WO2009107834A1 - シリコン単結晶引上げ用石英ルツボ及びその製造方法 - Google Patents
シリコン単結晶引上げ用石英ルツボ及びその製造方法 Download PDFInfo
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- WO2009107834A1 WO2009107834A1 PCT/JP2009/053886 JP2009053886W WO2009107834A1 WO 2009107834 A1 WO2009107834 A1 WO 2009107834A1 JP 2009053886 W JP2009053886 W JP 2009053886W WO 2009107834 A1 WO2009107834 A1 WO 2009107834A1
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- crucible
- single crystal
- pulling
- quartz
- quartz crucible
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/09—Other methods of shaping glass by fusing powdered glass in a shaping mould
- C03B19/095—Other methods of shaping glass by fusing powdered glass in a shaping mould by centrifuging, e.g. arc discharge in rotating mould
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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
-
- 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
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
- C30B35/002—Crucibles or containers
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
- Y10T117/1032—Seed pulling
Definitions
- the present invention relates to a high-purity quartz glass crucible used for pulling up a silicon single crystal ingot for semiconductors, and more particularly, a silicon melt taken into a large-diameter silicon single crystal ingot being pulled (hereinafter simply referred to as a single crystal ingot).
- a silicon melt taken into a large-diameter silicon single crystal ingot being pulled hereinafter simply referred to as a single crystal ingot.
- High strength and high strength that can reduce SiO gas in the liquid, thereby enabling a significant reduction of pinhole defects caused by the SiO gas in the single crystal ingot and preventing the occurrence of deformation and distortion.
- the present invention relates to a purity quartz glass crucible (hereinafter simply referred to as a quartz crucible).
- a high-purity quartz glass powder having an average particle diameter of 200 to 300 ⁇ m and a purity of 99.99% or more is used as a raw material powder.
- the graphite mold was filled in a gap formed by the inner surface of the graphite mold and the outer surface of the core, for example, a gap of 30 mm while rotating at a speed of 60 to 80 rpm [see FIG.
- the core is taken out, and while rotating the graphite mold at a speed of 50 to 100 rpm, a three-phase AC arc discharge device using a graphite electrode is inserted from the upper opening, and this is reciprocated up and down along the inner surface of the graphite mold.
- the graphite mold is heated to about 2000 ° C., and the raw material powder is melted and solidified while evacuating the graphite mold through an air passage formed in the inner surface of the graphite mold. For example, the thickness becomes 10mm It is known to produce English crucible [see FIG. 4 (b)].
- the quartz crucible obtained as a result has a bubble content ratio (expressed as a percentage of the total volume of bubbles contained in quartz glass per unit volume): 1 to 10%, purity: 99.99% or more It has a double laminated structure of an outer layer of high-purity amorphous quartz glass and an inner layer of high-purity amorphous quartz glass having a bubble content of 0.6% or less and a purity of 99.99% or more, and the inner side It is also known that the ratio of the thickness of the layer and the outer layer is usually adjusted to a ratio of 1: 1 to 5 [see FIG. 6].
- the single crystal ingot is charged with a high-purity polycrystalline silicon lump in a quartz crucible mounted on the graphite support, and along the outer periphery of the graphite support.
- the polycrystalline silicon lump is melted by a heater provided to form a silicon melt, and the temperature of the silicon melt is heated and held at a predetermined temperature within a range of 1500 to 1600 ° C., while rotating the quartz crucible.
- the silicon seed crystal is produced by bringing it into contact with the silicon melt surface while rotating it in an Ar gas atmosphere under reduced pressure and pulling it up.
- the silicon melt falls in the quartz crucible from the bottom of the single crystal ingot to the bottom of the crucible, and from bottom to top along the inner surface from the bottom of the crucible.
- the silicon melt (Si) reacts with the inner surface of the crucible (SiO 2 ) to generate SiO gas during the convection toward the bottom of the single crystal ingot. It moves to the surface of the silicon melt on the flow of gas, where it is released into the reduced-pressure Ar gas atmosphere, removed, and taken into the single crystal ingot being pulled up, and the pulling conditions are set to prevent pinhole defects. Manufactured with adjustment.
- the crystallization accelerator is interposed between the inner and outer layers of the quartz crucible, or is applied along the outer peripheral surface of the upper end of the crucible opening, and the action of the crystallization accelerator during melt molding Efforts have also been made to improve the strength of the quartz crucible by changing the amorphous structure to a crystalline structure.
- the use of a quartz crucible having a high-strength crystal structure becomes unavoidable, but the amorphous structure is changed to a crystal structure by the action of the crystallization accelerator described above.
- the crystallization accelerator present in the crucible causes crystallization during pulling. As the process proceeds, the crystal grains become finer and the crystal grain boundaries further increase.
- the gist of the present invention is as follows. (1) In a quartz crucible for pulling up a silicon single crystal made of quartz glass and having a two-layer structure of an outer layer and an inner layer, the inner layer is pulled up at least on the silicon melt surface of the silicon melt surface when viewed in a cross section on the crucible side. When the distance from the top end of the crucible opening to the start position of pulling the silicon single crystal is 100, the top end of the opening A quartz crucible for pulling up a silicon single crystal, characterized in that only the crucible part from the position to the position corresponding to the range of 40 to 100 is crystalline.
- the inner surface shape of the inner layer is such that the distance between the peak position of the peak and the deepest position of the valley is 0.1 to 3 mm, and the distance between the peaks of the peak is 10 to 100 mm.
- the silicon single crystal pulling start position is The silicon single crystal pulling method according to (1) or (2), wherein the height position range is 50 to 95 from the bottom, and the end position of pulling the silicon single crystal is a height position range of 0 to 10 from the bottom of the crucible. Quartz crucible.
- the proportion of the crystallization accelerator blended in the ring-shaped cut-out portion is set to 0.01 to 1% by mass. If the proportion is less than 0.01% by mass, the upper end of the crucible opening When the distance from the opening of the silicon single crystal to the starting position of the silicon single crystal is 100, only the crucible part from the upper end of the opening to the position corresponding to the range of 40 to 100 cannot be made crystalline. A desired high strength cannot be ensured, and as a result, a large-diameter quartz crucible having an inner diameter of 610 to 810 mm may be deformed or distorted due to insufficient strength.
- the quartz crucible of the present invention even if the crucible is enlarged to an outer diameter of 610 to 810 mm, for example, for pulling up a large single crystal ingot having a diameter of 200 mm to 300 mm, the formed crucible and valley portions are provided. Due to the reaction between the inner surface of the crucible and the silicon melt, a large amount of SiO gas generated as the diameter of the crucible increases due to the reaction between the inner surface of the crucible and the inner surface of the crucible.
- the silicon melt surface is maintained until it grows to a size not affected by the silicon melt convection, and when the generated SiO gas is agglomerated and coarsened to have a large buoyancy, the silicon melt surface is separated from the ring groove at once. As a result, the generated SiO gas that moves to the bottom of the single crystal ingot being pulled up by riding on the silicon melt convection is remarkably reduced. It is possible to achieve a significant reduction of pinhole defects generated in the crystal ingot. Furthermore, by making only the crucible portion from the upper end of the opening to a position corresponding to the range of 40 to 100 crystalline, it is possible to secure high strength capable of preventing the quartz crucible from being deformed or distorted.
- the inner surface of the crucible that is substantially in contact with the silicon melt substantially retains the amorphous structure during the pulling of the single crystal ingot.
- the reaction with the silicon melt on the inner surface of the crucible is further suppressed as compared with the crystal structure. As a result, it is possible to suppress the occurrence of pinhole defects in the single crystal ingot caused by the generated SiO gas. It is.
- FIG. 4 is a schematic vertical sectional view showing a main part of the quartz crucible of the present invention, where (a) shows a wavy inner surface shape having peaks and valleys, and (b) schematically shows the behavior of generated SiO gas on the inner surface of the quartz crucible.
- FIG. It is a schematic longitudinal cross-sectional view which shows the half part of this invention quartz crucible raw material. It is a schematic longitudinal cross-sectional view showing the manufacturing process of a quartz crucible, (a) is a figure which shows the filling aspect of raw material powder, (b) is a figure which shows the melt molding aspect of a quartz crucible. It is a schematic longitudinal cross-sectional view which shows the pulling aspect of a single crystal ingot. It is a figure which shows typically the behavior of the SiO gas generated on the inner surface of the conventional quartz crucible.
- a quartz crucible for pulling a single crystal is a quartz crucible for pulling a silicon single crystal made of quartz glass and having a two-layer structure of an outer layer and an inner layer, wherein the inner layer is seen in a crucible side cross section, Between the starting position and the ending position of pulling up the silicon single crystal on the silicon melt surface, it has a wavy inner surface shape with peaks and valleys, and from the upper end of the crucible opening to the starting position of pulling up the silicon single crystal. When the distance is 100, only the crucible portion from the upper end of the opening to the position corresponding to the range of 40 to 100 is crystalline.
- the SiO gas generated by the reaction between the silicon melt and the inner surface of the quartz crucible at the time of conventional pulling has a diameter of 50 to 200 ⁇ m immediately after the generation, and is schematically shown in FIG.
- it moves by the silicon melt convection along the inner surface of the crucible, and most of them are released from the silicon melt surface into the reduced pressure Ar gas atmosphere while maintaining the above dimensions and removed, but the remaining slight amount
- the generated SiO gas moves to the bottom of the single crystal ingot that is being pulled up and is taken into this, causing pinhole defects.
- the ratio of the generated SiO gas taken into the single crystal ingot is the ingot and the crucible. There is a problem that it increases dramatically as the diameter increases.
- the inner surface between the ingot pulling start line and the pulling end line of at least the silicon melt surface on the inner surface of the quartz crucible is a wavy inner surface shape having a peak and a valley," as schematically shown in the main part schematic longitudinal sectional view in FIG. Since the inside of the ring groove forming the wavy inner surface shape is a staying zone that is not affected by the flow of the silicon melt, the SiO gas generated at the bottom of the crucible rides on the flow of the silicon melt and enters the inner surface of the crucible.
- the SiO gas stays attached to the inner surface of the ring groove and moves sequentially into the ring groove.
- the SiO gas that moves to the bottom of the single crystal ingot in the inside and is taken into this and causes pinhole defects can be significantly reduced. This phenomenon does not change even if the diameter of the single crystal ingot and the quartz crucible is increased.
- the pulling start position of the silicon single crystal shown in FIG. 2 (a) means that the height position of the bottom of the quartz crucible is 0 and the height position of the upper end of the opening is viewed from the side cross section of the quartz crucible.
- the height position range of 50 to 95 when 100 is assumed.
- the end position of the pulling of the silicon single crystal is 0 as the height position of the bottom of the quartz crucible and 100 as the height position of the upper end of the opening. It is preferable to refer to a height position range of 0 to 10.
- the corrugated inner surface shape is a quartz crucible straight body portion, with the upper end being a position 5 mm to 10 mm below the upper end of the crucible opening as seen from the crucible side cross section, as viewed from the crucible side cross section. It is preferable to be provided up to the lower end.
- the upper end of the wavy inner surface shape is located above 5 mm from the upper opening end of the crucible, the wavy shape exists up to the vicinity of the upper end of the opening, so that sufficient crucible strength cannot be obtained and the quartz crucible is deformed.
- the lower end of the wavy inner surface shape is set to the same height position as the lower end of the quartz crucible straight body part. Normally, the end position of the pulling up of the silicon single crystal is such that the silicon melt is from the straight body part. If the end of the wavy inner surface shape is located above the straight body part, the SiO gas cannot be sufficiently suppressed and a pinhole defect may be caused. This is because, when the inner surface shape is located below the straight body portion, the suppression effect of SiO gas is improved, but the manufacture of the quartz crucible becomes complicated.
- the straight body of the quartz crucible refers to the body of the quartz crucible, and more specifically, until the curvature changes when transitioning from the upper end of the quartz crucible to the bottom. The crucible part in the range.
- the quartz crucible of the present invention the depth and width of the ring groove constituting the wavy inner surface shape having a peak and a valley are determined based on various experimental results as described above.
- the depth and width satisfy the above numerical conditions (the distance between the peak position of the peak and the deepest position of the valley is 0.1 to 3 mm, and the distance between the peaks of the peak is 10 to 100 mm), The occurrence of pinhole defects in the crystal ingot can be sufficiently reduced. On the other hand, if any of the depth and width of the ring groove is out of the above numerical range, the desired pinhole defect reduction effect may not be obtained.
- FIGS. 2A and 2B show a case where the waveform of the inner surface of the quartz crucible in the longitudinal section is a “sine wave”, but the above-described peak may be obtained even if this is a deformed waveform. If it is within the dimension range of the distance between the apex position of the part and the deepest position of the valley part and the distance between the apexes of the peak part, a remarkable effect can be obtained.
- the quartz crucible when the distance from the upper end of the crucible opening to the starting position of pulling the silicon single crystal is 100, only the crucible portion from the upper end of the opening to the position corresponding to the range of 40 to 100 is made crystalline.
- the strength of the quartz crucible during pulling up of the single crystal ingot is determined by the strength of the upper end of the crucible opening, so if the upper end of the crucible opening can secure high strength, only the upper end of the crucible opening is made of a high-strength crystal structure,
- the quartz crucible retains its high strength during pulling of the single crystal ingot even when other parts (substantially below the ingot pulling start line on the silicon melt surface) are made of an amorphous structure. It becomes possible to prevent distortion.
- the crystalline crucible portion is a crystallization accelerator (preferably an oxidizing agent).
- Aluminum hereinafter referred to as Al 2 O 3
- CaO calcium oxide
- BaO barium oxide
- CaCO 3 calcium carbonate
- BaCO 3 barium carbonate
- at least one kind is contained in an amount of 0.01 to 1% by mass, and a quartz crucible material is melt-molded with a ring-shaped cut-out portion extending upward from the upper end of the crucible opening. The crystal structure is formed. Due to the action of the crystallization accelerator, as shown in the quartz crucible of the present invention in FIG.
- a part of the quartz crucible becomes crystalline, and if this crystalline part is adjusted in the blending ratio of the crystallization accelerator,
- the portion corresponding to the range of 40 to 100 from the upper end of the opening can be made crystalline, in which case the inner diameter is Even with a large-diameter quartz crucible of 610 to 810 mm, it is possible to obtain a high-strength quartz crucible that does not cause deformation or distortion when the single crystal ingot is pulled up.
- the crystallization accelerator does not exist, so that the non-crystallization during the pulling of the single crystal ingot. No further crystallization of the crystalline part (the remaining part except the crystallized part between the upper opening of the quartz crucible body and the ingot pulling start line of the silicon melt surface) occurs, and the amorphous structure Therefore, the generation of SiO gas is remarkably suppressed as compared with the crystal structure, and as a result, the generation of pinhole defects in the single crystal ingot can be suppressed. This phenomenon is the same for a large single crystal ingot having a diameter of 200 to 300 mm.
- Example (A) According to the manufacturing process shown in FIGS. 4 (a) and 4 (b), for the purpose of forming a crucible body under normal conditions, as a raw material powder, a purity having an average particle size of 250 ⁇ m: a high of 99.998% by mass Using pure quartz glass powder, fill the 30 mm gap formed between the inner surface of the graphite mold and the outer surface of the core while rotating the graphite mold and core at a speed of 65 rpm, and further upward from the upper opening of the crucible body.
- the raw material powder is blended with crystallization accelerators in the proportions shown in Table 1 and mixed.
- the raw material powder is filled in the same way, and after filling, the core is taken out, and while rotating the graphite mold at a speed of 65 rpm, a three-phase AC arc discharge device using a graphite electrode is inserted from the upper opening, and this is inserted into the graphite mold.
- the graphite powder is heated to about 2000 ° C.
- the quartz crucible material of the present invention having the structure shown in FIG. 3 composed of a ring-shaped cut-out portion having a height (width): 20 mm containing the crucible body and the crystallization accelerator is formed by solidification, After cutting and removing the ring-shaped cut-out portion from the quartz crucible material of the present invention using a diamond cutter, the groove depth and width of the ring groove are formed on the inner surface of the crucible between the ingot pulling start line and the pulling end line on the silicon melt surface.
- the height (width) of the ring-shaped cut-off portion is 40 mm, and the ratio of the crystallization accelerator blended therein is as shown in Table 1, and the ingot pulling start line on the silicon melt surface
- the inner surface of the crucible between the pulling end line and the inner surface of the crucible has a sine wave shape and a corrugated inner surface in which the inner surface of the ring groove has the groove depth and groove width as shown in Table 1, respectively.
- the outer diameter is 810 mm, the depth is 435 mm, and the thickness is 16 mm in the same manner as the manufacturing method for the quartz crucibles A-1 to A-9 of the present invention in (A) above except that is formed by grinding.
- the ingot pulling start line on the silicon melt surface is at a position 100 mm from the upper end of the opening, the pulling end line is at a position 335 mm from the upper end of the opening, and the bubble content is 0.2%, and the purity is 99.998%.
- Thickness: 6mm of high purity quartz glass It has a double layered structure consisting of a side layer and an outer layer of high purity quartz glass with a bubble content of 5%, purity: 99.997%, thickness: 10mm, and a crystallization accelerator at the top of the crucible
- the core was taken out, and the graphite mold was rotated at a speed of 65 rpm.
- a three-phase AC arc discharge device using a graphite electrode was inserted from the upper opening, and this was reciprocated up and down along the inner surface of the graphite mold to heat the temperature inside the graphite mold to about 2000 ° C., while the graphite Mo
- the crystallization accelerator is melted and solidified in the inside of the crucible through the air passage provided in the inner surface of the inside and melted and solidified to reach a position 20 mm below the upper end of the opening at the upper end of the crucible.
- It has a double layer structure consisting of an inner layer and an outer layer of high-purity quartz glass with a bubble content of 5%, purity: 99.997%, and thickness: 10mm, and promotes crystallization at the upper end of the crucible.
- the inside of the crucible is formed with a corrugated inner surface with peaks and valleys.
- Five conventional quartz crucibles D-1 to D-9 each having a diameter of 300 mm for pulling a single crystal ingot were manufactured.
- the crucible opening of the quartz crucibles A-1 to A-9 and B-1 to B-9 of the present invention after pulling up the single crystal ingot and the conventional quartz crucibles C-1 to C-9 and D-1 to D-9 are also the same.
- the ratio of crystallization from the upper end is observed using an optical microscope, and when the distance from the upper end of the crucible opening to the starting position of the silicon single crystal pulling is 100, the ratio is expressed as an average value of five crucibles. 1 and 2 (column after pulling up the ingot).
- Quartz crucible strength Furthermore, with regard to the strength of the quartz crucible, a ruler is applied to the outer surface of the straight barrel part extending in the vertical direction of the quartz crucible after being used for pulling, and the gap between the outer surface of the upper end opening and the ruler (mm) was measured with a vernier caliper, and the average value measured at a total of four locations on the outer periphery of the crucible was calculated as the upper end opening deformation (mm) to evaluate the strength of the quartz crucible.
- the quartz crucibles A-1 to A-9 and B-1 to B-9 of the present invention were used for pulling up a large single crystal ingot having a diameter of 200 to 300 mm. Even when the outer diameter is increased to 610 to 810 mm, when the distance from the upper end of the crucible opening to the starting position of pulling the silicon single crystal is set to 100, it is formed at a position corresponding to the range of 40 to 100 from the upper end of the opening.
- the crystal structure has high strength capable of suppressing crucible deformation when pulling up the single crystal ingot, and since there is no crystallization accelerator at the upper end of the crucible opening, the crystallization action by the crystallization accelerator Progression does not occur, and the inner surface of the crucible substantially in contact with the silicon melt retains the amorphous structure during pulling of the single crystal ingot, and the ingot pulling of the silicon melt surface of the inner surface of the crucible of the amorphous structure starts. From the line The wavy inner surface shape having raised ends peaks and valleys formed over the line, the number of occurrences of pinhole defects in the single crystal ingot was found to decrease significantly.
- the conventional quartz crucibles C-1 to C-9 and D-1 to D-9 have a crystal structure at the upper end of the crucible opening, so that the crucible deformation at the time of pulling up the single crystal ingot can be suppressed.
- it has strength, since there is a crystallization accelerator at the upper end of the crucible opening, it goes beyond the ingot pulling start line on the silicon melt surface not only when melting the crucible but also when pulling the single crystal ingot.
- the existence of a zone where the crystal structure comes into contact with the silicon melt is unavoidable. In this zone, the generation of SiO gas at the crystal grain boundary is further activated as described above.
- C-10 which has a small proportion of the crystal structure at the upper end of the crucible opening, does not have sufficient strength, so the amount of deformation of the crucible is large, and the upper part of the crucible is tilted upward during the pulling. Will be suspended.
- the quartz crucible of the present invention is particularly suitable for use in pulling a large-diameter single crystal ingot having a diameter of 200 to 300 mm, and greatly improves the yield and quality of a large-diameter silicon single crystal wafer. It contributes.
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Abstract
Description
さらに、単結晶インゴット引上げ中の石英ルツボの変形及びゆがみを防止して、石英ルツボの使用寿命の延命化を図る目的で、例えばアルカリ土類金属の酸化物、水酸化物、及び炭酸塩などからなる結晶化促進剤を、石英ルツボの内側層と外側層の間に介在させたり、あるいはこれをルツボ開口上端部の外周面に沿って塗布し、溶融成形中に前記結晶化促進剤の作用で非晶質組織を結晶組織に変化させて、石英ルツボの強度を向上させる取り組みもなされている。
(1)石英ガラスからなり、外側層と内側層の2層構造を有するシリコン単結晶引上げ用石英ルツボにおいて、前記内側層は、ルツボ側断面で見て、シリコン融液面の少なくともシリコン単結晶引上げの開始位置と終了位置間にて、山部と谷部をもつ波状の内面形状をもち、かつ、ルツボの開口上端からシリコン単結晶引上げの開始位置までの距離を100とするとき、前記開口上端から40~100の範囲に相当する位置までのルツボ部分のみが結晶質であることを特徴とするシリコン単結晶引上げ用石英ルツボ。
本発明による単結晶引上げ用石英ルツボは、石英ガラスからなり、外側層と内側層の2層構造を有するシリコン単結晶引上げ用石英ルツボであって、前記内側層が、ルツボ側断面で見て、シリコン融液面の少なくともシリコン単結晶引上げの開始位置と終了位置間にて、山部と谷部をもつ波状の内面形状をもち、かつ、ルツボの開口上端からシリコン単結晶引上げの開始位置までの距離を100とするとき、前記開口上端から40~100の範囲に相当する位置までのルツボ部分のみが結晶質であることを特徴とする。
一方、上記の従来石英ルツボに見られる通り、石英ルツ内に結晶化促進剤が存在した状態で実用(単結晶インゴット引上げ)に供すると、前記結晶化促進剤の作用で単結晶インゴット引上げ中に石英ルツボの更なる結晶化が進行して、結晶は微細化し、この結果結晶粒界が増大し、結晶粒界でのSi+SiO2反応が活発に起こるようになって引上げ中の単結晶インゴットおけるピンホール欠陥の発生が促進するようになるが、石英ルツボ中に前記結晶化促進剤が存在しなければ、引上げ中の石英ルツボに結晶化進行作用(結晶粒界増加作用)を防止できるためである。
(A)図4(a),(b)に示される製造プロセスに従い、通常の条件で、ルツボ本体を形成する目的で、原料粉末として、平均粒径:250μmを有する純度:99.998質量%の高純度石英ガラス粉末を用い、これを黒鉛モールド内面と中子外面で形成された30mmの間隙に前記黒鉛モールド及び中子を65rpmの速度で回転させながら充填し、さらにルツボ本体の開口上端から上方に20mmの高さ(幅)で伸長し、これと一体となったリング状切り捨て部を形成する目的で、前記原料粉末にそれぞれ表1に示される割合の結晶化促進剤を配合し、混合した混合原料粉末を同じく充填し、充填後、前記中子を取出し、前記黒鉛モールドを65rpmの速度で回転させながら、黒鉛電極を用いた三相交流アーク放電装置を上方開口より挿入し、これを黒鉛モールド内面に沿って上下に往復動させて黒鉛モールド内温度を約2000℃に加熱し、一方、前記黒鉛モールド内に、これの内面に開口して設けた通気路を通して真空引きを行いながら、前記原料粉末を溶融し、固化することにより、ルツボ本体と結晶化促進剤を含有した高さ(幅):20mmのリング状切り捨て部からなる図3に示される構造の本発明石英ルツボ素材を成形し、ついで、前記本発明石英ルツボ素材からリング状切り捨て部をダイヤモンドカッターを用いて切断除去した後、シリコン融液面のインゴット引上げ開始ラインと引上げ終了ラインの間のルツボ内面に、リング溝の溝深さ及び溝幅をそれぞれ表1に示される寸法とし、かつ縦断面内面形状を正弦波形状とした山部と谷部をもつ波状の内面形状を研削加工により形成し、研削加工面を酸素バーナーを用いて平滑化仕上げ処理することにより、外径:610mm、深さ:380mm、厚さ:10mmの寸法を有すると共に、シリコン融液面のインゴット引上げ開始ラインがルツボ開口上端から50mmの位置、同引上げ終了ラインが開口上端から300mmの位置にあり、かつ、気泡含有率:0.3%にして、純度:99.998%、厚さ:4mmの高純度石英ガラスの内側層と、気泡含有率:5%にして、純度:99.994%、厚さ:6mmの同じく高純度石英ガラスの外側層で構成された図1に示される2重積層構造を有し、ルツボ上端部に結晶化促進剤を含有しない直径:200mmの単結晶インゴット引上げ用本発明石英ルツボA-1~A-9をそれぞれ5個ずつ製造した。
(B)上記リング状切り捨て部の高さ(幅)を40mmとし、かつこれに配合される結晶化促進剤の割合を表1に示される通りとすると共に、シリコン融液面のインゴット引上げ開始ラインと引上げ終了ラインの間のルツボ内面に、リング溝の溝深さ及び溝幅をそれぞれ表1に示される寸法とした縦断面内面形状が正弦波形状の山部と谷部をもつ波状の内面形状を研削加工により形成する以外は、上記(A)の本発明石英ルツボA-1~A-9の製造手法と同じ方法にて、外径:810mm、深さ:435mm、厚さ:16mmの寸法を有すると共に、シリコン融液面のインゴット引上げ開始ラインが開口上端から100mmの位置、同引上げ終了ラインが開口上端から335mmの位置にあり、かつ、気泡含有率:0.2%にして、純度:99.998%、厚さ:6mmの同じく高純度石英ガラスの内側層と、気泡含有率:5%にして、純度:99.997%、厚さ:10mmの高純度石英ガラスの外側層で構成された2重積層構造を有し、ルツボ上端部に結晶化促進剤を含有しない直径:300mmの単結晶インゴット引上げ用本発明石英ルツボB-1~B-9をそれぞれ5個ずつ製造した。
(C)また、図4(a),(b)に示される製造プロセスに従い、通常の条件で、原料粉末として、平均粒径:250μmを有する純度:99.998質量%の高純度石英ガラス粉末を用い、これを黒鉛モールド内面と中子外面で形成された30mmの間隙に前記黒鉛モールド及び中子を65rpmの速度で回転させながら、最終ルツボ寸法から20mm短い位置まで充填し、ついで、前記原料粉末にそれぞれ表2に示される割合の結晶化促進剤を配合し、混合した混合原料粉末を最終ルツボ寸法になるまで充填し、充填後、前記中子を取出し、前記黒鉛モールドを65rpmの速度で回転させながら、黒鉛電極を用いた三相交流アーク放電装置を上方開口より挿入し、これを黒鉛モールド内面に沿って上下に往復動させて黒鉛モールド内温度を約2000℃に加熱し、一方、前記黒鉛モールド内に、これの内面に開口して設けた通気路を通して真空引きを行いながら、前記原料粉末を溶融し、固化することにより、ルツボ上端部に開口上端から20mm下の位置まで結晶化促進剤を含有し、外径:610mm、深さ:380mm、厚さ:10mmの寸法を有すると共に、シリコン融液面のインゴット引上げ開始ラインがルツボ開口上端から50mmの位置、同引上げ終了ラインが開口上端から300mmの位置にあり、かつ、気泡含有率:0.3%にして、純度:99.998%、厚さ:4mmの高純度石英ガラスの内側層と、気泡含有率:5%にして、純度:99.994%、厚さ:6mmの同じく高純度石英ガラスの外側層で構成された2重積層構造を有し、ルツボ上端部に結晶化促進剤を含有させ、ルツボ内面には山部と谷部をもつ波状の内面形状の形成を行なわない直径:200mmの単結晶インゴット引上げ用従来石英ルツボC-1~C-10をそれぞれ5個ずつ製造した。
(D)ルツボ上端部に開口上端から40mm下の位置まで結晶化促進剤を含有し、かつこれに配合される結晶化促進剤の割合を表2に示される通りとする以外は、上記(C)の従来石英ルツボC-1~C-9の製造手法と同じ方法にて、外径:810mm、深さ:435mm、厚さ:16mmの寸法を有すると共に、シリコン融液面のインゴット引上げ開始ラインがルツボ開口上端から100mm下の位置、同引上げ終了ラインが開口上端から335mmの位置にあり、かつ、気泡含有率:0.2%にして、純度:99.998%、厚さ:6mmの高純度石英ガラスの内側層と、気泡含有率:5%にして、純度:99.997%、厚さ:10mmの同じく高純度石英ガラスの外側層で構成された2重積層構造を有し、ルツボ上端部に結晶化促進剤を含有させ、ルツボ内面には山部と谷部をもつ波状の内面形状の形成を行なわない直径:300mmの単結晶インゴット引上げ用従来石英ルツボD-1~D-9をそれぞれ5個ずつ製造した。
次いで、上記の通りそれぞれ5個ずつ用意された本発明石英ルツボA-1~A-9及びB-1~B-9、並びに従来石英ルツボC-1~C-9及びD-1~D-9を用いて、図5に示される引上げ装置にて、通常の条件で、それぞれ直径:200mm及び300mmの単結晶インゴットを引上げ製造した。単結晶インゴット引上げ後の本発明石英ルツボA-1~A-9及びB-1~B-9、並びに従来石英ルツボC-1~C-9及びD-1~D-9について、同じくルツボ開口上端からの結晶化の割合を光学顕微鏡を用いて観察し、ルツボの開口上端からシリコン単結晶引上げの開始位置までの距離を100とするとき、これに対する割合で、ルツボ5個の平均値として表1,2(インゴット引上げ後の欄)に示した。
(1)ピンホール欠陥の抑制
また、上記の単結晶インゴット引上げ後の各種の石英ルツボについて、ルツボ開口上端の内径を内周に沿って10箇所測定したところ、いずれのルツボも最大値と最小値の差が1mm以下の範囲内にあり、変形のきわめて少ないものであった。さらに、上記の前記本発明石英ルツボA-1~A-9及びB-1~B-9、並びに従来石英ルツボC-1~C-9及びD-1~D-9における1種類の石英ルツボ毎に5本の単結晶インゴットが製造されることになるが、1本の単結晶インゴットから、直径が200mmのものからは、厚さ:725μmのウェーハを1000枚、直径が300mmのものからは、厚さ:775μmのウェーハを800枚切出し、それぞれ5本の単結晶インゴットから切出された合計ウェーハについて、ウェーハ上下面を検査装置を用いて検査し、直径:30μm以上の窪みが存在したウェーハをピンホール発生ウェーハとし、ピンホール欠陥の発生したウェーハの枚数を計測した。計測結果を表1,2に示す。
さらに、石英ルツボの強度については、引上げに使用した後の石英ルツボの鉛直方向に延びる直胴部外面に定規を当て、上端開口部の外面と定規の隙間(mm)をノギスにより測定し、ルツボ外周の計4箇所について測定した平均値を上端開口部変形量(mm)として算出し、石英ルツボの強度を評価した。
Claims (5)
- 石英ガラスからなり、外側層と内側層の2層構造を有するシリコン単結晶引上げ用石英ルツボにおいて、
前記内側層は、ルツボ側断面で見て、シリコン融液面の少なくともシリコン単結晶引上げの開始位置と終了位置間にて、山部と谷部をもつ波状の内面形状をもち、かつ、
ルツボの開口上端からシリコン単結晶引上げの開始位置までの距離を100とするとき、前記開口上端から40~100の範囲に相当する位置までのルツボ部分のみが結晶質であることを特徴とするシリコン単結晶引上げ用石英ルツボ。 - 前記内側層の内面形状は、山部の頂点位置と谷部の最深位置との距離が0.1~3mmであり、山部の頂点間距離が10~100mmである請求項1記載のシリコン単結晶引上げ用石英ルツボ。
- ルツボ側断面で見て、ルツボの底部の高さ位置を0、ルツボの開口上端部の高さ位置を100としたとき、前記シリコン単結晶引上げ開始位置が、ルツボの底部から50~95の高さ位置範囲であり、前記シリコン単結晶引上げ終了位置が、ルツボの底部から0~10の高さ位置範囲である請求項1又は2記載のシリコン単結晶引上げ用石英ルツボ。
- 請求項1、2又は3記載のシリコン単結晶引上げ用石英ルツボを製造する方法であって、前記結晶質ルツボ部分は、結晶化促進剤を0.01~1質量%含有し、ルツボ開口上端から上方に伸長するリング状の切り捨て部を設けた状態で、前記石英ルツボの溶融成形を行なうことで、結晶組織が形成されることを特徴とするシリコン単結晶引上げ用石英ルツボの製造方法。
- 前記結晶化促進剤が、酸化アルミニウム、酸化カルシウム、酸化バリウム、炭酸カルシウム及び炭酸バリウムのうちの少なくとも1種である請求項4記載のシリコン単結晶引上げ用石英ルツボの製造方法。
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Cited By (13)
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KR101395859B1 (ko) | 2009-09-10 | 2014-05-15 | 쟈판 스파 쿼츠 가부시키가이샤 | 실리콘 단결정 인상용 실리카 유리 도가니 및 그 제조 방법 |
JP5022519B2 (ja) * | 2009-09-10 | 2012-09-12 | ジャパンスーパークォーツ株式会社 | シリコン単結晶引き上げ用石英ガラスルツボ |
WO2011030657A1 (ja) * | 2009-09-10 | 2011-03-17 | ジャパンスーパークォーツ株式会社 | シリコン単結晶引き上げ用シリカガラスルツボ及びその製造方法 |
US8936685B2 (en) | 2009-09-10 | 2015-01-20 | Japan Super Quartz Corporation | Vitreous silica crucible for pulling silicon single crystal and method of manufacturing the same |
EP2385157A1 (en) * | 2009-12-11 | 2011-11-09 | Japan Super Quartz Corporation | Silica glass crucible |
EP2385157A4 (en) * | 2009-12-11 | 2012-08-22 | Japan Super Quartz Corp | SILICON GLASS CRUCIBLE |
US9115445B2 (en) | 2009-12-11 | 2015-08-25 | Sumco Corporation | Vitreous silica crucible |
WO2013088617A1 (ja) * | 2011-12-12 | 2013-06-20 | 信越石英株式会社 | 単結晶シリコン引き上げ用シリカ容器及びその製造方法 |
JP2013121902A (ja) * | 2011-12-12 | 2013-06-20 | Shinetsu Quartz Prod Co Ltd | 単結晶シリコン引き上げ用シリカ容器及びその製造方法 |
KR101504953B1 (ko) | 2011-12-12 | 2015-03-23 | 신에쯔 세끼에이 가부시키가이샤 | 단결정 실리콘 인상용 실리카 용기 및 그 제조 방법 |
US9382640B2 (en) | 2011-12-12 | 2016-07-05 | Shin-Etsu Quartz Products Co., Ltd. | Single crystal silicon pulling silica container and manufacturing method thereof |
JP2020097512A (ja) * | 2018-12-13 | 2020-06-25 | クアーズテック株式会社 | シリカガラスルツボ |
JP7280160B2 (ja) | 2018-12-13 | 2023-05-23 | モメンティブ・テクノロジーズ・山形株式会社 | シリカガラスルツボ |
Also Published As
Publication number | Publication date |
---|---|
TW200944625A (en) | 2009-11-01 |
KR101176968B1 (ko) | 2012-08-30 |
EP2251460A4 (en) | 2015-04-01 |
CN101965418A (zh) | 2011-02-02 |
KR20100112173A (ko) | 2010-10-18 |
US9150447B2 (en) | 2015-10-06 |
EP2251460A1 (en) | 2010-11-17 |
JP5234526B2 (ja) | 2013-07-10 |
US20110011334A1 (en) | 2011-01-20 |
EP2251460B1 (en) | 2017-01-18 |
CN101965418B (zh) | 2012-12-05 |
JPWO2009107834A1 (ja) | 2011-07-07 |
TWI378158B (en) | 2012-12-01 |
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