WO2010092955A1 - シリコン単結晶引き上げ用の石英ガラスルツボおよびシリコン単結晶の製造方法 - Google Patents
シリコン単結晶引き上げ用の石英ガラスルツボおよびシリコン単結晶の製造方法 Download PDFInfo
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- WO2010092955A1 WO2010092955A1 PCT/JP2010/051893 JP2010051893W WO2010092955A1 WO 2010092955 A1 WO2010092955 A1 WO 2010092955A1 JP 2010051893 W JP2010051893 W JP 2010051893W WO 2010092955 A1 WO2010092955 A1 WO 2010092955A1
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- Prior art keywords
- quartz glass
- glass crucible
- crystallization
- single crystal
- silicon single
- Prior art date
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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
- 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
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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
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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
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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 quartz glass crucible used for manufacturing a silicon single crystal used for a substrate of a solar cell or a semiconductor device, and a method for manufacturing a silicon single crystal using the same.
- Silicon single crystal is manufactured from polycrystalline silicon by FZ method or CZ method.
- silicon single crystals produced by the CZ method currently occupy more than 70% of the market.
- this CZ method polycrystalline silicon is put into a quartz glass crucible, melted by heating, and the silicon single crystal is pulled up using a seed crystal.
- Quartz glass crucible is an important member that determines the yield and quality of silicon single crystal as the only member in contact with silicon melt.
- the yield of single crystal silicon is that the crystallized material with the size of ⁇ 2 to ⁇ 6 ( Figure 4) scattered at the interface when the silicon melt reacts with the quartz glass crucible at high temperature is the inner surface of the quartz glass crucible. It is lowered by peeling off from the silicon and adhering to the edge of the silicon single crystal to be polycrystallized. Thus, it has been studied to uniformly crystallize the entire inner surface of the quartz glass crucible.
- Patent Document 1 discloses a method in which high-concentration barium is applied to the entire inner surface of a quartz glass crucible, and the inner surface of the quartz glass crucible is crystallized into a thick crystal layer entirely before use. .
- Patent Document 2 discloses a method for improving the yield of pulling up a silicon single crystal using the crucible of Patent Document 1 described above.
- Patent Documents 1 and 2 require a considerably high concentration of barium coating, and there is a concern that defects may be generated by barium mixed during silicon crystal growth. Further, in the case of growing a large-diameter silicon crystal, a severer thermal environment is required, so that the quartz glass crucible that has been thickly crystallized is significantly deteriorated. Moreover, handling becomes difficult by using high concentration barium.
- Patent Document 3 discloses a method for improving the durability of a crucible by forming a coating film or a solid solution layer of a crystallization accelerator within 1 mm of the inner surface of a quartz glass crucible.
- a group 2a element compound is used as the crystallization accelerator
- the solution is applied to the inner surface of the crucible and dried to form a coating film.
- a 3b group element compound as a crystallization promoter
- the solid solution layer is formed by sprinkling the powder doped with this during melting.
- Patent Document 4 discloses that the crystallization accelerator-containing layer on the inner surface of a quartz glass crucible is difficult to peel off, has a high crucible strength at high temperatures, and can stably pull up a silicon single crystal. Yes.
- the crystallization accelerator-containing layer In order to increase the strength of the quartz glass crucible during the pulling, the crystallization accelerator-containing layer must be thickened to 1 to 2 mm, and quartz powder that gradually increases the concentration of the crystallization accelerator must be deposited stepwise. In other words, it cannot be said that the layer formation efficiency is good.
- this method has a low concentration of crystallization accelerator, and when used at a low temperature such as a small-diameter quartz glass crucible, the crystallization rate is low and the crystallization material generated on the inner surface of the quartz glass crucible Is peeled off from the inner surface, and it is difficult to stably improve the yield of pulling the silicon single crystal.
- Japanese Patent Laid-Open No. 9-110590 Japanese Patent Laid-Open No. 9-110579 JP-A-8-002932 JP 2007-001806 A
- the inner surface is uniformly crystallized in order to suppress the separation and dropping of the crystallized substance having a size of ⁇ 2 to ⁇ 6 (FIG. 4) scattered on the inner surface of the quartz glass crucible. Therefore, no effective solution has been proposed for the separation of the crystal layer from the inner surface of the quartz glass crucible due to excessive crystallization.
- the present invention has been made in view of the circumstances as described above, and there is no occurrence of separation and dropping of crystallized substances scattered on the inner surface, and a crystal layer is formed on the entire inner surface. As described above, a part of the crystal layer does not exfoliate and a gas discharge hole is not formed, and the dissolved silicon can enter between the crystal layer and the glass layer below it from the gas release hole due to the micro exfoliation. It is an object of the present invention to provide a quartz glass crucible with which a high yield can be obtained and a method for producing a silicon single crystal using the same.
- the present invention is characterized by the following in order to solve the above problems.
- a silica glass crucible for pulling up a silicon single crystal having a crystallization accelerator-containing layer on the inner surface, and when pulling up the silicon single crystal, a crystallization accelerator has a patchy crystallization region on the inner surface.
- the patchy crystallized region is formed by continuously bonding crystallized substances generated in a scattered manner on the inner surface of a quartz glass crucible when the silicon single crystal is pulled up. Quartz glass crucible.
- the patchy crystallized region includes a unit region substantially having a closed peripheral edge and having an independent shape, and an area of the shape in the range of 10 to 100 mm 2.
- At least a part of the unit regions of the patchy crystallization region is such that the unit regions are further continuously connected to each other, and the entire area of the patchy crystallization region is 30 to 80 of the inner surface of the quartz glass crucible.
- the third quartz glass crucible characterized in that it occupies%.
- the crystallization accelerator is barium, and the crystallization accelerator-containing layer is formed by supplying and melting barium-coated high-purity silica powder on the inner surface of a quartz glass crucible.
- the quartz glass crucible according to any one of the first to sixth.
- Tenth The quartz glass crucible according to any one of the seventh to ninth, wherein the crystallization accelerator-containing layer has a barium concentration of 130 to 170 ppm.
- the present invention at the time of pulling a single crystal, there is no formation of scattered crystallized material on the inner surface of the quartz glass crucible, and a patchy crystallized region in which crystallized materials are continuously bonded is formed. It is formed. In this manner, the formation of the patchy crystallized region suppresses the separation of the crystallized material scattered on the inner surface of the quartz glass crucible.
- the crystallization accelerator in the depth direction of the inner surface of the quartz glass crucible, the crystallization of the patchy crystallization region proceeds in the depth direction of the inner surface. Therefore, it is possible to greatly suppress the detachment of the crystallized material that is scattered on the inner surface.
- the gas present in the quartz glass crucible is released from a region other than the patchy crystallization region on the inner surface of the quartz glass crucible. Therefore, the crystal layer in the patchy crystallized region does not exfoliate and a gas discharge hole is not formed, and the molten silicon enters between the crystal layer in the patchy crystallized region and the glass layer below it. There is no. Therefore, peeling of the crystal layer in the patchy crystallized region does not occur.
- the quartz glass crucible of the present invention does not cause the falling of the crystallized material scattered on the inner surface as in the conventional case, and the crystal layer is formed on the entire inner surface. A part of the crystal layer is not finely peeled to form a gas discharge hole, and dissolved silicon does not enter from the gas discharge hole by the fine peel between the crystal layer and the glass layer therebelow. Therefore, it is possible to provide a quartz glass crucible for pulling a silicon single crystal with a very high yield.
- FIG. 1 is a cross-sectional view schematically showing one embodiment of a quartz glass crucible for pulling a silicon single crystal of the present invention. It is the figure which showed typically the inner surface of the quartz glass crucible in which the spot-like crystallization area
- FIG. 6 is a photograph of a gas discharge hole of several tens of ⁇ m generated on the surface of a crystal layer on the inner surface of a quartz glass crucible of a comparative example.
- 4 is an electron micrograph of a gas discharge hole of several tens of ⁇ m generated on the surface of a crystal layer on the inner surface of a quartz glass crucible of a comparative example. It is the photograph of the state which melt
- FIG. 1 is a cross-sectional view schematically showing an embodiment of a quartz glass crucible for pulling a silicon single crystal of the present invention.
- the quartz glass crucible 1 of the present invention has a crystallization accelerator-containing layer 4 on the inner surface.
- the crystallization accelerator contained in the crystallization accelerator-containing layer is formed by reacting the inner surface of the quartz glass crucible with a high-temperature silicon melt when pulling up the silicon single crystal, and generating a crystallization substance at the interface.
- Specific examples thereof include the group 2a elements magnesium, strontium, calcium, barium and the like. These may be used alone or in combination of two or more.
- barium has a small segregation coefficient, and therefore has an excellent characteristic that it is difficult to be taken into the silicon single crystal when the silicon single crystal is pulled.
- barium is used as the crystallization accelerator. Is particularly preferred.
- a characteristic point in the present invention is that when a silicon single crystal is pulled, a patchy crystallization region is formed on the inner surface by a crystallization accelerator.
- reference numeral 5 denotes a patchy crystallization region.
- This mottled crystallized region is formed by continuous bonding of crystallized substances scattered on the inner surface of a quartz glass crucible when the silicon single crystal is pulled up. This is clearly different from the conventionally known scattered crystallized substances.
- the crystallized substances generated in a scattered manner are typically of a circular shape of ⁇ 2 to ⁇ 6 as shown in FIG. 4, and the shape and size are constant compared to the patchy crystallized region in the present invention. There is a certain order in the range. Most of the crystallized substances generated in a scattered manner have an area of less than 10 mm 2 .
- the patchy crystallization region in the present invention has an irregular and non-uniform appearance as a whole.
- the patchy crystallized region 5 includes a unit region 5 a exemplarily surrounded by a dotted ellipse in the figure, which has an independent shape with its peripheral edge closed. It is out.
- the spot-like crystallized regions are irregular and non-uniform as shown in the photograph of FIG. 3, and the unit regions 5a 1 , unit regions 5a 2 , unit regions 5a 3 and the like are shown as an example in FIG.
- the unit region 5a includes a continuous portion through a thin portion, the unit region 5a can be grasped as one that can be recognized as an independent shape with its peripheral edge substantially closed for visual convenience.
- This unit region is a crystallization accelerator in which a high-temperature silicon melt reacts with the inner surface of the quartz glass crucible when the silicon single crystal is pulled, and the crystallized material generated at the interface is contained in the inner surface of the quartz glass crucible.
- a typical unit region includes one having an area in the range of 10 to 100 mm 2 . Some unit regions have an area exceeding 100 mm 2 .
- the crystallized material on the inner surface of the quartz glass crucible By continuously bonding the crystallized material on the inner surface of the quartz glass crucible to form a non-uniform spot-like crystallized region, and further including a crystallization accelerator in the depth direction of the inner surface of the quartz glass crucible.
- the crystallization of the inner surface of the quartz glass crucible proceeds in the depth direction, and the separation of the crystallized material generated on the inner surface can be suppressed.
- the formation of a non-uniform spot-like crystallization region on the inner surface of the quartz glass crucible means that the gas existing in the quartz glass crucible is pulled into a region 12 other than the spot-like crystallization region in FIG. And the crystal layer of the patchy crystallized region can be prevented from peeling off from the inner surface of the quartz glass crucible.
- At least a part of the unit regions of the patchy crystallization region is composed of unit regions as illustrated in the unit region 5a 1 , unit region 5a 2 , unit region 5a 3, etc. of FIG. Further, they are continuously bonded, and the entire area of the patchy crystallization region occupies 30 to 80%, preferably 30 to 70%, of the inner surface of the quartz crucible.
- the gas that is contained in the quartz glass crucible and expands at a high temperature can be sufficiently released when the silicon single crystal is pulled up. It may disappear. In this case, the gas finely peels off the crystal layer to generate a gas discharge hole, and the gas is released from the gas discharge hole (FIG. 6). At this time, it has been confirmed by the present inventors that a lot of minute gas discharge holes of several tens of ⁇ m are generated in the crystal layer (FIG. 5).
- the molten silicon melted by heating put in the quartz glass crucible is a glass layer of the quartz glass crucible (transparent layer or an opaque layer on the outer periphery thereof) located under the crystal layer from a small gas discharge hole of several tens of ⁇ m. ) (FIG. 7), the glass layer is melted by the high-temperature molten silicon, the molten silicon enters between the crystal layer and the glass layer, and the crystal layer is separated from the quartz glass crucible (FIG. 8).
- the crystallization accelerator is barium
- the crystallization accelerator-containing layer is formed by supplying and melting barium-coated high-purity silica powder on the inner surface of the quartz glass crucible.
- the crystallization accelerator-containing layer thus formed preferably has a thickness of 30 to 200 ⁇ m.
- the crystallization accelerator When the crystallization accelerator is contained within 30 ⁇ m from the inner surface, the crystallization is not promoted unless the crystallization accelerator is contained at a high concentration as in the case of application to the inner surface, and the crystallization generated on the inner surface. The peeled material will peel off.
- the crystal accelerator when contained at 200 ⁇ m or more from the inner surface, crystallization proceeds and the entire surface of the inner surface of the quartz glass crucible is crystallized, so that a nonuniform spotted region cannot be obtained. That is, the crystal layer is peeled off from the inner surface of the quartz glass crucible.
- the crystallization accelerator-containing layer has a barium concentration of preferably 100 to 200 ppm, more preferably 130 to 170 ppm.
- the concentration of barium as a crystallization accelerator is low, so that crystallization is not promoted, and the crystallization substance generated on the inner surface of the quartz glass crucible may be peeled off.
- the barium concentration exceeds 200 ppm
- crystallization proceeds excessively, the entire inner surface of the quartz glass crucible is crystallized, and a patchy crystallized region cannot be obtained. For this reason, the crystal layer may be peeled off from the inner surface of the quartz glass crucible.
- the barium concentration in the crystallization accelerator-containing layer is set to 130 to 170 ppm, it is possible to reliably make 30 to 80% of the inner surface of the quartz glass crucible a patchy crystallization region. That is, the amount of heat applied to the quartz glass crucible among the conditions for pulling the silicon single crystal varies depending on the diameter of the quartz glass crucible and the like. The state of the spot-like crystallized region on the inner surface of the quartz glass crucible is influenced by the amount of heat applied to the quartz glass crucible, so that it is reliably 30 to 80% of the inner surface regardless of the conditions for pulling the silicon single crystal.
- a patchy crystallization region can be reliably formed on 30 to 80% of the inner surface within a barium concentration range of 130 to 200 ppm.
- the aperture size is 24 inches, a patchy crystallized region can be reliably formed on 30 to 80% of the inner surface within a barium concentration range of 100 to 170 ppm.
- a silicon single crystal ingot serving as a base for a silicon substrate used as an element for solar cells or semiconductors is manufactured under conventional conditions known in the past. be able to. That is, a general method for manufacturing a silicon single crystal ingot using this quartz glass crucible is that a quartz glass crucible is filled with a necessary amount of polycrystalline silicon, the inside of the silicon single crystal pulling apparatus is replaced with argon gas, and graphite heat generation is performed. The body is heated to 1500 ° C. to 1600 ° C., which is 1420 ° C. or higher, to dissolve the polycrystalline silicon.
- the temperature is gradually lowered and the temperature of the melt surface is adjusted to 1420 ° C., and then the seed crystal (6 to 8 mm prismatic shape) is immersed in the melt to dissolve the surface of the seed crystal.
- the diameter is 3 to 5 mm and the length is 100 to 300 mm at a relatively high pulling speed (1 to 5 mm / min). A narrow and long neck is formed.
- the temperature in the vicinity of the upper surface of the melt in the quartz glass crucible is lowered and the pulling speed is also slowed to 0.1 to 0.5 mm / min. A shoulder that increases in diameter is formed.
- the constant diameter portion is grown so that the crystal diameter is constant by adjusting the temperature and the pulling speed. When it reaches a certain length, the temperature is lowered slightly, and the pulling speed is increased to make the crystal thinner, the diameter gradually decreases from the constant diameter part, and a tail with a diameter of zero is formed, and the silicon single crystal ingot is melted.
- the pulling manufacturing work is completed when the distance is away from the substrate, and the silicon single crystal can be manufactured with a high yield.
- the thickness of the crystallization accelerator-containing layer is divided into three stages in the range of 30 to 200 ⁇ m, and divided into four stages in the range of the barium concentration of the crystallization accelerator-containing layer in the range of 100 to 200 ppm, and the diameter of the quartz glass crucible is 16 inches. And 24 inch quartz glass crucibles were prepared.
- the patchy crystallized region has an irregular and non-uniform appearance as a whole, and the unit region includes one having an area of 10 to 100 mm 2. It was. At least a part of the unit areas of the spot-like crystallized area is further continuously connected to each other, and the total area of the spot-like crystallized area occupies 30 to 80% of the inner surface of the quartz crucible. It was.
- any of the quartz glass crucibles of the present example peeling of the crystallized material generated on the inner surface is suppressed, and the crystal layer does not peel from the inner surface of the quartz glass crucible due to the generation of gas discharge holes, and a high single crystal of 75% or more. Achieved a chemical yield.
- the results are shown in Table 1.
- the thickness of the crystallization accelerator-containing layer is 10 ⁇ m or 220 ⁇ m
- the barium concentration of the crystallization accelerator-containing layer is 0 ppm, 70 ppm, or 230 ppm.
- 16-inch and 24-inch quartz glass crucibles were prepared. Using these quartz glass crucibles, the silicon single crystal was pulled up.
- Table 1 The results are shown in Table 1.
- the thickness of the crystallization accelerator-containing layer is less than 30 ⁇ m and 10 ⁇ m, a large number of crystallization substances having a size of ⁇ 2 to ⁇ 6 generated when the crystallization accelerator is not contained are generated on the inner surface of the quartz glass crucible, This crystallized material was peeled off from the inner surface of the quartz glass crucible. Therefore, the yield of single crystal pulling could not be improved.
- the thickness of the crystallization accelerator-containing layer is more than 200 ⁇ m and 220 ⁇ m, almost the entire surface exceeding 80% of the inner surface of the quartz glass crucible is crystallized, and gas discharge holes which are small holes of several tens of ⁇ m are formed on the crystal layer surface. Many were confirmed, and dissolved silicon penetrated between the crystal layer and the opaque layer from this gas discharge hole (FIG. 7). Therefore, the yield of single crystal pulling could not be improved.
- the inner surface of the quartz glass crucible is A large number of crystallized substances having a size of ⁇ 2 to ⁇ 6 generated when the crystallization accelerator was not contained were generated, and the crystallized substances were separated from the inner surface of the quartz glass crucible. Therefore, the yield of single crystal pulling could not be improved.
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Abstract
Description
2 石英ガラスの不透明層
3 石英ガラスの透明層
4 結晶化促進剤含有層
5 斑状の結晶化領域
5a 単位領域
6 ガス放出穴
7 シリコン
8 結晶層表面
9 結晶層
10 シリコン
11 石英ガラスの不透明層
12 斑状の結晶化領域以外の領域
<実施例>
回転するモールドに天然石英粉を投入した後に、黒鉛電極に電圧を印加し、電流を流す電気アーク加熱によって、モールド内面から石英ガラスルツボの不透明層を形成した。引き続いて、アーク火炎中に天然石英粉を徐々に散布供給し透明層を形成した。さらに連続して、本発明の結晶化促進剤であるバリウムを含有する溶液を天然石英粉にコーティングすることにより得た、バリウムをコーティングした天然石英粉を徐々に散布供給して、結晶化促進剤含有層を形成し溶融を終了した。その後は、公知の工程により、図1に示すように外周部に石英ガラスの不透明層2、その内側に石英ガラスの透明層3、さらにその内側に結晶化促進剤含有層4を有する石英ガラスルツボを作製した。
<比較例>
上記実施例において、結晶化促進剤含有層の厚さを10μmまたは220μm、結晶化促進剤含有層のバリウム濃度を0ppm、70ppm、または230ppmとし、それ以外は実施例と同様にして、口径寸法が16インチと24インチのそれぞれの石英ガラスルツボを作製した。これらの石英ガラスルツボを用いて、シリコン単結晶の引き上げを行った。その結果を表1に示す。
Claims (11)
- シリコン単結晶引き上げ用の石英ガラスルツボであって、結晶化促進剤含有層を内表面に有し、シリコン単結晶の引き上げ時に、内表面に結晶化促進剤により斑状の結晶化領域が形成されることを特徴とする石英ガラスルツボ。
- 斑状の結晶化領域は、シリコン単結晶の引き上げ時に石英ガラスルツボの内表面に点在的に発生した結晶化物質が連続的に結合して形成されることを特徴とする請求項1に記載の石英ガラスルツボ。
- 斑状の結晶化領域は、実質的に周縁部が閉じて独立した形状を有し当該形状の面積が10~100mm2の範囲にある単位領域を含むことを特徴とする請求項1または2に記載の石英ガラスルツボ。
- 斑状の結晶化領域の単位領域のうち少なくとも一部は、単位領域同士がさらに連続的に結合しており、斑状の結晶化領域の全面積が石英ガラスルツボの内表面の30~80%を占めることを特徴とする請求項3に記載の石英ガラスルツボ。
- 斑状の結晶化領域には、シリコン単結晶の引上げ時に10~100μmの微少穴が発生しないことを特徴とする請求項4に記載の石英ガラスルツボ。
- 結晶化促進剤は、マグネシウム、ストロンチウム、カルシウム、およびバリウムから選ばれる2a族元素の少なくとも1種であることを特徴とする請求項1から5のいずれかに記載の石英ガラスルツボ。
- 結晶化促進剤はバリウムであり、結晶化促進剤含有層は、バリウムをコーティングした高純度シリカ粉を石英ガラスルツボの内表面に供給し溶融させて形成したものであることを特徴とする請求項1から6のいずれかに記載の石英ガラスルツボ。
- 結晶化促進剤含有層は、厚さが30~200μmであることを特徴とする請求項7に記載の石英ガラスルツボ。
- 結晶化促進剤含有層は、バリウム濃度が100~200ppmであることを特徴とする請求項7または8に記載の石英ガラスルツボ。
- 結晶化促進剤含有層は、バリウム濃度が130~170ppmであることを特徴とする請求項7から9のいずれかに記載の石英ガラスルツボ。
- 請求項1から10のいずれかに記載の石英ガラスルツボを用いたシリコン単結晶の製造方法であって、多結晶シリコンを石英ガラスルツボ内に投入する工程と、多結晶シリコンを加熱溶解してシリコン融液とする工程と、種結晶を用いて石英ガラスルツボ内のシリコン融液からシリコン単結晶を引き上げる工程とを含むことを特徴とするシリコン単結晶の製造方法。
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
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US13/148,768 US20120006254A1 (en) | 2009-02-10 | 2009-02-09 | Quartz glass crucible for pulling single-crystal silicon and process for producing single-crystal silicon |
SG2011057502A SG173618A1 (en) | 2009-02-10 | 2010-02-09 | Quartz glass crucible for pulling single-crystal silicon and process for producing single-crystal silicon |
KR1020117018531A KR20120013300A (ko) | 2009-02-10 | 2010-02-09 | 실리콘 단결정 인상용의 석영 유리 도가니 및 실리콘 단결정의 제조방법 |
CN2010800073695A CN102317511A (zh) | 2009-02-10 | 2010-02-09 | 硅单结晶拉升用石英玻璃坩埚及硅单结晶的制造方法 |
EP10741232A EP2397582A1 (en) | 2009-02-10 | 2010-02-09 | Quartz glass crucible for pulling single-crystal silicon and process for producing single-crystal silicon |
Applications Claiming Priority (2)
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JP2009028444A JP4866924B2 (ja) | 2009-02-10 | 2009-02-10 | シリコン単結晶引き上げ用の石英ガラスルツボおよびシリコン単結晶の製造方法 |
JP2009-028444 | 2009-02-10 |
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WO2010092955A1 true WO2010092955A1 (ja) | 2010-08-19 |
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PCT/JP2010/051893 WO2010092955A1 (ja) | 2009-02-10 | 2010-02-09 | シリコン単結晶引き上げ用の石英ガラスルツボおよびシリコン単結晶の製造方法 |
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US (1) | US20120006254A1 (ja) |
EP (1) | EP2397582A1 (ja) |
JP (1) | JP4866924B2 (ja) |
KR (1) | KR20120013300A (ja) |
CN (1) | CN102317511A (ja) |
SG (1) | SG173618A1 (ja) |
TW (1) | TW201035392A (ja) |
WO (1) | WO2010092955A1 (ja) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2012055195A1 (zh) * | 2010-10-27 | 2012-05-03 | 杭州先进石英材料有限公司 | 一种石英玻璃坩埚及其制备方法 |
Families Citing this family (9)
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JP5610570B2 (ja) * | 2010-07-20 | 2014-10-22 | 株式会社Sumco | シリカガラスルツボ、シリコンインゴットの製造方法 |
JP5509189B2 (ja) | 2011-12-26 | 2014-06-04 | ジルトロニック アクチエンゲゼルシャフト | 単結晶シリコンの製造方法 |
JP5509188B2 (ja) * | 2011-12-26 | 2014-06-04 | ジルトロニック アクチエンゲゼルシャフト | 単結晶シリコンの製造方法 |
KR101680215B1 (ko) * | 2015-01-07 | 2016-11-28 | 주식회사 엘지실트론 | 실리콘 단결정 잉곳 제조 방법 및 그 제조방법에 의해 제조된 실리콘 단결정 잉곳 |
KR101829291B1 (ko) * | 2016-08-05 | 2018-02-19 | 에스케이실트론 주식회사 | 도가니 및 이를 포함하는 단결정 성장 장치 |
DE112017004764T5 (de) * | 2016-09-23 | 2019-06-27 | Sumco Corporation | Quarzglastiegel, Herstellungsverfahren dafür und Verfahren zur Herstellung eines Silicium-Einkristalls unter Verwendung eines Quarzglastiegels |
TWI651283B (zh) * | 2017-04-28 | 2019-02-21 | 友達晶材股份有限公司 | 坩堝結構及其製作方法與矽晶結構及其製作方法 |
DE102020000701A1 (de) * | 2020-02-03 | 2021-08-05 | Siltronic Ag | Quarzglastiegel zur Herstellung von Siliciumkristallen und Verfahren zur Herstellung von Quarzglastiegel |
CN115142121B (zh) * | 2021-03-31 | 2023-06-20 | 晶科能源股份有限公司 | 提高复投单晶硅成晶率的方法及单晶硅制备装置 |
Citations (3)
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US20030106491A1 (en) * | 2001-12-12 | 2003-06-12 | Heraeus Shin-Etsu America | Silica crucible with inner layer crystallizer and method |
JP2005145731A (ja) * | 2003-11-12 | 2005-06-09 | Kuramoto Seisakusho Co Ltd | 結晶化石英ルツボ |
JP2006021985A (ja) * | 2004-06-10 | 2006-01-26 | Kuramoto Seisakusho Co Ltd | 石英ルツボ |
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JP2003095678A (ja) * | 2001-07-16 | 2003-04-03 | Heraeus Shin-Etsu America | シリコン単結晶製造用ドープ石英ガラスルツボ及びその製造方法 |
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2009
- 2009-02-09 US US13/148,768 patent/US20120006254A1/en not_active Abandoned
- 2009-02-10 JP JP2009028444A patent/JP4866924B2/ja not_active Expired - Fee Related
-
2010
- 2010-02-09 WO PCT/JP2010/051893 patent/WO2010092955A1/ja active Application Filing
- 2010-02-09 CN CN2010800073695A patent/CN102317511A/zh active Pending
- 2010-02-09 SG SG2011057502A patent/SG173618A1/en unknown
- 2010-02-09 EP EP10741232A patent/EP2397582A1/en not_active Withdrawn
- 2010-02-09 KR KR1020117018531A patent/KR20120013300A/ko not_active Application Discontinuation
- 2010-02-10 TW TW099104108A patent/TW201035392A/zh unknown
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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US20030106491A1 (en) * | 2001-12-12 | 2003-06-12 | Heraeus Shin-Etsu America | Silica crucible with inner layer crystallizer and method |
JP2005145731A (ja) * | 2003-11-12 | 2005-06-09 | Kuramoto Seisakusho Co Ltd | 結晶化石英ルツボ |
JP2006021985A (ja) * | 2004-06-10 | 2006-01-26 | Kuramoto Seisakusho Co Ltd | 石英ルツボ |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2012055195A1 (zh) * | 2010-10-27 | 2012-05-03 | 杭州先进石英材料有限公司 | 一种石英玻璃坩埚及其制备方法 |
Also Published As
Publication number | Publication date |
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CN102317511A (zh) | 2012-01-11 |
JP4866924B2 (ja) | 2012-02-01 |
SG173618A1 (en) | 2011-09-29 |
KR20120013300A (ko) | 2012-02-14 |
EP2397582A1 (en) | 2011-12-21 |
US20120006254A1 (en) | 2012-01-12 |
TW201035392A (en) | 2010-10-01 |
JP2010184819A (ja) | 2010-08-26 |
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