WO2003091484A1 - Procede de production d'un cristal unique de silicium et plaquette de cristal unique de silicium - Google Patents

Procede de production d'un cristal unique de silicium et plaquette de cristal unique de silicium Download PDF

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Publication number
WO2003091484A1
WO2003091484A1 PCT/JP2003/005243 JP0305243W WO03091484A1 WO 2003091484 A1 WO2003091484 A1 WO 2003091484A1 JP 0305243 W JP0305243 W JP 0305243W WO 03091484 A1 WO03091484 A1 WO 03091484A1
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Prior art keywords
single crystal
crystal
region
silicon single
silicon
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PCT/JP2003/005243
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English (en)
Japanese (ja)
Inventor
Masahiro Sakurada
Tatsuo Mori
Izumi Fusegawa
Tomohiko Ohta
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Shin-Etsu Handotai Co.,Ltd.
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Publication of WO2003091484A1 publication Critical patent/WO2003091484A1/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
    • C30B15/32—Seed holders, e.g. chucks

Definitions

  • the present invention is directed to a defect-free area having no defects in any of the V area, the I area, and the OSF area as described later, and having no defects detected from the u deposition.
  • the present invention relates to a method for producing a silicon single crystal at high speed and in a stable manner. Background art
  • V vacancies
  • I interstitials-silicon
  • the V region is a region where there are many Vacancy, that is, recesses and holes generated due to lack of silicon atoms, and the I region. This is a region where dislocations and extra silicon atom lumps are generated due to the presence of extra silicon atoms.
  • Ma In addition, between the V region and the I region, there is a Neutran 1 (Neutra 1; hereafter, sometimes abbreviated as N) region with no (small) lack or excess of atoms. It will be.
  • the above-mentioned green-in defect (FPD, LSTD, COP, etc.) is the result of point defects agglomerating when V and I are over-saturated. It can be seen that point defects do not aggregate and do not exist as the above-mentioned glow-in defects, even if there is some deviation of atoms, even if there is a certain degree of saturation, if they are less than saturation. I came.
  • the concentration of these two point defects is determined by the relationship between the crystal pulling rate (growth rate) in the CZ method and the temperature gradient G near the solid-liquid interface in the crystal, and the boundary between the V region and the I region is determined.
  • OSF Oxidation Induced Stacking Fault
  • Defects Large Dislocations: LDSD, LSEPD, LFPD, etc. defects (Large Dislocation Clusters) which are considered to be caused by dislocation loops
  • the area where these are present at low density and these defects are present is called the I area (sometimes called the LZD area).
  • the OSF ring shrinks to the center of the wafer and disappears, and the entire surface becomes the I region (see the line in FIG. 6).
  • these N regions exist obliquely with respect to the growth axis direction when the growth rate is reduced, so that only a part of the N region exists in the aeah plane (see, for example, FIG. 6).
  • V.V.V oronkov For this N region, the Boronkov theory (V.V.V oronkov; Journal rystal G rowth, 59 (1992) 625-643) raises It is proposed that the VZG, a ratio of the velocity (V) and the temperature gradient (G) in the crystal-liquid interface axis direction, determines the total concentration of point defects. Considering this fact, since the pulling rate (growth rate) should be almost constant in the plane, G has a distribution in the plane. At the raising speed, a force was obtained that could only obtain a crystal whose center was in the V region, sandwiched the N region, and became the I region in the periphery.
  • the distribution of G in the plane was improved, and the N region, which existed only at an angle, was pulled up, for example, while gradually lowering the pulling rate (growth rate).
  • the pulling rate growth rate
  • the crystal in the entire N region in the length direction it can be achieved to some extent by pulling up while maintaining the pulling speed when the N region spreads laterally.
  • the pulling speed so that V / G remains constant, the growth direction will be more
  • the crystal in the entire N region can be expanded.
  • the entire surface is in the N region, and although it is a single crystal that does not generate an OSF ring when subjected to thermal oxidation and has no FPD or LZD on the entire surface. It was found that oxide film defects could occur significantly. This causes electrical characteristics such as oxide withstand voltage characteristics to deteriorate, and it is not sufficient to merely say that the entire surface of the conventional device is in the N region. Further improvement was desired.
  • the present invention provides a method for producing a silicon single crystal by the chiral scan method, in which a V region, an OSF region, and an interstitial silicon region of a vacancy rich are provided.
  • a V region, an OSF region, and an interstitial silicon region of a vacancy rich are provided.
  • the objective is to provide a defect-free silicon single crystal wafer with excellent electrical properties at a low cost.
  • the present invention it is housed in a crucible. After the seed crystal is brought into contact with the silicon melt, the seed crystal is pulled up from a rotating force S to grow a silicon single crystal by the Chiocular key method.
  • the crucible is rotated without rotating or in the same direction as the rotation direction of the seed crystal, and a ring shape is formed when the thermal oxidation treatment is performed.
  • the silicon is characterized by growing a crystal in an N region outside the OSF generated in the defect free region where there is no defect region detected by Cu deposition.
  • a method for producing a single crystal is provided.
  • the entire region includes defects such as FPDs in the V region and giant dislocation clusters in the I region (LSEPD, LFPD). ) And N region where OSF defects are not formed, and there are no defects and no defects (Cu deposition defects) detected by Cu deposition.
  • a silicon single crystal can be manufactured faster and more stably than before.
  • the seed crystal is pulled up while being rotated while rotating the silicon single crystal.
  • the crucible is rotated without being rotated or in the same direction as the rotation direction of the seed crystal.
  • the defect area detected by the Cu deposition remaining after the OSF ring disappears.
  • the crystal growth is controlled by controlling the growth rate between the boundary growth rate and the growth rate at the boundary where interstitial dislocation loops occur when the growth rate is further reduced.
  • a method for producing a silicon single crystal is also provided.
  • the rotation speed of the crucible is set in a range of 0 to 2 rpm.
  • a defect-free silicon single crystal wafer characterized by being sliced from silicon single crystal gas grown by the above method is provided. .
  • Such silicon wafers do not include V region defects such as FPDs, I region defects such as giant dislocation clusters, and OSF defects, and have a Cu deposition. It will be a defect-free silicon single crystal wafer with no defects, high breakdown voltage and excellent electrical characteristics, and will be inexpensive because it is grown at high speed.
  • FPD Flow Pattern Defect
  • a wafer is cut out from a silicon single crystal rod after growth, and the strained layer on the surface is etched with a mixed solution of hydrofluoric acid and nitric acid. After removal by etching, the surface is etched (Secco etching) with a mixture of K 2 Cr 2 O 7 , hydrofluoric acid and water. Cuts and ripples occur. This ripples The higher the FPD density in the wafer surface, the more the oxide film withstand pressure increases (see Japanese Patent Application Laid-Open No. 1991-92445).
  • SEPD Secco Etch Pit Defect
  • LSTD Laser Scatting Tomography Defect
  • a silicon monocrystal rod is cut out from a grown silicon single crystal rod, and the strained surface layer is mixed with hydrofluoric acid and nitric acid. After removal by etching with liquid, the wafer is cleaved. Infrared light is incident from this cleavage plane, and light emitted from the wafer surface is detected to detect scattered light due to defects existing in the wafer. And can be. Scatterers observed here have already been reported at academic meetings and are considered to be oxygen precipitates (Jpn. J. Appl. Phys. Vol. 32, P36). 79, 1993). Recent studies have also reported that it is an octahedral void.
  • COP Crystal Originated Particulate 1e
  • the diameter of this pit is less than 1 ⁇ m and is examined by the light scattering method.
  • L / D (Large D is 1 ocation) is an abbreviation of interstitial dislocation loop, which includes LSEPD and LFPD. These defects are thought to be caused by dislocation loops in which the aggregates aggregate.
  • LSEPD refers to those larger than 1 ⁇ among SEPDs.
  • LFPD refers to the above-mentioned FPDs whose tip pits have a size of 1 O / xm or more, and this is also considered to be caused by a dislocation loop.
  • the Cu deposition method accurately measures the position of defects in semiconductor wafers, improves the detection limit for defects in semiconductor wafers, and accurately measures even finer defects. It can be analyzed.
  • a specific method of evaluating wafers is to form an oxide film of a predetermined thickness on the wafer surface, and to destroy the oxide film on a defect site formed near the wafer surface to obtain a defect.
  • Electrode such as Cu is deposited (deposition) on the site.
  • a potential is applied to an oxide film formed on the wafer surface in a liquid in which Cu ions are dissolved, a current is supplied to a portion where the oxide film has deteriorated.
  • This is an evaluation method that utilizes the fact that the flow and Cu ions are precipitated as Cu. It is known that defects such as COP exist in portions where the oxide film is easily deteriorated.
  • the defect site of the wafer that has been Cu deposited can be analyzed under the condensing light or directly with the naked eye to evaluate its distribution and density.
  • a silicon single crystal in a defect-free region that does not include a V region, an OSF region, an I region, and a Cu deposition defect region is rapidly drawn. Can be raised. Therefore, silicon single crystals that can improve electrical characteristics such as oxide film breakdown voltage can be manufactured at high speed and in a stable manner, and defect-free silicon with high breakdown voltage and excellent electrical characteristics can be obtained. Can be provided at a low cost.
  • FIG. 1 shows an example of a silicon single crystal manufacturing apparatus that can be used in the present invention.
  • Figure 2 is a graph showing the defect-free region growth rate.
  • Figure 3 is a graph showing the relationship between the crucible rotation speed and the defect-free region growth rate.
  • Figure 4 is a graph showing the relationship between the crucible rotation and the temperature gradient in the direction of the crystal interface axis.
  • Figure 5 is a graph showing the relationship between crucible rotation speed and initial oxygen concentration.
  • FIG. 6 is an explanatory diagram showing a growth rate and a crystal defect distribution according to a conventional technique.
  • the present inventors have investigated in detail the vicinity of the boundary between the V region and the I region with respect to the silicon single crystal growth by the CZ method, and found that the OSF region is located between the V region and the I region. Outside the ring, a neutral N region was found in which the number of FPDs, LSTDs, and COPs was very small and L / D was absent.
  • the present inventors conducted a more detailed investigation on the N region by the Cu deposition method, and found that the N region outside the OSF region was used. Therefore, it is evident that some of the regions where oxygen precipitation is likely to occur after the precipitation heat treatment have regions where defects detected by the Cu deposition process are significantly generated. discovered. The inventors have also found that this causes deterioration of electrical characteristics such as oxide breakdown voltage characteristics.
  • a defect-free area growth rate By growing a single crystal at a rate between the above (hereinafter, sometimes referred to as a defect-free area growth rate), it is possible to eliminate the various types of green-in defects.
  • a defect-free silicon single-crystal silicon wafer capable of reliably improving the oxide film breakdown voltage characteristics and the like was obtained.
  • the growth rate of such a defect-free region needs to be lower than the conventional single crystal pulling rate, and the control range is narrow. Let's raise the cost of single crystal production. Therefore, it is necessary to improve the growth rate of the defect-free region.
  • the inventors of the present invention further investigated and found that there was a correlation between the number of rotations of the crucible and the growth rate of the defect-free region, and that the rotation of the crucible or seeding was not performed. It has been found that by rotating the crystal in the same direction as that of the crystal, the growth rate of the defect-free region can be increased.
  • the present invention has been completed on the basis of these findings, that is, without rotating the crucible or in the same direction as the rotation direction of the seed crystal.
  • the N region outside the OSF which is formed in a ring shape when subjected to thermal oxidation treatment when it is converted, and is detected by the Cu deposition.
  • the feature is to grow a crystal in a defect-free region where no defect region exists. It is a thing.
  • FIG. 1A shows an example of a single crystal pulling apparatus that can be used in the present invention.
  • the single crystal pulling apparatus 30 includes a pulling chamber 31, a crucible 32 provided in the pulling chamber 31, a heater 34 disposed around the crucible 32, and a crucible for rotating the crucible 32.
  • Holding shaft 33 and its rotating mechanism (not shown), seed chuck 6 for holding silicon seed crystal, wire 7 for pulling up seed chuck 6, and rotating or rotating wire 7 It has a winding mechanism (not shown) for winding.
  • a heat insulating material 35 is disposed around the outside of the heater 34.
  • the Norrebo 32 has a quartz crucible on the inner side for containing the silicon melt (hot water) 2 and a graphite crucible on the outer side. Further, a positive / negative rotation switching switch is provided so that the crucible holding shaft 33 can be rotated in either the left or right direction by a rotating mechanism. As shown in FIG. 1 (b), the crucible 32 is moved. The seed crystal can be rotated in the same direction as the rotation direction (upper axis rotation direction) or in the opposite direction.
  • An annular graphite cylinder (heat shield plate) 9 is provided in order to set the manufacturing conditions relating to the manufacturing method of the present invention, and an annular outer periphery is provided around the solid-liquid interface 4 of the crystal. Insulation 10 is provided.
  • the outer heat insulating material 10 is provided with an interval of 2 to 20 cm between its lower end and the molten metal surface 3 of the silicon melt 2. Further, a cylindrical cooling device for spraying a cooling gas or cooling a single crystal by blocking radiant heat may be provided.
  • the difference between the temperature gradient G c [° C / cm] at the center of the crystal and the temperature gradient G e at the periphery of the crystal becomes smaller.
  • the temperature gradient around the crystal is greater than the crystal center. It is also possible to control the furnace temperature to lower the temperature.
  • a superconducting magnet for applying a horizontal magnetic field (transverse magnetic field) to the silicon melt 2 in the crucible 3 2 is provided outside the pulling chamber 31 in the horizontal direction. 36 are provided.
  • the silicon single crystal can be pulled up by the so-called H-MCZ method, which suppresses the convection of the melt 2 and stably grows the single crystal.
  • the magnet 36 may be of a normal conduction type.
  • a high-purity polycrystalline silicon raw material is melted in a crucible 32 at a melting point (about 142 0 ° C) Heat to above and melt.
  • a melting point about 142 0 ° C
  • the tip of the seed crystal 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, and the wire 7 is wound while being rotated.
  • the seed crystal is pulled while rotating, and the growth of the single crystal is started.
  • a substantially cylindrical single crystal rod 1 can be obtained. It can be.
  • the rotation direction of the seed crystal that is, the rotation direction of the crucible and the rotation direction of the crucible are conventionally set to be opposite to each other, but in the present invention, when growing the silicon single crystal as described above,
  • the N region outside the OSF which is generated in a ring when the thermal oxidation treatment is performed, is performed. Therefore, the crystal is grown in a defect-free region where no defect region is detected by the Cu deposition.
  • a 250-cm (600 mm) diameter quartz crucible was charged with 150 kg of polycrystalline silicon as a raw material, and an 8-inch (200 mm) diameter was used. ), A silicon single crystal of orientation ⁇ 100> was grown.
  • the growth rate was controlled so that the growth rate gradually decreased from 0.8 mm / min force to 0.4 mm / mi ⁇ from the straight body of 10 cm to the tail. did.
  • Such an experiment of gradually decreasing the crystal growth rate was performed by setting the crucible to various rotation speeds. Specifically, the crucible is kept stopped (0 rpm), or in the same direction as the seed crystal rotation direction (upper shaft rotation direction), 0.1 rpm, 0.3 rpm, 0.5 rpm. rpm, 1.0 rpm, 2.0 rpm, 3.0 rpm, and 0.1 rpm, 1.0 rpm, 2.0 rpm in the opposite direction to the seed crystal. Set to a number.
  • a horizontal magnetic field was applied by a superconducting method so that the magnetic field strength at the center of the single crystal was 400 G.
  • the magnetic field strength is not particularly limited. For example, it is appropriate to apply a horizontal magnetic field having a center magnetic field strength of about 500 to 500 G.
  • each block is further divided vertically in the crystal axis direction.
  • the sample was cut to a thickness of about 2 mm.
  • Oxide film 25 nm
  • the Cu deposition was applied to the N region outside the OSF, which was generated in a ring shape during thermal oxidation treatment. A defect-free area where no defective area was detected was confirmed.
  • Figure 2 shows the relationship between such a defect-free region and its growth rate. From this figure, when the growth rate of the silicon single crystal during growth is gradually reduced, the defect area detected by the Cu deposition remaining after the OSF ring disappears disappears.
  • the N region outside the OSF is between the boundary growth rate and the boundary growth rate at which the interstitial dislocation loop (giant dislocation cluster: I region) occurs when the growth rate is further reduced. Thus, it can be specified as a growth rate (a defect-free area growth rate) that is a defect-free area where no defect area detected by the Cu deposition exists.
  • the defect-free region growth rate was determined for each silicon single crystal as described above, and is shown in Table 1.
  • the relationship between the crucible rotation speed and the defect-free region growth rate is graphed.
  • the growth rate of the defect-free region shown in Table 1 and Fig. 3 is the same as that of the Cu deposition defect disappearance rate.
  • Intermediate value with the dislocation cluster (LSEPD, LFPD) generation speed is the same as that of the Cu deposition defect disappearance rate.
  • the growth rate of the defect-free region increases as the rotation speed decreases. In any case, it will be less than 0.57 mm / min.
  • the crystal growth rate is 0.57 mm / min or more. Depressed area growth rate has been achieved. Therefore, for example, by rotating the crucible without rotating or rotating the crucible in the same direction as the rotation direction of the seed crystal at a rotation speed in the range of 0 to 2 rpm, at least 0.
  • the defect-free silicon is obtained.
  • a single crystal can be grown at a higher speed. Therefore, by slicing a silicon single crystal rod grown by such a method, the entire surface is free from defects, that is, V region defects such as FPD, and giant dislocations.
  • V region defects such as FPD
  • giant dislocations High-quality silicon with high withstand voltage and excellent electrical characteristics that does not include I-region defects such as clusters, OSF defects, and no defects detected by Cu deposition. It is possible to obtain efficiently.
  • the crucible should be rotated more than when the crucible is rotated in the direction opposite to the rotation direction of the seed crystal (the direction of rotation of the upper shaft). Rotating in the same direction (upper shaft rotation direction) increases the temperature gradient G in the crystal-solid interface axial direction.
  • the present invention is not limited to the above embodiment.
  • the above The embodiment is an exemplification, and any of those having substantially the same configuration as the technical idea described in the claims of the present invention and having the same function and effect will be described. Even so, they are included in the technical scope of the present invention.
  • the apparatus used for producing a silicon single crystal according to the present invention is not limited to the apparatus as shown in FIG. 1, and the crucible is formed in the same direction as the seed crystal.
  • Any device that can produce a silicon single crystal in a defect region can be used without limitation.
  • crystal growth may be performed without applying a horizontal magnetic field.

Abstract

L'invention concerne un procédé permettant de produire un cristal unique de silicium au moyen du procédé de Czochralski, selon lequel un cristal germe est mis en contact avec une fonte de silicium (2) maintenue dans un creuset (32) et le cristal germe est tiré tandis qu'il tourne, de manière à faire croître un cristal unique de silicium (1). Ledit procédé est caractérisé en ce que le creuset ne tourne pas ou tourne dans la même direction que celle de la rotation du cristal germe, et un cristal croît dans une région sans défaut qui est une région N présente hors OSF permettant de générer une forme en anneau au cours d'un traitement d'oxydation thermique et qui est exempte de région défectueuse détectée par dépôt de cuivre. Selon un mode de réalisation préféré, un champ magnétique horizontal est appliqué et le creuset tourne à un taux compris entre 0 et 2 rpm. Ce procédé garantit une stabilité à un taux de production élevé et permet la production d'un cristal unique de silicium qui n'appartient pas à une des régions parmi une région V riche en lacunes de réseaux, une région OSF et une région I riche en silicium interstitiel. Ce procédé permet d'établir l'amélioration des caractéristiques électriques, telles qu'une tension de claquage du film d'oxyde, qui débouche sur la fabrication, à moindre coût, d'une plaquette de cristal unique de silicium exempte de défauts et présentant une tension de claquage élevée et d'excellentes caractéristiques électriques.
PCT/JP2003/005243 2002-04-25 2003-04-24 Procede de production d'un cristal unique de silicium et plaquette de cristal unique de silicium WO2003091484A1 (fr)

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JP2002124900A JP2003321297A (ja) 2002-04-25 2002-04-25 シリコン単結晶の製造方法及びシリコン単結晶ウェーハ

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Cited By (1)

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EP2226412A1 (fr) * 2009-02-27 2010-09-08 SUMCO Corporation Procédé de croissance de silicium monocristallin et procédé de fabrication d'une tranche de silicium

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KR101105475B1 (ko) 2009-02-04 2012-01-13 주식회사 엘지실트론 공정 변동이 최소화된 단결정 제조방법
KR101729515B1 (ko) 2015-04-14 2017-04-24 주식회사 엘지실트론 실리콘 단결정 잉곳의 성장 방법
CN110129890B (zh) * 2018-03-30 2021-02-02 杭州慧翔电液技术开发有限公司 一种用于磁控直拉单晶的线圈结构及磁控直拉单晶的方法

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WO1998045507A1 (fr) * 1997-04-09 1998-10-15 Memc Electronic Materials, Inc. Silicium a faible taux de defectuosites precipitant idealement l'oxygene
US5954873A (en) * 1995-05-31 1999-09-21 Sumitomo Sitix Corporation Manufacturing method for a silicon single crystal wafer
EP0964082A1 (fr) * 1998-06-11 1999-12-15 Shin-Etsu Handotai Company Limited Plaquette de silicium monocristallin et procédé pour sa production
US6048395A (en) * 1997-11-21 2000-04-11 Shin-Etsu Handotai Co., Ltd. Method for producing a silicon single crystal having few crystal defects
JP2001261495A (ja) * 2000-03-23 2001-09-26 Komatsu Electronic Metals Co Ltd 無欠陥結晶の製造方法

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US5954873A (en) * 1995-05-31 1999-09-21 Sumitomo Sitix Corporation Manufacturing method for a silicon single crystal wafer
WO1998045507A1 (fr) * 1997-04-09 1998-10-15 Memc Electronic Materials, Inc. Silicium a faible taux de defectuosites precipitant idealement l'oxygene
US6048395A (en) * 1997-11-21 2000-04-11 Shin-Etsu Handotai Co., Ltd. Method for producing a silicon single crystal having few crystal defects
EP0964082A1 (fr) * 1998-06-11 1999-12-15 Shin-Etsu Handotai Company Limited Plaquette de silicium monocristallin et procédé pour sa production
JP2001261495A (ja) * 2000-03-23 2001-09-26 Komatsu Electronic Metals Co Ltd 無欠陥結晶の製造方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2226412A1 (fr) * 2009-02-27 2010-09-08 SUMCO Corporation Procédé de croissance de silicium monocristallin et procédé de fabrication d'une tranche de silicium

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