109013A (ja) * 1994-10-12 1996-04-30 Tokuyama Corp シリコン種の製造方法
JP2007296471A (ja) * 2006-04-28 2007-11-15 Nippon Steel Materials Co Ltd 多結晶シリコンの破砕方法
JP2010540395A (ja) * 2007-10-02 2010-12-24 ワッカー ケミー アクチエンゲゼルシャフト 多結晶シリコン及びその製造法
JP2011046594A (ja) * 2009-07-28 2011-03-10 Mitsubishi Materials Corp 多結晶シリコンロッドのクラック発生方法及びクラック発生装置
JP2011068558A (ja) * 2009-09-24 2011-04-07 Wacker Chemie Ag 改善された破砕特性を有するロッド状ポリシリコン

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DE19741465A1 (de) * 1997-09-19 1999-03-25 Wacker Chemie Gmbh Polykristallines Silicium
US7223303B2 (en) * 2004-08-26 2007-05-29 Mitsubishi Materials Corporation Silicon cleaning method for semiconductor materials and polycrystalline silicon chunk

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01249618A (ja) * 1988-02-18 1989-10-04 Union Carbide Corp シリコン棒材から予め大きさを定めた粒子を形成する方法
JPH06271309A (ja) * 1993-03-22 1994-09-27 Sumitomo Sitix Corp 多結晶シリコンの破砕方法
JPH0761808A (ja) * 1993-08-26 1995-03-07 Koujiyundo Silicon Kk 多結晶シリコンの破砕方法
JPH08109013A (ja) * 1994-10-12 1996-04-30 Tokuyama Corp シリコン種の製造方法
JP2007296471A (ja) * 2006-04-28 2007-11-15 Nippon Steel Materials Co Ltd 多結晶シリコンの破砕方法
JP2010540395A (ja) * 2007-10-02 2010-12-24 ワッカー ケミー アクチエンゲゼルシャフト 多結晶シリコン及びその製造法
JP2011046594A (ja) * 2009-07-28 2011-03-10 Mitsubishi Materials Corp 多結晶シリコンロッドのクラック発生方法及びクラック発生装置
JP2011068558A (ja) * 2009-09-24 2011-04-07 Wacker Chemie Ag 改善された破砕特性を有するロッド状ポリシリコン

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