WO2002000970A1 - Procede de production de monocristal de silicium - Google Patents

Procede de production de monocristal de silicium Download PDF

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Publication number
WO2002000970A1
WO2002000970A1 PCT/JP2001/005361 JP0105361W WO0200970A1 WO 2002000970 A1 WO2002000970 A1 WO 2002000970A1 JP 0105361 W JP0105361 W JP 0105361W WO 0200970 A1 WO0200970 A1 WO 0200970A1
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WO
WIPO (PCT)
Prior art keywords
single crystal
crystal
silicon single
producing
crucible
Prior art date
Application number
PCT/JP2001/005361
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English (en)
Japanese (ja)
Inventor
Makoto Iida
Yoshihiko Yamada
Original Assignee
Shin-Etsu Handotai Co., Ltd.
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Publication date
Application filed by Shin-Etsu Handotai Co., Ltd. filed Critical Shin-Etsu Handotai Co., Ltd.
Priority to JP2002506276A priority Critical patent/JP4007193B2/ja
Publication of WO2002000970A1 publication Critical patent/WO2002000970A1/fr

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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
    • 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
    • C30B15/203—Controlling or regulating the relationship of pull rate (v) to axial thermal gradient (G)

Definitions

  • the present invention relates to a method for producing a silicon single crystal by the Chiral Clarke method (CZ method).
  • Control factors in the method of manufacturing CZ silicon single crystals to achieve various quality requirements include impurity concentration and thermal history during crystal growth.
  • the ratio VZGs between the pulling speed V and the temperature gradient Gs of the crystal-solid interface can control two types of point defects: vacancies and interstitial silicon. It is a parameter that has attracted attention as a control factor for the growth-in (Grown-in) defect and oxygen deposition characteristics.
  • VGs may be set to be larger than a certain value over the entire surface in the crystal radial direction.
  • the crystal is grown at a higher pulling speed than the Gs.
  • the maximum pulling speed V max that can be pulled without causing such crystal deformation is determined by a function including G s.
  • Gs is determined by the temperature distribution of the internal structure (hot zone: HZ) of the pulling device, and the maximum pulling speed is determined by that Gs.
  • the crystal is grown at a pulling speed lower than the maximum pulling speed determined here.
  • VZGs For example, in order to prevent the occurrence of the OSF ring, it is necessary to set VZGs over a certain value over the entire surface in the radial direction of the crystal.
  • G s has a distribution that is higher in the periphery in the radial direction of the crystal, whereas V is constant in the radial direction. The value of s becomes smaller.
  • the maximum pulling speed without deformation is determined by the minimum value of G s, that is, the value of G s at the center of the crystal. Therefore, when the in-plane distribution of G s is large, the peripheral V / G s value cannot be made sufficiently large at the maximum pulling speed determined by the central G s, and the OSF ring around the periphery May not be suppressed.
  • Another method is to increase the maximum pulling speed without deformation for G s.
  • the temperature gradient G1 just below the melt interface which is another parameter that determines the maximum pulling speed without deformation, may be reduced.
  • the MCZ method magnetic-field-applied and zochralski method
  • MCZ method equipment The investment was expensive and the maintenance costs were high, all increasing the cost of the crystal. Disclosure of the invention
  • the main object of the present invention is to provide a method for producing a silicon single crystal that can be made large and that can reliably suppress the generation of OSF rings in the plane.
  • a method for producing a silicon single crystal according to the present invention is directed to a method for producing a silicon single crystal by the Czochralski method.
  • the inner diameter of the crucible to be accommodated is set to 2 to 2.5 times the target diameter of the silicon single crystal to be manufactured, and the pulling speed V and the solid-liquid interface temperature gradient G s in the crystal diameter direction are determined. It is characterized in that it is pulled up so that the minimum value of the ratio V / Gs becomes 0.3 mm 2 / K ⁇ min or more.
  • a crucible having an inner diameter of 2 to 2.5 times the target diameter of a silicon single crystal to be manufactured is used as a crucible for accommodating the raw material silicon.
  • G 1 can be reduced, and the maximum pulling speed V max at which the deformation of the silicon single crystal with respect to G s does not occur can be increased.
  • the pulling is made so that the minimum value of the in-plane V / Gs in the radial direction of the pulled crystal becomes 0.3 mm 2 / K ⁇ min or more, the entire in-plane Since V / Gs is at a high level, it is possible to reliably suppress the generation of the OSF ring, and it is possible to produce a high-quality silicon single crystal with high productivity.
  • a silicon single crystal doped with nitrogen can be pulled up.
  • VZGs when pulling a silicon single crystal doped with nitrogen, VZGs is set to 0.3 mm 2 ⁇ ⁇ mi 11 or more, for example, when a silicon wafer made from this single crystal is used to make an epitaxy wafer, Even at a relatively low nitrogen concentration of 1 ⁇ 10 14 / cm 3 or less, it is said that the epilayer defect is reduced and the gettering ability is improved by the high BMD density in the bulk. These two effects can be achieved simultaneously.
  • another method for producing a silicon single crystal according to the present invention is a method for producing a silicon single crystal doped with nitrogen by the Czochralski method.
  • the crucible for accommodating a cone is pulled up using a crucible having an inner diameter of 2 to 2.5 times the target diameter of the silicon single crystal to be manufactured. .
  • the target of the silicon single crystal to be produced is used as a crucible for accommodating the original family silicon.
  • G 1 can be reduced, and the deformation of the silicon single crystal with respect to G s occurs.
  • the maximum pulling speed V max can be increased, and crystals can be produced efficiently.
  • the inner diameter of the heater be 2.5 to 3 times the crystal diameter.
  • the inner diameter of the heater placed around the crucible is desirably 2.5 to 3 times the crystal diameter. Because, for heater diameters that are too large, more than three times the crystal diameter, the convective distribution of the melt in the crucible changes significantly, and the pulling rate for G s is low. They may not be as fast.
  • the rotation speed of the crystal be 5 to 25 rpm.
  • the rotation speed of the crucible is 0.1 to 20 rpm in the method for producing a silicon single crystal.
  • the present invention it is possible to further improve the maximum pulling speed at which a pulled single crystal does not deform, and to obtain a high-quality silicon that avoids the generation of an OSF ring.
  • the present invention can provide a manufacturing method capable of growing a silicon single crystal at a lower cost.
  • Figure 1 shows the relationship between the crystal solid-liquid interface temperature gradient G s and the maximum pulling speed V max at which the crystal is not deformed, as seen by the ratio c / d between the inner diameter c of the quartz crucible and the diameter d of the pulled single crystal. It is the figure which did.
  • FIG. 2 is a result diagram showing the in-plane distribution of the solid-liquid interface temperature gradient G s in the crystal diameter direction during pulling in Example 1 and Comparative Example 1.
  • Figure 3 shows the in-plane distribution of the ratio V raax / G s between the maximum pulling rate V max in the crystal diameter direction and the temperature gradient G s of the crystal solid-liquid interface in Example 1 and Comparative Example 1. It is a figure.
  • FIG. 4 is a schematic diagram qualitatively showing the relationship between cZd and Vmax / Gs.
  • FIG. 5 is a schematic explanatory diagram of a single crystal pulling apparatus by the CZ method used in the present invention.
  • the present inventors have found that in the ordinary CZ method that does not require a large investment and maintenance cost such as the MCZ method, the temperature gradient G1 of the melt is reduced and the maximum pulling rate with respect to Gs is increased. It is considered that the factors that may determine the temperature gradient of the melt c, which have been studied extensively, are the temperature distribution in the furnace and the convection of the melt. Therefore, when experiments were conducted with various norameters considered to be effective for these, the ratio between the crystal diameter and the crucible inner diameter was large in the temperature gradient G1 of the melt. The inventor has discovered that the influence is exerted, and reached the present invention.
  • the crucible inner diameter of the crucible is usually about three times the diameter of the crystal, sometimes called the triple law.
  • a 22-inch (about 55 Omm) or 24-inch Quartz crucibles (about 60 Omm) are usually used.
  • the integrated heat transfer analysis software FEMAG F. Dupret, P. Nicodeme, Y. Ryckmans, G s was calculated using PW outers, and M.J.Crochet, Int.J.Heat Mass Transfer, 33, 1849 (1900), and the crystal was experimentally obtained.
  • V max with respect to G s is up to a level comparable to the maximum pulling speed when pulling up by applying a magnetic field using a crucible with a normal inner diameter according to the triple law, regardless of the application of a magnetic field. It was confirmed that it was increasing.
  • V max / G s 0 in the method (magnetic field application teeth) in the center which uses the conventional large crucible. 3 5 mm 2 / K ⁇ min, been made at 0. 2 mm 2 / K ⁇ min approximately around
  • V max / G s 0.47 mm 2 / K-min, It is now possible to grow around 0.32 mm 2 /K.min around. As a result, it is possible to achieve high VGs over the entire surface in the crystal diameter direction at low cost without installing expensive equipment necessary for applying a magnetic field. But it was hot.
  • the temperature gradient G 1 of the melt becomes smaller, the maximum pulling rate with respect to the temperature gradient G s of the crystal becomes larger, so that the inner diameter of the crucible should be smaller than usual. It is inferred that the temperature gradient of the melt became smaller.
  • the rotation speed of the crystal is 5 to 25 rpm.
  • the rotation speed of the crucible it is preferable to set the rotation speed of the crucible to 0.1 to 20 rpm. If the crucible does not rotate at all, the convection will change because the melt is not agitated. When the crucible rotation speed exceeds 20 r, the melt surface vibrates, which may cause deformation and disorder of the crystal. is there.
  • the single crystal pulling apparatus 30 includes a pulling chamber 31, a crucible 32 provided in the pulling chamber 31, and a crucible 32 disposed around the crucible 32.
  • the crucible 32 is provided with a quartz crucible on the inner side for containing the silicon melt 2 and a graphite crucible on the outer side. Further, a heat insulating material 35 is arranged around the outside of the heater 34.
  • an annular solid-liquid interface heat insulator 8 is provided around the solid-liquid interface of the crystal, and an upper surrounding heat insulator 9 is placed thereon.
  • the solid-liquid interface heat insulating material 8 is provided with a gap of 3 to 5 cm between the lower end thereof and the molten metal surface of the silicon melt 2.
  • the upper surrounding insulating material 9 may not be used depending on the conditions.
  • a cylindrical cooling device 36 for spraying a cooling gas or cooling a single crystal by blocking radiant heat may be provided.
  • a method for growing a single crystal using the single crystal pulling apparatus 30 shown in FIG. 5 will be described.
  • a crucible 32 a high-purity polycrystalline silicon material is melted by applying heat to a temperature higher than the melting point (about 144 ° C).
  • the tip of the seed crystal 5 is brought into contact with or immersed substantially in the center of the surface of the melt 2.
  • the crucible holding shaft 33 is rotated in an appropriate direction, and while the wire 7 is being rotated, the winding seed crystal 5 is pulled up to start single crystal growth. Is done. Thereafter, by adjusting the pulling speed and the temperature appropriately, it is possible to obtain a substantially cylindrical single crystal rod 1.
  • the ratio c / d of the inner diameter c of the crucible accommodating the raw material to the diameter d of the pulled crystal is 2.0 to 2.5. .
  • Figure 4 qualitatively shows the relationship between c / d and Vmax / Gs. is there.
  • d is less than 1
  • crystal growth also occurs from the inner wall of the crucible, which is released. It is not appropriate because it causes problems such as dislocations in the pulled crystal and makes pulling extremely difficult.
  • 1.6 to 2.0 single crystal growth is not impossible, but it lacks the stability of continuous operation, so it is not suitable for an actual mass production system that requires low cost.
  • the specific inner diameter of the crucible is 12 to 15 inches, respectively. (300 to 375 mm), 16 to 20 inches (400 to 500 mm), and 24 to 30 inches (600 to 750 mm) Can be used. This made it difficult to satisfy the conventional pulling method using a crucible with an inner diameter exceeding 2.5 times the diameter of the pulled crystal without applying a magnetic field.
  • the pulling condition that s is 0.3 mm 2 / K ⁇ mi ⁇ or more can be extremely easily achieved.
  • V / Gs is not sufficient at the periphery of the crystal by simply using a crucible having an inner diameter of 2.5 times or less the diameter of the pulled crystal, a heat insulating material constituting HZ should be used. With simple improvements such as removal, it is possible to further increase V max and consequently increase V / G s; ⁇ FEMAG ( This was confirmed by a thermal analysis simulation using the above method.
  • the VZG s value should be larger than 0.3 mm 2 / K'mi ⁇ , but if it is too large, the crystal will be deformed.
  • the limit is usually about 0.55 mm 2 / K ⁇ min.
  • Nitrogen with a diameter of 8 inches (200 mm), p-type, and crystal orientation of 100> was doped under the conditions shown in Table 1, respectively.
  • a silicon single crystal was pulled.
  • Nitrogen is doped by introducing a predetermined amount of silicon wafer with a nitride film into the raw material, and the nitrogen concentration at the shoulder of the pulled crystal is calculated to be 2 ⁇ 10 13 / cm It was set to be 3 .
  • the in-plane distribution of G s in the crystal diameter direction during the pulling was calculated from FEMAG and shown in Figure 2.
  • the in-plane distribution of V max / G s is shown in FIG. 3 ⁇ V max is about 1.05 mm Z min for Example 1 and about 1.1 mm Z min for Comparative Example 1 force. Therefore, V max itself is slightly smaller in the first embodiment, as shown in FIG. 3 and Table 1 and as shown in Table 1, V max against G s, that is, V max / G s Example 1 is overwhelmingly larger in Example 1, and only Example 1 satisfies V max / G s ⁇ 0.3 mm 2 / K Power.
  • Example 1 a slab having a thickness of about 2 mm was cut out from the crystals grown in Example 1 and Comparative Example 1 perpendicularly to the crystal axis direction, and the surface distortion was reduced with a hydrofluoric / nitric acid-based mixed acid. Removed. Next, the sample was subjected to an oxidizing heat treatment in a wet oxygen atmosphere at 115 ° C. for 100 minutes, and the presence or absence of an OSF ring was confirmed in the sample that was selected and etched. As a result, no OSF ring was generated in the crystal of Example 1, but an OSF ring was generated in the periphery of the crystal of Comparative Example 1. .
  • Example 2 Using the same pulling device as in Example 1, an 8-inch single crystal doped with nitrogen was pulled up under the same pulling conditions as in Example 1 with a structure in which some heat insulating material of HZ was removed.
  • V max is obtained at 1.33 mm / min
  • V max / Gs around 10 mm around is 0.350 mm 2 / K ⁇ min.
  • the improvement of G s was confirmed.
  • Table 1 shows the pulling conditions and results.
  • Example 2 As to the crystal of Example 2, it was confirmed whether or not an OSF ring was generated in the same manner as in Example 1, and it was found that generation of an OSF ring was not recognized.
  • Ratio to inner diameter c Inner diameter times fe3 ⁇ 4 Gs in rotation speed (mm / min) Vmax / Gs of Gs near Vmax / Gs
  • Example 1 1 8 2.25 21.5 8 20 1.05 2.38 0.441 3.07 0.342
  • Example 2 1 8 2.25 21.5 8 20 1.33 2.75 0.484 3.80 0.350 Comparative Example 1 2 2 2.75 25.8 8 18 1.10 3.20 0.343 4.30 0.256 CO
  • Example 3 the presence or absence of the generation of the OSF ring was confirmed in the same manner as in Example 1. As a result, no OSF ring occurred in the crystal of Example 3, but an OSF ring was observed in the periphery of the crystal of Comparative Example 2.
  • the present invention is not intended to prohibit the application to the pulling method to which a magnetic field is applied, but may be applied to the so-called MCZ method.
  • V max with respect to G s is larger than that in the case where the above-mentioned magnetic field is applied to the printing force [J without pulling the ordinary CZ method.
  • the improvement effect is small, some improvement effect can be expected.

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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)

Abstract

L'invention concerne un procédé de production de monocristal de silicium selon la technique CZ, à savoir que le diamètre intérieur (c) d'un creuset (32) contenant un matériau de silicium brut est 2 à 2,5 fois le diamètre escompté (d) du monocristal (1) de silicium à produire. Ledit monocristal de silicium est tiré de façon que la valeur minimale d'un rapport (V/Gs), dans le sens du diamètre d'une vitesse (V) de tirage vers un gradient de température (Gs) à l'interface entre le solide et le liquide dans le cristal, soit d'au moins 0,3 mm2/K.min. Le procédé permet d'abaisser le gradient de température (G1) dans un bain de fusion, d'augmenter la vitesse maximale du tirage, et de supprimer la survenue d'un anneau OSF, d'utiliser la technique classique CZ, avec facilité et simplicité, et à un coût réduit.
PCT/JP2001/005361 2000-06-27 2001-06-22 Procede de production de monocristal de silicium WO2002000970A1 (fr)

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JP2002506276A JP4007193B2 (ja) 2000-06-27 2001-06-22 シリコン単結晶の製造方法

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JP2000192317 2000-06-27

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002076007A (ja) * 2000-08-31 2002-03-15 Mitsubishi Materials Silicon Corp エピタキシャルウェーハの製造方法及びその方法により製造されたエピタキシャルウェーハ
WO2005010242A1 (fr) * 2003-07-29 2005-02-03 Shin-Etsu Handotai Co., Ltd. Procede et dispositif destines a la production d'un monocristal

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10310485A (ja) * 1997-04-30 1998-11-24 Sumitomo Sitix Corp 単結晶育成方法
WO1999057344A1 (fr) * 1998-05-01 1999-11-11 Nippon Steel Corporation Plaquette de semi-conducteur en silicium et son procede de fabrication
JP2000211995A (ja) * 1998-11-17 2000-08-02 Shin Etsu Handotai Co Ltd シリコン単結晶ウエ―ハおよびシリコン単結晶ウエ―ハの製造方法
JP2000277527A (ja) * 1999-03-26 2000-10-06 Mitsubishi Materials Silicon Corp シリコンウェーハ及びその製造方法。
JP2000351690A (ja) * 1999-06-08 2000-12-19 Nippon Steel Corp シリコン単結晶ウエーハおよびその製造方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10310485A (ja) * 1997-04-30 1998-11-24 Sumitomo Sitix Corp 単結晶育成方法
WO1999057344A1 (fr) * 1998-05-01 1999-11-11 Nippon Steel Corporation Plaquette de semi-conducteur en silicium et son procede de fabrication
JP2000211995A (ja) * 1998-11-17 2000-08-02 Shin Etsu Handotai Co Ltd シリコン単結晶ウエ―ハおよびシリコン単結晶ウエ―ハの製造方法
JP2000277527A (ja) * 1999-03-26 2000-10-06 Mitsubishi Materials Silicon Corp シリコンウェーハ及びその製造方法。
JP2000351690A (ja) * 1999-06-08 2000-12-19 Nippon Steel Corp シリコン単結晶ウエーハおよびその製造方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002076007A (ja) * 2000-08-31 2002-03-15 Mitsubishi Materials Silicon Corp エピタキシャルウェーハの製造方法及びその方法により製造されたエピタキシャルウェーハ
WO2005010242A1 (fr) * 2003-07-29 2005-02-03 Shin-Etsu Handotai Co., Ltd. Procede et dispositif destines a la production d'un monocristal

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