WO2011071176A1 - Creuset en verre de silice - Google Patents

Creuset en verre de silice Download PDF

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Publication number
WO2011071176A1
WO2011071176A1 PCT/JP2010/072339 JP2010072339W WO2011071176A1 WO 2011071176 A1 WO2011071176 A1 WO 2011071176A1 JP 2010072339 W JP2010072339 W JP 2010072339W WO 2011071176 A1 WO2011071176 A1 WO 2011071176A1
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WO
WIPO (PCT)
Prior art keywords
silica glass
glass crucible
crucible
marking
silica
Prior art date
Application number
PCT/JP2010/072339
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English (en)
Japanese (ja)
Inventor
俊明 須藤
岸　弘史
真喜子 小玉
Original Assignee
ジャパンスーパークォーツ株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by ジャパンスーパークォーツ株式会社 filed Critical ジャパンスーパークォーツ株式会社
Priority to EP20100836095 priority Critical patent/EP2385157B1/fr
Priority to US13/148,457 priority patent/US9115445B2/en
Priority to KR1020117019517A priority patent/KR101248915B1/ko
Priority to JP2011540648A priority patent/JP4875229B2/ja
Priority to CN201080008269.4A priority patent/CN102325928B/zh
Publication of WO2011071176A1 publication Critical patent/WO2011071176A1/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
    • 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
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
    • 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
    • C03C19/00—Surface treatment of glass, not in the form of fibres or filaments, by mechanical means
    • 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
    • C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0005—Other surface treatment of glass not in the form of fibres or filaments by irradiation
    • C03C23/0025—Other surface treatment of glass not in the form of fibres or filaments by irradiation by a laser beam
    • 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
    • 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
    • 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 silica glass crucible for pulling a silicon single crystal.
  • Silicon wafers are indispensable for the electronics technology that supports today's IT society, and for the production of semiconductor devices used there.
  • One of the features of this silicon wafer is microdefects such as oxygen precipitates, dislocations, and oxygen stacking faults. While these micro defects have the beneficial effect of capturing heavy metal contamination that occurs in the device process, they can also cause device failure. Therefore, the oxygen concentration in the crystal needs to be adjusted to a predetermined concentration depending on the type of device or the device process used.
  • CZ method a manufacturing method of pulling a single crystal of silicon called Czochralski method (hereinafter referred to as CZ method) is common.
  • CZ method Magneticfield-applied CZ method
  • MCZ method Magneticfield-applied CZ method
  • a seed crystal silicon rod is put on the surface of the silicon solution, the seed crystal or silica glass crucible is rotated, the seed crystal is made thin (no dislocation) and then pulled up, single crystal silicon having the same atomic arrangement as the seed crystal The ingot is obtained.
  • the silica glass crucible is for storing a silicon melt when melting polycrystalline silicon and pulling it up as a single crystal. And the quantity of the molten silicon in a silica glass crucible decreases according to the pulling-up amount of a silicon single crystal, and the position of the liquid surface (henceforth a molten metal surface) of molten silicon changes in a silica glass crucible.
  • the position where the molten metal surface fluctuates is generally monitored visually, but with this, there is a problem that it is impossible to accurately measure the decrease in the volume of the silicon melt due to the variation of the molten metal surface position. there were.
  • the special region could not be identified from its appearance.
  • the carbon susceptor that supports the silica glass crucible reacts with the outer surface of the silica glass crucible during the pulling of the single crystal silicon, and the inner diameter of the carbon susceptor changes with each use. Even if the crucible is charged, the initial hot water surface position does not become the same position. Therefore, even if the distance between the initial molten metal surface position and the molten metal surface position that has fluctuated during pulling is known, the relative position between the molten metal surface and the special region provided in the silica glass crucible cannot be accurately grasped.
  • the present invention is a silica glass crucible provided with a special region for suppressing hot water surface vibration during pulling of single crystal silicon in view of the above-mentioned present situation, and the silica glass crucible is partly due to the weight of the molten silicon.
  • the purpose is to accurately grasp the position of the hot water surface and the position of the special area even when the shape is deformed.
  • the present invention can accurately realize the optimum pulling speed while accurately controlling the position of the molten metal surface and the position of the special region in this way while suppressing the molten metal surface vibration during the pulling of the single crystal silicon. It aims at providing the silica glass crucible which gave the marking.
  • the gist configuration of the present invention is as follows.
  • a silica glass crucible for accumulating molten silicon wherein the silica glass crucible has a special region for preventing the undulation of molten silicon on the inner wall surface of the straight body portion, and has markings at least at the upper and lower ends of the special region Silica glass crucible characterized by that.
  • the special region is mainly composed of silica glass made from natural silica, and the transparent layer other than the special region is made mainly from silica glass made from synthetic silica.
  • Silica glass crucible as described in).
  • the special region is provided between 5 mm below the crucible opening edge and 100 mm above the center of the bottom of the crucible, and has a width of 1 to 100 mm.
  • the silica glass crucible according to any one of the above.
  • the present invention when pulling up the single crystal silicon, for example, even if the silica glass crucible is deformed by the mass of the silicon melt, it is possible to accurately grasp the variation in the position of the molten metal surface relative to the position of the special region. Can do. This makes it possible to increase the pulling rate of the single crystal silicon immediately after the molten metal surface passes through the special region for preventing molten metal surface vibration, which can greatly contribute to the improvement of productivity.
  • FIG. 1 is a sectional view of a silica glass crucible.
  • the silica glass crucible 1 according to the present embodiment has a special region 2 for preventing fluctuation of the molten metal surface on the inner wall surface of the straight body portion 5 of the silica glass crucible 1 used for pulling up single crystal silicon such as CZ method, And at least at the upper end and the lower end of the special area 2, it is characterized in that it has markings 4 that can be detected from the outside of the CZ furnace (for example, can be visually judged (visible)).
  • the silica glass crucible 1 of this embodiment may be used for either single pulling or multiple pulling.
  • the silica glass crucible 1 includes a corner portion 9 having a relatively large curvature, a cylindrical straight body portion 5 having an edge portion opened on the upper surface, and a straight line or a curvature that is relatively long. It has a mortar-shaped bottom 8 made of a small curve.
  • the corner portion 9 is a portion connecting the straight body portion 5 and the bottom portion 8, and is common to the bottom portion in that the tangent line of the curve of the corner portion 9 overlaps the straight body portion 5 of the silica glass crucible. It means the part up to the point with tangent.
  • the silica glass crucible 1 has substantially no bubbles from the inner surface side toward the outer surface side (the bubble content is less than 0.5%) (hereinafter, transparent layer 6), and the bubble content is 0. It has a silica glass layer (hereinafter referred to as bubble-containing layer 7) of 5% or more and less than 50%.
  • the bubble content means the ratio (w2 / w1) of the bubble occupation volume (w2) to the constant volume (w1) of the crucible 1.
  • FIG. 1 1 is the crucible opening edge
  • 2 is a special region for preventing the surface of the molten metal provided on the inner wall surface
  • 3 is the center of the bottom
  • 4 is the marking
  • 5 is such a marking. It is the range (straight body part 5) which can be performed.
  • the position where the marking 4 is provided is preferably selected from the range of the straight body portion indicated by 5.
  • the markings 4 can be provided at other positions of the straight body portion 5 in order to check the amount of the melt.
  • the special region 2 As described above, when the silicon lump is melted in the silica glass crucible 1 and pulled up as a single crystal ingot, the silicon melt swells (vibrates) on the liquid surface (water surface). ) In order to reduce the phenomenon, it is provided on the inner wall surface of the silica glass crucible 1.
  • the special region 2 can be made of natural silica glass in which natural silica is melted, and the inner wall surface of the transparent layer 6 of the silica glass crucible 1 other than that can be made of synthetic silica glass.
  • the silica powder (synthetic silica powder) for forming the synthetic silica glass means one made of synthetic silica, and the synthetic silica is a chemically synthesized and manufactured raw material. Since the raw material of synthetic silica is a gas or a liquid, it can be easily purified, and the synthetic silica powder can have a higher purity than natural silica powder. Synthetic silica glass powder is amorphous. The raw material for the synthetic silica glass powder is derived from a gaseous raw material such as carbon tetrachloride and a liquid raw material such as silicon alkoxide. Synthetic silica glass powder can reduce all impurities to 0.1 ppm or less.
  • synthetic silica glass powders those by the sol-gel method usually leave about 50 to 100 ppm of silanol produced by hydrolysis of the alkoxide.
  • Synthetic silica glass powder using carbon tetrachloride as a raw material can control silanol in a wide range of 0 to 1000 ppm, but usually contains about 100 ppm or more of chlorine.
  • alkoxide is used as a raw material, synthetic silica glass powder containing no chlorine can be easily obtained.
  • the sol-gel synthetic silica glass powder contains about 50 to 100 ppm of silanol before melting as described above. When this is vacuum-melted, silanol is eliminated, and the amount of silanol in the resultant synthetic silica glass is reduced to about 5 to 30 ppm.
  • the amount of silanol varies depending on the melting conditions such as the melting temperature and the temperature rise. Further, the amount of silanol in natural silica glass obtained by melting natural silica powder under the same conditions is less than 50 ppm.
  • synthetic silica glass is said to have a lower viscosity at high temperature than natural silica glass obtained by melting natural silica powder.
  • One possible cause is that silanol or halogen cuts the network structure of the SiO4 tetrahedron.
  • synthetic silica glass obtained by melting synthetic silica glass powder, when measuring light transmittance, UV light up to about 200 nm is well transmitted, and carbon tetrachloride used for ultraviolet optical applications is used as a raw material. It is considered that the characteristics are close to those of synthetic silica glass.
  • Natural silica powder means natural silica. Natural silica is a raw material obtained by digging raw silica existing in nature, crushing and refining, and natural silica powder is ⁇ - Made of quartz crystals. Natural silica powder contains 1 ppm or more of Al and Ti, and other metal impurities are at a higher level than synthetic silica powder. Natural silica powder contains almost no silanol. The amount of silanol in natural silica glass obtained by melting natural silica powder is less than 50 ppm.
  • the transmittance is drastically reduced when the wavelength is 250 nm or less due to Ti contained mainly as an impurity at about 1 ppm, and hardly transmits at the wavelength: 200 nm. .
  • an absorption peak due to oxygen defects is observed near 245 nm.
  • the glass material to be measured is natural silica, depending on whether the concentration of impurities contained, the amount of silanol, or the light transmittance is measured, or the fluorescence spectrum obtained by excitation with ultraviolet light having a wavelength of 245 nm is measured. Whether it is synthetic silica can be discriminated.
  • the transparent layer 6 can be prepared by reducing the pressure of the silica powder layer from the mold side at a pressure of ⁇ 50 to less than ⁇ 95 kPa. Further, after the transparent layer 6 is formed, the bubble-containing layer 7 can be formed outside the transparent layer 6 by reducing the pressure of the reduced pressure to +10 kPa to less than ⁇ 20 kPa.
  • silica powder is used as a raw material, but the “silica powder” here is not limited to quartz as long as the above conditions are satisfied, and silicon dioxide (silica).
  • quartz and quartz sand can be included as a raw material of the silica glass crucible.
  • the special region 2 in the present embodiment can also be constituted by silica glass containing bubbles. Furthermore, what is necessary is just to provide surface unevenness
  • the specific area 2 will be described more specifically. In the present embodiment, there is no particular limitation on how to provide each special area 2 described below, and a conventionally known special area 2 for preventing silicon surface vibration is known. Any of the providing methods can be suitably used.
  • the first is a special region consisting mainly of natural silica glass as described above.
  • the natural silica glass is present in a region having a thickness of about 2 mm from the inner wall surface, and the width in the height direction is preferably within 100 mm, more preferably about 30 mm.
  • the layer which has a natural silica glass as a main component means the silica glass layer formed from the raw material powder whose value of a natural silica powder mass / synthetic silica powder mass is one or more.
  • the second is a special region 2 made of silica glass containing bubbles.
  • the bubble means a bubble that can be detected with the naked eye using light scattering (about 5 ⁇ m or more). That is, the average bubble diameter at this time is preferably in the range of 5 ⁇ m to 50 ⁇ m, more preferably in the range of 10 ⁇ m to 40 ⁇ m, and particularly preferably about 30 ⁇ m.
  • the bubble density is preferably 10 / cm 2 or more, more preferably 20 / cm 2 or more, and particularly preferably 30 / cm 2 or more. About 40 pieces / cm 2 .
  • the bubble density is preferably 100 / cm 2 or less, and more preferably 70 / cm 2 or less.
  • the thickness of the special region 2 is preferably 1 mm or more from the inner wall surface, particularly preferably about 2 mm.
  • the width in the height direction of the special region 2 is preferably within 100 mm, more preferably about 40 mm.
  • the width in the height direction of the special region 2 is preferably 1 mm or more, and more preferably 10 mm or more.
  • the third is a special area 2 characterized by having surface irregularities.
  • the feature of the irregularities is that the average roughness of the ten-point average roughness Rz is preferably 0.1 mm or more, more preferably 0.3 mm or more, and particularly preferably about 0.5 mm. Further, the average roughness of the irregularities is preferably 1.0 mm or less, and more preferably 0.7 mm or less.
  • the width in the height direction of the special region 2 is preferably within 100 mm, and more preferably about 40 mm.
  • the width in the height direction of the special region 2 is preferably 1 mm or more, and more preferably 10 mm or more.
  • the surface is the inner wall surface of the silica glass crucible 1.
  • the fourth is a special region 2 characterized in that the above-mentioned surface irregularities are composed of a plurality of slits.
  • the average length is preferably 10 mm or more, more preferably 30 mm or more, and particularly preferably about 50 mm. Further, the average length of the slits is preferably 100 mm or less, and more preferably 70 mm or less.
  • the average width of the slits is preferably 0.1 mm or more, more preferably 0.3 mm or more, and particularly preferably about 0.5 mm. Further, the average width of the slits is preferably 1.0 mm or less, and more preferably 0.7 mm or less.
  • the average depth of the slit is preferably 0.1 mm or more, more preferably 0.3 mm or more, and particularly preferably about 0.5 mm. Further, the average depth of the slit is preferably 1.0 mm or less, and more preferably 0.7 mm or less.
  • the density of the slits is preferably 5 / cm 2 or more, more preferably 10 / cm 2 or more, and particularly preferably about 20 / cm 2 . Further, the density of the slits is preferably 50 / cm 2 or less, and more preferably 30 / cm 2 or less.
  • the width in the height direction of the special region 2 is preferably within 100 mm, more preferably about 40 mm. The width in the height direction of the special region 2 is preferably 1 mm or more, and more preferably 10 mm or more.
  • the position where the special region 2 is provided is preferably between 5 mm below the crucible opening end surface and about 100 mm above the center of the crucible bottom, and from 10 mm below the crucible opening end surface to the crucible. More preferably, it is provided between about 200 mm above the bottom center.
  • the width of the special region 2 in the height direction is preferably about 1 mm to 100 mm. In the present embodiment, the height direction refers to the arrow direction in FIG.
  • the shape of the marking 4 is a point (circular) or a line (rectangular) shape, and the number of points, the length of the line, etc. may be such that the marking 4 can be visually observed when pulling up the single crystal silicon (or optical measurement). Therefore, it may be selected appropriately according to the visibility of the actual CZ furnace or the like.
  • the individual depth is preferably from 0.1 mm or more to about 1/2 or less of the thickness of the silica glass crucible 1, and from 0.2 mm or more to 1 / th of the thickness of the silica glass crucible 1. More preferably, it is up to about 3 or less.
  • the diameter is preferably 0.5 mm or more, more preferably 0.7 mm or more, and particularly preferably about 1 mm.
  • the diameter is preferably 3.0 mm or less, more preferably 2.0 mm or less.
  • the individual depth is preferably from 0.1 mm or more to about 1/2 or less of the thickness of the silica glass crucible 1, and from 0.2 mm or more to 1 / th of the thickness of the silica glass crucible 1. More preferably, it is up to about 3 or less.
  • the width is preferably 0.5 mm or more, more preferably 0.7 mm or more, and particularly preferably about 1 mm.
  • the width is preferably 3.0 mm or less, more preferably 2.0 mm or less.
  • the marking 4 does not necessarily need to extend over the entire circumference of the horizontal plane of the silica glass crucible 1, but is preferably provided over a length of about 5 cm or more, and more preferably provided over a length of 10 cm or more.
  • the marking 4 in the present embodiment needs to be provided at least at the upper and lower ends of the special area 2 for the reason described above. At this time, since the marking 4 at the upper end is hardly or not in contact with the molten silicon during the pulling of the single crystal silicon, it is not necessary to consider the thinning of the silica glass crucible 1 itself.
  • the marking 4 in this embodiment can be provided between the upper and lower ends, or at the lower position of the lower end. That is, when the special region 2 is provided between the upper and lower ends, it can be used as a preparation point for changing the pulling conditions of the silicon single crystal. Further, when it is provided at a position below the lower end of the special region 2, it can be used as a guide for grasping the remaining amount of molten silicon.
  • the marking 4 used in the present embodiment is applied at an accurate position with respect to the special region 2 and clearly visible (or can be detected). Desirable is a laser marking to be applied or a diamond tool marking which is a marking 4 applied by a diamond tool.
  • a laser marking to be applied or a diamond tool marking which is a marking 4 applied by a diamond tool.
  • a diamond tool marking which is a marking 4 applied by a diamond tool.
  • all conventionally well-known methods such as marking by a cemented carbide drill, are applicable. That is, although the method is selected depending on the depth and length of the marking 4, it is preferable to provide the marking 4 with the diamond tool or laser, particularly the marking 4 with a carbon dioxide laser.
  • a conventionally known tool can be appropriately selected depending on the shape of the marking 4, and examples thereof include a diamond wheel and a drill with a diamond tip.
  • the marking 4 used in the present embodiment can be provided only on a part of the entire circumference. It may be provided.
  • Example 1 The marking described in the above embodiment was applied to a silica glass crucible having a diameter of 800 mm manufactured by a conventionally known method according to the following procedure.
  • the marking shape at that time was a 1 mm diameter spot.
  • [Laser marking procedure] A process of placing a 3-claw scroll chuck mechanism for centering the crucible and placing the crucible opening side down on a floor plate that has an opening for a laser processing machine in the center. 2. 3-claw scroll chuck Centering process of the crucible by the mechanism 3. The process of raising and lowering the laser processing machine on the inner wall surface side of the crucible 4. Adjusting the distance between the inner wall surface of the crucible and the laser irradiation port by the red semiconductor laser with a wavelength of 650 nm built in the laser device The process of providing marking with laser 6. The process of rotating the base plate with servo control mechanism and repeating the marking in sequence 7. The process of returning the laser processing machine to the origin position.
  • the irradiation conditions of a carbon dioxide laser are as follows.
  • Oscillation wavelength band 10.6 ⁇ m
  • Maximum output energy 10 J Beam divergence angle: 0.5 mrad Repeat: single, 0-12 Hz
  • Pulse width 180 ns
  • Jitter ⁇ 60 ns
  • Switching method Semiconductor switch method
  • Laser equipment dimensions W83 cm x H60 cm x D271 cm
  • Example 2 Next, the crucible used in Example 1 was heated to 1400 ° C. and deformed in a simulated manner. When the laser marking described in the above embodiment was applied, even when the crucible was deformed, a special region mainly composed of natural silica was visually recognized.
  • Example 3 The crucible used in Example 1 was loaded into a carbon susceptor with a gap of about 7 mm at the corner, and about 80 kg of polycrystalline silicon was placed in the crucible, placed in a CZ furnace, melted at about 1450 ° C., and 20 hours. Retained. At this time, visual observation was performed from the outside of the CZ furnace, but the location of the special region mainly composed of natural silica could be accurately visually confirmed.
  • the gap between the silica glass crucible and the carbon susceptor was measured after the crucible returned to room temperature, it was about 2 mm and was greatly deformed. That is, even when the corner portion of the crucible is deformed by about 5 mm, the silica glass crucible provided with the marking described in the above embodiment can accurately recognize the location of the special region mainly composed of natural silica.
  • Example 4 Laser marking was performed on the silica glass crucible having the same specifications as in Example 1 under the same conditions as in Example 1, and a silica glass crucible having the same specifications as in Example 1 without marking was prepared as a comparative example. Subsequently, each crucible was installed in a CZ furnace. Furthermore, after these silicon glass crucibles, when silicon is melted, about 100 kg of polycrystalline silicon lump is placed so that the molten metal surface is in a special region, and after maintaining an argon gas atmosphere (6.67 kPa), The temperature was raised from room temperature (20 ° C.) to 1500 ° C. over 10 hours, and kept at this temperature for a predetermined time to melt the silicon mass to form a silicon melt.
  • an argon gas atmosphere (6.67 kPa
  • the upper end marking was visible, but the lower end marking was not visible with the silicon melt.
  • a seed crystal was soaked in these silicon melts and gradually pulled up while rotating the crucible to grow a 400 mm diameter silicon single crystal in a length of 0.3 m, under the condition that the ripple was minimized.
  • the laser marking is visually recognized, but it is not particularly limited. That is, the position of the laser marking may be detected using an optical measurement device or the like instead of visual observation.
  • the present invention can accurately and easily use a special region effective for preventing liquid surface vibration of a silica glass crucible for storing molten silicon when pulling up single crystal silicon by the CZ method, the CZ method can be used efficiently.
  • Single crystal silicon can be pulled up.
  • a high-quality silicon single crystal ingot can be brought to an optimum pulling speed at a faster timing than before.

Abstract

Creuset en verre de silice muni d'une région spéciale qui minimise les vibrations de la surface de silicium en fusion qui se produisent lorsqu'un monocristal de silicium est en cours de traction ascendante, et sur laquelle sont appliquées des marques qui permettent de connaître avec précision une variation de position de la surface du silicium en fusion, ladite variation se produisant lorsque le monocristal de silicium passe par la région spéciale. Un creuset en verre de silice selon l'invention est muni d'une région spéciale qui empêche le silicium en fusion d'onduler, la région spéciale étant définie sur la surface de paroi intérieure de la section de corps rectiligne du creuset en verre de silice, et au moins les extrémités supérieure et inférieure de la région spéciale sont dotées de marques.
PCT/JP2010/072339 2009-12-11 2010-12-13 Creuset en verre de silice WO2011071176A1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
EP20100836095 EP2385157B1 (fr) 2009-12-11 2010-12-13 Creuset en verre de silice
US13/148,457 US9115445B2 (en) 2009-12-11 2010-12-13 Vitreous silica crucible
KR1020117019517A KR101248915B1 (ko) 2009-12-11 2010-12-13 실리카 유리 도가니
JP2011540648A JP4875229B2 (ja) 2009-12-11 2010-12-13 シリカガラスルツボ
CN201080008269.4A CN102325928B (zh) 2009-12-11 2010-12-13 氧化硅玻璃坩埚

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2009282138 2009-12-11
JP2009-282138 2009-12-11

Publications (1)

Publication Number Publication Date
WO2011071176A1 true WO2011071176A1 (fr) 2011-06-16

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PCT/JP2010/072339 WO2011071176A1 (fr) 2009-12-11 2010-12-13 Creuset en verre de silice

Country Status (7)

Country Link
US (1) US9115445B2 (fr)
EP (1) EP2385157B1 (fr)
JP (1) JP4875229B2 (fr)
KR (1) KR101248915B1 (fr)
CN (1) CN102325928B (fr)
TW (1) TWI369422B (fr)
WO (1) WO2011071176A1 (fr)

Cited By (4)

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JP2016064931A (ja) * 2014-09-22 2016-04-28 株式会社Sumco ルツボ測定装置
WO2022186067A1 (fr) * 2021-03-05 2022-09-09 信越石英株式会社 Procédé d'évaluation d'un creuset en verre de quartz et procédé de fabrication dudit creuset en verre de quartz, et creuset en verre de quartz

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CN107287652A (zh) * 2017-05-29 2017-10-24 德令哈晶辉石英材料有限公司 一种抑制熔融硅液面振动的石英坩埚及其制备方法
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JP2015218087A (ja) * 2014-05-19 2015-12-07 信越石英株式会社 単結晶シリコン引き上げ用石英ガラスるつぼ
JP2016064931A (ja) * 2014-09-22 2016-04-28 株式会社Sumco ルツボ測定装置
WO2022186067A1 (fr) * 2021-03-05 2022-09-09 信越石英株式会社 Procédé d'évaluation d'un creuset en verre de quartz et procédé de fabrication dudit creuset en verre de quartz, et creuset en verre de quartz

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US9115445B2 (en) 2015-08-25
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JPWO2011071176A1 (ja) 2013-04-22
TWI369422B (en) 2012-08-01
TW201131027A (en) 2011-09-16
JP4875229B2 (ja) 2012-02-15
EP2385157B1 (fr) 2015-02-11
KR20110119730A (ko) 2011-11-02
EP2385157A4 (fr) 2012-08-22
KR101248915B1 (ko) 2013-04-01
US20120260852A1 (en) 2012-10-18
CN102325928B (zh) 2014-02-26

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